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PUBLISHED BY
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VOLUME X, 1918
lb 1*
2$oart> of ^Dirore
Editor: CHARLES H. HERTY
Assistant Editor: Grace MacLeod Advertising Manager
• G. W. NOTT
Advisory Board
H. E. Barnard H. K. Benson F. K.
Cameron
B. C. Hesse
A. D. Little
A. V. H.
Mory
EASTON. PA.
ESCHENBACH PRINTING COMPANY
1918
Ti°
Tfte Journal of Industrial
and Engineering Gftemistry
Published by THE AMERICAN CHEMICAL SOCIETY
AT EASTON. PA.
Voi'ume X
JANUARY 1, 1918
No. 1
Editor: CHARLES H. HERTY
Assistant Editor: Grace MacLeod
Advertising Manager: G. W. Nott
ADVISORY BOARD
H. E. Barnard, H. K. Benson, F. K. Cameron, B. C. Hesse, A. D. Little, A. V. H. Mory M. C. Whitaker
Published monthly. Subscription price to non-members of the American Chemical Society. $6.00 yearly; single copy, 60 cents
Price per single copy to American Chemical Society members, 50 cents. Foreign postage, seventy-five cents. Canada, Cuba and Mexico
Entered as Second-class Matter December 19. 1908, at the Post-Office at Easton, Pa., under the Act of March 3. 1879
All communications should be sen! to The Journal of Industrial and Engineering Chemistry.
Telephone: Vanderbilt 1930 35 East 41st Street, New York City
Subscriptions and claims for lost copies should be referred to Charles L. Parsons, Box 505, Washington, D. C.
Eschenbach Printing Company. Easton, Pa.
TABLE OP CONTENTS
Editorials:
The Chemical Service Section of the National Army ... 2
A Chemists' Club lor France 2
The Chemical Alliance 3
Progress in Selective Service 3
Spruce Turpentine 4
A Regrettable Decision of the Directors 4
The Missing Five Thousand 5
Original Papers:
Recovery of Potash from Greensand. H. W. Charlton. 6
Toluol by Cracking Solvent Naphtha in the Presence
of Blue Gas. Gustav Egloff 8
The Estimation of Phenol in the Presence of the Three
Cresols. G. W. Knight, C. T. Lincoln, G. Formanek
and H. L. Follett 9
The Determination of Manganese in Steel in the Pres-
ence of Chromium and Vanadium by Electrometric
Titration. G. L. Kelley, M. G. Spencer, C. B. Illing-
worth and T. Gray '9
Reagents for Use in Gas Analysis. VI— The Absorp-
tion of Hydrogen by Sodium Oleate. R. P. Ander-
son and M. H. Katz 23
Reagents for Use in Gas Analysis. VII— The Deter-
mination of Benzene Vapor. R. P. Anderson.... 25
Research on the Detection of Added Water in Milk.
Halsey Durand and Reston Stevenson 26
The Loganberry and the Acjd Content of Its Juice.
Milo Reason Daughters 3°
Reaction of Hawaiian Soils with Calcium Bicarbonate
Solutions, Its Relation to the Determination of Lime
Requirements of Soils, and a Rapid Approximate
Method for the Determination of Lime Requirement
of Soils. Maxwell O. Johnson .1 '
Reverted Phosphate Carlton C.James 3i
Electric Furnace- Smelting of Phosphate Rock and Use
of the Cottrcll Precipitator in Collecting the Volatil-
ized Phosphoric Acid. J. N. Carothers 35
roRY and Plant:
A Constant Temperature and Humidity Room for the
Testing of Paper. Textiles, Etc P 1'. Veitch and
E. <» Reed 38
A Method for Determining the Absorbency of Paper.
E. O. Reed 44
The Use of Textile Fibers in Microscopic Qualitative
Chemical Analysis. E. M. Chamot and H. I. Cole. . 48
A Proximate Quantitative Method for the Determina-
tion of Rubidium and Caesium in Plant Ash. W. O.
Robinson 50
A Quick Method for Lime Cake Analysis. Alfred N.
Clark 5i
Recovery of Light Oils and Refining of Toluol 51
Addresses:
Chemical Microscopy. E. M. Chamot 60
The Bureau of Markets in Its Relation to the Conserva-
tion of Foods. Charles J. Brand 66
The Canning Industry — Some Accomplishments and
Opportunities along Technical Lines. H. A. Baker 6a
Edible Fats, in War and Law. David Wesson 71
CURRENT Industrial Nsws:
Perfumery for Siarn; Desulfuratiou of Hydrocarbons;
Lampblack Manufacture; Boric Acid and Borax;
Power from Refuse; Mineral Production in Canada;
Copper Amalgam as Metal Cement; Jute Sacks for
Argentina; Japan Peppermint Cultivation; Non-in-
flammable Plastic 1 1 rie Lamp Trade in
I ipan; Imitation Leather for Switzerland; New
a Alloy; Electro Steel Works in German] I
and Oils; New British Dye; Water-proof Goods for
South America; Japanese Glycerine; Water-proof and
Dust-proof Fabrics; Recovery of Platinum Metals
Canadian Nickel; Gutta Percha from the Shea
Butter Tree; British Papei Exports; Low-Grad
Utilization; Swedish Industrial Developments; British
73
Scientific Societies:
imial Index Patrons; Tenth mal teetin
ican Institute. 4' Chemical Engineers, St. Louis, Mo.,
■\ Pin;
The Nichols Med J Award; The Perkin Medal tarard. 77
Washington Letter 8o
Personal Notes 81
Industrial Notbs 82
Govbrnmi 84
88
89
Market.Rbport 9°
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. i
EDITORIALS
THE CHEMICAL SERVICE SECTION OF THE NATIONAL
ARMY
The importance of chemistry in the conduct of
the war has received a gratifying endorsement from
the War Department in the establishment of a new
division attached to the General Staff and designated
the Chemical Service Section of the National Army.
The two immediate purposes to be accomplished
by the formation of this division are, first, the unifica-
tion and more comprehensive development of the
various research activities now being conducted for
the War Department, and second, the creation of a
chemical organization, complete in personnel and
equipment, for service with the American Expeditionary
Forces in France.
The most significant feature in the formation of
this Section is the growing appreciation on the part
of the heads of the departments of the Army of the
value and necessity of chemistry in modern warfare.
General Pershing has urgently requested that a chem-
ical unit be organized and sent to France at the earliest
possible moment to care for the emergency problems
of vital importance which are constantly arising in
the conduct of the war. Both the personnel and
laboratory equipment of this force are being prepared
upon the basis that the American armies in France
have a right to the service of our ablest scientific
minds and the most complete and adequate facilities
for the work which it is possible for the United States
Government to supply.
This chemical unit will serve as adviser to General
Pershing on all chemical matters pertaining to the
war, and will be attached to his staff through Colonel
A. A. Fries, head of the Gas Warfare Division. It
will also act as the chemical eyes of the unit in this
country, transmitting information relative to chem-
ical problems of the war to the men at work here.
Able scientists throughout the country have responded
eagerly to this call to national service. The unit
will probably have sailed by the time this issue ap-
pears. The following have been recommended for
commissions:
I.IKITENANT-COLONEL
Raymond F. Bacon
Majors
Gilbert N. Lewis William A. rJamoi
Captains
II. II. Hanson
B. H. Nicolet
.1 II Hildebrand
F ( '. K
First i.hmh
A. K. Norton I.. II Cretchei
L. V.Walker Pannelee
J. K. Senior \\ I. Argo
T. D. Stewart
Second Lieutenants
P. G. Woodward
A. H. Hooker, Jr.
H. W. Nichols, Jr.
L. H. Ashe
G. S. Skinner
D. H. McMurtrie
J. J. Hast
J. W. MacMaugher
E. B. Peck
X. F. Hall
R. B. Hall
Allen Abrams
C. B. Spofford, Jr.
A K. Olsen
About twenty-five enlisted men, including some
of the best of the younger chemists of the country,
make up the remaining personnel as at present organ-
ized. The names of these enlisted men are not yet
available; they will be published in a future issue.
As the work develops, more men will be added so
that the laboratory will be in position to solve quickly
the many problems which the constant changes in
the methods and munitions of the war introduce.
In order that the information collected by this force
of scientific men may be of the greatest aid to the re-
search work now being conducted in this country,
Dr. William H. Walker, of the Massachusetts Insti-
tute of Technology, has been commissioned a Lieu-
tenant-Colonel, and will have charge of the unifica-
tion and coordination of many lines of research
now being so ably carried on here. It is not ex-
pedient to discuss the activities of these research
groups, but it is gratifying to know that real progress
is being made in practically every field.
The organization of this Chemical Service Section
will provide a means by which men drafted into the
service, and having special research ability, may be
enabled to serve the country as scientists in a way
which will produce results of the very highest value.
A CHEMISTS' CLUB FOR FRANCE
The war has effected in France, as in this country,
a remarkable stimulation of the chemical industries.
This has reflected itself during the past year in the
organization of a French Society of Chemical Indus-
try. The strong bonds of a common endeavor in
the struggle against the Teutonic menace has led
many of our chemists to join gladly in the formation
of an American section of that organization of French
industrial chemists.
Another evidence of that same activity has just
been received in the announcement of the organiza-
tion of the Cercle de la Chimie, located at 54 rue de
Turbigo, Paris, jt.
The association is composed, to quote from its
constitution, "ilc membres titulaires recrutes parmi
les chimistes de curriere, les industriels, les n^gociants,
les represcntants de l'industrie chimique. les construc-
teurs et toutes les personnes s'inteiessant au developpe-
ment de la Chimie."
The Association has for its object, to quote again,
"de permettre a tous ses adherents de discuter en
commun de leurs interfits materiels et moraux et de
Jan., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
s'interesser au deVeloppement de la science et de
l'industrie chimiques francaises."
The Revue des Produits Chimiques will be the official
organ of the Cercle de la Chimie. The club build-
ing will contain a reading room, a writing room, a
lounge room, indeed all the conveniences and comforts
of a modern club. Provision is made for the holding
of scientific meetings, and extensive literature will be
available.
To those of our chemists who will soon be in France
and to that still larger number who will go as the
American Expeditionary Forces increase, the prospect
of visiting such a chemistry home will indeed be
delightful. Opportunity will there be offered for meet-
ing the distinguished chemists of France and for that
fraternization among French and American chemists
which so quickly and so naturally develops whenever
representatives of the two countries meet. For our own
part, we could desire no stronger attraction to such a
spot nor need more certain guarantee of the genial
atmosphere which will abound than is afforded by the
presence of the name of Lieutenant Rene Engel in the
list of the charter members of the Cercle. During the
days of his connection with the French Mission in this
country Lieutenant Engel won a warm place in the
hearts of American chemists.
THE CHEMICAL ALLIANCE
One of the most interesting developments of the
past month has been the resuscitation of the Chem-
ical Alliance. This organization, formed at the sugges-
tion of the Department of Commerce, was incorpo-
rated during the past summer. Its primary object was
to assist in the clearing up of questions connected with
the importation of pyrites, a situation so acute at that
time. The Alliance, however, was not called upon for
this particular service. As originally organized, it con-
sisted of the chairmen of the sub-committees of the
Committee on Chemicals, provision being made for
associate members of allied groups. The officers were
Wm. H. Nichols, President, Horace Bowker, Vice-
President, and J. D. Cameron Bradley, Secretary.
With the gradual evolution of the war machine in
Washington all of the semi-official committees, such
as the Committee on. Chemicals, have been discon-
tinued. However, industrial advice is needed by the
War Industries Board, so each group has been asked
to organize a trade association, without any official
government connection, to which that Board can turn
for expert advice. To meet this situation the Chem-
ical Alliance has been revived. Dr. Nichols having
resigned the presidency of the original organization,
a meeting was held recently at which the following
officers were elected: Horace Bowker, President, Henry
Howard, Vice-President, and J. D. Cameron Brad-
ley, Secretary and Treasurer. These officers, together
with A. II. Weed, Secretary of the Manufa<
Chemists' Association, are now engaged in drafting
a constitution and by-laws for the new organization.
For the present, the Board of Directors consists of
the original members of the Committee on Chemicals.
All manufacturers of chemicals are eligible for mem-
bership and it is confidently hoped that all such will
become members at once. The members are to be
classified in groups, and at a meeting to be held soon
each of the groups will elect a director.
Such a representative organization of chemical
manufacturers has within itself great potentialities for
usefulness. It can act as a clearing house for priority
matters, and its recommendations may form the basis
of action by the War Industries Board, though ac-
corded no recognition in the form of official approval.
Furthermore, this close union in national service sug-
gests the approach of a day of more coordinated ef-
fort in a rapidly expanding industry, a coordination
which must be effected if the industry is to withstand
squarely the shock of the intense competition which
will assuredly have to be met in the days to come.
Individual effort has been able to accomplish much
under the unique conditions of a war period, but thor-
oughly coordinated and cooperative effort can alone
safeguard the future.
PROGRESS m SELECTIVE SERVICE
In so far as it applies to the wise utilization of chem-
ists, some semblance of order seems to be arising out
of the confusion incident to the immediate expansion
of the military forces through both voluntary enlist-
ment and the operation of the draft law. Many chem-
ists have been transferred from the line to chemical
service. In effecting these transfers splendid ser-
vice has been rendered by Dr. Charles L. Parsons.
In the next draft the new classifications issued by the
Provost-Marshall, General Crowder, give assurance
that the selective principle originally contemplated
in the enactment of the legislation will be substituted
for the lottery system which prevailed in the hurried
and inexperienced application of the first draft. The
regulations recently issued by the same officer remand-
ing drafted engineering students to' their universities
for completion of their courses partly insures a re-
serve of better trained chemical engineers. The or-
ganization of the Chemical Service Section of the
National Army furnishes an official medium for col-
lecting the scattered chemical forces. Finally, we
have been informed, though not directly, that the
Secretary of War grasps clearly the importance of
r61e the chemist must play in the great army we
are preparing to send abroad.
The disintegration of the Russian forces along the
Eastern front and the Italian reverses in the South
have brought clear conviction to this Nation that we
must prepare for a long war and on a great scale.
With characteristic American pluck our people have
accepted this situation, and with grim determination
have set themselves to the task of contributing the
maximum of men and means of which this country
is capable.
If this conviction should prove correct, and no one
loubts it, every possible means should bo re-
sorted to for preserving the 1 te sup-
ply of chemists and insuring full training of the younger
men now preparing for the profession of chemistry.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. i
To meet these two points we wish to urge upon the
military authorities careful consideration of the fol-
lowing suggestions:
First — It will be unfortunate if a literal application
of the term "chemical engineer" is made in applying
the new ruling as to return of engineering students
to their universities for completion of the course
necessary to graduation. In many institutions the
technical "chemical engineering" is not used to de-
scribe courses preeminently designed to supply chem-
ists trained for such engineering work as the country
needs. Moreover, chemists, just as much as, or even
more than, chemical engineers, will be needed in the
future for Government war work.
Second — For the training of these young chemists
and chemical engineers, competent instruction is a
prerequisite. The situation to-day is that many of
the ablest professors in our universities have been
detached from university work and are now engaged
upon special lines of research for the government,
while in the operation of the draft law, under the first
call, no consideration seems to have been given to the
question of exempting such instructors in chemistry
departments as are best qualified to carry on the work
of training the chemistry reserves.
Third — Many competent chemists are now in the
Army, serving as commissioned officers in the line.
The chemical ability of such men should be utilized
before further inroads are made for Government
chemical service upon the chemists now connected
with industrial establishments or upon the instruc-
tion staffs of educational institutions. For most of
these men no record exists in the census of chemists
compiled by the Bureau of Mines and the American
Chemical Society. The census, however, which is
now being compiled in each camp or cantonment by
the military authorities will doubtless contain the in-
formation which would make such men available.
Fourth — May we not hope that the War Depart-
ment will issue some general order directing all com-
manding officers to facilitate the transfer of chemists,
now serving in the line, to those branches of the ser-
vice needing men for chemical work!
If these four steps could be taken immediately the
future, in so far as it will be affected by chemists,
could be viewed with far greater equanimity than is
now the case.
SPRUCE TURPENTINE
From 1,500,000 to 2,000,000 gallons of "spru.
pentine" (sulfite turpentine) are going to waste an-
nually in the mills of the United States and Canada
using spruce pine for wood pulp. This oil is formed
during the cooking of the ehips in the sulfite digesters
and escapes with the steam in tin blowing out p
The term "turpentine," as applied to this mates
misnomer, for it contains only traces of terpenes; the
chief constituent, approximating ninety per 1 1
cymene. Recovery of I he crude product has been
carried out in a few mills, but no market was developed
sufficient to justify the expense of recovery. This
material assumes at the present time a greater im-
portance than hitherto accorded it because of its
possibilities as a source of toluol.
Patents have recently been issued to R. H. McKee
for a process in which the dried spruce turpentine is
heated with aluminum chloride to about the boiling point
of the turpentine. The products formed are toluol, pro-
pane and a small amount of tar. We are informed that
there is a plant in Philadelphia carrying on this process,
but so far only turpentine has been obtained to run
about one day a week; the sulfite mills have been
unwilling to take the trouble to collect and ship the
turpentine.
Moore and EglofI {Met. <ind Chem. Eng., Vol. 17
(191 7), 66), studying the action of aluminum chloride
on pure aromatic hydrocarbons, obtained a yield of
14.3 per cent of toluol from cymene.
Schorger (J. Am. Chem. Soc, Vol. 39 (1917), 2671)
studied the action of aluminum chloride on cymene
under varying conditions of temperature, time, amount
of reagent, etc. He mentions the interesting fact
that B. T. Brooks, by removing the light, low-boiling
reaction products as rapidly as they are formed, ob-
tained forty per cent of toluol by treatment of cymene
with seven per cent of aluminum chloride.
A still more interesting possibility is suggested by
the work of Boedtke and Halse (Bull, dc la Soc. < him.,
Vol. 19 (1916), 444). By heating cymene, dissolved in
ten times its weight of benzene, with aluminum chlor-
ide a true reversal of the Friedel-Crafts reaction was
obtained. Ninety grams of cymene yielded forty-four
grams of toluol and sixty-eight grams of cumene
(eighty and eighty-five per cent, respectively of the
theoretical yield).
If these results hold true on a commercial scale,
a new source of toluol for munitions and dyestuffs is
indicated. Furthermore, the ease of oxidation of
cumene to benzoic acid suggests the release of the
toluol which is now oxidized to benzoic acid.
It is unfortunate that Boedtke and Halse have in-
cluded so_few details of their investigation. The pub-
lished results are so striking that they suggest the neces-
sity of further work on this interesting reaction. Per-
haps the mills have been throwing away material of far
r value than they supposed.
A REGRETTABLE DECISION OF THE DIRECTORS
At the Annual Meeting of the Directors on De-
cember 8th a report was presented by the Pro-; and
Publicity Committee of the Society urging an appro-
priation of $^,500 for the continuance of the work
of that Committee during the year [918. In the light
of all of the estii presented to the
irs, the recommendation of the Committee
was not approved; instead, a renewal of the present
appropriation of $500 for this work was ordered,
this amount to be used in sending to .lie press each
month advanced copies of editorials in This Jolknal
which might be of public interest.
Jan., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
The press and publicity work during the past year
has been carried on largely by a fund contributed by
the New York Section from an available balance left
from the contributions to the expenses of the General
Meeting in New York City in 1916. This contri-
bution was supplemented by S500 appropriated by
the Society and by clerical help contributed by some
members of the Committee without charge. The
limited appropriation for the next year means there-
fore that the educational work carried on by the Com-
mittee through the newspapers of the country must
be practically abandoned, the valuable connections
of this service must be discontinued, and a well de-
veloped business representing a real asset of the So-
ciety must be discarded.
It is sincerely to be regretted that this important
educational work of the Society must be discontinued.
We sympathize fully with the critical and grave situa-
tion which the Directors faced in the preparation
of the budget for 1918. The necessity of larger issues
of the three Journals to supply the hoped-for increase
in members made heavy inroads upon the estimated
income; on the other hand, the uncertainties due to
the war situation led to grave apprehensions as to
what the actual income of the Society will be. This
situation, nevertheless, should become clear by April 1st.
If, then, the fears of decreased income have proved
groundless and the hoped-for increase has materialized,
we trust that the Directors will again take up this
matter, having before them the full information as to
the work of the Committee which can easily be placed
at their disposal.
We live in a democracy, and under such conditions
sure foundations can be laid only in broad educational
work from the bottom upward. Our people through
their newspapers should have opportunity to learn
more of chemistry treated in a popular way, and should
be brought into a more sympathetic relationship with
American chemists through the record of their achieve-
ments. Such work is preeminently the function of
the American Chemical Society, an organization which
has no propaganda to promote other than the wel-
fare of this country through increased appreciation
of chemistry. It was largely for this reason that the
newspapers of the country responded so sympathetically
to the suggestions of the Committee that more and
more of such material be carried in their columns. The
great mass of clippings collected by the Committee fur-
nishes ample proof of how wide-spread this response has
been. The arbitrary reduction of the mailing list at one
time to sixty papers was immediately followed by more
than two hundred requests for continuance of the ser-
vice. During the past year the work has been largely
enhanced by the creation of similar committees in
many local sections, whose work, in turn, has been
nated with that of the gi
This is too valuable a piece of machinery to be thrown
away. The best means to ensure its continuance
is a largely increased membership during ic
securing this increase each and every member of the
Society can take part.
It is time to get busy!
THE MISSING FIVE THOUSAND
The great increase in the number of members of
the American Chemical Society during the past year
has been a source of deep satisfaction to all — not be-
cause of the natural American love of bigness, but
from the conviction that when American chemists
speak through the medium of this organization it is
the voice of practically all chemists of the country.
Recently this feeling of satisfaction has had a rude
jolt. Secretary Parsons' records show that on
December 1, 191 7, the membership of the Society
reached the high total of 10,603. In the light
of the figures that marked the very gradual
growth during the years preceding the past decade
the present number of members seems enormous,
and it is so when compared with the membership
of similar organizations in European countries.
The magnitude of the figures, however, is consid-
erably dwarfed in the revelation made by the census
of American chemists recently compiled by the So-
ciety and the U. S. Bureau of Mines in cooperation for
purposes of possible war service. To the questionnaire
sent out for that census a little more than 15,500 replies
were received. This means that there are practically
5000 who stand ready to serve our country directly
and individually in this period of war, yet have not
felt disposed to serve it indirectly and collectively
through the medium of the national organization of
chemists. Why is this?
Can we be satisfied with reading the journals in
the library of the university or the plant, conscious
of the fact that these journals exist only as a result
of the joint effort of fellow chemists? Is it because
we take no interest in attending meetings of the So-
ciety? These meetings are of great help to all who
attend, and spread the gospel of chemistry in every
section where they are held. Moreover, the men who
to-day are serving the country so loyally in the solu-
tion of immediate war questions are the very men
who are most frequently seen at the meetings. In-
deed, Washington to-day looks like an adjourned
meeting of the American Chemical Society. Do we
feel that we cannot afford the expense of the ten dol-
lars a year dues? If so, let us watch carefully our
expenditures along the lines of purely self-interest
and see if the required sacrifice is indeed too great.
Are we waiting to be asked to join? That is not
necessary, for the doors are wide open to all reputable
chemists. Has it simply not occurred to us to
join?
To call attention to the opportunity before us is one
of the purposes of this editorial. Whatever the ex-
planation, the New Year is just upon us. Good resolu-
ned into deeds. Cooperation
Where. The closer union of the
0 gladly acclaimed M the fore-
runner ommon
Li lirable
union of chemical strength which D kil if we
are to win the fight for the welfare of our country
through the science which wc represent.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. i
ORIGINAL PAPERS
RECOVERY OF POTASH FROM GREENSAND1
Ily II. W. CnARLTON
In the original process as developed the material
adopted was feldspar, but it was later found that
glauconite, commonly called greensand, in many re-
spects possesses marked advantages, although carry-
ing a smaller percentage of potash. It exists in al-
most unlimited quantities in the Eastern states, par-
ticularly in New Jersey, and, unlike feldspar, requires
neither blasting nor crushing.
It is an accepted fact that any commercially suc-
cessful process of liberating potash in rocks, etc., must
include a method of profitably employing the residue.
In this case a building material is produced and has
the advantages of an unlimited market, as well as
being a superior product capable of being manufac-
tured at a remarkably reasonable figure.
The method consists in digesting under pressure
finely ground greensand with lime and water, thereby
obtaining caustic potash of remarkable purity and at
the same time converting the residue into a material
of value.
The reaction is carried out in large digesters or auto-
claves, heated by introducing into the charge high-
pressure steam in sufficient quantity to maintain the
desired pressure of about 225 lbs. for a period of from
2 to 4 hrs. To conserve the heat, at the completion
of each digestion the steam is allowed to escape and
be condensed in the greensand-lime-water mixture
next to be treated, and the contents of the autoclave,
which should have a cream-like appearance, is filtered
to separate the dissolved caustic potash from the
insoluble residue.
With sufficient lagging the unavoidable heat losses are
very moderate, especially as the chemical action
requires but little, if any, beyond the heat necessary
to raise the temperature of the mass to the reaction
point. For this reason the efficiency is largely de-
pendent upon the thoroughness of the heat insulation.
On filtering, the potash appears in the filtrate as
potassium hydrate associated with so few impurities
that on concentration it may be sold as a high-grade
product without further treatment.
Following is an analysis:
Per cent
KiO 77.2
SOi 0.90
Cli 0.35
SiOi 0.70
AUO» Pre*
From the origin of glauconite it would naturally
be supposed that the percentage of impurities would
be higher and the variety greater than is found to be
the case. According to standard works on mineralogy,
it is a hydrous potassium iron silicate, but this conclu-
sion was probably based on the simple analytical
figures, and there are very strong recent data to show
that this is not its true composition. As greensand
1 Presented at the 55th Meetiug ol the American Chemical Society,
Boston, Man., September 13, 1917.
is at the present time being carefully investigated, it
will very probably be shown to be a potassium iron
compound enveloping free silica, but not a silicate.
That it is of marine origin is undoubted, and its rich
green color is probably due largely, if not entirely, to
organic matter with which it is chemically combined.
The solid remaining on the filter, which is the in-
soluble portion resulting from the digestion, is em-
ployed in the manufacture of steam-hardened brick,
tile, artificial stone, etc. It acts as a binding or cement-
ing material and is incorporated with high silica sand,
as is customary in the manufacture of steam-hard-
ened products, but differs fundamentally in that,
whereas lime has always previously been employed
as a binding agent, in this case a pre-formed self-cement-
ing hydrous silicate performs this function.
In the past, steam-hardened brick, commonly known
as Sand Lime Brick, have not been the success pre-
dicted. They are not able to stand the weather
without more or less crumbling, and the edges and
corners are seldom perfect even in the freshly made
brick. This is due primarily to the fact that all the
binding power depends on the interaction of lime and
sand during steaming, with the resulting formation
of a surface coating of calcium silicate which binds
the sand particles. If any one of the many factors
governing this reaction are overlooked, the brick
is faulty. Imperfect slaking of the lime, improper
mixing, imperfect steaming, a deficiency or excess of
moisture, or dull cornered sand, would each be suffi-
cient in themselves to ruin the product. In fact,
every detail has to be rigidly observed and little lee-
way is permissible.
It is also found that the adhesion between the
sand and lime in the pressed but unsteamed brick is
slight in every case and that these "green brick"
crumble unless handled with the greatest care.
When employing the digestion solids as cementing
material these troubles are largely overcome. The
pre-formed cementing properties insure an unfailing
bond in addition to any chemical action that may
take place between the hydrous silicate and the sand
during steaming. Any type, such as bank, sea or
loamy sand is permissible. Ordinary ground rock will
serve the purpose. One of the most convincing
proofs of the self-cementing properties of the diges-
tion material is its ability to bond ground limestone,
with which there could not be any chemical action.
Sand and the cementing material may be mixed
in widely varying proportions ranging from oS and 2 to
40 and 60. In fact, it is almost true that the process
is "fool-proof."
The chemical composition of the autoclave residue
depends, of course, on the material treated. With
feldspar it is probably a complex calcium aluminum
, and with greensand a calcium iron silicate.
In both cases it possesses remarkable properties, being
to a degree self-cementing but capable of acting,
Jan., 1018 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
when subjected to steam pressure, as a powerful
binding agent, cementing sand so firmly that small
enclosed quartz pebbles fracture before the bond gives
way.
The cementing material resulting from the diges-
tion of feldspar is superior to that from greensand,
although the latter possesses sufficient cementing
power to meet the most rigid requirements and pro-
duces a brick of a pleasing light green shade at a
greatly reduced cost.
The feldspar brick are of a marble-like creamy
whiteness, entirely devoid of a lifeless milky tint,
and have surfaces so smooth that at a distance of a
hundred feet they cannot be distinguished from
marble.
If colored brick are desired, inorganic pigments
may be mixed with the binding material, and if an
ochre color is to be produced the coloring matter
may be obtained as a by-product in the general process.
It is necessary to calcine only a portion of the green-
sand-lime digestion product, under which treatment
it becomes a rich ochre, and add it to either the feld-
spar or greensand cementing material.
The properties of these brick are best illustrated
by tests on samples chosen from the general run by
an inspector from the Building Department of New
York City. The actual tests were carried out at
Columbia University and Pittsburgh Testing Labora-
tory.
Feldspar Required
Brick Standard
Crushing Strength, lbs per sq. in. 9267 2000
Modulus of Rupture, lbs. per
sq in 1060
Average Absorption.
4.44 per cent Under 15 per cent
The low absorption may be explained partially at
least by the voluminous, easily compressible, water-
repellent nature of the bonding material. On being
mixed with sand and subjected to the usual high
pressure in brick presses it oozes in and completely
fills all the interstices between the grains of sand.
Another feature, and in some respects perhaps the
most important, is the plastic nature of the binding
material which adds a toughness to the brick after
compressing and before steaming. This makes possible
the handling of the "green brick" without breaking
off the corners.
While brick is referred to particularly, it is not in-
tended to convey the impression that this is the only
marketable product. The particular advantage of
brick is the immense market.
In investigating the various factors governing the
yield of potash it was found that a high pressure and
a large excess of water were absolutely essential. In
treating feldspar it is necessary to use eight tin
weight of water, and ten is a fair amount. This
necessitated a great deal of evaporation, mal
reducing the capacity of the plant and requiring a
large outlay for initial heating.
After a series of experiments it \
a process of elimination that the alumina was the cause
of the trouble, and this naturally could not be removed
in the case of feldspar, K2O.Al203.6Si02, as it is an es-
sential element in its composition. The only remedy
consisted in the adoption of an alumina-free material,
or one in which this element was partially or wholly
replaced by a non-injurious one.
Greensand appeared very suitable and was tried.
Although its true composition is in doubt, the results
in this case were surprisingly satisfactory. It was
found that the concentration could be doubled or in
fact the water could be reduced to a point where it
was just possible to agitate the mixture.
A difficulty that has been met in every process of
recovering potash from feldspar is the invariable
liberation of soda at the same time. This is always
difficult and expensive to separate, and especially so
where both alkalies are liberated as hydrates. Theo-
retically potash feldspar is soda-free, but in practice
it invariably contains from 2 to 3 per cent.
Greensand is almost soda-free, which is all the more
remarkable from the fact that it is of marine origin,
being formed on the ocean bed by the selective ab-
sorption of potash from sea water by precipitated
colloidal silica and ferric hydroxide.
Another difficulty encountered in applying this
process to feldspar is the invariable presence of alumina
in the digestion liquors. Efforts to entirely overcome
this by adding more lime while reducing the amount
do not in any case remove it entirely. In the green-
sand-lime digestions there is not a trace. This is sur-
prising from the fact that the analysis of greensand
always shows a little alumina present probably in ad-
hering clayey matter. It must be present in some
combination that this process does not break up.
This is extremely fortunate.
Another important feature in the process is the em-
ployment of a high temperature and pressure in the
digestion. The reactions are not only speeded up,
as might be surmised, but are different. This is par-
tially due at least to the production of a chemically
active sub-hydrate of lime approximating the formula
CaO.CaO.HjO, which is formed at pressures of 200
lbs. and over.
That CaO.H20 should be partially dehydrated
during digestion in a large excess of water, such as an
amount equal to ten times the weight of the lime, ap-
pears to be paradoxical, but such is the case; and it
supplies a plausible explanation of the increased ac-
tivity of the lime in decomposing the feldspar at
pressures above 200 lbs. and corresponding tempera-
tures. It is found that the digestion of feldspar with
lime at 150 lbs. pressure for any reasonable length of
time scarcely liberates any potash, but above 200
lbs. pressure the reaction is ra]
Greensand, on the other hand, is less refractory and
may be liberated a1 Bsures, but it is 1
visable to employ them. '" and
oluble residue un-.
Considered from is be-
lieved that it is qu to adapl this process
nd, in conjunction
i,e production of a marketable by-product, to
8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol 10, Xo. i
operate at a profit when selling the potash at pre-
war prices. With feldspar, owing to the invariable
presence of soda, the mixed hydrate required to be
carbonated to effect a separation. The potash is
then sold as hydratcd carbonate. Carbonating is not
necessary in the case of greensand as high-grade caustic
potash is obtained in one operation. If potassium
chloride is desired it is necessary only to modify the
digestion by adding calcium chloride to the original
mixture.
It is found in the case of feldspar that the percentage
potash content does not give reliable data as to the
possible yield, this being dependent on unknown fac-
tors pertaining to each individual deposit. Often
feldspars that are valueless in pottery manufacture,
being weathered and mixed with mica, give the highest
yield, in some cases up to 90 per cent, while some very
high-grade samples yield as low as 30 per cent.
Greensand contains usually from 6 to 7 per cent
K20 and it may be almost completely recovered, but
it is found that 70 to 80 per cent of the total potash
is a satisfactory yield after considering such factors as
dilution, time of digestion, etc. This means the pro-
duction of about 100 lbs. of K20, and binder material
for from twenty to thirty thousand brick from each
ton of greensand.
If artificial stone, building blocks, roof, floor or drain
tile are manufactured, the resulting amount will vary
with the composition and weight of the products. If
desired, the digestion material without admixture
with sand may be molded in its plastic condition,
dried and employed as insulating fire-proof blocks.
On the other hand, it is believed that brick have the
most extensive market. The fact that the greensand
beds arc usually overlaid with a high silica sand
lessens the cost of manufacture. The overburden,
which has to be removed in any case, supplies the
necessary sai
The initial experiments and the commercial de-
velopment of the process have been made possible by
interest exhibited in the undertaking by
\\r_ Richmond Leverin] himself, borne the
1 in its development.
Kaolin Product* Corporation
120 Broadway, Nbw York
TOLUOL BY CRACKING SOLVENT NAPHTHA IN THE
PRESENCE OF BLUE GAS
1 '.I.OFF
red November 20, 1917
All past estimafc toluol which
Would I I in this war have been far too low.
May not the present estimate of Bri|
i of 22, 000,000 gallons of toluol1 required by
ber, toi8, also be far too low for our war
Tli. 1 more toll
One for increasing our toluol
ling carbureted v
and oil gas, by means of suitable scrul
I lilt- .!..! I ■ I
■ U*. .ind Chtm. Err., »« U9I7). 492. Mooic and Bfloff, IM., 17
(1917). 297.
for their toluol content. But, to pass the sorely needed
legislation, to change from a candle power to a heat
standard will take time, unless the War Department,
as a military necessity, commandeers or orders the erec-
tion of gas scrubbers in every commercial sized gas
plant in this country. But it will take time to build
scrubbers for the various gas plants. To quickly
add 2,000,000 gallons of toluol to our supply, it is
proposed in this communication to suggest the use
of water-gas machines to crack solvent naphtha and
produce toluol in the presence of blue gas.
It is calculated that there will be produced in the
year 1917, 15,000,000 gallons of solvent naphtha
from which, in round numbers, 2,000,000 gallons of
toluol can be made by cracking solvent naphtha in
carbureted water-gas machines. A more than suffi-
cient number of carbureted water-gas machines are
already installed throughout the country to more than
take care of the cracking of 15,000,000 gallons of sol-
vent naphtha from which 2.000,000 gallons of toluol
can be quickly made.
SOLVENT NAPHTHA USED
The solvent naphtha used in the following experi-
ment was derived from the thermal decomposition
of coal and analyzed, using a standard Engler flask
for distillation and the Westphal balance for specific
gravity.
■Distillation Analysis
Specific Gravity 0.867/15.5° C.
Temp. ° C. Per cent by Vol.
135.5 1st drop
140.0 49.1
150.0 87.0
160.0 91.5
170.0 96.3
180.0 98.5
183.5 Dry point
CRACKING TEST
The following test of cracking solvent naphtha
was conducted upon a Lowe 6' carbureted water-gas
set, over a period of 48 hrs. The operation of the
plant in cracking solvent naphtha in the presence of
blue gas for toluol is practically the same as when
cracking gas oil in ordinary carl iter-gas
making, with the exception that the gallonage per
hour of sob. la into the cracking zone is
higher. The data upon a 24-hr. basis averaged as
follows for a carbureted water-gas
Make per 6' set per day of pas formed 500,000 cu. ft.
Candle power of the gas 21 at 21° C.
Candle power of gas per gallon of oil 1 .75 at 21° C.
Solvent naphtha cricked per 1.000 cu. ft. of gas formed. . . . 12.0 gal.
Gas per gallon of solvent naphtha crackr,'. 83.3 cu. ft.
Coke used per 1,000 cu. ft. gas 46 0 lbs.
Steam used per 1.000 cu 38.0 lbs.
Temperature of superheater fa IRC . . . 825° C.
Tcinper.it lire of condenser outlet 15.56C.
Length of run 4 min.
Length of Mow 4 min.
Rati per hour solvent naphtha 250 gal.
Rate actual flow of solvent naphtha into system 500 gal.
of solvent naphtha passing throueh set in
6,000 gal.
Lighl oils collected in drips and seals. . 57 per cent
15 per cent
\\ \l VMS 01 1 loll I "II
The li.uht oil was distilled in a one-barrel still with '
steam to a temperature of 1700 C. This cut was
Jan., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY g
analyzed by a method1 already devised for the ben- vestigated the problem further and have published
zene, toluol and solvent naphtha content. methods in which they make use of the specific gravi-
The analysis showed on the basis of light oil recov- ties and solidifying points or solidifying points alone
ered from the cracking of solvent naphtha the follow- obtained by them for certain mixtures of phenol and
ing percentages of aromatic hydrocarbons: cresols.
Per cent The principal difficulty in working out a reliable
Refined Benzol 14.5 and satisfactory method for the determination of
RefinedToluol 23.7 , , . ., , , . .,
Refined solvent Naphtha 19.8 phenol in the presence of cresols in coal-tar products
Deadeoueayy. ..ap. . .?.'.\ .'.'.'.'.'.. ...... u'.b lies in the fact that in coal-tar distillates there is no
, , ., constant relation between the amounts present of any
On the basis of ioo gallons of solvent naphtha c ., . , ,, ,, , ,
, , ,, , , of the cresols, i. e., any of the three cresols may be
cracked the following percentage of aromatics can be . . . ,
B present in any amount varying over a very large
recover . ^ ^^ range, and this is more particularly true now since
Refined Benzol 8.3 m-cresol is being removed in some cases for making
Refined Solvent Naphtha.' .'.'.'.'.'.'. '.'. '.'.'.'.'. 1K2 trinitrocresol. Attention has been called to this fact
Dead!oiieavy. ..a.P.t. .a. '.'.'.'.'.'" '.'.'.'.'.'.'.'. s!o in the literature by Lunge,1 Ihle,2 Tiemann and Schot-
ten,3 Wegen,4 Schulze5 and even Weiss and Downs.6
In these critical times, with a high scarcity of toluol, Nevertheless, the methods of Weiss and Downs and
no quicker method lends itself to adding to our toluol Masse and Leroux have been partly based on the ar-
supply than the cracking of solvent naphtha in car- bitrary assumption that w-cresol and />-cresol occur
bureted water-gas machines. This being due to the in certain fixed proportions to each other in coal-tar
fact that there is more than a sufficient number of distillates or crude tar acids. Weiss and Downs
carbureted water-gas machines already in operation, assumed this proportion to be 50 per cent of m- to 50
which could be used at once without any change per cent of p-, and Masse and Leroux 60 per cent of
for the adding of 2,000,000 gallons of toluol to our m- to 40 per cent of p-cresol. Consequently, when
much needed supply. the interproportion of m- to />-cresol present in the
final distillate upon which the constants are determined
is different from that upon which their methods are
THE ESTIMATION OF PHENOL IN THE PRESENCE OF based, a condition very frequently met with in actual
THE THREE CRESOLS- practice, the results obtained by the use of either of
By G. w. Knight, c. T. Lincoln, g. Foemanek and h. l. Follett these methods are apt to be unreliable.
Received July 30. 1917 The following investigation was carried on in the
Of the many methods proposed for the estimation h°Pe of developing a method along similar lines that
of phenol in the presence of the three cresols, only would eliminate this and other weaknesses in these
those based on the determination of physical constants methods, be capable of wider application, give more
of mixtures of these substances would have much concordant results and be as short and concise as ac-
practical value in the analysis of coal-tar distillates, curacy would permit.
for the reason that small amounts of xylenols and experimental
other impurities that are apt to be present in the final In ordef tQ accomplish this end it was necessary
distillate would seriously affect the accuracy of any tQ obtain phenol> ^^sol, ^-cresol and m-cresol in
of the chemical methods. as pure a condition as possible and to work with as
Many methods of proximate analysis have been many samples from different sources as possible in
based on the determination of physical constants ordef to study the effect produced by slight amounts
such as the specific gravity, index of refraction, sohdi- of impurities on the constants of the different mix-
fying point, optical rotation, etc., of the substance tures
to be analyzed or a part of it that has been purified Various samples of the purest phenol obtainable
as much as possible. In the case of the determina- were procured from different commercial sources.
tion of phenol in the presence of the cresols, advantage A lafge number of sampies of the purest o-cresol made
can be taken of variations in the solidifying points commercially was obtained from American sources
and specific gravities of the various constituents to and also {rom England. Most of the samples of
determine the phenol. phenol were synthetic, while the o-cresol was all ob-
Part of the problem of working out along these tained directly from coal tar Some of the w.cresol
lines a really accurate method for the determination used jn the investigation was synthesized in this lab-
aol in the presence of the cresols was accom- oratory by the method of Staedel and Kolb,' while
by Lowe,' and also by Weiss.4 Very recently, some was of coal_tar origin obtained from commercial
and Leroux8 and Weiss and Downs' have in- sources Likewise some of the £-cresol used was
off, Met. b- Chcm. Ens.. 16 (1917), 259. ' "Coal Tar and Ammonia." 5th Ed., 1916, 784.
• Contributed with the permission of tin- Secretary of the Ti ■ /. t-rakt. Chcm.. (2], 14 (1876), 442.
•nd the U. S. Appraiser, Port of New York. ' Bar., 11 (1878). 767.
' Luntr. "Coal Tar and Ammonia," 5th Ed.. 1916, 782. • Z. angcu. Chtm., 1909, p. 391.
« J. Franklin 1ml.. 1912, 683. * Btr., SO (1887). 409.
• Compt rend.. 166 (1916). 361 V ' Loc. cil.
This Joitknal, 9 (1917). 569. ' Ann.. «69 (1890), 209.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. i
synthesized in the laboratory by the method of
Erdmann,1 while the rest was bought from commercial
houses, as having been obtained directly from coal tar.
The specific gravities and solidifying points of these
substances were determined by the methods and ap-
paratus described later on. The various samples
of phenol had solidifying points of from 40.4 to 40. 7 °
C. and specific gravities of from 1.0640 to 1.0647 at
45° C./450 C. Those of o-cresol varied in solidifying
point from 28.8 to 30. 2 ° C. and in specific gravity
(250 C./250 C.) from 1.0439 to 1.0451. The p-cresols
varied in solidifying point from 31.9 to 34.4 ° C. aud
in specific gravity (250 C./250 C.) from 1.0334 to
1.0335, while the m-cresols varied from — 3.3 to +3.00
C. in solidifying point and from 1.0248 to 1.0333 m
specific gravity (250 C./250 C). Of the various samples
the following were selected as being either the purest
or else freest from slight impurities that might intro-
duce serious errors:
Specific Gravity Solidifying Point
phenol 1.0647 at 45* C./45° C. 40.6° C.
o-Cresol 1.0439 at 25° C./25° C. 29.0° C.
e-Cresol 1.0335 at 25° C./25° C. 34.4° C.
m-Cresol 1 .0333 at 25° C./25° C. 3.0° C.
These samples were selected after a considerable
amount of preliminary work with mixtures of the
various substances to determine the impurity present,
if any, in each one. They represent as a rule those
having the highest solidifying points, although this is
not the case with the o-cresol. Another o-cresol sample
had a solidifying point of 30. 2° C. but was not se-
lected because it appeared to contain 2 or 3 per cent
of phenol.
The constants obtained by using these samples in
making up the necessary mixtures were used in the
final plotting of lines and calculation of formulae,
while those obtained by the use of the other less pure
samples were used for comparison and to study the
effect of varying amounts of the different impurities.
The following mixtures of the pure substances
mentioned above were made up and the constants
of the mixtures determined and plotted on cross-sec-
tion paper. Most of the constants obtained were
checked by two or more chemists working independently
in order to eliminate errors due to personal equation.
Mixtures of the o-cresol and the />-cresol were made
containing varying quantities of o-cresol from 95
to 70 per rent l>y weight and />-cresol from 5 to 30 per
cent by weight and the solidifying points and the specific
gravities at 250 C./250 C. of these mixtures were ob-
tained, using all precautions to have the data as ac-
is possible. The values obtained were plotted
using the specific gravities as abscissae and the solidi-
fying points as ordinates. Other mixtures were made
using varying proportions of o-cresol from 90 to 70
t by weight, ^-cresol from 5 to 25 per cent by
weight and phenol 5 per cent by weight in each mix-
ture. Similar mixtures containing decreasingly pro-
portionate amounts >>i 0-cresol and />-eresol and in-
creasing proportion* of phenol in series of increments
of 5 per cent were made up, the constants determined
and the values plotted as before. The results are
shown in rig. ' ■
■ Axlriluxt Z. Dirsl. Org. Prat.. l»»i.
This process was repeated using the m-cresol in
place of the />-cresol. The line representing mixtures
of the o-cresol and the m-cresol and no phenol is
shown in Fig. I, the lines representing those mixtures
containing the increments of phenol being omitted
to avoid confusion. Similar mixtures were made up
using the other less pure samples of the different cresols
and the constants determined and plotted. These
results, being used only for comparison, were not
plotted.
It was found that the tangent of the angle formed
by the line representing mixtures of the purest 0-
cresol and the purest />-cresol and no phenol and a
line drawn through the point representing 100 per cent
o-cresol parallel to the axis (X = O) is numerically
equal to 0.13. It was also found that the tangent of
the angle formed by the o-cresol + m-cresol line in
Fig. I and a line drawn through the point representing
100 per cent o-cresol parallel to the axis (X = O)
is equal to 0.22. These angles are represented in
Fig. I as "a o.p." and "a o.m.," respectively. Calcu-
lated from this data the tangent of the angle formed
by a line representing mixtures of o-cresol and a dis-
tillate composed of 50 per cent m- and 50 per cent
/>-cresol would be 0.175. The similar tangent calcu-
lated from the data obtained by Weiss and Downs
for mixtures containing the same percentages of 0-
cresol and a coal-tar distillate containing 50 per cent
p- and 50 per cent m-cresol using a line drawn through
the maximum number of nearest points obtained by
them was found to be 0.1S1, a very close agreement
with the above, notwithstanding the fact that the
constants themselves were very different.
With the other less pure samples various lines were
obtained depending on the purity of the o-cresol,
p-cresol or m-cresol used — the position of the line
indicating the impurity present.
As may be seen by referring to Fig. I, lines drawn
through the points represented by mixtures containing
no phenol, 5 per cent phenol, 10 per cent phenol,
etc., up to 30 per cent phenol, within the limits of the
plot, are parallel in the case of />-cresol. This is also
true of m-cresol and mixtures of m- and ^-cresol in
varying proportions. The general equation for the
pure o-cresol + /»-cresol lines, with or without phenol,
as may be seen by inspection, is
1000 (G0— G,) — 0.126 (T0— T„) = o.
That for the pure o-cresol + m-cresol lines, with
or without phenol, is
1000 (G0— GJ — 0.218 (T0— Tm) = o,
where G0 = sp. gr. 250 C./250 C. of the o-cresol,
Gp = sp. gr, 25 C. -'5° C. of the />-cresol,
G„ = sp. gr. 250 C./250 C. of the m-cresol,
T0 = solidifying point of the o-cresol,
Tp = solidifying point of the ^-cresol,
and Tm = solidifying point of the m-cresol.
These lines, in addition to being parallel, are also
equi-distant for equal increments of phenol, both in
se of />-cresol mixtures and m-cresol mixtures,
although for the same increments the distances between
the lines are greater in the case of m-cresol than in the
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Z5°C>
Specjf/c Gray/Mes 25 °c.
1035 1-036 1-037 1.038 1033 1-040 1041 1042 1043 1044 1045 1046 1047 1-048 1-043 1050 1-051 I05Z 1053 1054 1055 105a
case of />-cresol. In other word?, with mixtures of
o-cresol, />-cresol and phenol containing more than 70
per cent of o-cresol and less than 30 per cent phenol,
and of the same solidifying point, the per cent of phenol
varies directly with the specific gravity. The same
rule holds true with mixtures of o-cresol, w-cresol and
phenol and mixtures of o-cresol, phenol and varying
proportions of »re-cresol and p-cresol within the same
limits. In the case of mixtures of ^-cresol, o-cresol
and phenol, the solidifying point remaining the same,
it was found that each per cent of phenol increased
the specific gravity 0.0003367; in that of mixtures of
w-cresol, o-cresol and phenol, 0.0003600. in that of
mixtures of ^-cresol, w-cresol, o-crcsol and phenol
proportionately intermediate values depending on the
ratio of />-cresol to »j-cresol.
Similarly it was found that, the specific gravitv
remaining constant, each per cent of phenol depressed
the solidifying point 2.75° C. in case of the />-cresol
mixtures, and 1.71° C. in that of the w-crcsol mixtures.
These facts enable us to formulate an equation
which will give the percentage of phenol without
I III JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. i
having recourse to a plot in cases where (1) o-cresol,
/>-cresol and phenol, or (2) o-cresol, »»-cresol and phenol
are present in the mixtures, and 30 per cent of the
mixture has been mixed with 70 per cent of pure
o-cresol.
Per cent
2-73
(T0— TJ0)
0.0003367
Per cent phenol = 0.366 (T„
Per cent phenol = o.58s(T0 — Tso)
(G0— GJ0)
(I)
(ID
278o(G„— G30)
where T„ = solidifying point of the pure o-cresol used,
TJ() = solidifying point of mixture of 70 per cent
of o-cresol + 30 per cent of substance,
GJ0 = specific gravity 25° C./250 C. of mixture
of 70 per cent of o-cresol + 30 per
cent of substance,
G0 = specific gravity 25° C./250 C. of the pure
o-cresol used.
Since in the analysis of commercial products, as
has been said before, the proportion of m- to £-cresol
may vary over very wide limits, it is necessary to have
some means of obtaining a measure of the amount of
m- or ^-cresol present in the portion of distillate used
for determining the constants.
Specific Grarit-iea f£»£
1-030 1031 1032 1033 1034- 1035 M36 K)37 1038 1039 1-040
90%para-cr<rsol
io% phenol
In the hope of finding such a means, mixtures of
rent of pure />-eresol with to |
and also with to per ceir and io per cent of
ide up separately, and the constants
determined . ults are shi
Fig. II. As a study of the plot failed to throw any
light on the problem, this particular line of investiga-
tion was abandoned.
The effect of varying amounts of the different cresols
on the constants of pure phenol was studied by making
mixtures containing 90 to 70 per cent of the purest
phenol and io to 30 per cent of the purest o-cresol
and similar mixtures containing the same percentages
of the purest />-cresol and the purest w-cresol separately
in place of the o-cresol, determining the constants for
each mixture and plotting the points representing
them. The terminal points and the three lines drawn
through the nearest points representing the three
classes of mixtures are shown graphically in Fig. Ill
as "Phenol + w-cresol line," "Phenol + o-cresol line"
and "Phenol + />-cresol line."
The effect of using the slightly impure cresols was
also studied to determine the effect of the small amounts
of impurities present on the constants of the different
mixtures. The results clearly indicated the impuri-
ties present in the same way as was the case with the
mixtures of the different slightly impure substances
with 70 per cent or more of the different o-cresols.
A study of the results obtained with the pure samples
revealed the following facts:
The effect of the addition of each of the cresols on
the solidifying point of phenol is widely different as
may be seen by referring to Fig. III. Each per cent
of o-cresol added, within the limits of the plot, de-
presses the solidifying point of the phenol about 0.65 °
C, each per cent of »»-cresol depresses it about 0.55 ° C.,
and each per cent of ^-cresol about 0.83 ° C. Ob-
viously, under such circumstances it would be folly
to attempt to determine the per cent of phenol in a
mixture of the cresols by determining either the solidi-
fying point alone or the solidifying point and specific
of a mixture of phenol and cresols containing
70 per cent or more of phenol unless the relative pro-
portions of each cresol present in the mixture were
known at least approximately. Meta-cresol can be de-
termined by the Raschig method.1 A number of dis-
tillates were analyzed by this method after first being
purified and fractionally distilled. As the percentage
of w-cresol found by this method varied ov< r very wide
limits and there seemed to be no connection between
the distillation point and the amount of »;-cresol
found and as no way was devised for determining the
relative proportions of 0- and ^-cresol present it was
decided that this line of attack would be unproductive
ultS.
Further study of the results obtained on the mixtures
of phenol and the separate cresols containing more than
70 per cent of phenol showed that the effed of the ad-
dition of the different cresols on the -• - gravity
of the phenol is also diff< 1 may be
seen by referring to Fig. [II. cent of 0-
within the limits of I wers the
C.) of the phenol 0.00031,
each per cent of />-eresol lowers it 0.00040. and each
per cent of w-cresol, 0.00044.
■ 7.. «(«. Chtm.. 1900. 759.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
»3
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14
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No.
tan. aph.s. =
where G{
(III)
of phenol
The combined effect of each cresol on the solidifying
point and specific gravity of phenol is represented by
the three lines shown in Fig. Ill and is measured in
each case by the tangent of the angle formed by each
line and a line drawn through the point representing
the constants for pure phenol parallel to the axis
(X = o). These angles are represented in the plot as
"ctph.o." and "aph.m." and "ctph.p." Inspection of Fig.
Ill will show that "aPI,.0" = "otph.p.." consequently
tan. aph.o. = tan. ap^.p.
The value of this tangent was found to be numerically
equal to 0.482 by the formula
1000 (Gp — ■ GJt),
TP — Tsp
= specific gravity 45° C./450 C.
used,
GjP = specific gravity 450 C./450 C. of phenol +
cresol used,
Tsp = solidifying point of phenol + cresol used,
Tp = solidifying point of phenol used.
The same value was obtained by calculation from
the data obtained by Weiss and Downs for their sample
of pure phenol and their mixture of 70 per cent phenol
and 30 per cent of o-cresol in spite of the fact that the
constants obtained by them were very different from
those obtained by the writers.
The tangent of the angle formed by the "phenol +
w»-cresol" line (tan. aph.m) was found to be equal to
0.794, while that of a "phenol + (50 m + 50 />)-
cresol" line was equal to 0.65. The tangent corre-
sponding to the latter case calculated from the data
obtained by Weiss and Downs for their phenol and their
mixture of 70 per cent of phenol plus 30 per cent of a
coal-tar distillate containing 50 per cent of m-cresol
and 50 per cent of /(-cresol was found to be about 0.64.
Those results obtained by the writers for the tangents
of the angles that are comparable with those calculated
from the data obtained by Weiss and Downs, are in
remarkable agreement both in the case of the phenol
mixtures and the o-cresol mixtures, although the con-
stants themselves are widely different for the same
mixtures.
By a series of experiments it was shown that if 30
per cent of a pure cresol or a mixture of cresols con-
taining varying amounts of phenol were mixed with
70 per cent of pure phenol and the constants obtained
on this mixture, the value of the tan. ap*.j. calcu-
lated from the constants of the phenol and the mixture
by Equation III would be the same, within the limit
of error of the analytical work, regardless of the amount
of phenol present, provided the same cresol or mixture
of cresols were present and only the per cent of phenol
varied. Consequently by calculating the tan. ap*.j.
for a given mixture of cresols containing any amount
of phenol over 70 per cent the influence of any phenol
originally present before the 70 per cent was added
is eliminated and since tan. api,.i. for o-cresol and
also for />-cresol is equal to 0.482, any increase in the
value of tan. aph.s. over 0.4S2 gives a measure of the
amount of m-cresol present.
Now the "phenol + o-cresol line" in Fig. Ill is
coincident with the "phenol + />-cresol line" and no
matter how much phenol is present in the original
mixture of cresol and phenol the point representing
the constants after mixing with 70 per cent of phenol
will lie somewhere on the line if 0- or />-cresol alone
or mixtures of 0- and />-cresol in any proportion are
present. Likewise if 0- or />-cresol alone or mixtures
of 0- and />-cresol in any proportion are present, the
point representing the constants of a mixture of 30
per cent of the original mixture and 70 per cent of 0-
cresol will lie somewhere on the "o-cresol-/>-cresol
line" shown in Fig. I, or a line parallel to it if phenol
also is present. In this case tan. apt,.s. w"iU be equal
to 0.482, showing that 0- or />-cresol alone or mixtures
of 0- and />-cresol in any proportion are present only
and the per cent of phenol in the original mixture may
be calculated by Equation I. If the tan. aph.s. is
equal to 0.794, only m-cresol in addition to phenol is
present; the point representing the constants of a
mixture of 30 per cent of the original mixture and
70 per cent of o-cresol will lie somewhere on the "0-
cresol -m-cresol line" in Fig. I, if phenol is absent in
the original mixture, or, on a line parallel to this line
if phenol is present, and the per cent phenol present,
if any, is obtained by the use of Equation II. Now
if in addition to 0- or /(-cresol alone or 0- and />-cresol
in any proportion, m-cresol is also present, tan. api.s.
will be intermediate between 0.482 and 0.794; and the
difference between the value found and 0.482 will
give a measure of the m-cresol present in proportion
to the other cresols present, which, if multiplied by
the ratio of the difference between the tan. ap».m
and apuo. (Fig. Ill) to the difference between the
tan. a0.m. and a0.P. (Fig. I) will give the neces-
sary factor for correcting Equation I for varying
amounts of m-cresol present. The resulting equation
is derived algebraically as follows:
The difference between tan. otph.m. and tan. ap/,.0.,
or tan. aph.p., = 0.794 — 0.482, or 0.312. The
difference between tan. a0.p_ and tan. o0.m. is equiva-
lent to the difference between Equations I and II.
0.366 (T0— TJ0) — 2970 (G0 — G„) = % phenol
0.585 (T0— T„) — 2780 (Go — GJ0) = % phenol
or,
0.219 (To— T„) + 190 (G0 — G50) = o, for
equal percentages of phenol.
Dividing this equation by 0.312 gi
0.219
190
(T0— Tso) + "" ^Go— G„) = o
0.312 0.312
or, 0.702 (T0— TJ0) + 609 (G„— GJ = o.
Multiplying by (tan. aPk.s. — tan. op».J or (tan.
aph.s. — 0.482) which can be represented by the sym-
bol ht, meaning the tangential lowering of the constant
of phenol caused by the substance compared with that
caused by 0- or ^-cresol, gives
0.702 L, (T0 — TJ0) + 609 L, (G, — G„) = o.
Adding this equation to Equation I gives
(0.366 + 0.702 Ls) (To — TJ0) + ^09 L, — 2970)
(G0 — Gj0) = per cent phenol
or, (0.366 + 0.702 L,) (T0— Tso) + (:97c— 609 L,)
(Gjo — G0) = per cent phenol, (IV)
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
where
1000 (Gj, — Gsf)
0.482
in which GP = sp. gr. 45 ° C./450 C. of the phenol used,
G^ = sp. gr. 45° C./45° C. of the 70 per cent
phenol + 30 per cent cresol mixture,
Tsp = solidifying point of the 70 per cent
phenol + 30 per cent cresol mixture
and Tp = solidifying point of the 70 per cent,
phenol used,
and where G0 = sp. gr. 2s0 C./250 C. of the o-cresol
used,
Gjo = sp. gr. 25° C./250 C. of the 70 per
cent o-cresol + 30 per cent cresol
mixture,
Tso = solidifying point of the 70 per cent
o-cresol + 30 per cent cresol mix-
ture,
and T0 = solidifying point of the o-cresol used.
When the distillate analyzed is composed of o-cresol
or />-cresol alone or a mixture of these two cresols in
any proportion Ls becomes equal to 0.0 and Equation
IV is transformed into Equation I. As the propor-
tion of m-cresol to the other cresols present increases,
Lj increases in value until 100 per cent of w-cresol
is present, when Ls becomes equal to 0.312 and Equa-
tion IV is transformed into Equation II.
Although Equation IV does not give absolutely
accurate results with all possible mixtures of the three
isomeric cresols it does give them with any of the three
cresols alone, with all possible mixtures of 0- and p-
cresol and all possible mixtures of m- and ^-cresol.
Where o-cresol and w-cresol are present in varying
proportions and ^-cresol is absent or present in very
small quantities, results obtained are too low, the
error increasing as o-cresol increases and />-cresol
simultaneously decreases until the greatest is intro-
duced where />-cresol is absent and less than 50 per
cent of w-cresol and more than 50 per cent of o-cresol
is present. Even in this case the error is compensated
for, as the relative proportion of 0- to m-cresol increases,
by the factor (T0 — Tso) simultaneously decreasing
proportionately, so the ultimate error is never very large
in any case. Moreover, it is hard to conceive of a
case in actual commercial practice where 0- and tri-
cresol would occur together in the absence of, or in the
presence of a small amount of />-cresol, since no evi-
dence has ever been found that ^-cresol was removed
from a crude cresylic acid, as is the case with m-cresol,
and, owing to the fact that ^-cresol distils at a tempera-
ture between the boiling point of o-cresol and that of
fn-cresol, in the ordinary processes of distillation there
is more likely to be a dearth of 0- or w-cresol in a mix-
ture of the three cresols in commercial products than
of p-crcsol. This fact is confirmed by Ihle1 and by
Tiemann and Schotten1 who found "mostly 0- and
#-cresol with a little w-cresol" present, while
Schu'.ze2 found "about 40 per cent m-, 35 per cent
o- and 25 per cent /»-cresol" in tar oils. In the latter
case, as well as in practically all those cases ordinarily
• Loc. M.
met with in commercial practice, where all three
cresols are present in varying amounts, the probable
error would amount to only a few tenths of a per cent
in the final result, which is about the same as the prob-
able error inherent to the determination of the constants
of the different mixtures.
In the application of Equation IV to the determina-
tion of phenol in commercial products, such as crude
cresylic acid, it is necessary to remove completely
even small quantities of hydrocarbons, and to remove
effectively xylenols, higher homologues and bases,
inasmuch as it was found on practical application that
the presence of even very small amounts of hydro-
carbons would seriously affect the accuracy of the
results while the presence of bases, xylenols and other
higher homologues, though not affecting the ultimate
result to so great a degree as the hydrocarbons, never-
theless introduced serious errors when present in very
great amounts.
the hydrocarbons were found to be more effectively
removed by diluting the original sample with 2 volumes
of benzol before extracting with caustic soda solution.
In addition, this process in most cases renders un-
necessary the preliminary distillation in the case of
dark colored products.
the bases are effectively removed by the regular
process of separating the tar acids, being left behind
in the acid liquor on acidifying the carbolate solution.
The problem of separating effectively the xylenols
and higher homologues from phenol and the cresols
was investigated by comparing results obtained in
actual analysis, using most of the still-heads enumerated
and illustrated by Rittman and Dean1 in their article
on the analytical distillation of petroleum.
The results were far from satisfactory. Those
still-heads that effectively removed the xylenols choked
up and caused considerable annoyance and delay in
the process of distillation, while those that distilled
without choking up failed to remove the xylenols. To
remedy these defects a special still-head was designed
of the proper dimensions for this work. This still-
head is described later on. It has been used for a
long time now and has proved satisfactory.
Other details in the manipulation, the necessity for
which will be obvious, were worked out and owing to
the impracticability of obtaining thermometers and
still-heads of exactly standard dimensions the dis-
tillation temperatures are given corrected for emergent
steam, thus eliminating the necessity of having still-
heads and thermometers of certain dimensions.
description and method of use of the knight
still-head
This still-head is especially designed for use in
separating xylenols and higher homologues from phenol
and the cresols. It consists of three 2-in. bulbs joined
by 2 glass tubes '/18 in. long and having a %2-in.
aperture. The upper bulb is connected with a glass
tube open at the top ('/a in. inside diam. and 3 in.
long) and having a side tube (V32 in. inside diam.)
' This Journal. 7 (1915). 755.
i6
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING > 111 MISTRY -Vol. 10, No. i
which is joined on about iV< in. above the upper bulb
and is bent downward at any suitable angle and for
any desired length. The lower bulb has a glass syphon
tube (Vs in. inside diam.) joined to the side of the
bottom of the bulb and bent upward to slightly less
than half way up the side of the lower bulb and then
bent downward, following roughly the contour of the
bulb, and passing through and down the center of an-
other tube, 4'A in. long and >/« in. inside diam., along
3V2 in. of the lower part and 7/s2 in. inside diam.
Inside diameter s/e /n~
FitS-IK Inside
diameter
7/32 in-
KNIGHT T ..
Inside
o j_ - / / diameter
Otlll- 3/ein
head
4.-..
.?
Inside diameter '/s in-
Sca/e '/? in- = f/fh
along 1 in. of the upper part where it is joined to the
bulb of the still-head. The syphon tube en-
ters the ■/• in- diameter part of the lower tube about
1V2 in- from the bottom of the lower bulb and passes
t.hroiiK'' '' bottom as shown
The dimension of the constriction in the lowi ■
is so 1. to the comlt ■ of the bulb
of the still-head that when the distillation is carried
on at the specified rate more vapor will condense than
can run back into the distilling flask through the con-
striction; thus a layer of liquid collects in the bottom
of the lowest bulb and acts as a liquid condenser for
all vapors passing through it having a higher boiling
point than the temperature of the liquid layer. In
this way the xylenols and higher homologues which
tend to pass over with the phenol and cresols are re-
tained in the liquid layer, and the temperature of the
liquid layer is kept hot enough by the vapors to pre-
vent phenol from being condensed. When the height
of this layer reaches above the level of the top of the
outside portion of the syphon tube, the syphon auto-
matically empties the bulb of the liquid layer and de-
livers the condensed liquid back into the distilling
flask again, provided the rate of distillation is not too
fast. A Tirrell burner should be used as a source of
heat on account of the ease with which the rate of dis-
tillation may be controlled by its use.
Towards the end of the redistillation of the 100-
202° fraction, when all the phenol has been removed,
occasionally such a small amount of liquid remains
in the distilling flask that scorching is liable to occur.
In this case, and in other cases where it seems neces-
sary to carry a small amount of liquid layer in the
lower bulb, this may be accomplished by tipping the
top of the still-head away from the condenser so that
the still-head instead of being vertical is inclined at
an angle from top to bottom toward the condenser.
By regulation of this angle the syphon may be made
to empty as frequently as the operator desires.
Weigh out 100 g. of the sample (W)ina tared beaker
to centigrams. Pour the oil into a separatory funnel
(500 cc. capacity) ; rinse the flask with 200 cc. of benzol,
adding the rinsings to the sample contained in the
separatory funnel. Mix the contents of the separatory
funnel, add 100 cc. of a 20 per cent NaOH solution,
shake thoroughly for two minutes, allow to settle,
and draw off the lower layer1 into another separatory
funnel of 600-700 cc. capacity.
Repeat the extraction of the benzol layer with suc-
cessive ioo-cc. portions of 20 per cent XaOH solu-
tion, drawing off the lower layer as before until no
more tar acids are extracted, as shown by acidifying
the last portion (3 or 4 shake-outs are usually sufficient).
Shake the combined NaOH extracts out with 30-cc.
portions of benzol until any hydrocarbons that may
have been carried through ii - >H extracts
by benzol and tar acids have been removed as shown
by heating the NaOH solution in a beaker to a gentle
boil until the odor of benzol disappears and the charac-
teristic odor of coal-tar :1Q longer
be den h the combine ' ben
couple of times with to nt XaOH
solution and add the was] n solution.
.1 black tarry sample will be . oeounten with which it
will be difficult to .lislinguish tin U yets. In this
case it will he Decenary, first to distil enough ol . the sample to
be sure that all of the phenol has been r en pour the distillate
Into the Mparatory funnel, add the , ee<j ^ above.
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
17
Acidify the combined caustic soda extracts with
dilute sulfuric acid (50 cc. of concentrated acid mixed
with 150 cc. of water). The solution is conveniently
held in a i-liter Jena Erlenmeyer flask. The acid
must be added in small portions at a time, and the solu-
tion cooled by immersing the flask in water or hold-
ing it under a tap of running water so that the tempera-
ture does not rise above 40 ° C. as measured by a ther-
mometer placed in the flask.
As it approaches neutrality the solution becomes
light in color, and should be tested occasionally with
litmus paper. When neutral, add 4 to- 5 cc. more of
the dilute sulfuric acid, transfer to a 700-cc. separa-
tory funnel rinsing flask and allow to stand till the two
layers separate well (from 1 to 4 hours are necessary
according to the character of the sample).
Draw off the lower layer into another separatory
funnel. Shake the acid-water layer with 30 cc. of
benzol; allow the two layers to separate well, draw off
the lower layer into another separatory funnel and
repeat the extraction with 20-cc. portions of benzol
until no more tar acids are extracted, as shown by
evaporating a test portion just to dryness on the water
bath (usually 4 extractions are enough). Reject the
exhausted water layer, add the second benzol shake-
out to the first; add the third benzol shake-out to the
separatory funnel which had contained the second
benzol shake-out and then add it to the first two benzol
shake-outs. Repeat this process with the fourth
benzol extract, etc., rinsing out each successive funnel
with the last benzol extract, and combine all the shake-
outs with the first. Wash the combined benzol ex-
tracts with 10 cc. of saturated salt solution and draw
off and reject the salt solution. Draw off the tar
acids into a 300-cc. round bottom, short neck, distilling
flask, made of Jena or other heat-resisting glass; rinse
out the separatory funnel with the combined benzol
shake-outs of the acid-water layer, and add to the tar
acids in the distilling flask. Distil off the benzol and
water into a separatory funnel, using a medium size
Wurtz still-head having an inlet tube below the first
bulb »/j2 in. inside diameter (both will come off prac-
tically completely below 1700 C, and there will be
an abrupt rise beginning at about 100-1200 C). The
distilling flask should rest on a V< in. asbestos board
6 in. square with an opening in the center 3V2 in.
in diameter and be enclosed entirely in an asbestos
shield; the thermometer should be a standard ther-
mometer, calibrated by the Bureau of Standards and
accurate to Vs" C., over the range 170 to 2100 C;
the condenser should be long enough, and cooled with
sufficient cold water, to prevent loss by lack of proper
condensation; the top of the bulb of the thermometer
should be on a level with the bottom of the outlet
tube of the still-head, and the upper part of this still-
head and the one ussd later should be protected with
thick asbestos cloth held in place with copper wire
hoops and extending from the top of the upper bulb
to the top of the still-head. When water and benzol
are out of the condenser, stop the distillation (it does
not matter if some oil distils over with the water).
Allow the still to cool; rinse out the Wurtz still-head
with a small amount of benzol and add the rinsing to
the benzol and water distillate. Saturate the water
layer with salt, shake, separate, reject the salt water
layer, and extract the benzol layer with 5-cc. portions
of 20 per cent NaOH solutions until any tar acids in
the benzol layer are removed (as shown by acidifying
a test portion of the last shake-out with dilute sulfuric
acid.) (Usually 3 or 4 extractions are enough.) Acidify
the combined NaOH extracts with dilute sulfuric acid
as before, allow to stand, separate any tar acids that
collect, and add to the tar acids in the distilling flask.
Continue the distillation, using a Knight still-head
in place of the Wurtz still-head, and collect the dis-
tillate, first in a 10-cc. burette, until the oil passes over
clear, then change to a tared 100-cc. cylinder, weighed
to centigrams, and collect up to 193° C. (corr.).1
Meanwhile saturate with salt any water layer that may
be mixed with the tar acids in the 10-cc. burette and
allow to stand. At 193 ° C. (corr.) change the receiver,
stop the distillation, allow the still to cool, separate
the tar acids from the saturated salt water, if any,
contained in the 10-cc. burette, rejecting the salt water
and drawing off the tar acids into the distilling flask;
continue the distillation and collect the distillate up to
206 ° C. (corr.), distilling, as nearly as possible, at the
rate of 0.5 to 1.0 cc. per minute.
Transfer the distillate collected from 193 (corr.)
to 206° C. (corr.) to another flask and redistil at the
same rate as before, collecting the distillate up to
201 ° C. (corr.) in the same tared cylinder used for
collecting up to 193° C. (corr.) in the initial distilla-
tion. Weigh the cylinder containing the distillate
to centigrams and calculate the weight of the distillate
(D). Pour the distillate into a suitable size Erlenmeyer
flask and mix thoroughly by pouring back and forth,
and then stopper the flask.
Weigh out as accurately as possible 4. 5 g. of this
distillate and 10.5 g. of o-cresol (solidifying point above
28 ° C). Mix these two portions thoroughly; if neces-
sary, heat cautiously in warm water to dissolve any
crystals of o-cresol that may be undissolved, and keep
in a stoppered flask.
Determine the specific gravity (Gso) of this mix-
ture, at 25° C./250 C, in a carefully calibrated and
tared 10-cc. Geissler pycnometer, having a thermometer
carefully calibrated to within o.i° C. at 25° C, being
careful to make consecutive weighings and to wipe off
the pycnometer thoroughly between weighings, until
the weight is constant to a few tenths of a milligram.
Determine the solidifying point of the same mixture,
using the apparatus and method described below.
The solidifying point determination should be
1 This temperature and all subsequent distillation temperatures are
given corrected for stem exposure, using the formula: stem correction =»
0.00016 N (T° — 1°), where N = number of degrees exposed. T° = tem-
perature of the thermometer bulb, and /° = average temperature of the
exposed stem. This correction will make a difference of 3 to 40° C. at
these temperatures, but the corrected temperatures will be consistent re-
gardless of the thermometer used, provided it is a standard thermometer.
A corrected temperature of 193° C. will usually give an observed rciuliiiB
of 190° C. although this will vary slightly with different thermometers.
[8
I 111. JOURNAL OF INDUSTRIAL AND ENGINEERING CHI " ')" Vol. 10. Xo. i
made in an apparatus composed of a cylindrical glass
vessel 6 in. in diameter by 7V2 in. high filled with water
or iced water at a temperature about 50 C. below the
expected solidifying point and containing a cylindrical
salt-mouthed bottle of about 3V2 in. diameter and
about 6V« in. high, clamped in position so that the
bottle is almost completely immersed. The bottle
is closed with a cork stopper through which passes
a short test tube 4 in. long by 7/s in. diameter, fitted
snugly into the stopper so that none of the tube ex-
tends above the top of the stopper. The test-tube is
closed with a rubber stopper through which pass the
standard thermometer and a looped platinum stirrer.
The thermometer used should be a standard ther-
mometer reading to tenths and calibrated by the Bureau
of Standards to hundredths of a degree over the range
between 6 and 41° C. The determination should be
conducted as follows:
Pour enough of the mixture into the test-tube to
give a layer more than sufficient to cover the bulb of
the thermometer. Insert the thermometer and the
platinum stirrer passing through the rubber stopper
into the mixture; press the stopper tightly into the
test-tube and stir the mixture continuously with the
platinum stirrer till the temperature is near the expected
solidifying point. Then introduce a few fine crystals
of o-cresol into the mixture and continue the stirring
until the mass crystallizes, and the temperature rises
to a maximum point and remains constant. This
temperature is the solidifying point (TJ0).
Repeat the determination of the specific gravity
and solidifying point (Tsp) of the distillate, using
phenol of 400 C. or higher solidifying point, instead
of o-cresol, and determining the specific gravity at
45° C./450 C. (Gsp), instead of 250 C./250 C.
The following procedure should be followed in de-
termining the specific gravities:
In the case of phenol and phenol mixtures, where
the specific gravity is determined at 45° C, the pyenom-
eter with the cap and thermometer removed is filled
with the phenol or phenol mixture which has previously
been heated very cautiously in warm water at a tem-
perature of about 50° C. until the phenol crystals
have dissolved and the phenol reached a temperature
of about 450 C. The thermometer is then placed in
the pyenometer and the pyenometer immersed in
water at a temperature slightly higher than 450 C.
The water in the bath is then repeatedly adjusted until
it is at 45° C. at the same time that the pyenometer
thermometer registers 450 C. (The pyi
immersed in the warm water almost up to the point
where the thermometer enters the pyenometer.)
The pyenometer is then removed from the water, the
cap put on, the whole pyenometer carefully wiped
dry, weighed to tenths of a milligram, removed from
the scale pan, wiped again and weighed again until
two successive weighings check to within a few tenths
of a milligram.
In the ease where the specific gravity is determined
at 25° C. and the room temperature is above 25° C,
the mixture to be tested, after first being heated, if
necessary, in water at about 30-35° C. to melt any
o-cresol crystals, should be first cooled in cold water
to a few degrees below 2S°'C. and then the pyenometer
filled, immersed up to the neck in water slightly above
25° C, etc., the same procedure being followed as
described above. The cap in this case should have a
slight perforation at the top to relieve any pressure
that might raise the cap and cause loss.
The per cent of phenol in the original substance
is calculated in the following manner:
First calculate the relative tangential lowering of
the specific gravity of the phenol-distillate mixture
(L,) by the equation
L, =
1000 (Gp — Gsp)
Tf
T*
0.482.
Then calculate the per cent phenol in the sample
by the following equation:
Per cent phenol = 100 D [(T5 — TJO) (0.366 +
0.702 Ls) + (G„— G„) (2970 — 609 L,)]/3oW,
where Gt = sp. gr. 45V450 C. of the phenol used,
Gj^, = sp. gr. 4S°/4S° C. phenol + distillate
mixture,
Tp = solidifying point of the phenol used,
Tsp = solidifying point of the phenol + distil-
late mixture,
D = weight of total distillate below 197° C.,
G0 = sp. gr. 25°/25° C. of the o-cresol used,
Gj0 = SP- gr- 25°/2S° C. of the o-cresol + dis-
tillate mixture,
T0 = solidifying point of the o-cresol used,
TJ0 = solidifying point of the o-cresol + dis-
tillate mixture,
and W = weight of the sample used,
SUMMARY
For the determination of phenol in the presence
of the three cresols, a feasible method is developed
which not only obviates the necessity of referring to
a plot in calculating results, but gives concordant and
reliable results with all the different combinations and
percentages of the different cresols and phenol likely
to be met with in commercial practice; in addition,
the method is not dependent for its accuracy on the
purity of the particular o-cresol used by the investi-
gators for the derivation of their formula for calcula-
ting the per cent of phenol. In applying the principle
involved to the practical determination of phenol
in crude commercial tar acids, suitable provision
is made for the complete separation the small
amounts of hydrocarbons that are usually present
in crude cresylic acids, especially those made from
Mas; furnace tar. which would otherwise introduce
serious error. A new still-head, « designed
for this kind of work, is used for the more complete
and satisfactory removal of the xylenols and higher
homologues.
641 Washington Strbkt
Nkw York Cm
Jan., 1918
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
19
THE DETERMINATION OF MANGANESE IN STEEL IN
THE PRESENCE OF CHROMIUM AND VANADIUM
BY ELECTROMETRIC TITRATION
By G. L. Kelley, M. G. Spencer, C. B. Illingworth and T. Gray
Received July 14, 1917
The determination of manganese in steel in the
presence of chromium and vanadium has long offered
difficulties to the analyst in steel works laboratories.
Numerous methods have been developed with the
object of alleviating or overcoming these difficulties.
Cain1 and Watters2 recommend devices for the separa-
tion of the manganese. Cornelius3 and Dedericks,4
although not particularly concerned with the analysis
of steel, have recommended procedures available for
the quantitative separation of manganese from chro-
mium and vanadium. Talminger5 has proposed a
method of the latter type, using von Knorre's procedure,
viz., the precipitation of manganese by ammonium
persulfate. Koester6 has investigated Engel's method
for the electrodeposition of manganese in the pres-
ence of chromium, and finds chromium occluded.
Cain7 finds that the Ford-Williams method gives
high results due to the occlusion of chromium. Even
in the Volhard- Wolff8 method chromium and vanadium
interfere.
The two methods most in use for the determination
of manganese in steel are known as the persulfate and
bismuthate methods. In the first of these the man-
ganese in a nitric acid solution of the steel is oxidized
with ammonium persulfate and silver nitrate, after
which it is titrated with sodium arsenite. Wdow-
iszewski9 reports good results with this method, even
in the presence of i per cent chromium. In this
laboratory, however, it has been noted that the method
rapidly becomes less useful as the percentage of chro-
mium rises, owing to the obscurity of the end-point.
In the bismuthate method the manganese in a solu-
tion of the sample is oxidized with sodium bismuthate,
the excess filtered out and an added excess of ferrous
sulfate titrated with permanganate. Here even a
trace of chromium may cause trouble and this diffi-
culty rapidly increases with the larger percentage of
chromium often met in commercial steels. By cooling
the solution thoroughly with ice before oxidizing
the manganese the tendency of the chromium to oxidize
is depressed, and if this procedure is followed by rapid
filtration fairly satisfactory determinations of man-
ganese may be made even in the presence of 5 per
cent of chromium in the sample. The consistently
successful analysis of such material by this method,
however, requires a high degree of skill. Demorest10
suggests titrating the solution with sodium arsenite
until the color of the permanganate disappears. He
has tested this method by titrating solutions of steel
to which chromium corresponding to 3 per cent of
• This Journal, 3 (1911). 630.
• Met. b- Chem. Eng., 9 (1911), 244.
' Pharm. Zip,., 68, 427.
• Ibid., p. 446.
'Chcm-Ztg., 34 (1910), 1877.
• Z. Eleklrochem., 17 (1911), 57.
1 hoc. cit
•5/0*1 u. Ehen, 33 (1913), 633.
• Ibid . 28 (1908), 1067.
• Tuts Journal, 4 (1912), 19.
the weight of the sample has been added as chromate
immediately before titrating. Under the usual
conditions of analysis most of the chromium is present
as chromic salt and such amounts of chromium in
this state make the end-point obscure. In the pres-
ence of s per cent or more of chromium all of these
methods, except those which involve the separation
of manganese, are extremely uncertain.
In this paper we describe a method which has suffi-
cient accuracy for all technical purposes and which,
without the separation of chromium and vanadium,
is not interfered with by these elements under the con-
ditions of analysis. The oxidation of the manganese
in this method may be accomplished either by the bis-
muthate or persulfate procedures, and titration is
made electrometrically, using mercurous nitrate as the
reducing agent. In the course of the examination of
a long list of reducing agents this was the only reagent
found which would reduce permanganate quantita-
tively and rapidly at ordinary temperatures without
reducing chromates or vanadates.
THE STANDARDIZATION OF THE MERCUROUS NITRATE
SOLUTION
io. 5 g. of mercurous nitrate are dissolved in 150 cc.
of water to which 2 cc. of nitric acid have been added.
Any undissolved salt is removed by decantation and
the solution made up to a volume of one liter. This
is compared electrometrically on the apparatus made
for this laboratory by the Leeds & Northrup Com-
pany,1 with a solution of potassium permanganate
which has been standardized against sodium oxalate.
The permanganate solution contains 0.5 g. of Mn
per liter, each cc. being equivalent to 0.05 per cent
of Mn in a i-g. sample of steel. The medium in
which the titration is made is a solution containing
50 cc. of sulfuric acid (sp. gr. 1.58) and 200 cc. of
water. The ^temperature should not be above 40 °.
For purposes of this titration, permanganate is
added to the solution in any convenient amount and
titrated with mercurous nitrate. The details of the
titration will be given at a later point in this article.
THE REACTION
When titration is complete, the solutions have a
brown color suggesting dissolved manganese dioxide.
The solutions, however, appeared to be quite stable.
When solutions containing 10 cc. of permanganate
had been titrated and were allowed to stand in a
stoppered Erlenmeyer flask at room temperature, no
precipitates appeared after some weeks. Filtration
removed only a small amount of the solids. With
solutions containing as much as 40 cc. permanganate
solution, a faint turbidity appeared after 24 hrs. On
warming, even to 400, manganese dioxide was pre-
cipitated.
After titrating 40 cc. of the KMn04 solution with
mercurous nitrate, the titration was continued with
ferrous sulfate of equivalent concentration on the
sami apparatus. This was found to require 12 cc.
1 This Journal, 9 (1917), 780.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING < III 14 ■ T Vol. 10, No. i
of ferrous sulfate. It is believed that the latter re-
action was the reduction of quadrivalent manganese
to the bivalent state. Our efforts to prove this point
were not entirely successful. When the solutions after
titration were warmed, both in the original volume
of 250 cc, and diluted to larger volumes up to one
liter, the amount of MnO: precipitated varied in an
uncertain manner. Changing the temperature from
40 ° to boiling did not serve to indicate a procedure
■1 give consistent results. The Mn02 so
precipitated was collected on asbestos and, after
washing, mixed with dilute sulfuric acid. An excess
of ferrous sulfate was then added and the solution
titrated with permanganate electrometrically. From
8 to 10 cc. of ferrous sulfate were required for titra-
tion, an amount always less than that required for a
similar titration before precipitation. One possible
explanation of this is that the manganese dioxide as
formed is in a hydrated condition and while in this
condition it may be that it very readily undergoes
decomposition in part into manganous sulfate and
oxygen. That there is a diminution in oxidizing
ly precipitation is shown by the fact that the
oxidizing power of the precipitate and filtrate com-
bined is insufficient to oxidize 12 cc. of ferrous sulfate
as is done when the titration with ferrous sulfate is
made without precipitation.
In the foregoing discussion 40 cc. of the solution
were taken as a unit in the study of the quantitative
precipitation of manganese dioxide. In the discussion
which follows we shall adhere to this volume.
To determine the amount of mercurous salt present
in the mercurous nitrate solution 40 cc. were diluted
to 200 cc, and 200 cc. of a solution containing 5 g.
of sodium chloride gradually added with stirring.
This was followed by the addition of 10 g. of sodium
acetate in the form of a filtered solution. The pre-
cipitate was washed with water containing a little
sodium chloride and finally with water alone. It
was dried at 150°. Two determinations gave 0.3005
g. and 0.2999 g., respectively. The Hg (NO»)i pres-
ent in 40 cc. of this solution was found from the aver-
age of these determinations to lie 0.3.540 g.
lupplied bj the known concentra-
tions of tin p and mercurous nitrate solu-
tions, ai idizing power of the solution
ds ferrous sulfate after titration with perman-
ganati onstruct the following equation:
., Mnvu + 14 Hg1 = 3 Mn" + 1 Mnn + 14 Hg"
Basing our calculation on the known strength of the
permanganate solution, theory requires that the mer-
curous nitrate in 40 cc. should be 0.334b g.. which
• •nds closely with 0.3340 g. found. Corre-
spond.; found in that 1 .■ cc. <>f an equivalent
solution of ferrous sulfate would be required for the
reduction of three atoms of quadrivalent manganese.
While the reaction givei quite certainly in-
izing power of the solu-
left after titration, it lias seemed to us neces-
make an effort to secure additional information
in its support. We give below a brief outline of some
of our observations with their implications as under-
stood by us, omitting, however, experimental details
because of the inconclusive character of the work.
When manganous sulfate is added to the solution
of permanganic acid before titration with mercurous
nitrate, it has the effect of diminishing the amount of
mercurous nitrate necessary. The effect, however,
is not a regular one, for the addition of small amounts
of manganous salt produces a proportionately larger
effect upon the titration than large additions. Such
additions noticeably alter the color of the solution,
changing it from brownish yellow to brownish red,
suggesting the formation of manganic salts. Barne-
bey1 reviews the explanations which have been offered
to account for the effect of manganous salts upon
the titration of ferrous iron with permanganate in
the presence of hydrochloric acid. He quotes Vol-
hard as suggesting that the action of manganous
salts on the permanganate results in the formation of
quadrivalent manganese, while Birch suggests the
formation of trivalent manganese. When the solu-
tion after titration with mercurous nitrate is treated
with manganous salt, the same reddish color appears
as when the manganous salt is added before titra-
tion. If we are correct in our belief that the product of
the reaction is manganic sulfate in both instances,
this would constitute additional evidence of the pres-
ence of quadrivalent manganese in the titrated solu-
tion.
From the fact that we are unable to remove MnOj
from the solution by filtration after titration, this sub-
stance, if present, must be evident either as a sulfate
or in the colloidal condition. Witzemann,5 discussing
the conditions under which colloidal solutions of man-
ganese dioxide are stable, points out that small amounts
of either salts or acids cause immediate precipitation.
Evidence for the existence of sulfates of quadrivalent
manganese is. meagre. Fremy3 states that MnOCSOO
is formed by acting on hydrated MnO. with concen-
trated sulfuric acid in air. The fact that a moder-
ately high concentration of sulfuric acid is necessary
to prevent the precipitation of manganese dioxide in
this titration may be construe. 1 as indicating the forma-
tion of a sulfate of quadrivalent manganese.
From the reaction as given above it appears that
after titration one-fourth of the manganese is present
as manganous salt. W< . '.rivalent
cse by boiling a dilul and deter-
mined the manganese in the filtrate '!"'• ''.irate from
the titration of 40 CC of pert hould have
contained the equivalent of 10 ... of this solution.
We always found it to 1 ibout 15
might have beer. fact that
the mangant ways too
small in amount to corre-; Blum4
states that preci] • • is not
I .' Am Cl™. Sot., 3« (1914). 1441.
• Ibid 37
' Comfl rr*d . Si (1876). 475
• J. Am. Chrr: - 3«
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
oxidized by sodium bismuthate in nitric acid. We
added 30 cc. of nitric acid (sp. gr. 1. 13) to a solution
in which 40 cc. of permanganate solution had been
titrated and which therefore probably contained quad-
rivalent manganese. The solution was then oxi-
dized with sodium bismuthate, filtered through asbes-
tos and titrated. The average of four determinations
indicated a manganese content corresponding to 31.5
cc. of the permanganate solution. To test the com-
pleteness of oxidation of manganous salts under
these conditions, we oxidized a solution of manganous
sulfate in a similar mixture of acids and found the oxida-
tion to be complete. Our failure to secure an amount
or permanganic acid corresponding to 40 cc. of the
original solution of permanganate may have been
caused by the failure of the quadrivalent manganese
to oxidize completely, owing to the nature of the solu-
tion. A colloidal solution of manganese dioxide, if
it were possible for it to exist, might be expected to
react as in this case.
From the foregoing and other considerations, our
quandary as to the course of the reaction may be set
forth as follows: (1) The relation of permanganate
and mercurous salt seems to be definitely established.
(2) The presence of manganese corresponding in
oxidizing capacity to 3 Mn02 for 4 KMn04 reduced,
appears equally certain. (3) The presence of so large
an amount of Mn02 apparently in solution or suspen-
sion seems improbable. (4) The solution upon fil-
tration through paper or asbestos after titrating
leaves too much on the filter to correspond to complete
solution. (5) If we accept the statement that undis-
solved manganese dioxide is not oxidized by sodium
bismuthate in nitric acid solution, less than one-
fourth of the manganese can be present in that form
instead of three-fourths as shown in the reaction.
(6) The ease with which warming the solution precipi-
tates Mn02 from these solutions after titration might
correspond to the precipitation of suspended man-
ganese dioxide or to the decomposition of trivalent or
quadrivalent manganese sulfates. It is not impossible
that the reaction might lead to 2 Mn(S04)2 + Mn2(S04)3,
but the color of the solution after titration does not in-
dicate the presence of manganic salt. (7) The red
color produced by the addition of manganous salts
to the titrated solution is probably due to the forma-
tion of manganic salts and therefore furnishes evidence
of the probable presence of compounds of quadri-
valent manganese. The fact that a red color is not
produced by interaction between the MnIV and Mn"
shown in the reaction we explain as due to the low con-
centration of Mn11, for the effect described appears
only when relatively large additions of manganous
salt are made. (8) Since the final equilibrium corre-
sponds to the disappearance of septivalent manganese
and the formation of compounds of quadrivalent
and bivalent manganese, we are at a loss to under-
stand why the reaction should not have been either
2 M.iv" + 6Hgr = 2 MnIV + 6 Hg" or 2 Mnv" +
8 Hg1 = MnIV + Mn" + 8 Hg11 instead of the
more complex one first shown, which is the sum of
these.
THE TITRATION OF PERMANGANIC ACID IN THE PRES-
ENCE OF CHROMATES AND VANADATES
This titration is best carried out in the presence of a
moderately high concentration of sulfuric acid. We
have used 50 cc. of acid of sp. gr. 1 . 58, and 200 cc. of
water. With a lower concentration of acid, manganese
dioxide separates from solution and irregular results are
obtained in titration. Nitric acid does not interfere,
but it must be free from nitrous acid, which is best
accomplished by treating it with a small amount of
sodium bismuthate and filtering to remove the excess.
To titrate permanganic acid, the resistance of the elec-
trometric titration apparatus is adjusted to bring the
beam of light on the scale. During the addition of
the mercurous salt the beam remains stationary or
shows a slight anomalous rise of potential until the end
of the titration is approached. At this time the addi-
tion of more mercurous nitrate causes the beam to
move in the opposite direction from which it returns
more or less slowly after each addition until the end-
point is reached, when it usually remains off the scale.
The addition of a few drops of KMn04 serves to cause
it to return. The titration having been carried out
rapidly to this point, may be completed by adding
the mercurous nitrate solution drop by drop. The
end-point is sharp, and it is not affected by the pres-
ence of chromates or vanadates, but it is subject to
the influence of temperature.
Table I — The Titration op Potassium Permanganate with Mer-
CUROUS^NlTRATE IN/THE PRESENCE OF ChrOMATES AND VANADATES
Titrations made in 50 cc. HjSO< (sp. gr 1 . 58) and 200 cc. H.O
KMnOi Hgj(NOs)2 G. Cr as G. V as
Cc. Cc.
5.0
5
0
5.0
5
0
10.0
9
95
10.0
9
95
20.0
19
85
20.0
19
90
40.0
39
85
40.0
39
80
Tabee II-
—The Influe
Volume
an
i Concent
Temper-
KMnO.
ature
Cc.
20°
20.00
20°
20.00
40°
20.00
40"
20.00
60°
20.00
60°
20.00
80°
20.00
80°
20.00
Chromate
Vanadate
None
None
0.020
0.020
None
None
0.020
0.020
None
None
0.020
0.020
None
None
0.020
0.020
as in Table I
Hg!(N03)s
Cc.
19.90
19.90
19.95
19.90
19.90
19.95
21.1
21.4
The titrations shown in Tables I and II were made
with a solution of permanganate containing 0.0005 g.
of Mn per cc. This corresponds to 0.05 per cent Mn
in a i-g. sample of steel.
THE DETERMINATION OF MANGANESE IN STEEL AFTER
OXIDATION WITH SODIUM BISMUTHATE
This method of oxidation is carried out exactly as
described by Blair.1 After filtering, a small piece of
ice is added, followed by 50 cc. of sulfuric acid (sp.
gr. 1.58). The volume should be 250 cc. and the
temperature not above 400 at the time of titration.
The procedure in titration is then as described above
(Table I).
In Table III analyses of samples of steel issued by
the Bureau of Standards are given. To certain of
1 "The Chemical Analysis of Iron," 7th Ed., p. 122.
I III. JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. r
these, 0.02 g. Cr as chromatc w as added immediately
before titration.
Table III — Analyses op Stbbls with ash without Chromium Added as
chromate apter ozxdatxom with sodium bismuthate
Md Found
No Cr
0.020 g.
Sample
Added
Cr Ad
Mn Present!
9o
0.895
0.910
0.915
9a
0.910
0.905
19a
0.850
0.850
o.^so
19a
0.860
0.850
30*
0.560
0.560
0.563
30
0.565
0.560
31*
0.155
0.155
• 0.156
31
0.160
0.155
32*
0.215
0.216
32
0.220
0.215
35
0.305
0.305
0.300
35
0.310
0.305
Where such large amounts of chromium are present
(over 30 per cent) it would be safer to oxidize both
the chromium and the manganese.
Table V — The Eppect op Time upon the Ma.nc.nese F01 no when thb
1 ages op Doth Manganese and Chromium Are High
* Sample 30 contains 1.35 percent Cr and 0.21 per cent V; Sample
31 contains 3.51 per cent Cr and 19.55 per cent W; Sample 32 contains
0.89 per cent Cr.
t Bxcept on Samples 30 and 31 the official values given throughout
this paper are those obtained by bismuthate oxidation.
In oxidizing manganese with sodium bismuthate
in steel containing chromium, it is customary to add
large amounts of ice and to filter quickly, for in cold
solutions in which the bismuthate is allowed only a
short time to act the oxidation of chromium is reduced
to a minimum. Success in this method, however, de-
pends largely upon compensating errors, for some
chromium is always oxidized and the oxidation of
manganese tends to be slow or incomplete at these very
low temperatures. In this new method we had much
better success by oxidizing between 20 and 35°.
The only danger here is that after the removal of the
bismuthate the permanganate may oxidize some of
the chromic salt, being itself reduced. When the titra-
tion is made with ferrous sulfate and permanganate
in the ordinary way this causes no error. That it
does not cause error in this method can be due only
to the fact that at temperatures below 40 ° the oxida-
tion of chromium by permanganate proceeds slowly.
It is at once evident, however, that with high per-
centages of either chromium or manganese the danger
of error from this source will be diminished (1) by
oxidizing in the neighborhood of 200, (2) by adding
ice after oxidation is complete and before filtering,
and (3) by titi iting immediately after nitration.
Table IV — Determination of Manganese in Steels Containino
17 Per Cent op Chromium
Mn Found Mn by Electro-
Samples after Separation metric Titration
A 1201 0 0.395
A 1204 0.260 0.258
In Table IV manganese is shown as determined in
steels containing 17 per cent of chromium. Since
these steels are not readily soluble in nitric acid, the
samples wen I in hydrochloric acid and re-
peatedly evaporated to a small volume with nitric
acid. The solutions were then oxidized with sodium
bismuthate as usual. Manganese was also deter-
mined in tli' on with am-
monium persulf 1
In Table V the influence of time is shown where
the pen chromium and manganese are both
high. Bureau of Standards' Sample Oil was treated
with 1 g. of potassium dichromate before solution
and 1 g. afterwards. This gave rise to a very large
amount of chromil well as much chromate.
These solutions were then titrated after different
ml ei \ als.
: of Standing
r Filtration]
Percentage
Percentage
Minutes
Found
Present
1
0.895
0.915
0.910
10
0.875
10
0.815
20
0.830
20
0.885
To test the suitability of the method for determin-
ing the higher percentages of manganese, we dissolved
the Bureau of Standards sample of manganese ore,
No. 25, in hydrochloric acid and evaporated with
sulfuric acid until fumes appeared. It was then di-
luted to a liter. To portions of this representing
0.04 g. of the sample, nitric acid and sodium bis-
muthate were added. Fourteen titrations gave re-
sults ranging from 56.17 to 56.44. The average
was 56. 27. Blum1 says that the most probable value
for the manganese in this sample lies between 56.20
and 56.30. While these results are good the
method is not recommended for determinations where
such a high percentage of accuracy is needed as is
the case in ores and ferro-manganese. In steels an
error of one- or two-hundredths of a per cent is almost
unavoidable under all methods and is rarely impor-
tant. It is in this field that the usefulness of the
method lies.
THE DETERMINATION OF MANGANESE IN STEEL AFTER
OXIDATION WITH AMMONIUM PERSULFATE
One of the advantages of the ammonium persulfate
method for determining manganese is that the filtra-
tion of the solution is not necessary. Where many
routine determinations are made this is a valuable
quality in a method because of the time saved. We
accordingly attempted to develop this method for
use on the electrometric apparatus. In titrating
permanganate in sulfuric acid with mercurous nitrate
in the presence of ammonium persulfate the relation
of one solution to the other is slightly different from
that which obtains when the persulfate is absent,
but the relation is definite. This titration has the dis-
advantage of being more sensitive to temperature
differences than is the titration in sulfuric acid alone.
However, it gives results generally accurate enough
for most technical purposes.
Table VI — The Titration op Potassium Permanganate in the Pres-
ence op Ammonium Psrsulpats
Solutions contained 50 cc. HjSOj (sp. gr. 1.58). 2 g. ammonium persulfate
and 200 cc. of water. Temperature
. MnO. <NOi)i Factor"
10.0 9.9 1.010
10.0 9.8 1.020
20.0 19.5 1.026
20.0 19.5 1.026
30.0 29.0 l o.H
30.0 29.1 1.031
4"0 38.8 1.031
40.0 38.8 1.031
' The subtraction of a blank of 0.1 cc. from the mercurous nitrate
makes the factor more nearly constant.
In Table VI titrations of potassium permanganate
at 20° are shown. The effect of temperature is demon-
strated in Table VII.
1 £<x .
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
23
Table VII — The Influence of Temperature upon the Titration of
Potassium Permanganate in the Presence of Ammonium
Persulfate
solution was identical
with
that used i
a Table VI
Cc. KMi
lO«
Cc.
Hg2(NO>)2
Factor
20
19.6
1.020
20
19.7
1.015
20
19.5
1.026
20
19.5
1.026
20
19.5
1.026
20
19.6
1.020
20
19. 8
1.010
20
19.8
1.010
20
20.5
0.97
20
20.0
1.00
20
19.8
1.01
20
21.0
0.95
20
21.6
0.93
20
21.8
0.92
20
21.6
0.93
20
22.0
0.91
It will be evident from the results shown in Table
VII that the temperature of the solution should be
kept close to 200 C. The increase in the amount of
mercurous nitrate used in titrating at the higher tem-
perature is undoubtedly due to the partial reoxida-
tion of the manganese. At low temperatures this
proceeds so slowly as to cause no trouble. Additional
difficulties arise in trying to work at temperatures
above 40 ° C. in that the behavior of the galvanometer
is irregular.
When the steel is dissolved in nitric acid it is not
generally possible to use more than 0.2 g. of the sam-
ple. We have found a preferable procedure to be
the use of a o. 5 g. sample in sulfuric acid. However,
where the manganese is below 0.5 per cent 1 g. sam-
ples may be used. Our method is to dissolve 0.5 g.
of the steel in 65 cc. of sulfuric acid of sp. gr. 1.20
and when solution is complete to oxidize with nitric
acid added dropwise. After boiling a minute or two
the solution is diluted with hot water to a volume
of 200 cc, heated to boiling and 10 cc. of silver nitrate
solution (2.5 g. in a liter) and 20 cc. of ammonium
persulfate solution (100 g. in a liter) added. Boiling
is allowed to continue about one minute when the solu-
tion is allowed to cool slowly, or rapidly with the
aid of ice, according to convenience. When the solu-
tion is nearly cool enough, a little more sulfuric acid
is added and the solution adjusted to about 20°.
Titration is then made.
At the time titration is made in this method all of
the chromium and vanadium present in the steel is
in the oxidized condition, while in the method pre-
viously described these elements are oxidized only in
part by the sodium bismuthate. In Table VIII
analyses of Bureau of Standards sample steels are
shown, some of which already contain chromium and
vanadium, but an additional amount of chromium as
chromate has been added in alternate determinations
to illustrate the independence of the presence of chromic
acid shown by this method. Samples weighing
o. 5 g. were used and titration was made with perman-
ganate and mercurous nitrate of such strength that
1 cc. was equivalent to 0.05 per cent in a half-gram
sample.
In this method it is not important to make the
titrations at once, as in the case after the filtration
following oxidation with sodium bismuthate. Eight
portions of Sample 35 were oxidized at the same time
Table VIII — The Determination of Manganese in Steels after
Oxidation with Ammonium Persulfate
Temperature, 10 to 25° C. Volume, 250 cc. Sample, 0.5 g.
Mi Present
0.915
0.850
0.563
0.156
. Mn Found
0.02 g. Cr
Added as
NoCr
Chromate
Added
0.896
0.896
0.900
0.902
0.844
0.844
0.830
0.850
0.545
0.556
0.556
0.558
0.158
0.154
0.165
0.144
0.205
0.220
0.299
0.301
0.298
0.309
0.216
0.300
and titrated at intervals during the succeeding 24 hrs.
The lowest result was 0.298 and the highest 0.314
less than 0.02 per cent difference.
The two methods have been in use in this labora-
tory during some months. Young men without
previous chemical training and with only a few weeks'
experience in laboratory work after a few minutes'
instruction have been able to make analyses of steels
containing chromium, vanadium, molybdenum and
tungsten, which could have been made by other
methods only by men of large experience and a high
degree of skill. Approximately a thousand determina-
tions have been made by these methods and compared
with other standard methods.
SUMMARY
I — A method has been shown for the determination
of manganese in the presence of chromium or vanadium.
II — A method in two modifications has been shown
for the electrometric determination of manganese.
Ill — A study of the reaction between permanganic
acid and mercurous nitrate has been made.
IV — The method does not require special skill for
its application.
Research Department
Midvale Steel Company
Philadelphia
REAGENTS FOR USE IN GAS ANALYSIS
VI— THE ABSORPTION OF HYDROGEN BY SODIUM
OLEATE
By R. P. Anderson and M. H. Katz
Received August 16. 1917
Bosshard and Fischli1 have suggested the use of
e. solution of sodium oleate containing nickel in sus-
pension, for the gas-analytical absorption of hydrogen.
Inasmuch as they did not determine definitely the
optimum conditions for the use of the reagent or its
specific absorption,2 experiments were undertaken
to obtain data on these points. At the very outset
the authors met with the difficulty of not being able
to duplicate the results of Bosshard and Fischli in
getting complete absorption of hydrogen. After various
attempts, the method was abandoned, and this note
has been prepared for publication in order that this
experience with the reagent may be placed on record.
The procedure that is recommended by Bosshard
i Z. angew. Chem.. 28, I (1915). 365.
' Anderson, This Journal. 7 (1915), 587.
THE JOURNAL OF INDUSTRIAL A.XD ENGINEERING CHEMIS1 io, No. i
and Fischli for preparing the catalyst and carrying
out the absorption, the one which the authors first
tried to duplicate, is as follows:
Metallic nickel is prepared by the reduction of
nickel oxide1 by hydrogen at 3400 C. The
nickel oxide is placed in a glass tube provided
with constrictions dividing it into compartments
of such size as to hold easily about 4.3 g. nickel
oxide each, and hydrogen is passed slowly through
this tube. After reduction of the nickel oxide, the
nickel is cooled in a current of hydrogen and the
constrictions sealed off, thus separating the nickel into
portions of about 3 g. in air-free containers. The
reagent, which consists of a concentrated solution of
sodium oleate in water to which about 3 per cent
nickel has been added, is placed over mercury in a
Hempel pipette, preferably modified by substituting
for the long capillary connection a short glass tube of
somewhat larger bore. To effect the absorption of
hydrogen from a sample of gas, the sample is shaken
with the reagent in the pipette for three minutes,
allowed to stand under diminished pressure for three
minutes as an aid in breaking up some of the trouble-
some foam which forms, and is then passed into a
second pipette along with the remaining foam. Here
the sample is shaken with the reagent for three minutes,
and then to it is added about 1 cc. of alcohol to de-
stroy the foam and enable the remaining gas to be
drawn back into the burette for the reading of the
decrease in volume.
Bosshard and Fischli used a lead bath for heating
the tube. The authors found it preferable to employ
a gas-heated combustion furnace of the usual form,
taking proper precautions to avoid local overheating.
After first employing the bulbed tube as suggested
by Bosshard and Fischli, and sealing off at the con-
strictions to preserve the nickel in an atmosphere of
hydrogen, the authors substituted for it a straight
tube about 3 cm. in diameter with a stopcock at each
end, one of them having a bore of about 5 mm. After
cooling the nickel in this tube in an atmosphere of
hydrogen, the stopcocks were closed, thus preserving
the entire product in one container. When a portion
of the catalyst was desired, the tube was placed in a
vertical position, with the stopcock of large bore at
the lower end, and the proper amount of nickel al-
lowed to pass out through the lower stopcock, pressure
being furnished by the admission of hydrogen through
the upper stopcock. This procedure simplified mate-
rially the preparation of the catalj
No figures are given by Bosshard and Fischli as to
the actual concentration of sodium oleate in the solu-
tion whi employed. The authors used a 10
per cent solution of sodium oleate for the greater part
of the experiments. Such a solution must be pre-
pared shortly before using since it jellies rather rapidly
inding. Stronger solutions solidify too rapidly
to be of use.
In the absence of any description of the method
of introducing the nickel into the solution of sodium
' Bosshard unci Fischli used nick die oxide; the authors used nickclous
oleate without access of air, the following procedure
was adopted: To the tip of the modified Hempel
pipette for use with mercury was attached a short-
stemmed funnel by means of a piece of rubber tubing.
The air was forced out of the pipette by filling the bulb
with mercury. With hydrogen flowing into the funnel
through a glass tube inserted almost to the bottom,
the desired amount of nickel was allowed to drop into
the funnel from the tube in which the product was
kept, the solution of sodium oleate being added im-
mediately and the mixture drawn into the pipette
by lowering the leveling bulb.
the reagent finally in the pipette, samples
of hydrogen were placed in contact with it, but with
practically no absorption. Many attempts were made
to obtain an active reagent, using metallic nickel pre-
pared from nickel oxide of various degrees of fineness
down to 200 mesh, but with no success. A temperature
of 80° C. was maintained in the reagent in one case,
but to no advantage. It was noticed, however, that
the solutions of sodium oleate to which nickel had
been added hardened much more quickly than those
of the same concentration that contained no nickel.
It was assumed that this was due to the "hardening"
of the solution by the hydrogen adsorbed by the nickel.
Accordingly, the preparation of nickel was modified
by substituting a current of nitrogen for the hydrogen
at the point when the reduction of the nickel oxide
had been completed, continuing the heating of the
material for a short time to drive off occluded hy-
drogen. The nickel was finally cooled in nitrogen
and stored in an atmosphere of this gas. When this
material was employed as a catalyst, the sodium
oleate showed no tendency to harden sooner than it
would have done in the absence of nickel, entirely
in accordance with the suggested explanation, but
the reagent thus obtained did not absorb hydrogen
from gas mixtures placed in contact with it.
At this juncture, the attempt to ascertain the con-
ditions under which complete absorption of hydrogen by
sodium oleate in solution might be obtained was aban-
doned, because of certain objections inherent in the
method which would make it of little value even when
standardized and found capable of giving satisfactory
results. Among these objections might be men-
tioned the following:
I — The time and effort required for the preparation
of the catalyst is considerable, and the necessity of
keeping it out of contact with air adds to the difficulty
of its use.
II — The reagent foams badly and this renders the
absorption process itself a lengthy and tedious opera-
tion.
Ill The rapidity with which even moderately
dilute solutions of sodium oleate solidify renders it
necessary to prepare fresh solutions Also,
old solutions must be discarded before -. y solidify
in the pipette, otherwise they can be removed only
with difficulty.
Cornell I'nivbrsity
Ithaca. Nkw York
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
REAGENTS FOR USE IN GAS ANALYSIS
VII— THE DETERMINATION OF BENZENE
VAPOR
By R. P. Anderson
Received August 16. 1917
In connection with the development of a new method
for the determination of benzene vapor in gas, a brief
history of the determination of this substance has been
prepared, and is here presented. Following this his-
torical summary, there is a brief statement of the prin-
ciple of this new method, upon which considerable pre-
liminary work has been done. The various methods
that have been employed are taken up in chronological
order.
FUMING NITRIC ACID METHOD
Berthelot1 appears to have been the first to suggest
a procedure for the determination of benzene vapor in
illuminating gases. A sample of gas whose benzene
content was desired was placed in contact with fuming
nitric acid and the approximate amount of benzene
determined either by weighing the dinitrobenzene
formed or by determining the decrease in volume of
the sample, defines were removed by bromine water
previous to the treatment with fuming nitric acid.
Treadwell and Stokes2 found that the volumetric
method gave unreliable results because treatment with
bromine water for the removal of defines results in the
absorption of some of the benzene, and because fuming
nitric acid, the reagent for benzene, also oxidizes carbon
monoxide. Drehschmidt3 found the method unsatis-
factory for the same reasons, and it does not appear
to have been used to any great extent.
DINITROBENZENE METHOD
The gravimetric method suggested by Berthelot
was developed by Harbeck and Lunge4 into one with
which accurate results can be obtained. The gas to
be examined is passed through a mixture of equal parts
of fuming nitric acid and concentrated sulfuric acid,
thereby quantitatively converting the benzene vapor
into dinitrobenzene. The separation of the greater
part of the dinitrobenzene from the acid is effected by
diluting with water and neutralizing with sodium
hydroxide. The crystals of dinitrobenzene which
separate from the liquid on standing are separated by
filtration, dried, and weighed. The dinitrobenzene
remaining in solution is recovered by extraction with
ether. The procedure recommended by Pfeiffer5 differs
from that just described in that the nitration is carried
out on a sample of gas enclosed in a special container
and in that the dinitrobenzene that is formed is not
weighed, but is titrated with stannous chloride accord-
ing to the method of Limpricht.6
COMBUSTION METHOD
Bunsen,7 by making combustions on samples of
illuminating gas before and after the absorption of
'Cornel, rind.. 82 (1876). 871. 927; 83 (1876). 1255; Ann. ckim. phys..
15) 10 (1877). 171; 12 (1877). 289; Bull. soc. chim.. 50 (1888), 660.
» Ber.. 21 (1888). 3131.
• Post. "Cham te. -lin. Analyse." 2nd Ed.. Vol. I. pp. 108. 179.
• Z. anon. Chem.. 16 (1898). 41.
• J. Casbel.. 42 (1899). 698; Chem.-Zlg.. 28 (1904). 884.
• Ber.. 11 (1878). 35.
' "Gasometrische Methoden." 1877, 2nd Ed., p. 142.
benzene vapor and defines by fuming sulfuric acid,
obtained data from which he computed the amounts
of benzene, ethylene, and propylene. The accuracy of
this method depends upon the amount of other hydro-
carbons, absorbable by fuming sulfuric acid, which may
be present in the gas.
ALCOHOL METHOD
Bunsen1 also determined the amount of benzene
vapor and other hydrocarbon vapors present in illumi-
nating gases by absorption in absolute alcohol. The
hydrocarbons thus removed from the gas, consisting
chiefly of benzene, are separated from the alcohol by
pouring it into a large volume of a concentrated solution
of sodium chloride, whereupon the hydrocarbons are
obtained as an oily liquid upon the surface of the salt
solution. Their amount is determined by weighing.
By the method of Hempel and Dennis,2 alcohol may be
employed • for the gas-volumetric determination of
benzene vapor by employing i cc. of absolute alcohol
in a pipette over mercury, and measuring the decrease
in volume that results from contact of gas with the
alcohol. Later Dennis and O'Neill3 showed that, while
concordant results may be obtained by the alcohol
method, absorption of benzene by this reagent is by
no means complete.
PHOTOMETRIC METHOD
Knublauch4 has devised a method for the determina-
tion of benzene and ethylene in illuminating gases
based upon the determination of the illuminating power
of the gas and the total amount of benzene and ethylene
present. From these data and a knowledge of the
illuminating powers of benzene and ethylene in the pure
state, the amounts of each can be determined. Graul5
has utilized the photometric method by comparing the
illuminating values of the gas before and after the re-
moval of benzene. In the method employed by Rein-
eke,6 the amount of benzene is determined from the
candle power of the flame, possible variations in the
luminosity due to other constituents of the gas being
disregarded.
CONDENSATION METHOD
Deville7 has developed a method for determining the
benzene vapor in gas mixtures by cooling to — 220 C.
and weighing the solid benzene which separates. Cor-
rection must be made for the vapor pressure of benzene
at the temperature employed. Application of the prin-
ciple of this method has been made by Neubeck.8
According to the procedure followed by Burrell and
Robertson,' the benzene vapor is condensed from a
sample of gas by using a mixture of solid carbon dioxide
and ether or acetone as a refrigerant. The gas which
remains is pumped out and then the benzene is allowed
1 "Gasometrische Methoden." 1877, 2nd Ed., p. 144
• » Ber.. 24 (1891). 1162; /. Casbel. 34 (1891), 414.
• J. Am. Chem. Soc. 26 (1903). 503.
« J. Casbel.. 22 (1879). 652; 23 (1880). 253, 274.
• U. S. Patent No. 1.163.654, December. 1915.
' German Patent No. 285,920, June. W14.
'J. Casbel., 32 (1889). 652.
• Ibid., 68 (1915), 616. Sec also anonymous article in Gas World,
64 (1916), 224.
• This Journal. 7 (1915). 669.
26
THE JOl AW, I/. OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. Xo.
to vaporize, the pressure exerted by the vapor being
determined from a manometer attached to the appa-
ratus. Knowing the atmospheric pressure, the per cent
by volume of benzene vapor is computed. A modifi-
cation of the apparatus employed by Burrell and
Robertson has been suggested by Whiton1 as being
more desirable for use in determining the efficiency of
the benzol scrubbers used on coke-oven gas.
I i MING SULFURIC ACID METHOD
The determination of the combined benzene and
ethylene content of an illuminating gas by fuming sul-
furic acid may be utilized for the indirect determination
of benzene when the amount of ethylene is determined
by some other method. Haber and Oechelhauser2
have employed this procedure, determining the ethyl-
ene content of the gas mixture by treatment with
standardized bromine water, and subsequent deter-
mination of the excess of bromine. Since benzene is
also absorbed by bromine water, the combined benzene
and ethylene content can be determined approximately
by bromine water, as well as by fuming sulfuric acid.
Haber and Lunge3 have described a method for deter-
mining ethylene in the presence of benzene by causing
the ethylene to combine with hydrogen in the presence
of platinum black. The amount of benzene is then
arrived at indirectly by taking the difference between
the combined benzene and olefine content, as deter-
mined by fuming sulfuric acid, and the ethylene content.
PARAFFIN Oil. METHOD
Muller4 has proposed that benzene vapor in illumina-
ting gas be determined by passing the gas through
cooled paraffin oil. The greater part of the benzene
vapor can be absorbed by this method. Nowicki6
had described a special absorbing device for carrying
out this determination. The method has been elab-
orated by Krieger.6 Neubeck7 has modified the pro-
cedure by distilling off the benzene taken up by the oil,
but doe: in ii recommend the method on account of
the difficulty in maintaining air-tight joints during
the distillation. Copp8 has described the procedure
adopted by him in obtaining more efficient absorption
of the benzene vapor.
SPECIFIC GRAM IV Mi
In Lunge's "Chi Untersuchungs-
methoden," Vol. 2 (1900), p. 586, there is described a
method for determining the benzene content of an
illuminating e,as from the specific gravity of the gas and
the amount of defines in it. This method is open to
the objection that possil ons in the amounts
of the other constituents of the gas
AMMONIACA] NICK] L CYANID1 If] I >
Dennis and O'Neill* developed a gas-volumetric
method for the determination of benzene, employing
' Tims JOURNAL, 8 (1916), 733.
* Btr.. 89 (18 <btl, S9 (1896), 804.
■ /. anori Ckem., 16 (IS98), 26.
* J. GuiM.. 41 (1898), *33.
« Ibid., 48 (190!
• Ibid.. 68 (191
' Ibid., 58 (191S). 815.
'Gas World 66
• J. Am. I hem Sdl . 28 (1903), 503.
as a reagent an ammoniacal solution of nickel nitrate.
Later Dennis and McCarthy1 suggested the use of an
ammoniacal solution of nickel cyanide instead of nickel
nitrate, having found that more uniformly reliable re-
sults could be obtained with the former reagent.
SULFURIC ACID METHOD
Morton2 has suggested the use of concentrated sul-
furic acid for the absorption of benzene vapor in the
presence of ethylene. Dennis and McCarthy* found
that this reagent does not give satisfactory results both
on account of the fact that some ethylene is absorbed
by it, and also because the absorption of benzene is
not complete.
SATURATION METHOD
The Soci6te" Roubaisienne d' Eclairage par le Gaz
and RR. L. H. Forrieres4 have developed a method for
benzene based upon the determination of the amount
of benzene that is required to saturate a known volume
of gas. After computing the amount that would be
required, under the conditions of the experiment, for
gas containing no benzene vapor, the benzene content
of the gas is gotten by difference.
THE NEW METHOD
During the summer of 1915, in attempting to develop
a method for determining benzene vapor in gas simply,
quickly, and accurately, the author did considerable
preliminary work upon a method which appears more
nearly to satisfy these requirements than any of the
methods that have been mentioned. In the proposed
method, a measured quantity of gas containing an un-
known amount of benzene vapor is placed in contact
with benzene in a special apparatus and the increase
in volume read. By determining what the increase in
volume would have been, had the gas contained no
benzene vapor, the amount of benzene vapor actually
present is easily computed. That this idea is not
entirely new was learned when a search of the literature
was made and reference to the German Patent described
under the previous heading was found. The procedure
that has been employed is, however, much simpler and
quicker than that described in the patent.
Owing to the failure of attempts to obtain, under
present conditions, apparatus considered essential for
the proper standardization of the method, its further
development has been temporarily postponed.
Cornell University
Ithaca. New Yore
RESEARCH ON THE DETECTION OF ADDED WATER
IN MILK
By Halsey Ditrand and Rbston Stbvbnson
Received September 13. 1917
At the annual meeting of the American Chemical
. . held in Xew York Ci 27, 1916,
the authors read a paper on "The 1 'election of
Water in Milk,"5 in which the importance of
devising a rapid and accurate method was brought
' J. Am. Chrm. Soc SO (1908), 233.
> Ibid.. J8 il*'r.
« Ibid.. 30
nnu Patent No. 267,491, M.iv. 1913.
' Tins Journal. 9 (1917V 44.
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
out and a review of the existing methods was pre-
sented.
The first was the determination of the refractive
index of the milk serum, which, while having the ad-
vantage of speed, proved unreliable for the detection
of less than 10 per cent of added water, vastly too
great a margin. The second was the determination
of the freezing point,1 the elevation above that of
normal milk indicating the percentage of added water;
this is an excellent method, but one requiring too much
time for a routine laboratory. A third method, the
determination of the specific gravity of the whole
milk and of the serum, was also mentioned as having
been in use for many years, but never having given
satisfactory results.
II — A second series of determinations was made,
in which weighed amounts of finely divided silver
nitrate was used for the coagulation. The procedure
was the same as described under I. The silver in 50
cc. of the serum was determined by titration with
N/10 ammonium sulfocyanate, after addition of nitric
acid and using ferric ammonium sulfate as indicator.
This method is much more accurate and rapid than
Method I, but the results show that the differences
in the number of cc. used, in milks of known purity,
are sometimes greater than those between whole milk
and samples watered in the laboratory. The method
was, therefore, abandoned as useless.
Ill — The third method, the determination of the
electrical conductivity by method of Kohlrausch
Table I — Preliminary Experiments
Cell
No. Sample
1 Whole Milk- a.
Table II — Tests Using Test-Tubes
as Cells
Temperature. 25°
Table III — Tests Using Cell No. 2, Accurately
b + 10% Distilled Water.
a + 10% Croton Water. .
c + 10% Distilled Water.
Whole Milk a
Milk
from
Individual Co
Suspicious
Sample
Sealect. Grade I
Temp.
Conduc-
•lo.
° C.
tivity
1
75.7
0.00577
7
75. 17
0.00520
71
75.15
0.00520
4
25.10
0.00479
5
75.17
0.00478
6
75.07
0.00466
7
24.95
0.00513
1
75.0
0.00572
7
25.0
0.00573
3
75.0
0.00522
4
75.0
0.00549
5
25.0
0.00517
6
25.0
0.00503
7
25.0
0.00585
8
25.0
0.00530
9
25.0
0.00521
II)
25.0
0.00571
11
25.0
0.00624
17
25.0
0.00755
13
25.0
0.00560
14
25.0
0.00515
IS
25.0
0.00569
Sample
Authentic Sample
No.
1
Conduc-
tivity
0.00543
Authentic Sample
2
0.00504
Same as 2
3
0.00504
Same as 1
4
5
Same as 2
0.00475
Authentic Sample
6
0.00504
Authentic Sample
7
0.00495
Authentic Sample
8
0 . 00460
Authentic Sample
9
0.00563
10
11
Sameas2
0.00605
12
0.00712
Same as 4
13
0.00727
Filled to Mark
Temperature, 25° C.
Conduc-
Sample
No.
tivity
1
0.00519
2
0.00519
Locust Farm Grade B, pasteurized. . .
3
0.00516
Milk from Individual
Holstein Cow
(Morning Milking,
4
5
6
7
8
0.00519
0.00516
0.00519
0.00513
0.00519
unpasteurized)
No. 4 4- 10% Distilled Water
9
0.00478
10
0.00478
4- 20% Distilled Water
11
0.00430
4- 50% Distilled Water
17
0.00307
4- 1.3% Distilled Water
13
0.00513
4- 3% Distilled Water
14
0.00503
4- 5% Distilled Water
15
0.00491
4- 7% Distilled Water
16
0.00482
4- 10% Distilled Water
17
0.00477
Grade A Milk from lA bottle (2 days
old)
IK
0.00503
19
20
Milk from 1 after Removal of Cream
0.00532
A brief outline was given, in which methods for
further research were proposed and the results obtained
are the subject of this contribution.
I — The first of these methods to be investigated
was based on the theory that added water would in-
crease the solubility of inorganic salts in the serum.
A series of determinations was made using a weighed
amount of anhydrous lead subacetate. The reagent
was that used in Home's methods for sugar analysis.
Experiment showed that 3 g. were required for the
■coagulation of 100 cc. of milk. After the addition
of the subacetate, the contents of the flask were vigor-
ously shaken to coagulate the milk thoroughly. The
contents of the flask were poured on a dry folded filter
and 50 cc. of the serum collected for the determination.
The lead was precipitated with 25 per cent of sulfuric
acid, and alcohol added to facilitate the precipitation.
The lead sulfate was collected in an alundum crucible,
washed with water and finally with alcohol, ignited
and weighed. Several determinations were made by
"the above method.
The results proved unreliable, in that a variable
amount of the subacetate in solution is adsorbed by
the coagulum, and that, owing to the slowness of the
filtration, it proved impractical to wash out all of the
organic matter not coagulated, this latter causing a
reduction of a portion of the lead sulfate when ignited.
' Chem. New*. 110, No. 2870, p. 259; No. 2871. p. 275; No. 2872. p.
of the whole milk, and of the serum after coagulation
with electrolytes and non-electrolytes, has been tried
out in an exhaustive manner during the past year by
the authors.
Through the courtesy of Dr. Charles Baskerville,
director of the Department of Chemistry, of the College
of the City of New York, permission was obtained to
carry on these experiments in the laboratories of that
institution.
The first series of experiments (Table I) was per-
formed in a cell used for conductivity experiments in
the laboratory, in which the electrodes were kept at
a uniform distance, but were placed in the cell after
filling without regard to their proximity to the sides.
This cell was designated as No. i. A constant tempera-
ture was maintained during all of the following de-
terminations, by warming the water by a coil of re-
sistance wire, and stirring by bubbling compressed air,
the current in the coil being regulated by a rheostat.
It will be observed from these results that there is a
decided similarity in the results on whole milk, and also
following the theory, the milks to which water has been
added give a lower conductivity.
In the second series of experiments, Table I, Cell 2,
a cell similar in construction to Cell 1 but of greater
capacity and with larger electrodes than the above,
was used.
Here as with Cell 1, the samples of known purity
gave excellent results. The results on the samples
28 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
, , . , , ,, . , ■• j __ Table IV — Tests'Usiko Special Cell
marked, in ice-box 2 days, are not to be relied on,
, , Timptraluri. 28° C.
as change in composition has probably taken place. sample op milk
In Table II, test-tubes, of the same commercial g^S^U,^^^*0'
size, were used to facilitate the work, as a number of *%Z*32*£ *?* ^ /.?.!??.?. ™^
tubes could be placed in the bath at the same time, to Grade B^pMteuri^d (Borden's
brine them to the required temperature. The same Same, another
to . . , Grade B pasteurized i Sheffield)
methods were used as in Table I. In this series a wide Grade b pasteurized rciover Farm)
deviation was observed on different tubes containing j^ ™ Pa!teuX^Mutuai-McDermo«t/
the same milk, amounting at most to 37.0 per cent in No. 4 + 2 per cent distilled water
, No. 4 + 5 per cent distilled water
the conductance. This was found to be due to tne no. 4 +10 per cent distilled water
.,_ . , . , 1 , .* _*. „r No. 7 -t- 2 per cent distilled water. .. .
difference in size ot the tubes and to the amount ot xo. 7 + 5 per cent distilled water
sample contained. To avoid a continuance of these n°- 8 + s per cent distilled water
_, , . , Grade B collected from shop
errors a file mark was made on Cell 2 and in tne
subsequent determinations the cell was carefully filled
to this mark.
The results in Table III for the whole milk are much »* • f2 'e""ted f" 5 ™inutes
Grade B collected from shop
more uniform than in the previous determinations,
but a variation still persists. The samples to which
No. 27 repeated
Ground G/aSS Stopper Grade B collected from shop
1
Mercury Contact Tu6e —
Lead G/ass fused Supports
40
41
Grade A' collected from shop 42
44
45
46
47
48
Grade A. mixed samples, 1st bottle 49
2nd bottle 50
Authentic sample 51
No. 51 second;reading 52
Authentic sample 53
55
No. 53 + 7 percent water 56
Ai-thentic Sample, unpasteurized 57
Milk from 3 or 4 mixed breed cows 58
Same as above after 10 minutes 59
No. 59 after 40 minutes 60
Same as No. 57 61
No. 62 second reading 63
Vol. io, Xo. i
Conductivity
0.00546
0.00540
0.00541
0.00563
0.00559
0.00559
0.00544
0.00569
0.00566
0 00563
0 00546
0 00537
0.00512
0 00536
0.00523
0.00541
0 . 00539
0.00541
0.00550
0.00560
0.00561
0.00555
0.00554-
0.00558-
0.00577
0.00579-
0.00535
0.00558
0.00536-
0.00560-
0.00575-
0.00554
0.00567
0.00566-
0.00563
0.00564-
0.00563
0.0057T
0.00554
0.OO53T
0.00546-
0.00555-
0.00552
0.00532
0.00534
0.00535
0.00530-
0.00548
0. 00450
0 00643
0.00843
0.00435
0.00555
0.00552
0.00565
0.00569
0.00575
0.00551
0.00545
SoJJJ $/ass Sea/ —
Ore u/a r P/at/num S/£-ctrodes
(/O x OS mm)
Sea/e-d So cj/ass
water has been added show a regular decrease in con-
ductivity as the amount of water added increases. A
search of the literature on electrical conductivity, while
discussing the size and distance of the electrodes and
the form of the cell, fails to make mention of the error
introduced by using varying amounts of solution. This
phenomenon is being made the subject of a s
investigation.
As a final effort to determine the cause of the
variations ill milk a special cell v-
as shown in the accompanying drawing.
This cell has the advantage that the electroi
sealed in a ; position, a constant distance
apart, and with the same amount of liquid above and
below them.
The results in Table IV are n
in that a wide discrepancy in conductivity exists
even in authentic samples. It was then decided to
separate the milk and cream and to determine the con-
ductivity of the skimmed milk. Through the courtesy
of 'Messrs. Paul and Terhune of the DeLaval Separator
Company, a cream separator was obtained and the
samples separated. Determinations were made on
whole milk, skimmed milk and cream.
The determinations in Table V were made under
ideal conditions. The cell was accurately filled to
the mark, the temperature kept at 2S.00 C. ^o.os
and correction made for each d( A large
number of the samples were collected under the personal
supervision of department inspectors so that there
could be no doubt as to their authenticity. The method
of measurement was sufficiently sensitive to detect
0.5 per cent of added water, and the fact that the cell
constant did not vary was confirmed 1 y frequent de-
terminations, using .iV/50 potassium chloride solution.
To preclude the possibility of error through improper
running of the separator, a representative of the:
Jan., 1918
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
29
Table V-
Authentic Samples.
Sample
Whole Milk, Can No. 1
No. 1 after separation
Whole Milk, Can No. 2
No. 2 after separation
Whole Milk. Can No. 3
No. 3 after separation
Whole Milk. Can No. 4
No. 4 after separation
Whole Milk. Can No. 5
No. 5 after separation
No. 5 after separation and filtering to remove air
bubbles
No. 4 after separation, coagulated with rennin and
filtered
No. 3 after separation, coagulated with pancreatin
and filtered
One Holstein cow producing 16 qts. per day
One Jersey cow producing 14 qts. per day
Mixed Jersey and Holstein herd
Holstein herd
No. 14 after separation
No. 15 after separation
No. 16 after separation
No. 1 7 after separation
No. 18 after separation.
No. 18 after separation ;
Grade B. pasteurized (Borden's)
Grade B. pasteurized (Sheffield)
Grade B. pasteurized (Clover Farms)
Grade A. pasteurized (Locust Farms)
Grade A. pasteurized (Sealect Sheffield)
No. 25 after separation
No. 26 after separation
No. 27 after separation
No. 28 after separation
No. 29 after separation
No. 29 coagulated with rennin and filtered.
No. 28 coagulated with rennin and filtered.
One Holstein cow
One Durham cow
Mixed Holstein and Durham herd
Determination on WbolS and Skimmed Milk and Cream
From 5 Cows. Milk from 4 Cows in Each Can. Morning Milkings (1-13)
Temperature, 28° C.
ad filtratio
No. 37 after separation.
No. 38 after separation.
No. 39 after separation.
No. 40 after separation.
No. 41 after separation.
Conductivity
0.00561
0.00590
0.00592
0.00629
0.00567
0.00605
0.00595
0.00621
0.00672
0.00643
0.00539
0.00601
0.00555
0.00547
0.00554
0.00576
0.00627
0.00596
0.00581
0.00586
0.00586
0.00565
0.00543
0.00580
0.00573
0.00560
0.00596
0.00581
0.00605
0.00599
0.00586
0.00611
0 . 00645
0.00590
0.00538
0.00560
0.00559
0.00560
0.00607
0.00574
0.00587
0.00599
0.00599
0.00538
0.00562
0.00561
0.00561
0.00603
DeLaval Company, separated the samples in Determina-
tions 59 to 72.
As the milk after separation contains air bubbles,
the milk was filtered to remove them. It was found
that the readings before and after_ filtration did not
vary (Nos. 10 and n).
As the samples were run through the separator one
after another, it was deemed advisable to determine
if the samples were affected by the ones preceding.
Four samples were mixed thoroughly, then divided
again into 4 samples and run through the separator
successively (Nos. 96 to 99). Three of these results
were fairly uniform.
It will also be observed that the average of the
readings on individual milks corresponds very closely
with the reading after mixing Nos. 88 to 94.
With all known sources of error eliminated the read-
ings on authentic samples still showed so wide a differ-
ence as to render the method useless.
In the freezing-point determination the fat and pro-
tein of the milk play no part and the constant depends
entirely on the concentration of the substances in
solution.
In the conductivity measurements, however, the
fat and protein of the milk decrease the specific con-
Sample
No. 47 after separation
No. 48 after separation
No. 49 after separation
No. 50 after separation
No. 5 I after separation
Separated cream from all samples mixed.
Separated milk from all samples mixed. . .
Separator run by representative of DeLaval Co.
Milk from single Holstein unpasteurized
No. 59 after separation
No. 60 after separation
No. 61 after separation
No. 62 after separation
No. 63 after separation
Mixed separated milk -f 5 per cent separated
cream
-f- 10 per cent separated
cream
Mixed separated milk, all samples
Mixed separated cream, all samples
Grade A. certified unpasteurized (Sheffield)
Grade A, pasteurized (Locust Farms)
Grade A. pasteurized (Sheffield. Sealect.)
Grade A. pasteurized (Sheffield. Sealect)
Grade A. pasteurized (Mutual-McDermott)
No. 73 after separation
No. 74 after separation
No. 75 after separation
No. 76 after separation
No. 77 after separation
Separated cream from No. 73
Separated cream from No. 74
Separated cream from No. 75
Separated cream from No. 76
Separated cream from No. 77
Grade B raw taken from cans
Nos. 88 and 89 mixed
Grade B raw taken from cans.
Nos. 91 and 92 mixed..
Nos. 88. 89. 91. 92 mixed
No. 89 second leading
Nos. 88, 89. 91. 92 mixed, after separation.
0.00574
0.00589
0.00616
0.00593
0.00632
0.00576
0.00555
0.00536
0.00606
0.00569
0.00606
0.00586
0.00569
0.00614
0.00610
0.00589
0.00602
0.00445
0.00554
0.00581
0.00573
0.00552
0.00547
0.00591
0.00619
0.00595
0.00575
0.00570
0.00448
0.00431
0.00435
0.00414
0.00417
0.00585
0.00592
0.00589
0.00545
0.00537
0.00540
0.00563
0.00555
0.00589
0.00596
0.00592
0.00594
ductance by decreasing the number of ions between
the electrodes in just the same manner as would glass
beads placed in the cell between the electrodes.
A final series of determinations (Table VI) was made
on samples of milk coagulated with basic lead acetate
Table VI — Tests Using Milk Sera
Conductivity
0.00653
0.00645
0.00647
0.00647
0 . 00649
0.00645
0.00645
0.00649
0.00643
0.00651
0 . 00649
0.00649
0 . 00653
0.00647
0 . 00647
0.00643
Temperattire:
, 28° C.
Chemical Analysis
Total
Sample
Solids
Fat
AA-223....
1 1 . 82
3.3
AA-226....
12.01
3.4
AA-227....
13.18
3.6
AA-228....
11.94
3.4
AA-230....
12.06
3.5
AA-232....
11.90
3.6
AA-233....
11.78
3.5
AA-234....
11.94
3.4
AA-235....
12.13
3.5
B-456....
11.94
3.4
B-457....
12.13
3.5
B-460
11.70
3.2
B-461
12.38
4.0
B-463
12.28
3.8
2A-501....
12.36
3.4
2B-505....
11.87
3.4
2A-505
Serum + 5
Serum from authentic milk Grade A raw.
As above -f- 5 per cent water.
4- 5 per cent water.
4- 10 per cent . i i . i
+ 10 per cent water
+ 20 per cent water.
+ 20 per cent water.
0 . 00653
(i 00682
n urn, .■>
II 11111,1,7
0.00682
0.00657
0.00667
0 . 006.19
n 00663
0 00628
ii iiiii.ii,
0 in.
0.00591
30
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. i
(Home's). One hundred cubic centimeters of the milk
were taken and 3 g. of the acetate accurately weighed
and added, thoroughly shaken and filtered to 50 cc.
Readings were then made on the clear sera.
The determinations made on laboratory samples
1 to 16 show a fair degree of uniformity. It will be
observed from a comparison of the conductivity and
the chemical analysis, that the differences in fat and
total solids content bear no relation to the differences
in conductivity. The sera from authentic samples
18 to 23 show a far greater variation than has been
observed in any of the foregoing determinations and
the results are entirely unreliable.
In the authentic samples adulterated in the labora-
tory (24 to 29) the water was first added to the samples
and 100 cc. of the adulterated milk were then taken
and coagulated as described above.
These results show great differences, even at the
same adulteration and these differences are greater
than those between the authentic and adulterated
samples. This is probably due to an irregular ad-
sorption of the lead salt by the coagulum, which would
account for the lack of uniformity in the results, as
was the case in experiments mentioned under Method I
at the beginning of this paper.
Having tried out the method and investigated all
of the modifications at hand in a most exhaustive
manner and being unable to obtain any uniformity
in results it was decided to abandon the method as
impractical.
It is to be regretted that this method proved ineffec-
tive, as a rapid and accurate method of this sort would
be of great value to the food analyst.
One of the authors, Durand, proposes at an early
date to continue this research, making use of the os-
motic pressure of milk, in a cell specially constructed
to measure the differential osmotic pressure between
milks and a standard saline solution.
Chemical Laboratory. Department or Health
AND
College of the City op New York
New York City
THE LOGANBERRY AND THE ACID CONTENT OF ITS
JUICE
By Milo Reason Daughters
Received September 24. 1917
Attention has been called to the composition of
loganberry pulp and juice and to the drying proper-
ties of loganberry oil.1 This paper gives the com-
position of the fresh, ripe, whole berry and some data
on the juice, with special reference to its acid content.
Table I — Composition op the Loganberry'
Per cent
Total Solids 20. 74
Moisture 79 . 26
Citric Acid (anhydrous) \.S2
Invert Sugar 7.15
Sucrose Absent
Protein! (N X 6.25) 4.55
Fat (ether extract) 0.613
Crude Fiber | , 38
Ash 0\571
1 This Journal. 9 (1917), 1043.
• Colby reported the analysis of a sample of California loganberries.
California Experiment Station Report. 1S96, 177.
The sample (Table I) was taken from 14 lbs. of berries
gathered at the close of a uniformly dry season. Total
moisture was obtained by heating in vacuo at 70° C.
to constant weight. An electric muffle furnace heated
to dull redness was used for the ash determinations.
Citric acid was estimated by the method given in
the Journal of the Association of Official Agricultural
Chemists, Vol. 2 (1916), 183.
Table II — Composition op thp. Juice
Sample No. I II III IV
Date of Collection (1917) July 18 July 25 July 28 August 7
Speci6c Gravity (25 ° C.) 1 . 0526 1 . 0548 1 . 0565 1 . 0599
Acidity (as anhydrous citric) 1.904 1.60 1.515 1.54
Citric Acid (anhydrous) 1.82 1.521 1.511 1.54
Volatile Acids (acetic) 0.048 0.025
Total Solids 12.84 12.49 14.74
Invert Sugar 8.55 8.80 9.06 8.74
Protein IN' X 6.25) 0.871 0.497 0.37
Ash 0.499 0.45 0.39
The first three samples of juice were pressed from
4 to 5 lbs. of berries purchased in the open market.
The berries were ground in a food chopper and then
pressed in a small fruit press lined with doubled
bird's-eye cotton cloth. Sample IV was obtained
in a similar manner in a larger press from 14 lbs. of
berries after removing the sample for the analysis
given in Table I. The specific gravity readings were
made by the pyenometer method on the juice which
was kept in a constant temperature bath at 25 ° C.
Dunbar and Lepper1 have made a study of the
Kunz! modification of Stahre's method3 for the quan-
titative estimation of citric acid and have announced
its applicability to fruit products. This method was
applied directly to the juice without preliminary pre-
cipitation of the citric acid as the barium salt in the
last three samples. Twenty-five grams of juice were
placed in a volumetric flask of 100 cc. capacity, and
2 cc. of dilute sulfuric acid and 3 cc. of freshly pre-
pared bromine water added, and then made up to the
mark with distilled water. Aliquots of 2$ cc. each
were used in the analysis. Approximately 40 cc.
of 5 per cent potassium permanganate were required
to complete the oxidation of the citric acid, pectins,
sugars, etc. Pentabromacetone separated in a very
satisfactory manner as a white semicrystalline solid,
leaving a clear supernatant liquid after the addition
of ferrous sulfate.
Samples II and III were examined for volatile acids,
which were found to be present in traces. Tartaric
acid was found in traces by Jorgensen's method.4
Dunbar and Bacon's5 uranyl acetate method for
malic acid was tried on Sample I, but with negative
results.
In conclusion, it may be stated that citric is the
chief acid of the loganberry. Traces of tartaric and
volatile acids are also present. Malic acid is absent.
Department op Chemistry
Oregon State Agricultural College
CoitvALua
1 Jr. A. O. A. C S (1916). 182; No. 4 (1917). 175.
» Arch. Chtm. Mikros., 7 (1914), 285; Chtm. Abs . 9 '1915), 687.
■ Sordisk Tidsskrift. 1 (1895). 141; Z. anal. Chrm . 36 1897). 19S.
• Z. .Vj/ir. Crnussm .. 17 (1909), 397; Abderhalden, "Handbuch Bio-
chem. Arbeitsmeth.," 1 (1910), 35; Chtm. Abs.. 3 (1909
• U S Dept. of Agr., Bureau of Chemistry, c 'main 76. Jr. A. O. A. C,
9 0917). 179; This Journal. S (1911). 826.
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
5i
REACTION OF HAWAIIAN SOILS WITH CALCIUM
BICARBONATE SOLUTIONS, ITS RELATION TO THE
DETERMINATION OF LIME REQUIREMENTS OF
SOILS, AND A RAPID APPROXIMATE METHOD FOR
THE DETERMINATION OF LIME REQUIREMENTS
OF SOILS'
By Maxwell O. Johnson
Received October 1. 1917
The importance of liming for the maintenance of soil
fertility is so well recognized that a number of methods
for determining the lime requirements of soils have been
proposed. Most of these methods are based on reactions
which do not parallel those occurring in the field.
Whether lime is applied as oxide, hydroxide or carbonate
the main reaction of the limed soil would appear to be
with calcium bicarbonate in solution.
Hutchinson and MacLennan2 and Maclntire3 have
proposed methods for determining the lime require-
ments of soils using calcium bicarbonate solutions.
In the Hutchinson- MacLennan method, 10-20 g.
of soil are shaken for 3 hours with 200 to 300 cc. of an
approximately 0.02 N bicarbonate solution. After
filtering, a portion of the filtrate is titrated with 0.1
N acid, using methyl orange as an indicator to deter-
mine the calcium carbonate absorbed by the soil. In
the Maclntire method 150 cc. of bicarbonate solution
are evaporated with 10 g. of soil to a thin paste and the
excess calcium carbonate estimated by the CO2
liberated with acid.
An investigation has been made of the reaction of
typical Hawaiian soils with calcium bicarbonate solu-
tions under various conditions. As a .preliminary
announcement of results, it may be stated that the ex-
tent of the reaction has been found to depend on the
usual factors influencing absorption, i. e., the nature
of the soil, the concentration of solution, the period of
contact and the ratio of soil to solution. This would
account for the variations in results obtained by the
Hutchinson-MacLennan and by the Maclntire methods
when slight variations are made in the methods of
procedure.4
The absorption by the soils from calcium bicarbonate
solutions increased with the period of contact and ap-
proached an equilibrium. As the concentration of the
bicarbonate solution was decreased, the absorption
decreased in amount but an increasing percentage of
the total calcium carbonate in the bicarbonate solution
was absorbed. This would show that by using solu-
tions of decreasing concentrations or by using increasing
weights of soil a point would be reached where absorp-
tion would be practically complete under prolonged
contact sufficient to insure equilibrium of the soil
with the solution. The total amount of calcium car-
bonate (calculated as per cent of the weight of the soil)
in the solution at and below whose concentration ab-
sorption by a given soil is complete, would appear to
express a definite absorptive capacity for that soil.
This definite absorptive capacity has been designated
1 Published by permission of the Secretary of Agriculture.
• J. Agr. Set.. [1)7 (1915). 75-105.
« This Journal, 7 (1915), 864-867.
« See Jour. Assoc. Off. Agr. Chtm.. 3 (1917). 133-149.
the "minimum absorption." An amount of calcium
carbonate slightly in excess of the minimum absorption
would appear to be the correct application to make in
the field as being sufficient to insure a slight alkaline
reaction. In theory, the lime requirements of a soil
by the Veitch method1 should lie very slightly above
the minimum absorption, since the Veitch method de-
pends, in principle, upon the satisfying of the minimum
absorption of a soil and the presence in the solution,
which is allowed to stand in contact with the soil over
night, of sufficient calcium bicarbonate to give an alka-
line reaction to phenolphthalein when 50 cc. are boiled
down to s cc- Under the practical conditions of the
method, however, some of the factors introduced may
cause the results to differ from the minimum absorp-
tion. The lime requirements of soils by the Hutchinson-
MacLennan method,2 by the Maclntire method,3
by the Tacke method,4 by Suchting's modification8 of
the Tacke method, and by the Vacuum method of
Gaither6 would be much greater than the minimum
absorption and depend on the conditions selected, since
the results are determined from the absorption when
the soil is in equilibrium with a large excess of calcium
bicarbonate in solution.
The minimum absorption of a soil may be determined
as defined above by subjecting to prolonged contact
a constant weight of soil with decreasing concentra-
tions of bicarbonate solution or increasing weights of
soil with a constant concentration of bicarbonate solu-
tion and determining the point where complete absorp-
tion occurs.
For the routine examination of soils, where great
accuracy is not required, a rapid approximate method
of determining lime requirements has been worked out
and appears to give good results. It was found that
when "acid " Hawaiian soils were shaken with solutions
of sufficient concentration to insure a fairly rapid con-
tact of solute with soil particles, an extemely rapid
absorption reaction takes place, approaching in velocity
that of an ionic reaction with a soluble acid, which reac-
tion is followed by a much slower increase in the absorp-
tion with the time. This is illustrated by the following
experiment:
200 cc. portions of 0.01 N calcium bicarbonate solu-
tion were measured out in 500 cc. Erlenmeyer flasks.
The soils used were three typical acid Hawaiian soils
and an alkaline station soil containing 1.63 per cent
CaO. 10 g. of soils were added to each flask and the
flasks immediately stopped and shaken vigorously by
hand for 1, 2, 3, 4, 5. 7 and 10-minute periods. At the
conclusion of the period of shaking, the flasks were
opened, and the contents filtered through a 24 cm. folded
filter paper, discarding the first 40 or 50 cc. of filtrate.
100 cc. of the filtrate were titrated with 0.1 A" HC1,
using methyl orange as an indicator. The absorption
was measured by the difference in titration between
'./our. Amcr. Chem. Soc, 24 (1902), 1120-1128; 26 (1904). 637-662.
1 Loc. cit.
• Ibid.
'Chem.-Zlg.tl (1897). 174-175.
• Z. angew. Chem.. 81 (1908). 151-153.
• This Journal. 8 (1916), 243-246.
;-'
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMIST : to, Xo. i
ioo cc. of the origii onate solution and of the
o.i cc. of o.i N acid difference in titration being
'iit to an absorption of o.oi per cent calcium
carbonate by the 10 g. of soil. The results are given in
Table I and in graphical form in Fig. i.
TaiiI.II I — AllSORPTION PROM CALCIUM BlCARDONATB SOLUTIONS BY
Hawaiian Soils undkr Various Periods op Contact
Absorption c.\| 11 [um carbonate in per cent of the weight
the soil
K:ii\viki Walpio Alkaline
Soil Soil Soil Station Soil
1 0. 17 l> .VI 0.24 0.03
2 0.20 0.39 0.29 0.04
3 0 114 1 0.3S 0.05
l 0.25 ii It 0.36 0.05
5 0.43 0.37 0.05
7 ') 4K 0.39 0.06
in 0.30 0.50 'i II 0.06
.. animation of Table I and Fig. I shows, with the
i! ind Kaiwiki soils, the very rapid reaction taking
place during the first minute of shaking and the much
slower absorption which follows. With the Waipio
soil, the rapid reaction apparently requires 3 minutes'
shaking for completion. The alkaline station soil
shows a slight, slowly increasing absorption. It should
be noted that the absorption during the first rapid
0.40
2 ° 0.2.0
O- z
0.10
Alkaline Sution so^l
a 3 4 5 & 7
TIME OF SHAK1N6
6 9 10 Mm.
Fio. I — Curvhs Showing tub Eppbct op tub Timb op Shaking upon
tub Adsorption uv Hawaiian Soils prom Calcium
blcardonatb solution
reaction corresponds closely with the lime requirements
by the Veitch method' which are 0.17, 0.^4, and 0.32
um carbonate fur the Haiku, Kaiwiki and
Waipio soils, respectively.
"1 of examination used in the above ex-
been applied to I .waiian soils,
and the absorption during the first rapid reaction ap-
! to offer quite an accurate measure of the lime
requirements of these soils. Determining the lime re-
iLoccU.
quirements of a soil by the absorption during a single
shaking of one minute appears sufficiently accurate
for routine soil examinations.
Due to the known peculiar nature of Hawaiian soils,
48 soil samples were secured for camparison from 8
different mainland states and the method used in the
above experiment applied to these samples. It was
found that the time of shaking could be shortened to
10 seconds for these mainland soils. The absorption
during this 10 seconds' shaking corresponded closely
with the lime requirements for these soils by the Veitch
method and with the amounts of lime which general
experience has found best in field trials, running from
1 to 3 tons of calcium carbonate per 2,000,000 lbs. of
soil for ordinary acid soils and about 6 to 8 tons for
acid peats. The method appeared to distinguish easily
alkaline from acid soils as the alkaline soils had but a
small absorption (less than 0.06 per cent calcium
carbonate). For mainland soils, the following procedure
is therefore recommended as a rapid, approximate
method of determining lime requirements:
Measure out 200 cc. of 0.01 N calcium bicarbonate
solution into a 500 cc. Erlenmeyer flask. Add 10 g. of
the soil to be examined to the flask, stopper and shake
vigorously by hand for 10 seconds. Filter through a
large folded filter paper, discarding the first 40 or 50
cc. of filtrate. Titrate 100 cc. of filtrate with 0.1 N
acid, using methyl orange as an indicator. The 0.1
difference in titration between 100 cc. of the filtrate and
of the original solution is equivalent to 0.0 1 per cent
calcium carbonate required. Multiplying by 10 the
percentage calcium carbonate required gives directly
the tons of calcium carbonate per 2,000,000 lbs. of soil,
which is the weight of soil per acre commonly assumed
as being in reaction with applied forms of lime. As
filtration is very rapid, it appears that the absorption
by this method is sufficient to induce flocculation. A
clear filtrate, easily titrated, is always secured, even
with peat soils.
For preparing calcium bicarbonate solutions, Mac-
Intire1 gives in detail a method of preparation by passing
carbon dioxide through a suspension of calcium car-
bonate. The method of preparation made use of by
Hutchinson and MacLennan1 is more convenient. A
refillable soda water syphon is used, which is charged
by means of small bulbs of compressed carbon dioxide.
In this laboratory, about 10 g. of C. P. calcium carbonate
ced in the carbonic syphon which is filled to the
mark with distilled water and charged. Solution is
sufficiently complete in about 15 min. if the syphon is
gently shaken. The syphon is then opened and the
contents poured into a 2.5-liter bottle and diluted to
about 1500 ee. After the solid calcium carbon
settled, the liquid is decanted, in portions, into a 600-cc.
beaker, from which, after settling, it | into a
large filter paper. A glass stirring rod placed in the
funnel along the sloping side underneath the filter paper
aids the rapidity of filtration. Decanting and filtering
in this manner makes the filtration a very rapid pro-
cess. The filtrate is shaken to insure unif irmity and
'Locctf.
Jan., 1918 j
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
50 cc. are titrated with 0.1 N acid, using methyl orange.
The filtrate is then diluted to the desired concentration,
which can be done with sufficient accuracy by measur-
ing the filtrate and the diluting water into a 4 -liter bottle
with a 500-cc. graduated cylinder. The accuracy of
the dilution is confirmed by titrating 100 cc. of the
diluted solution. A 0.01 N solution is used as this
concentration is fairly stable provided the containing
bottles are kept stoppered. It was not found necessary
to displace the air in the flasks with carbon dioxide
during determinations when this concentration was
used. The calcium carbonate which settled when the
liquid was decanted is returned to the syphon which is
recharged and set aside until a fresh solution of bicar-
bonate is required. While the 0.01 Ar solution is fairly
stable and may be kept under pressure, it is better,
however, to prepare the bicarbonate solution fresh
each day. Any solution remaining unused from the
previous day may be added to the fresh solution before
filtration.
Hawaii Agricultural Experiment Station
Honolulu, T. H.
Table I — Per cent Water-Soluble Phosphoric Ac
Allowed to Stand.
A — Acid Phosphate & Guano
Period of * Mixture
B — Lime Superphosphate & Lime
Mixture
Containing
Period of \5C,
REVERTED PHOSPHATE
By Carlton C. Jambs
Received August 28. 1917
As there has been so much published recently con-
cerning the reversion of acid phosphate, its value
after reversion, and its effect upon plant growth,
it seems advisable to set forth some of the work done
by the writer along these lines during the last eight
years.
This worl was inaugurated and continued in order
to control better the complete fertilizer mixtures,
and to provide a more effective phosphate for soil
conditions in Hawaii. Moreover, the contradictory
results and opinions of investigators and control
chemists elsewhere has made it necessary to verify
or disprove them when applied to conditions in Hawaii.
It has been generally held that iron and aluminum
phosphates are of little value as a source of phosphorus.
Now comes a recent publication by McGeorge1 show-
ing that in sand cultures with millet, ferric and alu-
minum phosphate produced more vigorous plants than
acid phosphate, sodium phosphate, phosphate rock
or Thomas slag. Similarly, it has been held that re-
verted phosphate is of less value than acid phosphate.
Considering the results obtained here by an acid
phosphate which has been reverted, we are inclined
to believe that under certain conditions prevailing
in Hawaii, reverted phosphate gives the better results.
EXPERIMENTAL
In a previous article2 the writer showed that some
reversion may be expected from the action of lime,
carbonate of lime, and a mixture of carbonate and
phosphate of lime in mixed fertilizers. In this article
methods, means and materials used to revert the acid
phosphate completely, are considered.
In the first experiment four laboratory samples
^Hawaii Agric Exp. Station. Bull. 41.
' This Journal. 9 (1917), 682.
fertoa of < mixture • Period of iSYo 3u%
Standing No. 1 No. 2 No. 3 No. 4 Standing Lime Lime
On mixing 9.1 8.6 7.6 7.5 On mixing 15.81 13.02
2 days 7.0 6.63 2 days 10 17 6.93
3 7.25 6.72 6 9.05 6.23
7 5.08 5.39 10 8.34 5.52
8 6.08 5.67 14 7.87 5.05
11 4.47 4.72 18 7.23 4.70
14 5.37 4.6 21 7.23 3.82
16 3.98 3.82 25 6.99 3.98
20 4.8 4.3 28 6.76 4.58
24 4.59 3.8 35 6.64 4.19
29 4.47 3.54 40 6.46 4.11
35 2.44 2.23 54 6.51 5.67
48 3.55 2.97 68 6.46 5.62
458 0.93 4.60
1580 0.48 2.90
were prepared, the constants of which were acid phos-
phate and brown guano, the name given to a low-grade
Laysan Island phosphate containing coral sand.
The variable was lime, CaO. Each sample contained
200 g. acid phosphate and 200 g. brown guano: in
addition, No. 1 contained 7.4 g. of lime, the theoretical
amount to revert all water-soluble lime phosphate,
disregarding whatever effect the calcium carbonate
in the brown guano might have. No. 2 contained
twice as much lime, 14.8 g. To Nos. 3 and 4 were
added 2 g. and 4 g. of lime, respectively. The samples
So/tf6/e phospfaric ocd
became appreciably warm, and one hour after mixing,
the temperatures in Nos. 1 and 2 were 35 and 36 °
C, respectively, a rise of 9 and 10° C. over room
temperature.
At intervals, analyses were made by the uranium
volumetric method for water-soluble phosphoric acid,
the results of which are shown in Table \A.
This table shows a reversion of from 5.16 to 5.63 per
cent of water-soluble phosphoric acid, and also that
the greater reversion is caused by the greater amount
of lime.
These points have been laid out diagrammatically
on quadrille paper and a smooth line drawn through
the points plotted to show the rapidity with which
the action takes place at first and how it is gradually
retarded. It will be seen that if the lines were ex-
tended, considerable time would elapse before all the
phosphoric acid would become reverted. While these
results were satisfactory, it was deemed advisable to
remove the brown guano as the supply was becoming
limited, and to try larger samples over a longer period
of time.
Some time later, with this in mind, another labora-
tory experiment was carried on with lime super-
phosphate, the analyses being made at close intervals
34
THE JOURNAL OF INDUSTRIAL
for about two months, the next analyses after 458
days, and the final complete analyses after 1580 days
or approximately 4 years and 5 months. To 1000
g. of acid phosphate in each of two bottles were added
150 and 300 g. lime, CaO. The analyses of water-
soluble phosphoric acid are shown in Table IB. On
mixing, the sample with 15 per cent lime contained
15.81 per cent water-soluble P2O5 and 17.18 per cent
total PjOj; after standing 1580 days, 0.48 per cent
water-soluble, 13.89 available, and 20.02 total PjOs.
The sample to which 30 per cent lime was added con-
tained on mixing 13.02 per cent water-soluble P2O5
and 14.15 per cent total P2O5; after 1580 days, 2.9
per cent water-soluble, 13.69 per cent available and
16.62 per cent total P205.
The sample containing 15 per cent lime shows a
AND ENGINEERING CHEMISTRY Vol. 10, No. 1
Table II — Factory Experiment op Mixing Acid Phosphate and Lime
Mixture Analyses op Mixture
( Acid Total Soluble and Water-Soluble
Percentages j Lime phosphate P:Oi Available P:Oi PsOi
No. 1 I" 90 19.16 2.18
2 15 85 18.56 17.16 2.92
3 20 80 1 7 06 1 . 50
4 25 75 16.70 15.33 2.88
Samples for analyses of the first series of experi-
ments with lime and acid phosphate were taken 18
hrs. after mixing. Reaction started from 10 to 20
mins. after mixing, and the material lost water rapidly.
At the same time it took on a lighter color and a more
friable powdery condition. One-half hour after mix-
ing, the temperature in Xos. 1, 2 and 3 was approxi-
mately 110° C, while in No. 4 it rose to 1900 C. The
results of this series of experiments are given in
Table II.
continued reversion over the whole period as was
expected, but what was responsible for the irregularity
in the sample with 30 per cent has not been explained.
It will be noticed that some reversion to tri-calcium
phosphate has taken place, but the greater part re-
mains as di-calcium phosphate.
Since these laboratory experiments indicated in a
general way the trend and rate of reaction it was con-
sidered advisable to continue experimenting on a
larger scale under factory conditions. Consequently,
the following series of experiments were conducted
with lots of one ton or more.
In Experiment 1, lime and acid phosphate
were mixed in a ball mill in proportions of 10 parts
lime to 90 parts acid phosphate. The material after
grinding through a coarse screen was caught in bags
and set out on the floor in order that the reaction could
go on to completion and the temperature drop to that
of the atmosphere. Experiments 2, 3 and 4 were
conducted in the same manner as Xo. 1, the only
difference being that the proportion of lime to acid
phosphate was increased in each succeeding experi-
ment.
The method of handling was not satisfactory, as the
id dust soon drove the nun away from the mill.
Unfertilized at Left: 90 Lbs. per Acre Reverted Phosphatb
at Right
The reaction goes on more rapidly as the percentage
of lime is increased. The water content of the acid
phosphate and also the length of time it ages in the
bin before mixing affect the rapidity of reaction and
intensity of heat generated.
Having studied the reverting action of lime, our
attention was next turned to carbonate of lime and
combinations of carbonate of lime with lime and acid
phosphate, the object being to obtain a fertilizer which
would contain a considerable part of the phosphoric
acid in the reverted form and also to effect a less
dusty mechanical condition. The dusty nature of the
reverted mixture makes a very difficult and dis-
agreeable product to handle on a large scale.
The results of experiments with calcium carbonate
(coral sand) and acid phosphate are given in Table
III. It will be noticed that reversion takes place
quite rapidly at first but as the time increases, the
rate of reversion diminishes. As with lime, the
Table III — Percentages Water-Soluoi.k PjOi in Mixtures op Acid
Phosphate and Cok\:
Phosphate: 80%
Mixture | Cobm Svm.
On mixing ■ 14.48
After :i hours 15.4 10.98
4S hours 9.58
120 hours 14.44 ' 11.18 8.86
11 dav> V 68 8.2
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
35
reversion increases with increasing proportions of car-
bonate of lime. With the carbonate of lime, however,
there is very little rise in temperature. It is unfortu-
nate that only the water-soluble phosphoric acid
determinations were made on this series of experi-
ments, as a comparison of the soluble and available
would have been valuable and interesting.
In an endeavor to get more satisfactory results with
lime and acid phosphate on a factory scale, mixtures
of 90 per cent acid phosphate and 10 per cent lime,
and also 85 per cent acid phosphate with 15 per cent
lime were again ground together in a ball mill. These
mixtures were allowed to cool and after 24 hrs. samples
were taken for analyses. The mixtures were sampled
again after one week.
I Table IV — Mixtures of Acid Phosphate and Limb
90% Acid 85% Acid
Phosphate & 10% Lime Phosphate & 15% Limb
Soluble Soluble
_ _ ( Water- and Water- and
Per cent PiOs (soluble Available Total Soluble Available Total
After standing
24 hours... 3.03 18.50 19.42 None 17.56 19.1
1 week 1.66 17.97 19.28 None 16.55 18.64
The reversion here was quite complete and little if
any of the acid phosphate was changed to the tri-
calcium form. The appearance of the material was
quite similar to precipitated phosphate. It was
found impractical to work this material through a
ball mill, however, on account of the gradual accumu-
lation of the mixture in the mill and also the heat
generated by the reaction.
A similar experiment was then undertaken with
mixtures of acid phosphate, lime and coral sand with
the object of obtaining the same result: i. e., a re-
verted phosphate, but with the idea of retarding and
tempering the violence of the reaction. The limited
capacity of the ball mill and its tendency to choke
and to accumulate heat led us to run the remaining
tests through a cage disintegrator. The reversion
which took place in this material is shown in Table V.
Table V — Experiment with Acid Phosphate. Lime and Calcium
Mixture:
Carbonate
85% Acid Phosphate
10% CaCCb + 5% CaO
Water- Soluble and
Per cent PaOj: Soluble Available Total
After standing
24 hours 4.94
10 days 4.52 15.64 17.36
80% Acid Phosphate
15% CaCOa + 5% CaO
Water- Soluble and
Soluble Available Total
14.77 16.48
The disintegrator makes a sufficiently homogeneous
mixture which passes rapidly through the machine,
and which is discharged almost before reaction begins.
Reaction attains its height about 30 minutes after
leaving the disintegrator, which allows sufficient
time for handling. The heat generated removes ex-
cess of moisture, causing a loss in weight of about
S per cent and leaving a free, dry powder, the phos-
phoric acid of which consists mainly of di-calcium
phosphate.
Thus with a 40-in. cage disintegrator, from 20 to
■ 1 per hour may be mixed direct into containers,
doing away with the handling of a very dusty material,
and avoiding excessively high temperatures.
AGRICULTURAL EXPERIMENTS
With regard to the effect of reverted phosphate on
growing crops, and also its commercial value, there
are differences of opinion. In 1914 the state chemists
of North Carolina, South Carolina, Alabama, Missis-
sippi and Georgia were all opposed to a reverted
phosphate. Dr. Cameron, then of the Bureau of
Soils at Washington, is also quoted as not favoring
lime being mixed with superphosphates.
Possibly in the majority of cases the water-soluble
phosphate is the one used. There are exceptions,
however, and we have found in numerous cases that
the reverted phosphate is just as valuable or even
more valuable than the water-soluble when applied
to cane upon upland soils. These soils are, as a rule,
highly ferruginous clays. On soils which have not
been cropped for several years, the reverted phosphate
gives excellent results. The accompanying photo-
graphs show the difference between cane unfertilized
and that receiving per acre 90 lbs. of phosphoric
acid in reverted form. In the check plot the canes
per stool ranged from 5 to 9 while in the reverted
phosphate plot the variation was from 9 to 15. These
photographs were taken in a series of experiments
run by the Hawaiian Sugar Planters' Experiment
Station, on land of the Oahu Sugar Co. Experiments
made by the U. S. Agricultural Experiment Station1
upon rice, also show favorable results from reverted
phosphate, particularly the Gold Seed rice which has a
long growing period. A gain of 132 per cent over the
check plot is recorded.
In view of these results and the fact that the re-
verted form is preferred by certain growers to any
other, it would seem that the practice of condemning
or setting arbitrarily a lower value on reverted phos-
phate is open to criticism.
Credit is due and acknowledgment hereby made to-
ri. M. McCance for aid in the analytical work re-
ported in this paper.
Pacific Guano & Fertilizer Company
Honolulu. Hawaii
ELECTRIC FURNACE SMELTING OF PHOSPHATE ROCK
AND USE OF THE COTTRELL PRECIPITATOR
IN COLLECTING THE VOLATILIZED
PHOSPHORIC ACID
By J. N. Carothers
Received October 8. 1917
The work described in this article is a continuation,
on a commercial scale, of preliminary work which was
carried on more than a year ago. In the preliminary
work,2 furnace operation was not continuous for a period
of days, consequently no conclusion could be drawn as
to cost of installation and operation.
The work of these later tests was made possible only
by the cooperation of the Bureau of Soils with several
' Hawaii Experiment Station Report 1907-1908.
» This Journal. 9 (1917), 26.
36
//// JOl RNAL OF INDUSTRIAL AND ENGINEERING CHEM1 rol. 10. No. i
firms which were interested in this line of investigation.1
The apparatus was installed near the plant of the R. B.
Davis Co., Hoboken, N. J. Fig. I is a view of the
precipitator and furnace housing. Power was secured
from the Public Service Co.
From the transformer ratings, the plant was a 200 K.
W. installation. The incoming power was quarter
phase, 2400 volts, which was transformed to 3 phase,
220 volts by a bank of Scott connected transformers.
A second bank of transformers, and a set of double-
throw switches made it possible to have either 220
volts or 1 10 volts in the furnace. This arrangement was
adopted so as to use the higher voltage for starting and
the lower voltage for operating. For the best operating
conditions no volts were found satisfactory.
The furnace consisted of a water-cooled crucible,
with the cooled section extending no higher than the
region of the molten slag. It_was lined with fire-clay
Fio. I — Prkci
Furnace Housi;
brick, but silica brick would prove more satisfactory.
The portion not exposed to the action of slag was lined
with a fire-clay l>rick. All gas mains and the cooling
tower had a fire-clay brick lini heat from the
gases served to harden the exposed surface, and thus
improve the service of the brick. The electrodes entered
through the top of the furnace, but below a line where
it Davis Co. of Hoboken. X J., first proposed the cooperative
plan, unci were instrumental in interesting some of the dealers of phosphate
rock, and electrical machinery. The Lakeland Phosphate Co. supplied
a high grade Florida pebble, the Cummer Lumber c't> a high-grade Florida
land rock, the Phosphate Mining Co. a screening and two suesof pebbles,
the Partners Ground Pho p ' lump of Tennessee rock,
the Central Phospl rown Tennessee rock in large lump, and the
m Co. a blue Tennessee rock in lump and line material
mixed.
pplicd all transformers and instruments
■ '■ with tlie Furnace. The Research Corporation furnished
used in connection with the treater for collecting
the g.e.. 1 ome veo helpful i<> treater design,
construction ami operati
the charge entered. Care should be taken in the
design of such furnaces that the angle of the electrodes
conform with the angle of repose of the charge. Thus
as the charge falls in a natural pile, the breakage of
electrodes is eliminated. Electrodes may be conve-
niently controlled by hand, or mechanically. Hand con-
trol was used in this experiment, with the control so
located that the switchboard and instruments could be
observed. Six-inch and four-inch graphite electrodes
were used. The life of a 4-in. electrode was about 7
days, while the 6-in. electrodes lasted on an average of 10
days under favorable conditions Thus it may be seen
that with such a low consumption, electrodes may be
operated by hand, since the chief movement of elec-
trodes is when they are consumed. In this experiment
the charge was fed by hand; however, this is obviously
impractical in a large installation where mechanical
apparatus should be used. During regular operation
about 2000 lbs. of rock were consumed per 12-hour
period.
A slag pit filled with water was used to quench the
molten slag as it flowed from the furnace. The slag
thus chilled slid to one end and was removed mechani-
cally. The P2OS content of the slag was approximately
2 per cent, although it is possible to reduce it to 1.5 per
cent or even 1 per cent for regular operation. The
P2O5 content of the slag is largely a matter of the mixing
of the charge, and using the proper proportions of rock,
sand, and coke.
The average production was 0.3 lb. H3PO4 per K.
W. hr. absorbed; however, there were periodic yields,
during times of good operating conditions, in which
0.4 lb. H3PO4 per K. W. hr. was produced. Judging
from the average results of this experiment it seems
reasonable to assume that a production of 0.6 lb.
H3PO4 per K. W. is possible. Of course, the production
is entirely dependent upon the efficiency of the furnace.
In the case of this work, no means were adopted to
utilize the heat absorbed by the water surrounding the
crucible, or in the gases carried over from the charge.
Also there were heat losses from the oxidation of phos-
phorus to phosphorus pentoxide (PjOs) and carbon
monoxide (CO) to carbon dioxide (C0S) which, if
utilized, would materially have increased the efficiency
of the process.
As the gases were removed from the furnace, they
passed through a cooling tower before entering the
treater. This tower was installed to afford sufficient
radiation, so that the gases entered the treater at 250
to 3000 C. Above these temperatures in the treater,
electrical and mechanical difficulties arise, which make
higher temperatures undesirable.
The treater consisted of a header of common brick,
with a reinforced concrete top to support the pipes,
and 20 treater tubes of vitrified sewer pipes, 1; in. in
diameter and 15 ft. in length. All joints were packed
loosely with silica to prevent air from enuring at these
points. The pipes were enclosed to prevenl cricking,
due to heat differences, and to maintain :ii even flow
of gas.
All pipes at the top were inclosed in a :nmon hood.
Supports for the conductors rested on insulators within
Jan., 1918 TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
37
High tension line
Transverse Section
the treater hood. Complete clearance was given to
2,000 cu. ft. of gas entering at 3000 C, with a velocity
of 3 linear feet per second (see Fig. II for diagrammatic
sketch of a transverse and a longitudinal section of the
treater).
Power was supplied the treater from a 150-volt
motor generator set, and transformed to higher voltages
by a 7.5 K. V. A. transformer. A 5-point switch on the
low-tension side of the transformer, connecting the
various turns of the coils, made a variation of voltages
possible. It was found that 70 kilo volts was sufficient
to give complete precipitation of the gases, at the
above stated volumes and velocity.
As the acid fell from the pipes it was caught in a re-
ceiving basin of vitrified brick set in acid-proof cement.
From this basin the acid flowed out and was disposed of
by pumping to a receiving vat. The concentration of
the acid collected was controlled by the temperature
of the gas in the treater. At a temperature of less than
iooc C. the concentration is not likely to exceed 50
per cent H3PO4, while a temperature of 250 to 300 ° C.
will yield an acid of 85 to 93 per cent H3P04. In one
case an acid of 97 per cent was produced. An acid
above 85 per cent H3PO4 will probably solidify when it
reaches atmospheric temperatures, and therefore the
pumping apparatus and pipe lines should be so con-
structed as to prevent clogging.
Any unscreened rock is undesirable for such a process
if a concentrated acid is to be collected; however, if a
dilute acid be collected no difficulties are encoui
The fine dust is carried over with the phosphorous
gases, and precipitated in the lower section of the
'.'.".-.y:'.^-f::;.A
Longitudinal Section Fiq-K
treater pipes. There it reacts with the concentrated
acid, and forms mono-calcium phosphate which is a
stiff paste under such conditions as exist in the treater.
This mass gradually accumulates until the distance to
the conductors is so close that disruptive discharges
set up.
It should be borne in mind that when a rock free from
dust is used, the only impurities likely to be in the re-
sultant acid are: carbon in the form of coke dust;
silica dust from the sand and rock; and any volatilized
fluorine or arsenic, which is absorbed in the acid as the
gases pass through the treater. Therefore, if an acid of
high purity is desired these impurities must be removed;
however, this is largely a matter of filtering apparatus,
and a question for individual installations.
Below is given an estimate as to the cost of operation
for such a plant. A 3,000 K. W. unit is nominally
chosen to show the production and cost of operation.
Total Annual Production 6.480.000 lbs. H1PO4
Material Needed for a 300-Day Year:
7.800 tons 34 per cent PiOs Phosphate Rock, assuming
90 per cent recovery
3.510 tons sand
1.758 tons coke (86 per cent carbon)
Items Cost
7.800 tons phosphate rock @ J 1.25 per ton $ 35.100.00
3.510 tens sand @ SI. 25 per cu. yd 3.327.00
1.758 tons coke @ $4.50 per ton 7,911 .00
25 tons electrodes @ $10 per 100 5.000.00
8 Laborers g %1 00 pel day 5.280.00
2 Electricians @ ?100 per mo >, 100 00
<■ S»o per ni.i 960.00
1 Superintendent @ $150 per mo 1.800.00
Power @ $25 per II P, V, (equivalent to 0.285 ct.
ii B '''"i II. P. Ilr 100 00 I 00
Power for machinery, lights, etc.. 100 K W 3.283.00
3«
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. i
Based on 0.3 lb. H3PO4 per K. W. hr. a 3,000 K. W.
furnace would produce 21,600 lbs. H3PO4 per 24-hour
day. Such a plant should average at least 300 operating
days per year.
On this basis the cost of acid per lb. H3PO4 is 2.55
cents or 3.37 cents per lb. PjOs for power labor, and
material, but exclusive of investment charges, main-
tenance, and depreciation.
The cost of installation is more difficult to determine
because of the present un-teady market conditions and
the character of construction employed; consequently
no attempt is made to make an estimate covering the
cost of installation. However, it may be said that most
equipment needed for a plant of this type is stock
material. The furnace must be built from design, and
is special. Stock transformers may be used, also
switches and instruments. Likewise, all elevator
equipment could be purchased from stock material.
The treater may be so constructed that little special
equipment is necessary. The treater base or header
may be constructed of common brick, with a lining of
vitrified brick or tile, while the top supporting the pipes
may be built of reinforced concrete. Vitrified sewer
pipes serve very well for treater tubes, although stone-
ware is better. If an exhaust fan be placed in the gas
main before the treater, no special hood is needed for
the top of the treater pipes; however, if it be desired
to have the exhaust after the treater, an air-tight hood
is necessary, which should be lined with vitrified sheet
asbestos or tile. Some of the brick for the furnace
might necessarily be of special shape, if standard shapes
were not available and it were not desirable to cut stand-
ard shapes to the desired form. The foregoing briefly
outlines the character of the equipment necessary for
an installation for the production of phosphoric acid
by means of the electric furnace, where electric precip-
itation is used to collect the volatilized gases.
Since most of the equipment is available from standard
stock sources, the cost of an installation of this character
is materially lower than it would be, were special equip-
ment required. Also the simplicity of collecting phos-
phorus pentoxide, or phosphoric acid, by electrostatic
precipitation is an improvement over the use of water-
absorption towers, not only in tower cost of installation
but in operation as well. Furthermore an acid of higher
concentration may be collected. By having a gravity
flow from the collecting basin to the receiving vat
all pumping equipment and many of the storage tanks,
which are necessary in the case of absorption towers,
are eliminated. Therefore, with a lower cost of installa-
tion and operation of the treater, as compared with the
absorption towers, the application of the Cottrell
precipitator in collecting phosphorus pentoxide, un-
questionably advances the possibilities in the applica-
tion of electric smelting along this line.
It should be pointed out that the yield of this ex-
periment was considerably below that of a furnace de-
signed to utilize the energy from the heat in the gases.
This very important feature is a large factor in the
development of the process of smelting phosphate
rock by means of an electric furnace.
Bureau op Soils
Washington. D. C.
LABORATORY AND PLANT
A CONSTANT TEMPERATURE AND HUMIDITY ROOM
FOR THE TESTING OF PAPER, TEXTILES, ETC.
By F. P. Veitch and E. O. Reed
Received July 23. 1917
Variations in the relative humidity of the atmos-
phere have a decided effect on the physical properties
of paper. The results of all physical tests on paper are
affected to a greater or less degree by the ordinary
variations of the relative humidity in the testing room
and certain tests are valueless unless conducted under
uniform temperature and humidity conditions. Es-
pecially is this true with the determination of the folding
endurance, a most important test for indicating the
flexibility and probable durability of paper. Though
it is generally understood that the physical qualities
of paper are affected by changes in humidity condi-
tions, there is but little appreciation of the rapidity
with which these changes affect it. so ex-
ceedingly sensitive to changes in atmospheric humidity
that, in order to obtain concordant results which may
be duplicated at other times and by other labor
it is necessary to make all physical tests upon it in
a room where both uniform temperature and relative
humidity are maintained.
All physical testing of paper done by the Bureau of
Chemistry, U. S. Department of Agriculture, has been
conducted since December, 1909, in a specially con-
structed and automatically controlled constant tem-
perature and humidity room. So far as is known, this
laboratory was the first in this country to maintain
uniform temperature and humidity conditions in the
testing of paper, textiles, leather, etc.
MEASUREMENT OP HUMIDITY
Humidity is expressed either as relative or absolute.
Absolute humidity is the weight in grains of the water
vapor in a cubic foot of air, while relative humidity
is the percentage of saturation of the air at any par-
ticular temperature and pressure. Saturation at the
designated temperature and pressure is taken as 100
per cent. The higher the temperature of the air the
more moisture required to give the same percentage
of saturation or relative humidity.
The measurement of humidity1 is preferably made
with a I". S. Weather Bureau sling psychrometer.
Thermometer d to o.i° F. should be used,
since every degree differ, ■ • the wet and dry
bulb temperatures gives from ; to 6 per cent variation
in relative humidity, at the ordinary temperatures
of from 50 to So0 F. A ratures this
variation increases, as for instance a1 3;° F. one de-
difference of 10 ih e humidity.
The sling psychroi miling and
1 "Pinal Report of the Committee on Standard Methods for the Ex-
amination of Air." .In. J. Pitb. Health. N'o. 1. 7, p. 54.
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
30
On the Floor in the Rear Will Be Seen Oi
The Method of Exposing Samples
Fig. I — View of Interior of Room Taken from the Doorway
e of the Fans for Keeping the Air Uniform within the Room and along the Left Side and Back of the Room
near the Ceiling Is the Outlet Flue,
to Be Tested by Suspending with Clamps from Wires Stretched across the Room Is Also Shown
tables necessary for calculating relative humidity and
dew point from the readings of the wet and dry bulb
temperatures are described by the U. S. Weather
Bureau.1 There are many instruments for recording
the temperature and humidity on charts, but these
instruments must be frequently checked with a stand-
ard sling psychrometer or other accurate form of wet
and dry bulb instrument.
INDOOR AND OUTDOOR HUMIDITY
During the six to nine months of the year when
artificial heat is required in most localities, the average
relative humidity indoors is as low as 20 to 40 per cent,
unless mechanical means for humidifying have been
installed, while the average outdoor relative humidity
in most localities in the U. S. is over 65 per cent.
These facts are not generally appreciated, and erroneous
statements on this subject are often made. Wilson2
states that during the winter months the normal out-
door relative humidity over the more populous por-
tions of the United States, especially east of the Mis-
souri and north of the Ohio Rivers, is 72 per cent and
that the average diurnal range is from 60 to 85 per cent.
In Table I arc given the indoor temperatures and
relative humidities for Dayton, Ohio, and Washington,
D. C, recorded by this laboratory, and the outdoor
1 Psychrometric Tables. U. S. Weather Bureau Bull. 23S.
3 "Atmospheric Moisture and Artificial Heating," Proceedings of the
Convention of Weather Bureau Officers, 1898.
readings for the same localities taken from the Annual
Reports of the Weather Bureau.
Table I — Average
Monthly Outdoor and Indoor Temperatures
and Relative Humidities
Outdoor
Indoor1
Outdoor
Indoor4
Dayton
Temp. Re
. Temp. Rel.
Washington Temp. Rel.
Temp. Rel.
Ohio
° F. Hun
1. ° F. Hum.
D. C.
° F. Hum.
0 F. Hum.
1911. Nov.
38.0 83% 74.5 29%
1912. Aug.
73.4 72%
83.5 49%
Dec.
37.8 80
74.5 28
Sept.
70.4 82
76.5 65
1912. Jan.
18.4 78
75.0 19
Oct.
59.3 75
75.0 46
Feb.
23.2 75
75.0 21
Nov.
46.9 67
74.5 39
Mar.
34.4 79
74.5 26
Dec.
40.4 69
74.0 35
Apr.
53.6 75
75.0 35
1913. Jan.
43.6 72
73.0 35
May
64.4 75
75.5 43
Feb
36.6 63
74.5 31
June
68.4 69
76.0 44
Mar.
49.0 66
74.0 31
July
74.9 76
79.5 58
Apr.
55.5 60
76.5 33
Aug.
71.0 80
78.0 60
May
64.4 65
77.5 41
Sept.
68.2 76
77.0 56
June
72.8 66
80.0 49
Oct.
56.6 71
72.5 41
July
77.6 66
87.0 44
Average
50.7 76
75.5 38
Average
57.5 68.5
77.1 41.5
i Read
ngs taken
by the Burea
i of Chemistry
in the Mercantile Cor-
poration Factory.
2 Readings taken in laboratory room Bureau of Chemistry. As open
steam baths are located in all rooms used for laboratory purposes the indoor
humidity is slightly higher than was found in other buildings.
The results given in Table I are representative of
the average indoor conditions at Dayton, Ohio, as
determined by observations made during several
years. It has been observed in Washington, in several
of the different government bureaus and in offices
using large amounts of paper, that the average yearly
indoor relative humidity during working hours is be-
tween 35 and 40 per cent. The average yearly indoor
relative humidity is close to 40 per cent both in Dayton,
Ohio, and Washington, D. C, but in no case does it
approach the average outdoor relative humidity,
4°
THE JOURNAL OF INDUSTRIAL AND ENGINEERING ( II i Vol. 10, Xo. i
averaging from 30 to 40 per cent less. These results
are in close agreement with those quoted by Wilson,1
to the effect that the indoor relative humidity in heated
buildings in several widely separated parts of the
country on the coast and in the interior varies from 24
to 33 per cent and that during the winter months
the indoor relative humidity is about 42 per cent
lower than the outdoor.
The average winter indoor humidity in the United
States is lower than that of the driest climate known.1
This fact has led to investigations as to the physio-
logical effects of temperature and humidity for the
purpose of setting standards for the best living and
working conditions. Such work has been conducted
by the New York State Commission on Ventilation for
several years.2
Fig. II — Vikw OP Tin: Am [m Tumiersd Air
and Moisturb to Tin-; Room
Back or the Baffle Plate Will Bi Seer thi Motor of the Sirocco Fan.
which Serve; to Circulate Air through the System; in Front of It the
Other Fan which Is Used to Distribute the Air throughout the Room
STANDARD TESTING CONDITIONS
The German Imperial Testin tory at Gros-
rfelde found the variations in atmospheric
ity to produce such a di ct on the re-
sults of i ' 1 sts of paper, that it v.
to make all tests under cot. ive humidity
II !.' Al» Mil 1 :- 1 :
65 per ceil re humidity for all physical testing
1 "Atmo ture and Artificial Heating;11 Proceedings of the
Convention of Weather Bureau Officers, 1898.
IC Results of thi Work of the New York State
in," /lm. J. Pub. Health. No. 2. 8, p. 85.
■ UiUluiluntm "• d. K Tecknischn I rrsuihuntsattslaUen. 7 (1889), 2
8 (1890), 8 to I';.
of paper. It is not made clear why 65 per cent rela-
tive humidity was selected, but it appears to have
been taken because of the fa< the average
outdoor relative humidity is more than 65 per cent
and the indoor humidity somewhat lower, it was easier
to add moisture to the air than to remove it.
This condition has been gei pted in this
country, apparently without investig; on. Since the
average yearly indoor humidity in this country is,
according to the data available, but 35 to 40 per cent,
it does not seem rational to test paper at a relative
humidity rarely obtained indoors. The testing should
be done under humidity conditions more nearly like
those under which the p. per is used It is doubtful,
however, if it would be advisable to set the relative
humidity for such work as low as 40 per cent or even
45 per cent, since for about five months of the year
it will be necessary to dehumidify to secure these
percentages. A relative humidity of 50 per cent is
probably as low as can be maintained throughout the
year without elaborate equipment. Even at this
percentage it will be necessary to dehumidify the greater
part of the time during the months of July, August
and September.
Not only has humidity a marked effect on the re-
sults of physical tests, but also on the handling and use
of paper. The printer, engraver, stationer, librarian
and others using large quantities should standardize
their working and storing conditions to secure the
best and most satisfactory results at all times of the year.
The most suitable humidity conditions for their re-
spective purposes should be determined by investi-
gation and means should then be taken to maintain
these conditions throughout the year. The paper
maker and consumer would undoubtedly profit by the
maintenance of uniform humidity conditions most
satisfactory for their purposes. Suggestions from the
Bureau of Chemistry have led to the elimination of a
number of difficulties in printing and engraving es-
tablishments of the government caused by variations
in atmospheric humidity.
In most texts on paper testing it is suggested that
certain definite humidity conditions may be had by
placing the samples in small containers, in which the
definite temperature and humidity required are main-
tained for 12 to 24 hours, then removing from the con-
tainers and testing under the atmospheric conditions
prevailing in the room. A lis cannot be
1 in this v.. e folding en-
durance tester. As will be see' :•. m able II, results
made with this machine ar s made under
uniform humidity conditions. it been found
possible to apply accurately r correction
where the tests have been 0 a different
humidity than 05 per cei is of paper
or even runs of the same kii necessarily
permit the application of tl tion factors
— a fact that is clearly shown he results
in Table II, Columns .- and s 6 and 7,
respectively.
The results in Table II show ical quali-
ties of the paper change very hanges in
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Table II — Results Showing Rapidity with Which the Folding En-
durance is Affected by Humidity
Samples of Uncoated Blue-Print Paper. Results Given are Averages of
10 Tests Each
Exposed Exposed
( 12 hrs.. 71° F. 71° F. and 12 hrs.. 65° F. 6S° F. and
Exposure^ and 30% 30% and 65% 65%
/ rel. hum. rel. hum. rel. hum. rel. hum.
Ilmmedi- Immedi-
ately at ately at
71 ° F. 65° F. 65° F. 74° F.
and 30% and 65% and 65% and 25%
rel. hum. rel. hum. rel. hum. rel. hum.
Paper Double Folds Double Folds Double Folds Double Folds
No. Long. Trans. Long. Trans. Long. Trans. Long. Trans.
28541 316 411 852 804 1431 1298 468 347
28538 104 186 229 269 843 416 329 214
loeirt i/>c 1f»£ 111 AACi K<;l AA 1 \T»» tnn*nJ
28519
305 296 373 440 1561 641 Not tested
the relative humidity of the air. They show that
papers should not be exposed to a certain humidity
condition and tested under other conditions even
though the tests are made at once. They indicate
further that paper loses moisture faster in passing to
a lower relative humidity than it gains moisture
in passing to a higher relative humidity. The length
of time for which it is necessary to expose a paper to
a certain humidity condition before it reaches equi-
librium can be definitely determined by means of the
Fig. Ill — Diagram Showing Operation of Room as Described in Text
folding endurance tester as well as by weighing the
paper. Articles dealing with the effects of humidity
on paper are in preparation and will be published in
the near future.
DESCRIPTION OF THE BUREAU OF CHEMISTRY CONSTANT
TEMPERATURE AND HUMIDITY ROOM
For general testing work this room has been operated
up to the present at 700 F. and 65 per cent relative
humidity. The temperature was at first set at 65° F.
with 65 per cent relative humidity. At 65 ° F., the
men were decidedly uncomfortable and developed
frequent colds. It was, therefore, deemed advisable
to adopt 70° F. as the standard temperature with
the relative humidity at 65 per cent. The room can
be operated automatically at any relative humidity
from 20 to 85 per cent and any temperature from 40
to 95° F. Investigational work has been carried on
at different humidities and temperatures to show the
effects on paper and on tests made with various testing
machines.
The room is 10 ft. 6 in. X 14 ft. 3 in. X 9 ft. 3 in.
high and contains 1410 cu. ft. It was constructed in
connection with the refrigeration plant of the Bureau.
The walls and ceiling of the room are 8 in. thick and
consist of an outside sheathing, 4 in. of ground cork,
a thin partition and two layers of sheet cork, each
1V2 in. in thickness, the inner layer finished on the
inside with cement, which is painted to prevent ab-
sorption of moisture. The floor is insulated in the
same manner, cemented and covered with linoleum.
The door is of the regular cold storage type. The
insulation of the room is such that when the automatic
controls are turned off the temperature will remain
constant for several hours.
Air is drawn into the room by means of a sirocco
fan (Fig. Ill, C) , from the intake flue A , through which
the tempered air and moisture are supplied. It is
delivered into one corner of the room near the ceiling,
against a slotted baffle plate, D. Two fans, E and F,
are located within the room to keep the air uniform
throughout; E is placed in front of the baffle plate
where the air enters, and F on the floor in the diagonally
opposite corner. These fans are essential in order
to prevent the air from stratifying. The outlet flue
B is located near the ceiling along the two sides of the
room opposite the intake, and has three openings, each
with an adjustable hand damper, through which air
is removed from various parts of the room. This
flue is connected with a fresh air flue, G, outside of the
room, which supplies air to the tempering coil chambers
H and I. The sirocco fan located in the intake flue
maintains the air circulation, drawing air into the room
and forcing it out through the outlet flue. Careful
experiment shows that the two fans as placed within
the room insure even humidity throughout the room.
The tempering coils, steam and refrigerated brine
are located in well insulated chambers on the outside
of the room and are connected both with the inlet and
outlet flues. All air supplied to the room is drawn over
one or the other of these coils as the demands of the
room may require. The steam coil H contains ap-
proximately 28 sq. ft. of heating surface, and the brine
coil I approximately 113 sq. ft. of cooling surface.
They have been found ample at all seasons of the year
for maintaining any temperature within the range of
the controlling thermostat, 40 to 95° F. In order
to obtain maximum efficiency it is necessary to keep
the brine coil free from ice, and this is accomplished by
opening the chamber once every two or three weeks
and allowing the ice to melt off.
The automatic operation of the plant is obtained
by means of air pressure and automatic air pumps
maintain a pressure of approximately 12 lbs. The
operating valves and dampers are worked by dia-
phragms. Automatic diaphragm-operated valves are
located on the pipe lines leading to each of these coils;
the brine valve 71 opens when air pressure is supplied
to the diaphragm operating it and the steam valve
H ' when the air pressure is released from the operating
diaphragm. Each coil chamber is fitted with an auto-
matic diaphragm-operated damper, I1 and H2, leading
into the main flue to the room. These dampers work
by means of their respective diaphragms at the same
THE JOl RNAL OF INDUSTRIAL A XI) ENGINEERING I HEM1 i Vol. 10. Xo.
time as the corresponding brine and steam valves
on the coils. The autom these valves
and dampers is controlled by a thermostat within the
room to be described later. The two valve diaphragms
and the two damper diaphragms are all on the same
air-pipe line, the air pressure of the line being con-
trolled by the thermostat within the room, which
makes and breaks the circuit of air.
Moisture for humidifying is supplied by means of
a steam jet, K, located immediately outside of the room
in the intake flue. This steam jet consists of a brass
pipe about 8 in. in length, perforated and wrapped
with cotton wicking, which removes any water which
may be in the steam. This produces a finely divided
steam vapor, which has been found the most satis-
factory method of humidifying. Two automatic
diaphragm-operated valves, Kl and K2, are located
on the steam line leading to this humidifier; A"1 is
operated by the hygrostat within the room and opens
Fig. IV — Vmw OF Tkmi-braturb and Humidity Controlling Instru-
ui rs Located within the Room
tnostat on the Ki^ta. Hygrostat on tin- Left
when the hygrostat releases the air pressure on the
diaphragm; A."2 is a safety valve which closes with the
release of the air pressure to its diaphragm and is
Lth the main air-supply line of the system.
Since the valve controlled by the hygrostat opens with
the release of air pressure, in break in the
main air supplj line of the plant tins valve would not
close and an excessive amount of Steam would be
supplied to the room. The safety valve is to prevent
lent of this kind. The supply of steam to the
humidifying jet is controlled by a needle valve, A.'".
It is important that the Supply to the jet be regulated
according to the
furnish amount nor an insufficient amount
Of moisture for the room. A steam trap for removing
the water in the steam is plaeed in the line in front of
bhl I alves.
The room is automatically opera. - separate
controls, one for maintaining temperature and the
other humidity. Roth controls are located withjn the
room itself.
The temperature control was installed at the time
the room was constucted and entire satis-
faction. The temperature in the room varies less
than i° F. This thermostat operates the valves on
the brine and steam coils and the dampers leading
from these coil chambers into the room, previously
described. When the room requires warm air, the
thermostat releases the air pressure and the valve on
the steam line and the damper to the steam coil cham-
ber are opened, while at the same time the valve on
the brine line and the damper to the brine coil chamber
are closed. When cool air is required the above opera-
tions are reversed, the thermostat permitting the air
pressure to be on the operating diaphragms. The
above describes the principle of operation of the equip-
ment. As a matter of fact the action of the thermo-
stat is gradual, allowing the room to be supplied
with both warm and cool air at the same time.
Several makes of equipment for automatically con-
Fio. \ Yn v. Ol rsiDB ok thb Room Showing Brine (a), and Steam
Coils and Chambers (*), thb Intaki «d tub Humidity
ENS ((/).
trolling the humidity of the room have been tried.
The hygrostat now used controls the relative humidity
within less than _> per cent variation. The room has
perated fairly well by means of other controls,
but none, so far used, has pr iable as the
instrument now in use in giving uniform and accurate
automatic control at all seasons of the year. The
instrument is a Type F hygrostat, in which the ac-
tuating material is silk fiber. This instrument operates
the diaphragm-operated valve Kl on steam line
humidifying jet. When the need of more moisture is
indicated by contraction air pres-
sure to the diaphragm is relea the valve
and admitting steam to the jet humidity
is reached, whereupon the valve is closed with the ex-
pansion of the silk fiber.
Previous to the installation of the present humidity
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
43
controller the room was operated by passing all air
from the tempering coils over a vaporizing pan, in which
a constant temperature was automatically maintained.
This system usually gave fairly satisfactory results,
but when sudden changes in the outdoor temperature
or humidity occurred these were not automatically
taken care of within the room. The vaporizing pan
was 12 X iS in. and built immediately outside the
room in the intake flue. The pan contained 2 in. of
water in which was located a thermostat connected
with an automatic diaphragm-operated valve, placed
in the steam line, to an open coil in the pan for heating
the water. By this method moisture was uniformly
and continually added to all air passing into the room.
It was impracticable to take much fresh air into the
room under these conditions and consequently the same
air was continually recirculated, which facilitated
maintaining very constant conditions but did not per-
mit proper ventilation. The thermostat regulating
the temperature of the vaporizing pan required fre-
quent attention to allow for the changing outdoor con-
ditions of temperature and humidity. In summer the
temperature of the water in the vaporizing pan was
held at 120 to 1600 F. and in winter 160 to 185° F.
especially where exact testing conditions are desired.
It is much easier to maintain uniform humidity con-
ditions, when the temperature remains constant.
II — The source of the humidity supply should not
be located within the humidity room. Experience
shows that steam vapor is more satisfactory than water
spray for increasing the humidity. If water spray
vapor is used, mechanical moisture is likely to be de-
posited on the walls of the room, on the apparatus
and on the materials to be tested. A steam jet or
vaporizing pan has been found to be satisfactory for
supplying the steam. If a water spray is used it must
be installed outside of the room and the humidified air
passed through a series of baffle plates to remove all
excess of mechanical moisture before entering the
room.
Ill — Uniform conditions within a room can be
maintained only by the use of a number of properly
located small fans. Without these the air will be
stratified.
IV — Humidity may be controlled within limits in
almost any room or building. It is unnecessary,
even for testing laboratories, to construct such an
elaborately insulated room as has been described,
SATURQAY
Record of Temperature and Humidity for One Wee
Top Line — Temperature.
in order to maintain 65 per cent relative humidity
within the room. With the present system it is possi-
ble to take all air directly from outdoors or to add any
amount of fresh air to that exhausted from and to be
returned to the room without seasonal resetting of the
controlling instrument.
As has been previously stated the room has been
uniformly maintained at the desired temperature
and humidity with only regular inspection to insure
the proper mechanical condition of the operating equip-
ment. It is not unusual for both temperature and
relative humidity to be maintained constant for several
weeks at a time as shown by the accompanying copies
of the autographic records, which by the way are
confirmed several times each day by wet and dry
bulb readings.
CONCLUSION AND SUGGESTIONS
Seven and a half years' experience with and in de
veloping a constant temperature and humidity room
has led to the following conclusions and suggestions:
I — Owing to the intimate relation between tem-
perature and humidity, both should be controlled,
K BY ThERMO-HyGROGRAPH RECORDING INSTRUMENT
Bottom Line — Humidity
although a well insulated room is a great advantage.
However, the best results will be obtained when the
room has no outdoor exposure or windows. It is
believed that a room constructed within another,
leaving an air space of at least 12 inches between the
walls, can be maintained at constant temperature and
humidity by the control system described herein.
The walls of the room may be of 7/s in. lumber and
should be practically air-tight.
V — Humidity and temperature systems must be
controlled more closely in paper and textile testing
laboratories than in most factories, and for laboratories
more or less difficulty may be experienced with many
automatic systems, which are entirely satisfactory for
commercial and manufacturing plants. It is, there-
fore, advisable to submit any installation to a thorough
trial before reaching a conclusion as to its efficiency.
As temperature and humidity are so closely related,
a temperature effect on the actuating material of a
humidity control instrument must be properly com-
pensated for. Naturally if a humidity control is
in tailed in a room in whirl] the temperature is closely
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CUE./ Vol. 10, No. i
controlled this practically eliminates the effect of room
temperature on the humidity controller. All materials
used for humidity controls are subject to tempera-
ture changes to a greater or lesser degree.
VI — Not only is the control of humidity of importance
in the testing of materials, but also in many industrial
lines as well. Many of the troubles and complaints
of the pressman and engraver are due to humidity
effects on paper and could be remedied by maintain-
ing more uniform humidity conditions in the press
and storage rooms. Low indoor humidity in winter
is the cause of much inconvenience in printing, causing
the paper to curl and shrink and thus interfering
greatly with the work of the presses. Paper is more
flexible at high humidity. This fact is of direct im-
portance to the manufacturer of envelopes and in the
folding of paper, the humidity of the room determining
whether the folding is smooth or cracked. The hu-
midity of the drying loft and the calendering end of
a paper machine undoubtedly plays an important
part in the finishing of paper. The expansion and
contraction of the sheet caused by variations in at-
mospheric humidity are of controlling importance
in map and chart making and in certain special uses
of paper. This could be easily overcome by keeping
the paper at a uniform humidity from the time it is
received until the work is finished.
VII — There are many other industries in which the
maintenance of uniform humidity is absolutely neces-
sary. Among these are the manufacture of textiles,
fuses for munitions, motion picture films, tobacco
and many others. Humidity control is being applied
to the ripening of fruit, curing of cheeses, drying of
lumber, manufacture of leather goods and to many
other important industries.
Leather and Paper Laboratory
Bofbau op Chemistry. U. S. Department of Agriculture
Washington. D. C.
A METHOD FOR DETERMINING THE ABSORBENCY
OF TAPER
By E. O. Reed
Received November 13, 1917
The serviceability of blotting paper, paper towels,
filter paper and copying paper is largely dependent
on their absorptive properties for the measuring of
which several methods have been used. Since blotting
is the most important of absorptive papers, the methods
proposed have been especially adapted to the testing
of this class of paper.
Absorption is most commonly determined by meas-
uring the rate a1 which distilled water rises in a ver-
tically suspended strip usually 15 mm. in width,
the lower end of which dips beneath the surface of
water contained in a trough. Either the time which
it takes the water to rise to a given height or the height
to which the water rises in a given time, is noted.
The latter is the more common method. Apparatus
for conducting this test, which is known as the "mount-
ing test," has been Klemm1 and by S
Spa ifii ations for this quality in blotting paper usually
1 "Hiimlbuch (k-r Pupierkundc." p. 318.
• "Paper Mill Chemist." p. 229.
require that absorption shall be not less than a certain
number of millimeters in 10 min. The absorption in
each minute can also be noted, though specifications
generally state only the total absorption in 10 min.
There are several disadvantages in the use of the
mounting test for determining the absorptive proper-
ties of a blotting paper. The strips are suspended
vertically wh;le the blotting paper is always used flat.
The use of ink in this test is not practicable, due to
the large surface exposed to evaporation in making
the test and since most writing inks contain a col-
loidal precipitate, the blotter will tend to absorb only
the liquid portion. There is considerable difference
in the absorption of water and of ink by blotting paper.
To get the true ink absorptive value, ink must be em-
ployed in the test. The chief drawback of the mount-
ing test, however, is that it is unaffected by the bulk
or weight of the paper which necessarily has a rela-
tion to serviceability. In this procedure an unlimited
quantity of water is in contact with a variable thick-
ness or bulk of paper for a definite time and the height
to which the liquid rises in this definite time is re-
corded. Neither the width, thickness nor weight
of the strip affects the results. Two papers of differ-
ent bulk may give the same height of absorption,
but the lighter will undoubtedly not absorb as much
water as the heavier nor as rapidly. This is clearly
shown in Table III, which will be discussed later.
Bromley1 suggests determining the actual weight of
water absorbed. This procedure shows clearly that
the mounting test does not take into consideration
the bulk of the blotter, which is one of the chief fac-
tors determining the amount of water absorbed in a
specified time.
Other methods have been suggested for indicating
the absorbency of blotting papers. Sindall2 describes
a test for determining the absorptive qualities of
blotting paper, which consists of noting the time re-
quired to absorb 0.5 cc. of ink delivered drop by drop,
allowing each drop to be absorbed before another
falls. Methods somewhat similar but differing in
details of manipulation are described by Cross and
Bevan,' and by Stevens.4 The size and character
of the zones formed are also noted. The thickness or
bulk of the paper unquestionably pi an important
part in determining the size and character of the zones.
It has also been suggested that the absorptive capacity
and the loss of absorbent qualities of blotting paper
on repeated use can be determined by soaking it in
ink, allowing to dry, and then noting the time re-
quired for the absorption of quantity of
ink dropped upon it.6
The same criticism — failure to include the effect
of thickness or bulk of the j uantity of
ink or water absorbed in a given time applies also
to the methods suggested 1>\ I Fromm.7
1 "Notes on the Requirements ol Ccn .,.rs 0f Paper,"
Paper Maker and British Paper Trade Journal. 6», 59.
* "Elementary Manual of Paper Tcchoologs ." p. 119.
' "1'jpcr Making," 4th Ed , p. 389.
» "Pupcr Mill Chemist," p. 231.
» Ibid i
• La PapttrU, 1894.
; Wockbl. Papitrfabr., 1909, 4172.
Jan., 1918
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
4 5
In both of these methods absorption is measured
with the paper in a horizontal position. By Favier's
method the time required to saturate a square deci-
meter of the paper under a uniform pressure of water
is noted. The absorption value is calculated by divid-
ing the amount of water absorbed by the time re-
quired to saturate the paper. By Fromm's method
five circular pieces of blotting paper are floated to-
gether on a trough of water and the time required to
saturate the top piece is noted.
Though each of the methods referred to above is
faulty in some particular, the results obtained with
them, while varying with the procedure employed,
are serviceable in judging the quality of blotting paper,
if the limitations of the methods are kept in mind. It
has long been felt, however, that none of the methods
for indicating absorption give a true measure of the
serviceability of absorbent papers, especially of blot-
ting papers.
Investigations of the several procedures for the
testing of absorbency indicate that by a modifica-
tion and standardization of the procedures described
by Sindall, Cross and Bevan and by Stevens, more
accurate information as to absorptive qualities may
be obtained than by the mounting test or the other
methods mentioned. The procedure finally adopted
consists in noting the time required for the absorption
of one cc. of a specified standard ink or of distilled
water under definitely prescribed conditions.
PROCEDURE
Place a 4-in. square of blotting paper over a
beaker or tumbler and arrange a support in such a
manner that a i-cc. pipette is held in a vertical posi-
tion with the delivering tip '/2 in. above the cen-
ter of the surface of the paper. A suitable apparatus
may be made by boring a hole in a cork through
which the stem of the pipette will pass freely. Clamp
it in a ring stand, so that the pipette when placed in
position has the tip at the correct distance above the
surface of the paper. Select a pipette with a delivery
time for distilled water at 700 F. temperature of ap-
proximately 4 sec. Fill the pipette with distilled
water or standard ink at 700 F. temperature. Place
it in position in the support and permit the contents
to flow upon the surface of the paper and record by
means of a stop-watch the time required for the com-
plete absorption of the liquid. Triplicate determina-
tions should be made and the results averaged to
secure the absorption time of the paper.
A 4-in. square of blotting paper is sufficiently
large and it should be placed over a beaker or tumbler
having a diameter somewhat greater than the blot
made by the liquid, in order that the edge of the blot
may not extend to where the paper rests upon the
glass, as this may affect the time of absorption. It
is important in placing the square of blotting paper
upon the tumbler to dish it slightly, so that the water
or ink will be received in one pool and thereby pre-
vent buckling of the paper. If the paper is allowed
to buckle, uneven distribution of the liquid will be
caused and the time of absorption considerably af-
fected, thereby rendering the test valueless. Check
tests with this method in most cases differ but 2 or 3
sec. on papers absorbing the ink in less than 25 sec,
and from 5 to 10 sec. on papers absorbing the ink in
from 50 to 100 sec.
The results obtained using a specified standard
ink are more indicative in the case of blotting paper
than when water is employed. It is impossible to
depend upon ink purchased on the market for use in
a standard test of this character. It is therefore
absolutely essential for the analyst to prepare the
standard testing ink in accordance with a definite
standard formula. For this purpose the formula
for U. S. Government Standard1 blue-black writing
ink has been adopted. This formula is as follows:
Grams
Pure dry tannic acid 23 . 4
Gallic acid, in crystals 7.7
Ferrous sulfate 30.0
Dilute hydrochloric acid (U. S. P.) 25 . 0
Carbolic acid 1.0
Dye, Bavarian blue (D. S. F), Schultz and Julius
No. 478 2.2
Make to a volume of 1,000 cc. at 60° F. with distilled water.
All of these chemicals should be of U. S. P. quality and in addition
the purity of the tannin should be determined by the hide powder method.
Dissolve the tannic and gallic acids together in
about 50 cc. of warm water and allow to cool; dissolve
the ferrous sulfate in about 150 cc. cold water. Add
the hydrochloric acid to the ferrous sulfate and im-
mediately mix the solutions. Add the dye dissolved
in water and the carbolic acid and make up with dis-
tilled water to 1000 cc. Mix thoroughly and allow
to stand for at least 4 days at room temperature.
When ink is to be used for tests, draw out without
shaking the bottle. Formulas for standard inks
are also given in Bureau of Chemistry Bulletin 109,
revised, page 43, and Bureau of Standards Bulletin
on "Some Technical Methods of Testing Miscellaneous
Supplies," page 43. These formulas differ slightly
from the one adopted in that gum arabic is added
and the soluble dye is not included. The formula
adopted gives an ink closely agreeing in composition
with the normal commercial inks furnished under
the above quoted formula.
To prevent oxidation and evaporation of the ink
when not being used, it is essential that the ink be
poured into 50-cc. dark bottles, tightly corked and
stored in a dark, cool place. The use of 1 cc. of water
or ink gives a sufficiently wide range in the absorption
results between different papers. In the case of fil-
ter paper, copying paper and very light-weight blotting
paper, a smaller amount of water or ink (0.5 cc.)
should be employed.
There are several factors which affect the results,
namely, the temperature of the liquid, the delivery
time of the pipette, the distance of the tip above the
surface of the blotting paper and the amount of liquid
used. These should be standardized, if accurate and
comparable results are desired. In most cases there
is little difference between tests made with either the
felt or wire side of the blotter up. It is advisable,
however, always to place the same side of the paper
up, preferably the wire side, as on that side the ab-
sorption is mpre uniform.
Table I shows the effect of the time of delivery
I "General Schedule of Supplies, 1917-1918," General Supply Com-
mittee, Item 1128, p. 60.
46
THE JOURA I/. "/• INDUSTRIAL AND ENGINEERING I /// Vol. 10, No. i
from the pipette on the time required for absorption
of the water by the blotting paper. Ten i-cc. pipettes
were used. The pipettes were supported so that their
tips were approximately '/j inch above the sur-
face of the paper. The temperature of the distilled
water was 700 F. and the wire sides of the papers
were up.
Table I — Relation between Speed of Delivery and Time of Absorp-
tion of Water
Time Rbquiksd fur Absorption
Time of Sample Sample Sample
32286 32751 32288
Sec. Sec.
There is considerable difference in the results ob-
tained with rapid and slow delivery pipettes. How-
ever, the results obtained with pipettes delivering the
water in 3 to 6 sec. are practically the same. This
is explained by the fact that with a slow delivery the
rate of absorption of the fluid by the paper is nearly
the same as or exceeds the rate of delivery from the
pipette. Since the most uniform and accurate re-
sults are obtained with quick delivery, a pipette de-
livering 1 cc. in 4 sec. is regularly used in this test.
The last drop delivered upon draining, unaided, is
included in the test but not in noting the time of delivery.
Table II shows the effect upon the time of absorp-
tion of the distance of the point of delivery above the
surface of the paper. The same pipette delivering in
4 sec. was used in all cases and the temperature of
the distilled water was 700 F.
Table II — Effect on the Time of Absorption of Distance of Point
of Delivery above the Paper
Timi: RxgUTJUSD for Absorption
Distance of tip Sample Sample Sample
above surface 32751 32735 32926
In. Sec. Sec. Sec.
■/, 10 26 38
»/• 10 26 39
The distance of point of delivery above the surface
of the paper has very little effect on the time of ab-
sorption, though a slightly faster absorption with in-
creasing distance is noted. Practically no difference,
however, is observed in the average time of absorp-
tion when the tip of the pipette is from ', « to '/i
inch from the paper. When the tip of the pipette
is an inch or more above the surface of the paper, the
liquid spatters, covering a Largi d the time of
absorption is lessened. This difficulty
when the tip of the pipette is placed approximately
V« inch above the paper.
In Table III there are given comparative results
obtained by the mounting test and by the procedure
a set of white blotting papers of
me composition and weighing m. 3a, 45, 58, 72,
;oo sheets, respec-
The stock of these papers is all rag and the
ash content varies only from 1 . .• - cent.
Distilled water at 70' F. temperature was used in
both methods. The mi 1 strips were all
cut transversely of the sheet 15 mm. in width.
Table III— Comparative Absorption I " Mot rcrrrNG Test
am. the 1 Cc. Absorption Test
Ream V. Mountini 1 Time Required for
Sample 19X24-500 l.Min. A!. sorption of 1 cc.
No. Lbs. Mm Mm. Sec.
32791 (•) 19 20 54 111*
32792 32 20 54 100
32793 45 19 54 61
32794 58 58
32795 72 20 36
32796 96 18 50 37
32797 140 20 55 11
(*) This sample is very thin and allowed 4 drops of water to filter
through, reducing the amount absorbed by that quantity.
The absorption values of these samples obtained by
the mounting test are practically the same, though the
weight of the paper varied from 19 to 140 lbs. per
ream. These results are in harmony with the known
fact that the rate of rise of water in the mounting
test is independent of the weight of the paper. On
the other hand, the speed of absorption in the cubic
centimeter absorption method increases inversely
with the weight of the paper. The effect of the weight
or bulk of the blotter on the absorption value is clearly
indicated by the time required for the absorption
of 1 cc. of water in the horizontal position. This
test shows that the speed of absorption increases
with the increase in bulk of the paper and that the
heavier the blotting paper the better its absorption
properties.
In Table IV there are given the analyses and ab-
sorptive values of several typical samples of blotting
paper measured by three different methods. Results
are given by the mounting test, using distilled water,
and by the 1 cc. absorption method, using distilled
water and also U. S. Government Standard ink.
The water and ink were used at 70° F. temperature.
The samples are arranged in the order of their ab-
sorptive values as indicated by the time required
for the absorption of 1 cc. of standard ink. The order
would be changed completely if the samples were
arranged in the order indicated by the values ob-
tained by the mounting test or by the absorption
time for 1 cc. of distilled water. It will be noted
throughout that the values by the mounting test do
not give the same relative rating for absorptive quali-
ties as those obtained by the 1 cc. time absorptive
method using water or ink. It will be noted that
here, too, the effect of weight is shown by the results
obtained with the 1 cc. absorption method. By the
1 cc. absorption method the time varies from 9 to 203
sec, by the mounting test from 44 to 101 mm. Thus
the possibility of differentiating between papers is
much greater with the former than with the latter
method. The resull cc. of stand-
ard ink are undoubtedly tical value.
In this paper it is not the pur] r the fac-
tors in the n which affect
the absorption quality, as this will be fully dealt with
in a later publication. Hi'V color, stock,
and ash content of the pa] the weight,
will be found to explain the r ases.
If these samples
that is. all samples (oc
60 lb. classes, the resuh - ral pn
still si values,
though
The propose. 1 method maj 1 to g
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Sample
No.
32960
28018
32956
32959
28020
32925
28129
32961
32924
32955
32799
32968
32758
32969
32965
32966
32927
32929
28030
28024
32760
32976
32962
32926
33852
32973
32974
32970
32963
32922
32921
31748
28136
32936
Table IV — Analyses of Typical Samples op Blotting Paper with Comparative Absorption Values
Color
White
White
White
Gray
Blue
White
White
Gray
White
White
White
White
White
Gray
Gray
White
Pink
Pink
White
White
White
Gray
White
Pink
White
Gray
White
White
Gray
White
White
Blue
Blue
(All Physical Tests Made
at 70° F
and 65 Per cent Relative Humidity)
Weight
Bursting
Time Required for
Mounting Test
19 X 24
Stock
Ash
Thickness
Strength
Absorption of
Rise in
500
Rag
Soda
Per
Av.
Ink Water
10 Min.
Lbs.
Per cent Per cent
cent
Inch
Points
Sec. Sec.
Mm.
139'A
81
19
8.3
365
27.0
9 9
96
125
100
1.0
340
34.0
10 16
65
102
79
21
7.7
285
21.0
13 11
101
II81/1
70
30
7.9
330
30.0
14 10
86
123 'A
100
2.6
330
30.5
15 16
65
139
71
29
5.2
345
38.0
15 21
60
97 'A
80
20
2.3
290
21.0
15 16
80
135'A
59
41
5.5
360
31.0
19 19
65
119>A
72
28
5.5
320
35.0
19 24
56
7 7 'A
84
16
7.4
230
19.0
19 19
97
100
100
1.3
250
19.0
21 18
61
139'A
48
52
20.1
335
21.5
21 18
67
133
22
78
27.0
320
16.5
23 17
69
137
49
51
18.4
330
26.0
24 18
63
95 'A
52
48
17.0
260
19.5
26 16
78
124 'A
51
49
19.9
305
23.5
30 22
68
82'A
85
15
4.7
220
23.5
30 20
75
124
68
32
5. 1
310
38.0
30 28
48
93 1 A
81
19
5.8
230
28.0
31 25
63
101 'A
61
39
14.5
245
23.5
32 33
64
114
22
78
25.5
260
24.5
38 23
69
139
35
65
19.1
305
23.5
40 25
57
80
66
34
14.4
215
18.5
40 26
80
62
85
15
4.4
170
15.0
42 42
60
63>A
68
32
13.1
170
16.0
45 27
86
102
26
74
20.2
240
19.0
49 29
67
120
32
68
25.6
270
18.5
57 38
57
83
26
74
19.8
195
17.5
62 50
66
77
51
49
16.9
200
19.0
65 33
71
77
62
38
7.6
190
26.0
65 47
63
65 >A
68
32
6.3
150
22.0
74 85
57
99 'A
60
40
23.9
230
2d.0
104 69
56
102
44
56
27.9
215
14.5
147 98
49
58
37
63
16.0
132
13.5
203 197
44
indication of the total absorptive capacity of a paper
or the loss of absorptive qualities on repeated use.
In using this method to secure an indication as to the
capacity of a blotting paper, a piece of paper of definite
size (2 in. square is a convenient size) must be used.
The test may be carried out in two ways: The paper
may be saturated by running upon its surface succes-
sive i-cc. portions of standard ink until it is com-
pletely saturated and will absorb no more. Although
completely saturated with liquid in this manner, upon
thoroughly drying the paper will still absorb more
ink. Another plan is to allow the blotting paper to
thoroughly dry between each 1 cc. of ink. Consid-
erable time is required in the procedure, but after a
certain number of applications of ink the absorption
begins to decrease rapidly until finally a point is
reached when the paper will absorb no more. By
either procedure the number of centimeters of ink
used and time required for the absorption of each
centimeter is noted. The results by the procedures
outlined do not give the same relative results and it
is believed that the last suggested is the most indica-
tive of the total capacity of blotting paper under
service conditions.
However, the life or capacity of a blotter is so
largely dependent upon the treatment it receives in
service, that the results obtained by such a determina-
tion are of but little practical value. If a blotter
is saturated with ink and allowed to dry, although
somewhat stiffened, it will still absorb satisfactorily in
most cases. In fact, it has been found that many
blotting papers may be repeatedly saturated with
ink and dried without materially lowering their blot-
ting qualities. But in service the surface of the paper
becomes covered with a coating of dried ink, rubbed,
sed and filled with dust, which renders it use-
less long before it is completely saturated with ink
absorptive capacity gone.
ta on speed of absorption will not give an in-
dication of the total absorption capacity of a blotting
paper. For example, in Table IV, Samples 32955,
32799 and 32968 show practically the same absorptive
values by the 1 cc. time absorption method for ink.
Tests indicate that rated for total capacity of ab-
sorption the order would be 32799, 32955 and 32968,
or in this case inversely as their ash content.
CONCLUSION
As the rate of rise of a liquid in the mounting test
is independent of the bulk, an accurate indication of
the absorptive qualities of a paper cannot be ob-
tained with this test. It is our experience that the
measurement of the zones formed by blots of ink on
a blotting paper does not afford a reliable test for
rating absorption qualities of different papers since
the area of the blot is greatly affected by the thick-
ness or weight of the paper even though the same
amount of ink be used with each.
By the 1 cc. time absorption method suggested in
this paper, the results obtained are apparently more
indicative of the true absorption value of paper than
can be obtained by other known methods. The method
also has two distinct advantages: the test is made with
the paper in the horizontal position and it is possible
to use ink in making the test. The use of ink, pro-
vided a standard ink be used in all cases, gives the
most serviceable indication as to the absorption value
of blotting paper. The absorption value as indicated
with water is not always the same as with ink.
The method has also been used in determining
the relative absorptive values of paper toweling with
very satisfactory results. In the case of copying paper,
filter paper and very light weight blotting paper only
0.5 cc. of water should be used.
I- 1 hud is very simple and convenient, and a
number of closely agreeing results can be obtained
in a very short time.
rnKK and Paper Laboratory
1 < op Chemistry
Washington, D. C.
48
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHI ■ < I Vol. 10, No.
THE USE OF TEXTILE FIBERS IN
MICROSCOPIC QUALITATIVE CHEMICAL ANALYSIS
By E. M. Ciiahot and H. I. Cole
Received September 28. 1917
III THE DETECTION OF BORON BY MEANS OF TURMERIC
VISCOSE SILK FIBERS'
The reaction of boric acid with turmeric paper, in-
volving a color change from yellow to rose, was first
described by Trommsdorff ■ in 1 8 1 5 . Later investigators
showed that this rose color was changed to blue or
greenish black upon the addition of alkali.
In this reaction curcumine, the yellowish coloring
matter in the turmeric root, is changed by the boric
acid into another substance, rosocyanine, first described
and named by Schlumberger3 in 1866. It was so-called
by him because of the fact that it forms rose colored
solutions and blue colored metallic salts. Upon
analysis he found that the rosocyanine contained no
boron, though the latter was necessary to bring about
the reaction.
Ivanow-Gajewski,4 Ciamician and Silber,6 Milo-
bedzka,8 and Jackson and Clarke7 have since worked
on this curious and interesting reaction and they found,
as did Schlumberger, that rosocyanine does not contain
boron. Here, then, is another of those curious chemical
reactions where an element plays a mysterious r61e,
for it is strange that boron alone among the elements
should be able to induce a molecular rearrangement of
curcumine into rosocyanine.
Emich8 suggested that the blue color is due to a
reaction of cellulose. Jackson and Clarke,9 however,
obtained the blue color when no cellulose was present
and our results as given are in accordance with their
findings.
In testing for boric acid in the usual manner with
turmeric paper, addition of the alkali almost invariably
yields a greenish black color when boron is present
instead of the much more characteristic blue color. In
applying this test microscopically, however, using in-
dividual fibers instead of strips of paper dyed with
turmeric, it is always possible to obtain a distinct blue
color. Having experienced difficulty with flax and
cotton fibers impregnated with turmeric, it was thought
worth while to test out the various controlling factors
for the production of the best and most sensitive fiber.
After various methods of dyeing with turmeric were
tested, the following one was selected as being the most
satisfactory. A 50 per cent alcoholic, alkaline solution
of turmeric is prepared by boiling approximately 10
g. of ground turmeric root with 50 cc. of alcohol and
adding to the filtered solution an equal volume of water
and V2 to 1 cc. of dilute sodium hydroxide (10 per cent).
The fibers are immersed in this solution which is then
evaporated on a water bath to a syrupy consistency.
The fibers are removed and immediately dipped in 95
per cent alcohol, pressed between tiller paper, dipped
1 For P*rti I unci II see This Journal. 9 (1917), 967.
> J. 1'harm.. 16 (1815). 96.
• Bull. soc. chim.. |2) 8, (1866). I'M
' 1-i 6 IX
• Com. chim. Hal.. 87 (1897). 561.
• Ber.. 43 (1910). 2163.
'.1., i c htm /.. SB (1908). 696; 48 (1914). 48.
• Aft*.. SB1 (1907). 429.
• ,1m Ch,m. J.. S9 (1908). 69(.. 46 (191
in a dilute aqueous solution of sulfuric acid, washed with
water and dried. The transference of the fibers from
the hot dye to the alcohol must be done quickly as
otherwise the turmeric adhering to the fibers is removed
only with difficulty. Too long an immersion in the
alcohol tends to remove the adsorbed dye as well as t.he
excess dye.
If the fiber still appears to have any unadsorbed
turmeric adhering to it (with viscose silk this is easily!
noted by the lack of luster) it can once more be dipped
in alcohol and washed with water. Any unadsorbed
turmeric interferes with the formation of the blue color
in the boron test. This method as given yields a beauti-
ful golden yellow product which was found to be
eminently satisfactory.
Curcumine of different degrees of purity was also
tested but since the delicacy of the reaction obtained by
using the ordinary turmeric extract is exceedingly
great, there is no necessity for other purification than
that given in the above described method.
To determine the influence of the nature of the fiber
on the delicacy of the reaction, the common textile
fibers, flax, cotton, wool, mohair, raw silk, purified
silk, viscose silk (cellulose xanthate), lustron silk
(cellulose acetate) and coarse fibers of cupra-am-
monium silk were dyed in turmeric solutions as stated
above and then used for the boron test.
Flax, cotton, raw silk, purified silk and viscose silk
dyed with turmeric give the typical boron test described
below, while wool, mohair, lustron silk and cupra-
ammonium silk more often give a green instead of the
typical Prussian blue color upon addition of the alkali.
Of the various fibers tested, viscose silk gives by far
the best color reaction, flax being next best but less
satisfactory in comparison. Xo preliminary treatment
of the viscose silk to render it more adsorptive was
found to be necessary.
Of the various methods tested for applying the
turmeric fiber test for boron, the following procedure
gives the most satisfactory results: Place a drop of the
solution of the material to be tested upon an object slide
and acidulate with dilute hydrochloric acid to decom-
pose any borates that may be present. In this drop,
place a turmeric fiber about 5 mm. long and allow to
evaporate spontaneously, or by gently warming, to
compute dryness. Cool and examine the fiber under the
microscope. A rose or violet-rose color indicates boron.
To confirm the test, place a drop of a i per cent solution
of sodium hydroxide upon the rose colored fiber. The
rose color immediately turns to a beautiful Prussian
blue color which gradually changes to violet. Too high 1
a temperature in the evaporation or failure to allow'
the fiber to go to complete dryness ma) lead to negative ;
results. Too concentrated a solution of the alkali will
interfere with the formation of the blue color. The
fiber must be observed imnv addition of
the alkali as the blue color is thei most intense.
A mineral acid alone fiber on
evaporation to dryness gn brown color,
not the rose or pink color o\>' >ron is also
present. Furthermore, add: irGp of alkali
yields, instead of a blue, a yi ^ing to the
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
49
characteristic mahogany color produced by alkali on
the turmeric fiber.
It must be remembered that a test for boron as sensi-
tive as this one, must not be performed upon an object
slide made from resistance glass containing boron as
one of its ingredients. It follows also that apparatus
made from such glasses cannot be used for solutions
which are to be tested for the presence of boron.
The presence of hygroscopic salts is objectionable,
since they prevent the complete drying of the fiber.
However, when the solution to be tested contains more
than traces of boron, a satisfactory test may be obtained
even in the presence of large amounts of such salts.
Any strong bleaching agents, such as hydrogen perox-
ide or a hypochlorite, must be destroyed before the
test can be applied.
Much free phosphoric or silicic acid render the de-
tection of boron difficult though not impossible. In
the turmeric paper test for boron as commonly applied,
it has been pointed out that molybdenum, titanium,
zirconium, columbium and tantalum may lead to
error, because under certain conditions these elements
give a color reaction somewhat similar to that obtained
with boron when the alkali is added. This source of
error has been carefully studied and we find that the
presence of these elements leads to no misinterpreta-
tion of the color changes nor could we obtain with any
of these elements the blue colored fiber, characteristic
of boron, when no boron was present.
Boric acid can be distinguished from a simple borate
in the following manner: Evaporate to dryness with-
out the addition of a mineral acid. A rose-pink indi-
cates boric acid; undecomposed borates yield no rose
color. Add the alkali. Boric acid gives the character-
istic blue color, borates do not. Commercial borates
of ammonium, sodium, potassium, calcium, barium,
iron, lead, nickel, copper and manganese tested as
described, gave a boron test from aqueous solutions
only after acidification with hydrochloric acid. Ferric
borate, however, failed to give a positive test in very
concentrated solution.
It must be remembered that in the presence of in-
organic salts which have the power to decompose a
borate, a test for boron may be obtained without the
addition of an acid.
The sensitiveness of this reaction was tested accord-
ing to the method already described.1 A positive test
can be obtained by means of turmeric viscose silk, in
one drop of a N / 16,000 solution of boric acid or of a
borate, normality being computed with respect to the
amount of boron present. The amount of boron actually
present in a drop of a solution of this concentration is
0.000,025 mg-
SUMMARY
I — Viscose silk, dyed with turmeric, gives an ex-
ceedingly sensitive microscopic method for the de-
tection of boron in boric acid or in borates.
II — It is possible by this method to differentiate be-
tween boron as boric acid and boron combined as
borate, providing substances which will set free boric
acid from borates are absent.
1 Lot. cil.
Ill — A drop of a solution containing 0.000,025 mg.
of boron gives a positive test for boron by this method.
IV— THE DETECTION OF THE HEAVY METALS BY MEANS
OF ZINC SULFIDE WOOL FIBEES
The use of fibers impregnated with zinc sulfide,
as a microscopic means of detecting the heavy metals,
was suggested by Emich and Donau1 in 1907. They
used cotton and guncotton as the carriers for the zinc
sulfide. In making these fibers, according to their
method, we found that it was extremely difficult to
impregnate the fiber with the zinc sulfide. In order
to overcome this difficulty, we endeavored to make
artificial fibers containing a zinc salt and ultimately
to change this salt to zinc sulfide, as follows: An ether
solution of zinc chloride was mixed with a solution of
collodion or "parlodion." Artificial fibers were then
made from this solution by forcing it through a fine
capillary opening into a solution of sodium sulfide.
The resulting fibers, while sensitive enough, were
generally imperfectly formed and the manipulation
necessary for their satisfactory production required
such a great amount of skill and practice that the
method, after many attempts, was abandoned as un-
reliable.
The following modification of this method was also
tested. Finely divided and colloidal zinc sulfide
was mixed with the collodion and then made into
fibers, by extruding into a coagulating liquid, by dry
spinning and by making thin films of the mixture and
subsequently cutting them. Fibers made by this method
also proved unreliable.
The common textile fibers were then tested as to
their suitability. Fibers of cotton, true silk, viscose
silk, lustron silk, flax, ramie, wool and mohair were
immersed in solutions of zinc chloride for several hours,
washed with water and placed in solutions of sodium
sulfide for 2 hrs., then washed and dried. Of the fibers
treated in this manner, in reagent solutions of different
concentrations, wool and mohair alone adsorbed
enough zinc sulfide to give a satisfactory color reaction
with the heavy metals.
The preliminary treatment of the wool was found to
be important. Fat-free and swelled fibers adsorb more
of the zinc sulfide then the untreated fibers. The fat
may be removed from the wool by a mixture of alcohol
and ether. For swelling the fibers the best results
were obtained by soaking the wool over night at
room temperature in a 1 per cent solution of sodium
hydroxide. This gives the maximum swelling with the
minimum detriment to the fiber.
Various zinc salts and methods of impregnating the
wool with the salts were tested. It was found that zinc
acetate is adsorbed to a slightly greater extent than
either zinc sulfate or zinc chloride. The following
method for making zinc sulfide fibers was finally
adopted: The defatted wool is swelled by soaking over
night at room temperature, in a 1 per cent solution of
sodium hydroxide. It is then washed and dipped 5 or
6 times alternately in solutions of 10 per cent zinc
acetate and 10 per cent sodium sulfide, pressing out the
1 Ann.. SB1 (1907). 432.
5o THE JOl n \L Of INDl l KIM. AM) ENGINEERING I HI ' >°- No. i
excess solution but not washing between dippings. For the determination, 20 or more grains of the dry-
After the final dipping, the impregnated wool is washed plant are carefully ashed in a muffle where the tem-
and dried by pressing between filter paper. Zinc perature does not ex C. The ash is dissolved ■
sulfide wool fibers made in this way are sensitive to in hydrochloric acid and the iporated off.
0.001 mg. of copper. The sodium sulfide solution An excess of freshly slaked lime is added to precipi-
should be freshly prepared by passing H2S into a solu- tate the phosphoric acid, magnesium, etc. The
tion of NaOH until a portion removed fails to yield a solution and precipitate are boiled a few minutes and ;
precipitate with MgClj. The fibers thus prepared are then filtered. The calcium in the filtrate is then
employed as follows: precipitated with ammonia and ammonium carbon-
(a) Place a drop of the solution to be tested upon ates and filtered. For the sake of prei aution, a second
an object slide and add a drop of dilute HC1. Intro- precipitation of the calcium should be made. The
duce into the drop a zinc sulfide wool fiber about 5 combined filtrates are evaporated to dryness, and the
mm. long and examine under the microscope. ammonium salts expelled. This operation must be
(b) Evaporate to dryness, add a drop of dilute most carefully done, for the rare earth chlorides are
ammonium hydroxide, examine the fiber again and extremely volatile. It is best done in a muffle kept
introduce into the drop a new fiber to serve as a means just below redness. The remaining alkali chlorides
of comparison, in order that slight changes in color are filtered off with hot water, a few drops of hydro-
may be better discerned. These color changes are chloric acid added and then about 0.05 g. of
yellow, orange, brown or black. platinic chloride. The solution is stirred well and
In acid solution the fiber is evaporated to pastiness. Meanwhile a small carbon
straw-ydiow Tin filter is prepared by drawing out a hard glass tube
Lcmon-yriiou. ,wnic.Cadmium of ^ .q or less diameter A perforated platinum
B^JftSk*^:::::::.::: «K5Si. copper. Mercuric Mercury, foil serves to hold a small mat of asbestos. The un-
M^rfa?eK Ni3c*d)meS Cobalt' Iro"- changed chlorides of potassium and sodium are rapidly
Black (brown in very dilute solu- dissolved in the minimum amount of hot water and
tions Silver, Lead, Gold. Mercurous Mercury .
the chloroplatinates of the rare alkalies with some
In acid solution no color, but in alkaline solution potassium chloroplatinates washed on to the asbestos
the fiber may turn brown or yellow-brown if cobalt, iron. parj wjtj, g0 per rent alcohol. Care must be taken
manganese or nickel is present. These elements, how- not t0 use too iarge an amount of hot water to dis-
ever, rarely give goi h the fibers. solve and wash the unchanged chlorides. The platinic
It must be remembered that the color of the fiber, clilorides of potassium, rubidium and caesium are
as usually observed with transmitted light, varies with ,jlen reduced by connecting the carbon filter to a
the amount of the metal present. For example, a yel- hydrogen generator and heating gently with a Bunsen
low or orange color, if deep enough, may appear brown burner. The reduction takes place easily, becoming
black. On the other hand, an element giving spontaneous when some platinum black is left on
usually a brown or black color with the fiber may color t^e pad from a pri mination and the pad is
it a light brown or yellow when only traces of the SOmewhat moist with alcohol. The chlorides of the
element are present. alkalies are washed through the niter with hot water,
si mmaky ,-^g titrate evaporated t" .cry small,
I A reliabli .-mil sensitive method for the preparation lipped, platinum dish. then taken up
of zinc sulfide fibers has been descril with four drops of strong hydrochloric acid and fil-
II — Zinc sulfide wool offers a satisfactory test in tered through a tiny filter into a vial of about 2 to 5
minute quantities of materials for the presence or cc. capacity. A number of these vials are graduated
yielding colored sulfides. to hold the same volume. The rare alkali chlorides
Laboratory Ciikmicai. Microscopy are taken up and til' portions of
1 1 rnvBRsriY, Ithaca, n v. acid of four drops each (. s portion being
blown through the filter. The solution is made up
A PROXIMATE QUANTITATIVE METHOD FOR THE to volume and is real. Standard^
DETERMINATION OF RUBIDIUM AND arc madc up bv treating know, ■ ounts of caesium
CAESIUM IN PLANT ASH and rubidium chlorides and , potassium
lu xv " Ro1 chlorides with Stl I
Received Novei \ Bunsen burner is . of heat
This method on the removal of the major and ii must be carefullj :•-. the observer.
of potassium chloride by fractional precipi- The cl e lasts only
with platini ad, further, by precipita- a few moments. Caesium is i the d
rith strong hydro id. The resulting 4215. 6 and 4201 1 double lines
solution containing all the rubidium and caesium 4593-3 aIU' 4555-4- '
chlorides and a large amount of potassium chloride is and the observer must rem lit ii \.rk ro
compared S] ally with a standard solution at least an hour before tl m< Si
he method outlined by Gooch and enough.
Phinney.1 The comparison is ma • g a coil of:
'. Sci., U (1892). 392. platinum wire of sufficient hdraw a very
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
large drop.1 The coil is carefully dried high above
the flame or on a radiator, taking care to avoid spat-
tering. The unknown solution is matched with stand-
ards by means of the brilliancy of the line. An ac-
curacy of from 5 to 10 per cent is easily obtained by
different observers.
Bureau of Soils
Washington, D. C.
A QUICK METHOD FOR LIME CAKE ANALYSIS
By Alfred N. Clark
Received November 5, 1917
The usual procedure in lime cake analysis has been
to weigh out 50 g. of the sample in a sugar weighing
dish, add acetic acid, mix to a thin mud in the weigh-
ing dish, transfer the contents to a 200-cc. flask, add
lead subacetate solution, and fill to the mark with water.
All the textbooks describe a method similar to the
above, and in which a flask is used. Such a procedure
has four serious drawbacks which are avoided in the
method described below. With the flask method,
lime is liable to foam over the sides of the sugar dish
when acid is added; it is difficult to thoroughly mix in
such a small dish without sp'lling; there is danger of
spilling when transferring from the weighing dish to the
flask ; and the whole procedure is a slow, disagreeable one.
The writer weighs the sample of lime cake in a coun-
terbalanced, nickel-plated, copper beaker of about
300 cc. capacity, adds the calculated volume of acetic
acid solution from a pipette, mixes with a small pes-
tle, adds a charge of lead subacetate solution from a
Sachs-LeDocte or a Kruger pipette, again mixes with a
pestle, and pours onto a filter. The dish is large enough
to avoid foaming over, and the mixture is not trans-
ferred from the weighing dish until ready to filter.
1 A No. 27 wire B. & S. gauge, coiled
makes a good coil.
und a Vn rod,
The following examples will explain the calcula-
tion required for adopting the Sachs-LeDocte or
Kruger sugar pipettes to lime cake analysis:
A Sachs-LeDocte pipette delivers 177 cc. of lead
solution and uses a normal weight of 26 g. There-
fore, 200 cc. of solution must be added to the dry mat-
ter of the lime cake, and if it is assumed that the cake
contains 50 per cent moisture, we have 13 + 10 +
177 = 200 cc. As it is necessary to add acetic acid
or ammonium nitrate to decompose saccharates, the
strength of acid is so adjusted that 10 cc. are required.
When the filtered sample is polarized in a 200 mm.
tube twice the scale reading is the per cent sugar in
the cake.
With the Kruger automatic pipette the normal
weight is adjusted to the size of the pipette; for
instance, if the pipette delivers 123.6 cc, the normal
weight is 41 . 2 g. for beets, and the same weight is used
for lime cake. The amount of solution to add to the
dry matter of the lime cake is 158. 5 cc, and if the lime
cake contains approximately 50 per cent of moisture
the solution is made up of 20.6 + 14.3 + 123.6 =
158.5 cc. Here 14.3 cc. of acetic acid solution are
used, and the polarization in a 200-mm. tube is the
per cent sugar in the cake.
If the moisture content of the cake varies apprecia-
bly from 50 per cent the volume of acetic solution
added is adjusted accordingly.
When "free" sugar is to be determined, water is
added instead of acetic acid.
By the use of normal lead acetate solution in the
place of subacetate solution, no acetic acid need be
added, but in that instance a different weight of lime
cake should be used in order to give the proper dilu-
tion.
900 N. Washington Avenub
Lansing, Michigan
RECOVERY OF LIGHT OILS AND REFINING OF TOLUOL
Report prepared by th
u of Standards in response to n:
was submitted to, and revised in accor
i, municipalities, manufacturers of gas, a
of Standards at the request of the COnfe
inquiries for information regarding recovery of light oils and the refining of
ith suggestions of the committee, consisting of representatives of the Public
rs of toluol recovery equipment, organized under the chairmanship of Dr. E. B.
ich met at the Bureau July 31, August 1 and 2, 1917.
PART I THE TECHNICAL RELATION OF THE GAS INDUSTRY
TO THE MILITARY NEEDS OF THE NATION
I. HIGH EXPLOSIVES MANUFACTURED FROM GAS BY-PRODUCTS — ■
The importance of high explosives in the present war has been
amply demonstrated. While nearly all kinds of explosives are
used in some way, those which are most in favor for filling
high explosive shells are manufactured from benzol and toluol,
which substances have their most important commercial
source in manufactured gas of one kind or another. The gas
industry thus becomes directly and vitally connected with the
conduct of the war and a survey of the demands which will be
made upon it, and its preparedness in a technical way to meet
is very important at the present time.
J CITY OAS PLANTS MUST SUPPLEMENT COKE-OVEN PRODUC-
TION— The constituents of illuminating and fuel gas which are
important in the manufacture of explosives at the present time
arc benzol and toluol, especially tin- latter. The removal of
: I it in-nts from the gas which is a by-product of Coke-
D practiced for some time. Plants manu
factoring city gas, however, have not generally removed these
:u the gas since they contribute to its light- and
ml the substitution of other sub tance
to maintain the gas quality up to prescribed standards has not
usually been considered profitable. Even now, although several
months have elapsed since the United States entered the war,
comparatively few city plants are equipped to recover these
materials, but the prospects are that in the near future they
must do so if the requirements for high explosives are as great
as is anticipated. Major Burns of the Ordnance Department
at the conference held at the Bureau of Standards on August i
stated that the Army is dependent upon toluol for the manu-
facture of T. N. T. for shell filler. The amount of toluol needed
depends upon the number of men engaged and how engaged.
The present estimates are that toluol for shell filler will be
needed in the coming year for our own army, for the allies, and
the navy at a rate considerably in excess of the present or
anticipated supplies from works under construction. There is
at the present time about 4 million pivunds per month of T. N. T. ni-
trating 1 apacity and sufficient toluol is not now available to utilize
it; it is therefore now impossible to place more orders for T. N. T.
primarily because more toluol is not available. It is probable
that any and all explosives including the picratcs will be neces-
,ai y eventually.
V MANUFACTURING PROCESSES IN USE IN THE UNITED STATES
The manufactured gas distributed in the United States is of
three principal kinds: Coal gas, carbureted water gas, and oil gas.
5?
TUE JOURNAL OF IS DUST RIAL AND ENGINEERING CHI 10, Xo. i
The manufacture of water gas consists essentially of an inter-
mittent process in which a bed of anthracite coal or coke is
brought to a high temperature by an air blast and then steam
under pressure is blown through the fuel, forming carbon mon-
oxide, hydrogen and a small amount of carbon dioxide, by re-
action with the carbon in the fuel. The residtant gas, called
blue water gas, has a heating value of approximately 300 B. t. u.
per cu. ft. and almost no luminosity when burned in an open
flame; it is conducted into a fire-brick-lined chamber called
the carbureter, which contains staggered rows of fire bricks,
called checker brick, heated to incandescence during the blow
period. Gas oil or fuel oil is sprayed into the carbureter
while the gas is passing through, forming an oil gas which en-
riches the blue water gas to any desired heating value or candle-
power. Another cheeker-brick-filler chamber, called the super-
heater, converts most of the oil gas vapors into permanent gases,
which will not condense again upon cooling. During the forma-
tion of the oil gas certain portions of the hydrocarbons which
compose the oil are changed in their composition to form benzol,
toluol, and related hydrocarbons, called aromatic compounds.
Considerable tar is formed at the same time. This is condensed,
scrubl ed, and washed out of the gas by various means, but usually
at a temperature which permits most of the aromatics to go for-
ward with the gas. The sulfur in the gas is removed by iron
oxide purifiers and the gas is metered and leaves the plant at,
or slightly above, atmospheric temperature.
The manufacture of coal gas is essentially different from that
of water gas. In this process certain classes of bituminous coals
are distilled in fireclay or silica retorts or ovens and the result-
ing gases are condensed, scrubbed, washed, and purified to re-
move water vapor, tar, ammonia, and sulfur. As in the water-
gas process, certain of the hydrocarbons given off by the coal
are transformed by the heat of the retort to aromatic com-
pounds. A small part of these aromatics are washed out of the
gas by the wash water and tar. but the larger part remains in
the gas; in fact, the cooling of the gas is usually so regulated that
most of these substances will remain in the gas to increase its
heating value and candle power. Coal gas retorts take a variety
of forms; among these are coke ovens, chamber ovens, hori-
zontal D-shaped retorts, vertical retorts, inclined retorts, etc.
Even those of a given class differ among themselves in details
of construction. In most of them the distillation is an inter-
mittent process, but some continuous methods are used. In
all these processes the gas produced consists of the same con-
stituents in somewhat different proportions. The form of ap-
paratus used in a given case depends largely upon economic
considerations or is governed by certain special qualities which
are desired in one or more of the products produced. In all of
these coal-gas processes, coke remains in the retort after dis-
tillation. In some of them, as for example in coke ovens, coke
is the principal product; but in city gas plants, gas is the chief
product. The operation is carried out in any case to give
most satisfactory- qualities to the principal product and at the
same time obtain as high yields and good quality as possible
of the secondary or by-products.
Mixed gas is usually understood to be a mixture of carbureted
water gas and coal or coke-oven gas. It is supplied in many
cities in the United States where the requirements permit of
a mixed gas being supplied,
The manufacturing installation for mixed gas is practically
two complete installations, one for coal gas and one for car-
bureted water gas, with their auxiliary scrubbing, condensing,
purifying, and metering apparatus entirely independent and
separate The manufactured mixed gas, however, is stored in
common holders and delivered through a single distribution
system.
The coal and water gas thus supplement each other. The
uniform, but more cumbersome coal-gas production furnishes
coke as fuel for the wa1 at; this in turn takes care of
;ularities of the output and where necessarj
i 1 v of the gas 1 n duction, especially where a high can-
dlepower standard is in ford
The oil-gas process is at present confined chiefly to the Pacific
Coast states, where comparatively cheap oil and expensive
coal make the coal- and water-gas processes less feasible. In
oil-gas manufacture, oil alone is used as fuel for heating the
checker bi icks ol the fixing chambi 1 • and <"l is sprayed
into the chambers where in contact with the bricks, lampblack
and permanent gases are formed. In this iromatic
compounds are included among the constituents of the gas.
4 AVERAGE CONTENT OP LIGHT OILS in VARIOUS GASSS — The
amount of benzol and toluol formed in any one of these processes
is bj no means definite. It depends upon the operating condi-
tions and the quality of the raw materials (coal or oil). It
would therefore be impossible to predict exactly what the yield
in a given case would be, but an extensive inquiry into the opera-
tion of several typical plants has given the following approx-
imate figures for the various processes. These figures are aver-
ages of the results obtained in the several plants; individual
results may vary widely from them in a particular case:
Data from Twelve Plants Investigated
Approximate Yield op Crude Light Oils
Horizontal-retort coal gas 3 gal. per short ton coal carbonized
Coke-oven gas 2.6 gal. per short ton coal carbonized
Continuous-vertical retort coal gas" 1 .8 gal. per short ton coal carbonized
Carbureted water gas 10 per cent of volume of gas oil used
Composition op Crude Ligbt Oils'
Solvent
naphtha,
wash oil,
naphtha-
Benzol Toluol lene, etc.
Per Per
cent cent cent Paraffins
Horizontal-retort coal gas 38 16 46 Less than 2 per cent'
Coke-oven gas 55 14 31 Less than 2 per cent'
Continuous vertical-retort coal
gas1 15 15 58 12 per cent
Carbureted water gas 42 25 33 Less than 2 per cent4
Yield op Pure Products
Benzol Toluol
Horizontal-retort coal
gas 1 .32 gal. per short ton 0.45 gal. per short ton
coal carbonized cowl carbonized
Coke-oven gas 1 .47 gal. per short ton 0.35 gal per short ton
Continuous vertical-re- coal carbonized coal carbonized
tort coal gas' 0.27 gal. per short ton 0.26 gal. per short ton
coal carbonized coal carbonized
Carbureted water gas' 0. 15 gal. per 1000 cu. 0.07 gal. per 1000 cu. ft.
ft. of gas of gas
1 Results from only one continuous vertical installation included here.
* The yield of toluol is variable according to amount of oil used in
manufacturing the gas. being equivalent to about 2.0 to 2.2 per cent of
the gas oil used in the plants investigated, but perhaps only about 1.6 in
many cases.
8 Data obtained from various sources.
4 This amount may be exceeded under some operating conditions, but
paraffins can usually be kept down to this figure except in unusual condi-
tions or with certain fuels.
No specific data are available for the amounts of toluol present
in oil gas, though it is understood that the oil gas distributed on
the Pacific Coast contains at least as much toluol as does coal
gas.
Assuming that a ton of coal gives 10,000 cu. ft. of gas and
that 3.5 to 4 gal. of gas oil are used per 1000 cu. ft. of car-
bureted water gas, it is evident from the table that the amount
of toluol obtainable per 1000 cu. ft. of rich water gas is consid-
erably greater than that obtainable from coal or coke-oven gas.
5. prospective toluol sources — It does not seem likely
that it will become practicable in the near future for plants
having outputs less than 100 million cu. ft. per year to recover
light oils. A survey of plants of that size and larger indicates
that there are about 1 1 2 plants having an aggregate annual
gas output of about 135 billions cu. ft., of which about 97 bil-
lions are water gas, 25 billions coal gas. and 13 billions oil gas.
What annual output of toluol could be expected from washing
all this gas is problematical. It seems, however, that at least
0.05 gal. of toluol per ioco cu. ft. of gas could be expected,
which would give a prospective toluol recovery from all these
companies of about 7,000,000 gal. per year. It seems likely
that with an adjustment of standards the ben/n! production
from the same amount of gas would be between three and four
times as much as the toluol production, or approximately 18,-
000,000 gal. These yields are by no means the maximum ob-
tainable, since the production in some existing plants is higher
than O.05 gallon Of toluol per 1000 cu. ft. A few of the
included in this estimate art \iring part
of their toluol and benzol, but by far the greater part of the avail-
ipplies are not J I I
PART II PRINCIPLES UNDERLYING BENZOL AND TOLUOL
RECOVERY
1 RELATION TO CAS PLANT OPBJ (TONS — Benzol,
toluol, and the related hydrocarbons lively will
condensable
nd are associated with othi of the olefine
and paraffin -cries which possess ■ r iperties sim-
ilar to them. To separate some ol ices, especially
the paraffins, from the light oil bj •■ ,„is. is well-
nigh impossible ami therefore it to control
the conditions of gas manufactun ,f these sub-
stances will be present in the li( sjble. The
Jan., 191S
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
53
presence of more than 2 per cent of paraffin compounds in
toluol is said to make it unfit for the manufacture of explosives.
Only by careful attention to the temperatures and other opera-
ting conditions maintained in the gas making process and by
the use of suitable raw materials can the gas manufacturer be
certain that the toluol obtained from his light oils will be sala-
ble. For example, in the recovery of light oils from water gas
not only the temperature, but the rate of oil injection, spacing
of checker bricks, etc., affect results. Dirty checker bricks
are said to be a very common cause of high paraffin content
in the toluol produced. The favorable conditions can be de-
termined only by trial in each particular case.
For the successful operation of plants in which partial or total
rectification of the light oils is carried out, careful technical
control seems to be a prime essential. In smaller plants where
only light oil is recovered technical supervision should be avail-
'able in starting the plant and for such a time afterwards as will
enable the regular operators to become familiar with the funda-
mentals of operation and establish a routine. It might be
feasible for several small plants within a certain district to re-
tain the services of a technical man who would divide his time
among them, and make the more elaborate tests which are oc-
casionally required for successful operation.
2. removal OF light oils from the gas — To recover light
oils from the gas, the method now almost universally employed
is to bring the gas into contact with an oil which has a solvent
action upon the light oils. Oil washing of gas is accomplished
by a variety of apparatus. In any case to obtain complete ab-
sorption it is necessary that an adequate amount of oil at a suffi-
ciently low temperature be brought into contact with the gas.
The temperature of the wash oil should not exceed 30 °C. (86° F.).
The temperatures obtainable in practice will, of course, depend
upon the facilities available for cooling the oil. It is desirable
to have the oil a little warmer than the gas to prevent condensa-
tion of water from the gas into the oil which gives trouble in
the further stages of recovery. The amount of wash oil circula-
ted through the washers will depend upon the amount of light
oil vapors present in the gas, the temperature of the oil, the
amount of gas to be washed, and the saturation of the wash
oil which it is feasible to obtain. About 10 gal. of wash oil
per 1000 cu. ft. of gas washed, seems to be an average figure.
The oil now usually employed for this purpose in this coun-
try is a petroleum distillate called from its color, "straw oil;"
some plants use a creosote oil obtained from the distillation of
coal tar. The choice seems to depend largely upon which is
available in a given case. The qualifications which a wash oil
should possess seem to be substantially as follows:
A creosote oil upon distillation should yield not to exceed 5
per cent up to 200 ° C, and not less than 90 per cent between
200 and 300 ° C. The oil should not contain more than 7
per cent naphthalene and should not show any marked increase
in viscosity down to 4° C. The oil should be as fluid as possible
under the working conditions and should have as small capacity
for heat as possible.
The characteristics of a straw oil for this purpose, as obtained
from some operators, are substantially as follows:
I — Specific gravity not less than 0.860 at 15.5° C.
II — Flash point in open cup tester not less than 1,15° C.
Ill — Viscosity in Saybolt vjscosimeter at 37.7° C. not more than 70
IV — The pour test shall not be over — 1 . 1 ° C.
V — When 500 cc. of the oil are distilled with steam at atmospheric pressure,
collecting 500 cc. of condensed water, not over 5 cc. of oil shall have
distilled over.
VI — The oil remaining after the steam distillation shall be poured into
a 500-cc. cylinder and shall show no permanent emulsion.
VII — The oil shall not lose more than 10 per cent by volume in washing
with 2Vj times its volume of 100 per cent sulfuric acid, when vigor-
ously agitated with acid for 5 mins. and allowed to stand for
2 hrs.
Some operators claim to have successfully used ordinary gas
oil or water-gas tar. It is claimed by other operators, however,
that when gas oil is used the paraffin and olefine compounds
in it are likely to contaminate the light oil and that on account
of emulsification this oil soon becomes unfit fur use. Water-
gas tar, it is said, soon becomes too thick for use and soon leads
to serious naphthalene deposits in the distribution system. The
advantages claimed for these materials are their general avail-
ability and lower cost, and the fact that most gas companies
already have adequate storage facilities for these materials.
3 stripping wash on. — To separate the light oils from the
wash oil in which they are dissolved, some form of still is em-
ployed; the difference in boiling points makes possible the
separation. In large plants there are used continuous stills,
in which steam comes in contact with the wash oil and boils off
the light oils. The light oil vapors together with the uncon-
densed portion of the steam ascend upward through a series of
chambers, which will be described more in detail later. In
their ascent they come in contact with descending wash oil
carrying light oils which they assist in freeing. The light oil
vapors together with some steam, naphthalene, sulfur com-
pounds, etc., pass away from the still and are condensed. Some
of the wash oil is also carried along with the light oils, and has
to be separated in the subsequent treatment. In small plants
either continuous or intermittent stills may be used.
4. refining — To obtain from the light oils those constit-
uents which are most in demand, a further separation by dis-
tillation and chemical treatment is necessary. The light oil is
distilled in some form of a still, usually equipped with a recti-
fying column and dephlegmator or planer which will be described
in more detail later. The latter apparatus acts as a partial
condenser in which part of the vapor is condensed and falling
downward through the rectifying column meets the ascending
vapors and washes from them a portion of the high-boiling
constituents. Only the light low-boiling constituents are able
to pass the dephlegmator uucondensed. What vapors shall be
allowed to pass on to the condensers depends upon the temperature
maintained at the dephlegmator. This temperature is regula-
ted according to the particular oil which it is desired to separate
from the light oil mixture at any particular stage of the distilla-
tion. By the use of the dephlegmator and rectifying column
it is possible to obtain much more definite separation of the benzol,
toluol, and other aromatics than would otherwise be possible.
In making the first distillation of the light oil, it is usual to col-
lect the distillate in three successive portions or fractions, mak-
ing the "cuts" at predetermined temperatures. The first frac-
tion is collected in a containing vessel or receiver until the tem-
perature at the top of the still is ioo° C. This fraction is called
crude benzol, since benzol is its chief constituent. The flow of
distillate is then diverted into another receiver and collected until
a temperature of 120° C. is reached. This fraction is termed
crude toluol, from its chief component. The fraction collected
above 1200 C. is called crude solvent naphtha from the use to
which it is put, as a solvent of various materials. The boiling
point of pure benzol and pure toluol are 80 ° and 1 1 1 ° C, respec-
tively. It will be noted that one of the changes of fractions or
cuts is made midway between these boiling points while the boil-
ing point of pure toluol is midway between the other cuts.
That the first separation is by no means complete is shown
by the following analysis, which is typical of a crude toluol
fraction :
Per cent
Benzol HI
Toluol 64.4
Solvent 8.9
Residue, etc 15.6
Totai. 100.0
The above procedure is not universal. Some operators col-
lect the crude benzol and toluol together and subsequently
separate them. Some of the impurities present in the crude
fractions have boiling points so close to those of benzol and
toluol that they cannot be separated from them by distillation.
To remove a certain class of these compounds, called defines,
the fractions are washed successively with strong sulfuric acid,
caustic soda, and water. The defines form a thick, tarry mass,
which settles out by gravity upon standing and is drawn off.
The fractions are then redistilled in stills with very high recti-
fying columns and fractions are finally obtained which boil
within a single degree of the temperatures which have been
determined as the boiling points of pure benzol, toluol, etc.
Some operators prefer to distil the toluol fraction from water-gas
light oils in a still without a rectifying column, previous to final
distillation in a column still. The vapors from the still in this
case pass directly through a condenser coming out in liquid
form. This liquid passes upward through a tank containing
a solution of caustic soda. By this process any sulfonated
defines which remain in the toluol are removed. Otherwise
i!.| In broken up in the column still and have a destruc-
tive action on the dephlegmator and condenser. The condenser
coil and connections of this intermediate still should be made
of lead.
The final distillates are considered as substantially pure ma-
terials if their specific gravities also agree with those which have
been determined for the pure constituents. If, however, the
specific gravity is lower than that of the pure benzol or toluol,
it is an indication of the presence of paraffins, and to ;i
extent the lowering is a measure of the amount of paraffins
present.
u
THE JOl l<\ l/. "/• INDUSTRIAL AND ENGINEERING »' Vol. 10. Xo. i
It is understood that there is no commercially feasibli
separatin tdinthi ca i of toluol, if the amount
2 per cent, tin toluol is unfil for the manufacture of
explosives. Ii i tors that by regulating
I of distillation it i ile to make the
paraffins distil into other than the toluol fraction, even when
pri si in in excess in the crude toluol; but the real remedy is to
adjust the gas-making condition so that the paraffins will not
be produced. It is evident that special knowledge and skill
are necessary from beginning to end of the recovery process.
5. effect on gas QUALITY- -(a) Oil Washing. As has been
stated above, the removal of benzol and toluol from the gas
reduces its heating value and candle power. The amount of
reduction will depend on the original quality of the gas before
washing, the thoroughness of washing, and the process of gas
making employed.
Operators of benzol recovery plants differ considerably in
their opinion as to just what the average reduction would be,
but the general opinion seems to be that the complete removal
of light oils from gas results in reduction of at least 50 per cent
in the open-flame candlepower and from 1 V2 to 8 per cent in
tin heating value (averaging about 5 per cent). Various opera-
tors have endeavored to establish ratios between light oil re-
moval and heat reduction. One operator states that for every
0.1 of a gal. of light oil removed per 1000 cu. ft. of gas, the heat-
ing value will be reduced between 13 and 14 B. t. u. per cu. ft.
and the candlepower between 2V2 and 3 candles. Another
states that the reduction of heating value is 10 B. t. u. for every
0.1 gal. of liquor oil remained.
Mr. J. W. Shaeffer, manager of the Milwaukee Coke and Gas
Co., who has made some studies of the subject, states that the
following expression gives very closely the heating value of oil-
washed coal gas:
I — 35 ''
in which (a) is the heating value of the gas before washing,
(b) is the number of gallons of light oils removed per cubic foot
of gas washed and 35 is the number of cubic feet of vapor per
gallon of light oil. The constant 121827 is the product of 17567
(the heating value per lb. of the light oils;, 7.3 (the weight per
gallon of these oils) and o . 95 (a factor to correct for the amount
of wash oils in the light oil, which is assumed to be 5 per cent).
From calorimeter tests he concludes that the theoretical loss is
practically the same as the actual loss.
(b) Re-enrichment. If it is desired to recover toluol and
still maintain a fairly high standard of gas quality, various
methods may be employed, as follows:
(1) The light oils may be entirely removed from the gas,
fractionated, and the benzol fraction returned to the gas by
some suitable method.
(21 The gas may be only partially washed of its light oils
by the use of insufficient wash oil for complete removal of the
light oils.
(3) All the light oils may be washed from the gas and no
enrichment up to the desired quality be-
ing accomplished by the addition of volatile petroleum distil-
lates.
The decision as to which method should be employed in a
given c.tsc would depend upon nidations. A
partial scrubbing of the was bj Proci ss i would
1111 nt [01 plants which did not tract lit oils, but the
I recovery would be considerably less than in
1 and 3. i ould require the purchase of
petroleum distillates, the price of which might make the method
unprofitable. It is stated by some 0p1.rat.1rs that more distil
lates must be added to gas than the quantity of light oil removed
to compensate for their removal, especially where a candle-
tandard is in tone, since petroleum distillates do not
contribute to thi open flame candlepower to anything like the
extent that benzol does. In order to have the re-enrichment
effective the distillate would have to possess certain qualities.
One operator state-, that it should \olatili/c completely below
1500 C. and have a hi 000 B. t. u. per
lb.
ndard in force iii B given locality would
also, to a considerable extent, determine the method of re-en-
richmenl and the toluol yields 0i.tam.1Me A company which
'nig under a ( i.llcpowcr standard is forced
p. re enrich heavily or to in- satisfied with a small toluol recov-
ery. A lowei standard obviates this difficult]
able extent One operator in a large cits which maintains
a 22-candlepowei standard, states thai a plant now making gas
of that quality could, if relieved of the candlepower requirement,
-till maintain over (,<*> B. t. u. with a recovery of 0.05 gal.
toluol and 0.08 gal. benzol, even though no light oils were re-
turned to the gas. In plants making other gas qualities, the
yields of toluol and effect upon gas quality would, of course,
be different.
Figures as to the value of the light oil- in water gas from
various plants indicate that for medium candlepower gas,
viz., 12 to 17 candles, 0.1 gal. of benzol per 1000 cu. ft. returned
to the gas raises the candlepower about -' candles. The effect
on the heating value in these particular cases is not known,
but it seems probable that Mr. Shaeffer's conclusions would also
apply in these cases. This would give about 12.2 B. t. u. per
cu. ft. as the increase in heating value due to the addition of 0.1
gal. of benzol per 1000 cu. ft. of gas.
PART III CONCENTRATION AND OPERATION OF LIGHT-OIL
RECOVERY PLANT
1. scrubbers — The apparatus in which the gas is brought
into contact with the washing oil is known as the "scrubber"
r In different plants it assumes different forms;
that is, it may be of the rotary type, some form of bubble type,
the spray type, or the tower and hurdle type, this latter being
in use in most of the plants at the present time.
(a) Rotary Scrubbers. A rotary scrubber may be constructed
somewhat as follows: The shell is of cast-iron approximately
cylindrical in shape, with the axis parallel to the floor. It is
divided into a number of compartments by means of plates
which are the full size of the cross section of the shell and which
have circular openings at their centers; a second set of plates
placed alternately with the first reach from the bottom up to
the middle of the shell.
The shell is traversed lengthwise by a shaft, the axis of which
coincides with the axis of the shell, and which is supported by
suitable bearings on the end plates and on the second set of cross
plates mentioned above. On the shaft are fastened gas baffles
in the form of discs made up of wooden slats, there being one
disc for each compartment of the shell, built up so that the gas
can travel between the slats either from circumference of the
shell to the center or vice v<rsa, but not straight across the discs
parallel to the shaft. The central openings of the discs are alter-
nately closed and opened in such a manner in conjunction with
the arrangement of the cross plates that, when the scrubber is
filled with the washing medium to the proper level, the gas is
forced to travel through the upper half of the discs from circum-
ference to center and from center to circumference, alternately.
A small engine, or some other motive power, is used to rotate
the shaft and the attached discs.
The spaces between the slats are very narrow, and thus the
gas in passing through the scrubber flows in thin streams over
surfaces which are kept continually wet as the shaft rotates
by dipping into the washing medium in the lower part of the
shell. The washing medium is admitted to the end opposite
that at which the gas enters, and is carried by suitable overflows
from one compartment to the other until it finally leaves the
scrubber at the gas inlet end. In this way the gas most thor-
oughly washed, comes into contact with the freshest oil.
(b) Bubble-Ty A scrubber of the bubble type
usually consists of a series 1 ae mounted
upon the other, and constructed of cast it section has
a circular opening raised above it- bottom, and covered with a
hood or bell, the edges of which thai
flowing though the opening can pass out onl> under the edge of
the hood, which edge is kept »i tli rashing medium.
Likewise an overflow for thi - provided for
each section. The was enters t!u i ott mi of the washer and,
passing up, bubbles through th( seal of wash oil in each section.
Fresh wash oil is introduced at the top, and tills the top tray
to the height of the overflow pi] h it drains to
the next section. The process 1- therefot ~. arranged that
the gas most nearly washed is brought into contact with the
freshest oil.
•ray-Type Scrubbers. In thi spray-type scrubber the
wash oil eutets the top -, , •, .;criraposed
sections through .1 syphon and pas .raying cone
from which it is hurled by centrifug _h the per-
forations in the cone in a very fini ins tilling the
entire gas space with a mist of wash oil. The oil flows into the
next lowei section through tl .11 brought
into contact with the gas in r tere, finally leaving
the bottom of the washer it ition. The gas
enters from the bottom and passes upward through the succes-
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
5 5
sive washing sections. Power is supplied to the centrifugal
spraying cones by a small steam engine.
(d) "Hurdle-Tower" Scrubbers. The "hurdle-tower" scrub-
bers are the most common type used at the present time; they
usually consist of cylindrical steel shells about 6 to 7 times as
high as the diameter. Two such shells are shown as A and A 1
on the diagram. These shells contain a great number of grids
or trays, commonly called "hurdles," made of white-pine slats
5 or 6 in. high by 1 in. wide. Except for spaces at the bottom
and top of the scrubber these grids are practically superimposed
one upon the other, with the openings staggered, separated by
small spacing strips.
At the top of the tower the wash oil is sprayed in from a num-
ber of nozzles; after passing through the interstices in the grids
it collects at the bottom in a reservoir. The gas enters the tower
at the bottom and rises through the interstices in the grids by
this means coming into intimate contact with the washing
medium. Thus the freshest wash oil, introduced at the top,
comes into contact with the most nearly washed gas.
In one plant designed to scrub about 10,000,000 cu. ft. of gas
per day in which the tower is about 75 ft. high and 1 1 ft. in diam-
eter, there are 84 grids, arranged in 4 banks of 21 each. The
space at the bottom of the tower is about 8 ft. high, that at the
top is about 5 ft. Spaces of about 3 ft. separate the various
sets of trays. In the top are 12 oil nozzles. The foundation of
such a tower is constructed of concrete and extends down about
7 ft. The size of the washer is, of course, dependent upon the
capacity of the plant; 30 cu. ft. of scrubber capacity per 1000
cu. ft. of gas washed per hr. is a figure given by some engineers.
In some plants, notably in those utilizing existing tanks or
towers, the grids are replaced by trays on which coke is piled
or by one tray set near the bottom of the tower on which coke
is piled to nearly fill the tank.
The wash oil is pumped by a circulating oil pump from the
oil storage tank T<y or circulating tank T3 to the nozzles in the
top of the scrubber. From these nozzles the oil is sprayed into
the scrubber at a temperature of 30° C. or lower. When several
scrubbers are required they may be arranged either in series
or in parallel. In the former case the wash oil which has passed
through one scrubber is pumped to the top of the next scrubber
and flows down through this scrubber also. The gas passes
from the top of the first scrubber to the bottom of the second and
up through the second scrubber in the same manner as pre-
viously described. In those plants in which the scrubbers
are arranged in parallel, each scrubber acts as an individual
unit. An additional oil pump is required for each tower scrub-
ber which is being used.
2. heat exchangers — In order to utilize the heat which
would ordinarily be wasted, several pieces of apparatus known
as heat exchangers or interchangers may be used. One of these
is known as the "vapor-to-oil" and the other as the "oil-to-oil"
heat exchanger. Each of these may assume a different form in
different plants, or the order of succession may be different; in
some plants one or the other may be eliminated, and in very
small plants, especially those which are home-made, both are
frequently missing.
(a) Vapor-to-Oil Heat Exchanger. The wash oil containing
the light oils is pumped from the bottom tank of the tower
scrubber to the vapor-to-oil heat exchanger, shown as E on
the diagram. This piece of apparatus usually consists of a
cylindrical steel shell which contains a number of tubes. The
outer shell may be twice as long as it is in diameter; in one plant
designed to scrub 10,000,000 cu. ft. per day it is about 8 ft. long
and 4 ft. in diameter, containing about 150 tubes 2 in. in diam-
eter. The cold bcnzolized wash oil flows through the tubes,
while hot vapors from the top of the continuous still (hereafter
described) pass around the tubes, being directed by a series of
baffle plates. At the outlet of this heat exchanger the tem-
perature of the benzolized wash oil is about 72 °C. A heavy cov-
ering of heat-insulating material aids in the conservation of the
heat. It is understood that this apparatus is controlled by tin
patents of a single manufacturer of recovery apparatus.
(b) Oil-to-Oil Ileal Exchanger. After leaving the vapor-to-oil
heat exchanger, the benzolized wash nil passes to and through
an oil-to-oil heat exchanger, shown as (' on the diagram In
some plants this apparatus 1 an oblong box, in which the hut
de benzolized wash oil from the still pas ' pipe coils,
tin- benzolized oil passing around tin- outside of these coil in
other plants this apparatus is built up of a numl ei oi
tions, joined at the curls. Each pipe contains a number of smaller
1 iii hut de benzolized oil from the base of the still passes
through tin- smaller pipes, tin in nzolized oil passing around them.
The larger pipes are arranged in several banks one above the
other. The banks are connected together at each level, but the
superimposed pipes are connected only in pairs.
In one plant of the size above mentioned this heat exchanger
is constructed of S 10-in. pipes, heavily covered with insulating
material. Each of the large pipes contains 14 '/2-in.
tubes. The overall length is about 26 ft., the height about 7 ft.,
and the width about 3 ft.
At the outlet of this heat exchanger the temperature of the
benzolized wash oil is about 94° C. and that of the de-benzolized
wash oil about 87 ° C.
3. superheater — Passing from the oil-to-oil heat exchanger
the benzolized wash oil enters a superheater, sometimes called
a preheater, shown on the diagram as F. This piece of apparatus
usually consists of a cylindrical tank made of steel, and is about
twice as long as it is in diameter. Inside of the shell are a num-
ber of small tubes, and several baffle plates. The benzolized wash,
oil flows around, and steam passes through the tubes. la
the plant above mentioned this superheater is about 10 ft. in length
and 4 ft. in inside diameter; in this shell are about 160 2-inch
tubes. The superheater is heavily insulated, and owing to great
corrosive action a duplicate is usually provided. ' Likewise, the
parts are so arranged as to be removable without great difficulty.
A safety valve is placed on top of this piece of apparatus.
The temperature of the benzolized wash oil leaving the super-
heater is usually about 145 ° C, although this temperature varies
in different plants.
4. continuous stripping stills — After the benzolized wash
oil leaves the superheater, it passes into the continuous stripping
still, in which the wash oil is freed from practically all of the en-
trained light oils. This still, shown as D on the diagram, is
usually constructed in two main portions — each of which is
built up of superimposed individual sections. The total height
is usually about 4 to 5 times the diameter of the lower portion,
while the diameter of the upper portion is usually three-fourths
that of the lower. Each section is made of cast iron, and is
from 12 to 14 in. in height. The upper portion of the still
usually has about half as many sections as the lower, and acts
as a partial rectifying column assisting in retaining some of the
wash oil in the still, which might go over with the light-oil vapor.
In construction these sections are similar to those described
under the "bubble" type of scrubbers, there being a number of
openings arranged in a circular manner in each section. How-
ever, the edges of the sealing bells are not serrated.
The benzolized wash oil enters the still at the base of the up-
per portion and passes down through the large portion of the
still, rapidly giving up the light oil which it contains. Steam is
admitted at the bottom and passes up through the still, bubbling
from under the sealing bells of each tray and carrying upward
the light oil in the form of vapor from the wash oil which seals
the bells. The steam and these vapors pass through each indi-
vidual section of the still in the manner just described and
mingle in the upper sections of the still with the vapor set free
there.
In one plant designed for 10,000,000 cu. ft. of gas per day the still
is about 27 ft. high. The lower portion is about 6 ft. in diame-
ter and the upper about 4V2 ft. in diameter. The lower portion
consists of about 12 sections and the upper of about 6 sections.
The temperature of the light-oil vapor leaving the top of this
still is about 104 ° C, while the wash oil, stripped of all light
oils, leaves the bottom at a temperature of 1300 C. In some
types of light oil recovery plants, the light oil vapors after
leaving the top of the still column pass through some type of
dephlegmator or planer through which a regulated amount of
cooling water flows so that while the light oils are permitted to
pass uncondensed, the water vapors and any wash oil vapors
present condense out and run into a collecting tank. From this
tank the water is drawn off and the wash oil which contains some
light oil is pumped again with the benzolized oil into the still.
or, if tun heavy to be handled by the stripping still, it is some-
times put into the light oil to be subsequently refined in the crude
still.
5. wash-oil cooler. — The de-benzolized wash oil leaving the
base oi the continuous still passes into the oil-to-oil heat ex-
changer where it b tnpi rature is low end to about 87° C. From
this piece of apparatus the wash oil drains to a hot oil drain
tank, / s. after winch it is pumped through a wash oil cooler,
shown as /i on Hie diagram. This consists of a number of pipe
mils, tin cooling water being showered upon the outside of the
coils, while the wash oil Hows through the inside.
In the plant above mentioned these coils are made up of 2-in.
pipe with return bends at the ends, the whole being about
s«
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEM1 TRY Vol. 10. Xo. r
10 ft. high. At this plant there are 6 of the sets of coolers parallel
to each other.
In some types of recovery plants the wash-oil cooler consists
of pipe coils immersed in a tank of water. This apparatus is
sometimes designated as the temperature regulator, since it
determines the approximate temperature at which the oil is
in i uii i the gas scrubbers.
From these coolers the wash oil passes to a wash-oil storage
tank shown as 7'3, from which it is pumped to the top of the
tower scrubber to again pass through the system.
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In some plants the wash oil may be pumped directly from
the oil-to-oil heat exchanger through the coolers, and into the
wash-oil circulating tank.
6. condenser and separator— The crude light-oil vapors
leaving the top of the continuous still with a temperature of
about 104° C. pass into the vapor-to-oil heat exchanger before
described. From lure they pass into a condenser, shown as G
on the diagram. This condense! is usual] y of cylindrical shape,
being about 21/: times as long as it is in diameter. Inside of
the outer shell are a number of tubes into which the vapors
pass and in which they are condensed to liquid fi >rm by water
passing around the tubes. The light oils leaving the condenser
have a temperature of about 30° C. In the plant under dis-
cussion this condenser is about 9 ft. long and 4 ft. in diameter.
In many large plants it was found advantageous to install
a pipe connection with a small blower or steam jet between
the outlet of the light-oil condenser and the outlet of the last gas
scrubber. By this means a considerable amount of non-con-
densable olefines leaving the stripping still may be returned
to the gas, thereby re-enriching it to a considerable extent.
From this condenser the light oil enters a separator, or de-
canter, shown as H on the diagram. Here any water entrained
in the light oil is decanted or separated, due to the difference
in specific gravity. This piece of apparatus usually consists
of a small cylindrical shell provided with 2 outlets, one for oil
and one for water. The water connection extends down inside
of the shell nearly to the bottom, the oil outlet being near
the top. The water passes off to a sewer and the crude light oils
pass either to a crude light-oil storage tank, shown as 7"6, or di-
rectly into the crude rectifying or "boiler" still, if the plant is so
arranged as to do away with this tank.
7. crude rectifying stills — From the crude light-oil
storage tanks, the crude light oil is pumped into the crude
rectifying still, or boiler still. This still is composed of 3 parts, the
boiler, shown as / on the diagram, the rectifying column,
and the dephlegmator L.
The boiler still consists of a cylindrical shell having bumped
heads, internally braced; it is designed to handle from 5000
to 12,000 gal. of crude light oil, according to the size of the
plant. The shell is covered with insulating material in order
to reduce heat losses. The distillation is carried out by the use of
live steam, this being introduced into coils placed in the bottom
of the still. There is also a perforated pipe in the bottom of
the boiler so arranged that live steam can be utilized to aid in
the distillation, although this latter is not frequently made use of.
Vacuum connections are also provided so that the distillation
may be aided in the latter part of the cycle.
In a plant designed to wash 10,000,000 cu. ft. of gas per
day this still, designed to handle a charge of 5,000 gal. of crude
light oil. is made of steel, 7 ft. 6 in. in diameter and 16 ft. long,
overall. The steam coils are made of 2-in. pipe, and a ball
and lever safety valve is attached to the shell.
The crude light oils are pumped into the boiler still until
lis capacity is reached, the distillation being carried out at
the temperature previously described (see p. 53). The residue
which remains in the still is known as the still residue, and con-
sists of wash oil, naphthalene, etc. It is drained to the naphtha-
lene pans which are described later.
After the charge is fractionated a fresh charge is placed in
the still The time required to complete a run varies; in some
plants 40 hrs. are required while in others 24 hrs. are deemed
sufficient,
The vapors from the still pass into the rectifying column,
shown on the diagram, as they are distilled off. This col-
umn consists of a number of cast-iron sections, mounted one
upon the other, each section being from 12 in. to 14 in. in thick-
ness. It is mounted upon the top of the boiler still close to
one end, and is usually about 3 times as high as it is in diameter,
being heavily lagged with insulating material. In construction,
each section is similar to those already described. There are
openings in each section, the covering bells having their
edges serrated. The vapors rise through the openings and bub-
ble through a seal composed of the heavier portions of the de-
scending oils, which are condensed in the dephlegmator and
which drain back down the rectifying column.
In this plant this rectifying column is about 1 2 ft. 6 in. high
and 4 ft. in diameter, and is built up of 10 sections.
Mounted on top of the rectifying column is the dephlegmator
or planer shown as L on the diagram Here the vapors rising
from the rectifying column are cooled by a circulation of water.
The heavier portions condense and drain back down the recti-
fying column as before described.
The dephlegmator usualrj a i>ox-shaped shell
about two thirds .1- huh and » it lining a num-
.itei tubes. Baffles direct th< . of the vapors
through the dephlegmator. In this pi ni the dephlegmator
is about 5 ft 6 in. long and 3 ft. 6 in and it con-
tains about 14S water tubes each 1 r.eter.
In another plant one rectifying column am dephlegmator is
provided for two boiler stills. By this means a continuous flow
of light-oil vapors is obtained.
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
57
In some cases the crude rectifying still and stripping still
may be combined. In plants producing from 15 to 40 gal. of
light oil per hour (about 1 to 3 million cu. ft. of gas per day) it
may be found advantageous to have the stripping still of such
size that it can strip in say 16 hrs. all the benzolized wash oil
produced in 24 hrs. and to have such accessories to the still pro-
vided that it can be used as a crude rectifying still during the
remaining 8 hrs. of the day. When a still is to serve both
purposes it should usually be equipped with some form of de-
phlegmator, or planer, and with an auxiliary still base which
can be valved off and used as a light-oil storage tank while the
still column is stripping wash oil. This still base is equipped
with closed steam coils and a live steam connection and is so
connected with the still column that when in use rectifying light
oil, it corresponds in effect to the boiler part of a regular recti-
fying still. In plants producing more than 40 gal. of light oil
per hour it would probably be more practicable to have entirely
separate rectifying and stripping stills. In plants producing
less and probably in some producing more than 15 gal. of light
oil per hour when advantageously situated, it would usually
be impracticable to attempt fractionation of the light oil at all
at the gas works.
8. naphthalene pans — The still residue, containing wash
oil, naphthalene, etc., is drained from the bottom of the boiler
still into the naphthalene pans, shown as Z on the diagram.
Here the naphthalene separates out on cooling in the form of
crystals and the wash oil drains back to the circulating wash-
oil tank. The naphthalene may be further dried by using a
centrifugal machine.
In plants scrubbing the light oils from water gas, no naph-
thalene will usually be encountered.
9. condenser and separator — The benzol, toluol, and sol-
vent naphtha vapors leaving the dephlegmator enter a con-
denser, shown as M on the diagram. This is a cylindrical
tank about 3 times as high as it is in diameter. Inside are a
number of tubes through which water circulates; a series of
baffle plates direct the flow of vapor around the coils. In this
condenser the various light-oil vapors are condensed into liquid
form.
In the plant above mentioned this equipment is about 8 ft.
6 in. high and 3 ft. in diameter, and contains about 90 tubes,
each 1V2 in. in diameter.
From the condenser the benzol, toluol, etc., pass to a water
separator, shown as N, which is similar to the one described
above.
10. receivers or sampling Tanks — From the separator the
benzol, toluol, etc., drains into one of two receivers, shown as
O and Oi on the diagram. These are small graduated cylinders
of about 100-gal. capacity, and are used as sampling tanks.
One may be filling while a sample from the other is being tested
to determine its character.
From these receivers the crude benzol, toluol, or solvent
naphtha is drained into the proper one of the crude storage
tanks, shown as Ti, T8 and Tg on the diagram.
1 1 . agitator — If the plant is one which produces chemically
pure products, the crude benzol, toluol, or solvent naphtha is
pumped from the crude storage tanks into an agitator shown
as Q on the diagram. This agitator consists of a large lead-
lined, vertical, cylindrical, steel vessel nearly as high as it is in
diameter. It has a conical bottom, and contains power-driven
paddles. In one plant the agitator is about 8 ft. in diameter
and 6 ft. high.
In the agitator the benzol, or toluol, etc., is washed with
sulfuric acid, which is supplied from a small storage tank
shown as Ri. The paddles are located at a height which
permits of discharging the acid in the bottom of the washer
near the level of the benzol or toluol, and the distribution of it
in such a manner as to obtain a thorough mixture. This mixing
or washing is carried out for 30 to 90 min., after which the agi-
tator is shut down and about 30 min. are allowed for the used
acid to settle to the bottom of the agitator. The acid is used
to separate the unsaturated hydrocarbons, principally olefines,
which settle with the residue to the bottom of the agitator.
The sludge is run off and the acid contained in it is regenerated
for further use. The benzol or toluol is washed with water,
after which a caustic soda solution is run into the agitator to
neutralize any remaining traces of the acid in the benzol or toluol.
This latter solution is stored in the tank shown as R2 on the dia-
gram. After properly mixing with the light oil the soda is al-
lowed to settle and is then drained off, the benzol or toluol be-
ing again washed with water to remove any traces of caustic
soda. From the washer the washed benzol, toluol, or solvent
naphtha drains into the washed-oil tanks, shown as 7*io, T11,
and 7"i2.
12. rectifying still — From these tanks the washed benzol,
toluol, or solvent naphtha is pumped into the pure rectifying
still. This still consists of three parts: the boiler still, shown as
5 on the diagram, the rectifying column U, and the dephleg-
mator V. Each of these three parts fulfills the same function
and is similar in construction to those described for the crude
rectifying still. However, the rectifying column is usually
about one-half again as high as that on the crude still, in order
that closer fractionation can be accomplished. If benzol is
introduced into the still, pure benzol is distilled over at a tem-
perature between 80 and 81 .5 ° C. If toluol is introduced
into the still, pure toluol will distil over between no and
1 1 1 . 5 ° C. The time of distillation is usually about 5 times as long
as in the crude still, and the size of the still is usually greater.
The residue is usually returned to the tanks containing the
washed products while the vapors leaving the dephlegmator
pass through a condenser, shown as W on the diagram, and then
through a water separator, shown as X. These two pieces of
apparatus are similar in all respects to those described above.
From the separator the "C. P." benzol, toluol, or solvent
naphtha is run into one of thre<> sampling tanks, shown as Ki,
Y2, and Y3, similar to those marked 0 and Oi, after which it
passes to the pure tanks, shown as T13, T14, aud T15.
13. location relative to existing plant — The relative
position occupied by the light-oil recovery plant in reference
to the remainder of the manufacturing plant varies in different
localities. In some plants, the washing of the gas takes place
before the gas goes to the purifiers, while in others after the
gas passes the purifiers. However, in any plant in which quan-
tities of tar and ammonia are produced, the oil washing of the
gas should take place after the tar and ammonia are removed.
The relative arrangement of the equipment depends largely
upon the existing manufacturing plant. If possible, it should
be close to the necessary steam and water supplies, and all of
the parts should be so arranged that there would be only the
minimum of all classes of piping required.
14. space required — Sufficient space is required for the
necessary number of tower scrubbers, if the plant is to be of this
type; for the building to house the stills, pumps, and other
necessary accessories; and for the storage and circulating tanks
and other outdoor equipment. The entire recovery plant
should be in as compact form as possible, yet should not be too
crowded.
The amount of floor space which is required for the building
in which the stills are located, and in which some of the acces-
sories must be placed, depends largely upon the products re-
covered and the daily capacity of the plant. Sufficient floor
space must be provided for the stills, and the pumps should
also be provided for, in estimating the amount of floor space
required. It is possible to put much of the remaining apparatus
at a higher level, thus economizing in floor space.
It is impossible to state with any degree of exactness the
floor space requirements, but in several plants, from 2400 to
3000 sq. ft. of floor area are required for the recovery of "C.
P." products. In another plant 1200 sq. ft. are required for
the recovery of crude benzol, toluol, etc.
15. storage of materials — The question of storage of ma-
terials, viz., wash oil, both benzolized and debenzolized, the crude
light oil produced in the continuous stripping still, the crude
benzol, toluol, solvent naphthas, etc., the refined products if
plant carries the process to this extent, is one which must be
considered carefully. Lack of adequate means of storage often
means the discontinuance of the plant, unless it is possible to
utilize some other equipment in the plant.
In all plants an extra supply of wash oil must be stored. It is
advisable to have as a reserve from one-half to the full amount
of wash oil circulated through the system in one day. This pref-
erably should be stored in one tank, which should have a capac-
ity at least equal to twice that of a tank car so that the unload-
ing of incoming cars may be done promptly. It is also advisa-
ble to have sufficient tank capacity for all the wash oil being
utilized in the system, one-half for the benzolized wash oil and
one-half for the de-benzolized wash oil.
It is also necessary to provide a tank for the light oil recov-
ered from the continuous still. This tank should have a capacity
equal to that of the fractionating still unless there are two frac-
tionating stills with one rectifying column, as is the case in
some plants. If the plant is not equipped for fractionating the
light oil, sufficient storage capacity to tide over any interrup-
tion of shipping facilities should be provided ; it is suggested that
capacity for a week's production should be available, but where
practicable the capacity should be not less than twice that of
an average tank car.
58
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CEEMIl TRY Vol. 10, Xo. t
If tin- plant recovers crude benzol, toluol, etc., bul di
further Fractionate these, sufficient toragi capacity should be
i led 1 the crude fractions, so thai no dan
ger of a lack oi toragi will bi met in everal plants the stor-
age capacity for benzol is about twice thai ol thi toluol, solvents,
etc. It is suggested that capacity for a week's oiitp.it of each
of these liquids be provided. If the plant produces "C. P."
products, sufficient storage capacity Foi tch o thi crude liquids
should lie provided, so that the pure still will be able to operate
long enough to refine the preceding crudi
The C. 1'. benzol, toluol, etc., likewise requires sufficient
storage space so that if any interference with shipments occurs
it will not be necessary to curtail the operation of the plant in
any way. Here also the benzol storage should be about twice
that for the toluol. In addition, in a C. P. plant storage must
be provided for the sulfuric ai id, As a summary, approximately
Mi; torage capacity indicated is required for the following
materials:
When crude liuhl oil only is recovered:
Old wash oil de-benzolized
Bqual to one-half the amount in circulation.
u|, I wash oil l,i-nzolized
Equal lo one-half the amount in circulation.
New wash oil
From one-half to full amount in circulation, at least 2 car-loads.
Crude li
Equal to capacity of crude still,
large enough to avoid difficultie
least 2 car-loads.
When crude benzol, toluol, etc., are recovered:
Same as above and
Crude toluol
Crude benzol
Crude solvent naphthas
Heavy naphtha
Crude intermediates
Henzol storage about twice as great as other fractions.
If further refilling is done, should be large enough to allow refining
stills to work necessary time. If no refining', tanks should be
large enough to avoid difficulties caused by shipping delays.
When C. P. products are recovered:
Same as previously stated, and
Washed benzol
Washed toluol
Washed solvent naphthas
Henzol about twice as great as other fractions.
Sufficient capacity to allow refining still to operate requisite length
of time.
Sulfuric acid
Pure toluol
Pure benzol
Pure solvents
Henzol about twice as great as other fractions.
> nough to avoid difficulties caused by shipping delays.
In addition, one or two spare tanks would be advisable.
Tin- location of these tanks is largely dependent upon local
conditions. In some plants they are placed underground, in
othei plants they are located in water-tight pits, while m still
other plants part or all of the tanks are above the ground sur-
face. They may be grouped together or they may be
into dilTi largely depending on the amount of avail-
able spai e. or local lire regulations.
[6 SAFETY IN OPERATION— The buildings for a light-oil re-
covery plant should lie located as far as practicable from other
plant structures; or if sufficient distance is not obtainable,
owing to existing conditions, the building should i« n
individual unit, by bricking up or otherwise closing all openings
into adjacent buildings I adei any conditions, .t is desirable
that the still be located al out 21 0 ft. from any source of flame,
since the heavj benzol vapor is quite prone to travel along the
ground 1 iderable distance without dilution to a suffi-
cient device lo prevent inflammability.
The buildings should be constructed of fireproof material
throu bout, and should be well ventilated and equipped with
ind metal lire doors. If practii
should bi located awaj from railroad tracks or sidings, and the
ra should bi removed as far as practicable from
■ ■ t (1m plant
No open Barnes should I" brought neai any portion of a light-
oil reco\ 1 1 v plan! . and 1 encased
teeth e w iie casing around
the globe, should be used ai of a light-oil
plant hi ease portable lights are required, small stoi
tery light should i» used All electric wiring throughout the
plant houid be encased In iron pipe conduits, and no extension
cords should be used
\ sufficient numbei of fire extinguishers, of the type capable
of extin • and buckets containing clean, dry
sand shoul not only inside of the build-
ing, but also outside. A plentiful supprj of water, under
in h pressure, should also be readilj
efficient corps of nun. trained in fire extinguishing, should
be available at all times
Smoking should not be permitted in or near the light-oil
plant at any time.
All stills and superheaters should be equipped with a positive-
safety valve set to blow at about 10 lbs. pressure. Likewise
all tank cars and tank wagons should be equipped with safety
valves. All tanks should vent to the atmosphere, the vents
being provided with a screen of fine wire in order to prevent the
ignition of the vapors by sparks.
All joints in the piping, stills, tanks, or any other apparatus
should be kept tight so that leaking vapors do not accumulate
in the buildings or their vicinity. All condensers should be sup-
plied with adequate cooling water to prevent the escape of
vapor into the air.
When necessary to clean stills special precautions are neces-
sary to prevent the workmen from being asphyxiated. Xo one
should enter the stills until they have been thoroughly purged
of all vapors and are cool. All connecting valves should be
closed and locked, and if the valves are not tight, the piping
should be disconnected. At least two openings should be main-
tained in the still to allow a circulation of air throughout. The
man entering should be provided with a life belt and rope and
another man should be stationed outside of the still to assist
in case of necessity. He should obtain additional assistance
before entering the still to aid the man overcome by the vapors
in the still.
17. TECHNICAL control — In the operation of a light-oil re-
covery plant, in order to obtain efficient results and good quality
of product, an adequate laboratory equipment must be main-
tained and at least one observer, skilled in making the neces-
sary tests, must be employed. The extent of the tests in a
given plant will depend upon the final products produced by
the plant. Obviously a plant producing pure benzol, toluol,
etc., will require much more elaborate tests than a plant selling
unrefined light oil only.
The following is a list of tests usually required in the opera-
tion of a pure products plant as furnished by the Chief Chemist
of a large operating company:
A— Tests of Gas
1 I iting value and candlepower of gas entering scrubber.
(2) Determination of light oil in gas entering scrubbers.
(3) Heating value and candlepower of gas leaving scrubber.
(4) Determination of light oil in gas leaving scrubbers.
B — Tests for Wash-Oil Still Operation
termination of light oil in benzolized wash oil.
(2) Determination of light oil in de benzolized wash oil.
(3) Tests of the light oil
'j. Boiling point
b. Determination of wash oil.
C — Tests for Crude Still Operation
(1) Receiver tests; i. e., boiling-point tests made to control frac-
tionation.
(2) Boiling-point tests of fractions (crude benzol, crude toluol, etc>
and residues sampled from their respective storage tanks.
D — Tests for Agitator Operation
istillation and acid tests of washed benzols.
(2) Tests for S< benzols.
(3) Specific gravity of regenerated sulfuric acid.
E— Tests for Pure Still Operation
(1) Receiver tests; i. e., boiling-point tests made to control fractiona-
tion.
a. Boiling Point.
b. Acid lest.
(2) Tests of pure products sampled from storage or running tanks or
from shipin
a. Boiling Point.
b. Acid test
,-. Specific Gravity.
d. Freezing Point (occasional in case <
(3) Boiling-point tests of still residues.
F— Tests of Materials Used in Operation
:,!l dil.
Specific Gravity.
b. Vi
•■tv
ition.
d. Cole.
illation.
\cid — Specific Gravity,
It is evident that in a plant shipping light oil away for further
refining, many of these tests could be omitted In a very small
i.r the routine was ,] tcsts'on gas
before and alter scrubbing and of the wash oil and light oil
would probably suffice
IS. ADAPTATION OP LIGHT-OIL RECOVERY ro SMALL PLANTS
While the somewhat complicated system of I 1 hangers and the
careful design of stills, described in connection with the layout
of ,1 typical light-oil recovery plant, an vi important in ef-
fecting economy of operation, the) are not absolutely essential
to tin recover] of tins material. equipment of a
small plant recovering only light oils consists of some form of
scrubber to oil wash thi . the wash oil.
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
59
a condenser for condensing the light oils, and some tanks for the
storage of the various materials. A plant which is so fortunate
as to possess or to be able to obtain cheaply some old gas making
or power-plant equipment might find it profitable to construct
and operate a small plant. An old ammonia washer, water-gas
scrubber, shavings scrubber, or even an old water-gas genera-
ting shell could be readily adapted for use as an oil washer by
filling with wood grids, coke, or other materials which would
furnish a large surface wet with the wash oil for contact with
the gas. For a stripping still, an old boiler surmounted by a
section of large diameter pipe filled with stones could be used
and the process made an intermittent one. In this case tanks
would, of course, be necessary so that a portion of the wash oil
could be circulated while another portion was being de-benzol-
ized and cooled. An old feed-water heater of the type in which
the exhaust steam comes into direct contact with the cold water
might be used as a continuous still, by connecting the top of it
with a condenser of some kind and admitting the wash oil near
the top and live steam near the bottom. For a condenser, a
coil of pipe in a tank of water, an old closed coil-feed water heater,
or similar apparatus, might be used. In such an improvised
plant no fractionation of the light oil would probably be feasi-
ble. The light oil would be shipped to a larger plant or to a
benzol refinery. In a simple plant of this kind the cool wash
oil would be pumped from its storage tank to the top of the
scrubber. From the bottom of the scrubber the benzolized
oil would flow to a storage tank from which it could be pumped
to the still. The hot de-benzolized oil from the still would be
run into a storage tank to cool while another portion of benzol-
ized oil was being distilled. After cooling, it would be again
circulated through the scrubber. A fourth tank would be
necessary for the storage of the condensed light oil. If sufficient
old materials were available it might be possible to construct crude
heat exchangers which would improve the economy of the plant.
Whether or not a given small plant should attempt to make
crude fractions would depend upon local conditions. In general,
it does not seem practicable for a plant producing less than
1,800,000 cu. ft. of gas per day to do so.
It would hardly be expected that a simple plant of crude con-
struction would recover the benzol as completely or economically
as a large well-designed plant, but a large number of such plants
would increase the total benzol and the toluol resources very
materially.
In the small plant as well as in the large one all reasonable
precautions should be taken to make the operation safe both
to the operators and to the plant in general. The highly in-
flammable character of the materials handled and the explosive-
ness of the vapors when mixed with air should always be guarded
against. The benzol plant should be located where in case of
fire it will not endanger the rest of the plant. The fact that old
equipment is used in the construction should put the operators
on the outlook for leaks, which occur more or less frequently
even in well-constructed plants.
19. TIME REQUIRED AND COST OF PLANT INSTALLATION — -The
time required for the construction of light-oil recovery plants
seems to vary greatly. The two essentials to normal construc-
tion are sufficient labor to conduct the work in an expeditious
manner, and the necessary material either at hand or arriving
at a steady rate to carry on the work in logical sequence. In
this period of shortage of efficient labor and of congestion
of shops and railroads, the period of construction may be
prolonged far beyond the normal period or it may perhaps even
be halted. Of course the amount of construction and the clear-
ing and preparing of the site necessary are large factors in the
length of the construction period even in normal times.
If there is no difficulty in obtaining labor and material a plant
to scrub about 10 million cu. ft. of gasper day should take approx-
imately, 3 to 4 mo. to build. One such plant, recovering C. P.
products, actually took 6.5 days to build. Another plant, re-
covering crude benzol, toluol, etc., took about 4 months to build.
One plant of home-made construction throughout, and scrub-
nit three-fourths of a million cu. ft. of gas per day, pro-
1 rude light oil only, took 35 days to construct and put
1 ation
To present any definite figures as to the cost of installing a
plant for the recovery of light oils is impossible, '["his is par-
ticularly true at the present time, when the price of labor and
1 teadily mounting. Bach plant must lie figured
as a unit, and the cost is dependent upon a number of factors
each individual plant. If tin- plant is to
tructed of appa ,. <l for the specific purpose, and prac-
tically oo old equipment is utilized, it will, of course, cost more
than sui b a plant utilizing existing equipment,
■ if the plant, the completeness of recovery, Un-
available steam supply, and the available supply of condensing
and cooling water are factors which must be given considera-
tion in any estimate. The steam and water supply capacity
especially should have very careful consideration since the re-
quirements of a benzol recovery plant for steam and water
are very considerable. Likewise, the location of the plant with
reference to the source of material supply is of importance.
Among a number of plants visited no agreement as to cost
was obtained. The figures were, in most cases, only approx-
imate, and therefore no great reliance can be placed upon
them. The year in which the plant was constructed also had
a great bearing on its cost.
For example, one plant scrubbing about 1 1 million ft. of gas a
day, and recovering C. P. products, is said to have cost about $200,-
000, while another plant scrubbing about the same amount of
gas, but recovering only crude products, is said to have cost
about $225,000. Still another plant scrubbing only 4V4 mil-
lion cu. ft. of gas a day, and recovering C. P. products, is said
to have cost about $200,000.
In one plant where some existing equipment was utilized 7
million cu. ft. of gas a day is scrubbed, light oil in the crude
only being recovered; the cost is said to have been $25,000.
Another plant, utilizing some old equipment, and scrubbing
about one-half million cu. ft. of gas per day, producing only
crude light oil, is said to have cost about $40,000. Another
plant, made from odds and ends without heat exchangers or any
other such devices, and with only a few pieces of apparatus bought,
is said to have cost about $10,000. This plant scrubs about
650,000 cu. ft. of gas per day.
From the above examples it will be seen that it is impossible
to draw any general conclusions as to the cost of a light-oil re-
covery plant. However, it will be seen that an efficient plant
costs several hundred thousand dollars, but that the cost may
range considerably lower for plants constructed from existing
equipment, depending upon the amount of such equipment
used.
20. ITEMS ENTERING INTO COST OF LIGHT-OIL RECOVERY The
Bureau is unable to give any estimate of the cost of light-oil
recovery. This would necessarily vary greatly in different
localities. We can only indicate some of the principal items
which enter into the cost. These items are raw materials,
steam, water, electric power, wages, overhead expenses, fire
insurance, maintenance, depreciation, and in some cases cost
of re-enriching the gas to the prescribed standard of quality.
The materials include wash oil, lubricating oils, packing and
repair materials; and in plants producing pure products, sulfuric
acid and soda are also needed. The wash oil consumption
varies considerably in different plants, depending upon the kind
of gas washed, the tightness of the circulating system and the
method of operation. While wash oil does not enter into the
final product, replacement is necessary at regular intervals,
due to losses, depreciation of quality, etc. Some operators re-
place a certain percentage of wash oil each day while others re-
place the whole amount at stated intervals. The percentage
of loss varies greatly. Operators claim a replacement of wash
oil all the way from 2 to 10 per cent of the number of
gallons of light oil recovered. Prices of wash oil at the present
time range, according to information available, from 7V2 to 12
cents per gallon. These prices are continually changing, so no
definite figure can be assigned.
In a pure product plant, sulfuric acid and soda are necessary
for washing the distillates. The amounts used by various opera-
tors differ and are, of course, dependent upon the amount of
the various constituents which must be washed out of the prod-
uct. An average figure seems to be from 0.3 to 0.5 lb. of sul-
furic acid per gallon of light oil produced, and about '/io as much
soda. Some operators give the amount of sulfuric acid re-
quired for washing the crude toluol as 0.8 pound per gallon
of the toluol treated. The present price of acid was stated as
about 4 cents per lb. and soda at about 8 cents per lb., making
the cost of the materials about 1.6 cents and 0.3 cent, re-
spectively, per gallon of light oil produced.
No figures are available as to the cost of lubricating oils for
the numerous pumps, packing, gaskets, etc., but from the
nature of the materials handled it seems likely that these ex-
penses are rather heavy.
The consumption of steam, cooling water, and electric power,
varying according to local conditions and the cost of the separate
items are, of course, variable. The steam consumption for the
and accessories alone is estimated by various operators
as from 40 to 65 lbs., or even more is omi cases, per gallon
Of light "il produced. The consumption depends largely upon
lent 1.1 which the heats of the still 1 fflui n1 and distillate
are utilized to heat the incoming benzolized oil. One operator
6c
THE JOURNAL OF IX DUST RIAL AXD ENGINEERING CHEMISTRY Vol. ra, Xo. i
who recovered crude fractions only from 14 million cu. ft of
lean by-product oven gas per day, stated that his steam consump-
tion was about 65 lbs. per gallon of light oil, distributed as
follows:
Pounds
Stripping still 14.2
Superheater 48.8
Crude still 2.0
Total, 65.0
In this case there was no vapor-to-oil heat exchanger in use
ami the oil-to-oil exchanger was an improvised apparatus.
The lower figure, 40 lbs. per gallon, was quoted by the operating
ti ndent of a chain of several plants as the requirement
of the stills and accessories Xo estimate could be obtained
ti am consumption of the various pumps in these plants.
In many cases there seems to be no careful record kept of these
items. In one plant washing about 12.5 millions cu. ft. of
mixed gas per day, and producing pure products, it was stated
that 250 boiler horse power was required for the entire recovery
plant. As this plant produces about 3100 gallons of light oil
per day, this would be equivalent to about 57 lbs. steam per
gallon, assuming that the boiler horse power used was correctly
estimated. One operator having several plants under his super-
vision gives 8 to 9 lbs. of steam per pound of pure products as an
average figure in a plant having two heat exchangers. The
question of installing elaborate heat exchangers in a given case
to save steam must be decided by local conditions. If the cost
of steam production in a plant is very low it may not be ex-
pedient to install all the equipment necessary' for the fullest
utilization of the waste heat In a small plant, especially, it
might not be feasible to install all this equipment and the use
of steam could hardly be expected to be as low per gallon of
product as in a larger plant.
The water used in a light-oil recovery plant for cooling pur-
poses is also a very important item. In order to obtain efficient
scrubbing of the gas the wash oil must be cooled to 300 C. or
uts. and the conden hlegmators must have
an adequate supply of cooling water or light-oil vapors will be
lost. The amount of cooling water used will depend to a great
extent upon the temperature of the water supply. A plant which
is so fortunate as to have a supply of very cold water will be
able to use considerably less than a plant in which the water
is relatively warm. A requirement of about 60 gallons of cool-
ing water per gallon of light oil produced seems to be an average
amount. One operator of several plants gives 1 r gallons of
water per gallon of wash oil circulated as an approximate figure.
A plant which is favorably laid out may find it possible to utilize
a portion of the cooling water for other purposes after it has-
passed through the coolers; much water may also be saved in
some cases by recirculating. The cost of cooling water will in
be a controlling factor and will determine how elaborate
th.e layout with a view to savinj water Water cam
be used for cooling in many cases which would not be fit for boiler
feed unless treated. In contemplating any light-oil recovery
installations, especially in a small plant, one of the first con-
siderations should be the adequacy of the existing steam and
water supplies.
The labor expense in operating a benzol plant is a variable-
item for which only an approximation can be given. In start-
ing a plant and establishing a routine a larger force is required
■ r the plant is under regular operating conditions. A
superintendent who has general charge of the operation of s vera!
plants states that the regular opera' ing force for a plant pro-
ducing crude fractions consists of seven men during the 24 hrs.
lay, assuming that each man works an eight-hour shift.
Of this force one man should be a technical man who under-
stands the testing connected with the process. The actual
operators are men of average attainments, usually of the same
degree of skill as water-gas makers.
In some plants where very crude fractionations are made
even a smaller force is sometimes employed, though whether a
smaller force could carry on the process efficiently is questionable.
In one coke-oven plant washing 14 million cu. ft. per day it was
stated that the actual operation of the recovery plant required
ordinarily only 2 hours of one man's time on each 12-hr. shift
and about 6 hrs. of a chemist's time in 24 hrs. It was also stated
that the operation of the recovery plant was much less trouble-
some than the operation of the ammonia equipment of the same
plant.
No figures were obtainable which would permit even a rough
estimate of the overhead expenses, fire insurance, maintenance,
and depreciation of a light-oil recovery plant Frederick H.
Wagner, in his book entitled "Coal Gas Residuals," published
in 19,14. allows 10 per cent of the original cost of the plant to
cover these items We have no information to substantiate or
disprove this estimate. In view of the uncertainty of the benzol
and toluol market in the future and the fact that it might not be
profitable for city gas companies to recover benzol and toluol
without the exceptionally high prices for these products now
prevailing, especially if re-enrichment of gas were necessary,
it seems as though a value of to per cent would be much too low
an estimate for a company to safely calculate upon.
ADDRL55L5
CHEMICAL MICROSCOPY1
By E. M. Chamot
A speaker who has the temerity to address a joint meeting of
two different technical societies always finds himself in an awk-
ward predicament. He feels that he must present his subject
from the viewpoint of each group of men, that he must lay equal
emphasis upon all branches of the sciences represented by his
audience. I find myself very much embarrassed, realizing this,
and in doubt whether I am here in the guise of a microscopist or of
a chemist
This, gentlemen, is the introductory paragraph of the paper I
had originally prepared. Since that time we have entered the
-tea' w.u and I know where I stand. I come to you as a chemist
to make an appeal for a wider and more intelligent application of
the microscope in every day chemical pi u
If the talk appears rambling and fragmentary I trust you will
bear with me, for with several momentous issues in the hands of
my department 1 have had little opportunity to prepare a new
paper and none to make new lantern slides. I will, however, at-
tempt to stick to my text — -Chemical Microscopy. To my mind
there is no such thing as microchemistry as opposed to macro-
chemistry, and the term microchemical methods is a misnomer.
1 Ailtlrcss delivered before a joint meeting "f the Chicago Section of
the Aiiu-ii. Society and t'> Soccty of
Illinois, at the City I A V. H.
Mory. Chairman of the Chemical Society, and N. S. Amstutz. President
of the Microscopical Society, pn
A microchemical reaction or test may be one performed upon
minute amounts of material without necessarily having recourse
to the microscope.
Chemical Microscopy, on the other hand, requires that some
type of magnifying optical instrument enters into the work. By
chemical microscopy, therefore, we mean simply the appli-
cation of microscopic methods to the solutions of problems
arising in the chemical laboratory or in the chemical industries.
No instrument at our command can do so much or throw so
much light upon obscure problems with so little an expenditure of
time, labor and material. We chemists have been wasting golden
hours and slaving over sloppy methods to accomplish ends which
could have been reached easily and leisurely and with a degree of
certainty unsurpassed by anything we have had at our command
with test-tubes and beakers. Why spend hours upon a qualitative
analysis that can be better done through the medium of the
microscope in several mini:
The time has come w hen we can no longer 1 >e satisfied with time-
consuming operations. Industries must be speeded up, produc-
tion increased, better inspection methods introduced, quality
1 aised and final cost inconsequence reduced. I am simply
preaching good conservation. If we fail in th 1 ar and disappear
as a nation it will be because we have failed in our industries to
produce the necessary material and the requisite quality. I can-
not recall a single great industry to day where microscopic methods
intelligently applied will not lead tp more or less marked improve-
ments.
Jan., 1918
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
61
MICROSCOPIC METHODS NOT APPRECIATED
The causes of our failure to fully appreciate the value of micro-
scopic methods are not hard to find. In the first place, in the edu-
cational system of our chemists no adequate training has been
given in the multiplicity of uses of the microscope and its poten-
tial industrial applications. In the second place, too much em-
phasis has been laid upon biologic microscopy, so that the gen-
erally accepted view is that this instrument is intended for
studies in biology or medicine. As a result, the development of
the modern so-called high-grade microscope has followed strictly
biological lines and has drifted farther and farther away from
stands applicable for general work in the chemical laboratory.
For example, the best of our present-day stands no longer have the
mirror mounted upon a swinging bar capable of movements far
to one side, or even above the stage for oblique illumination. In
refractive index work, in the observation of melting points, in
the study of fatigue failure in metals, in the general examination
of alloys, cements, protective coatings, etc., and in the prepara-
tion of photomicrographs of certain preparations, this old device
now abandoned is really essential, and it is necessary to remove
the mirror from the stand and fasten it to a holder of some sort
in order that it may be properly employed.
It is also unfortunate that the objectives of small angle, long
available working distance and marked penetrating power are
not obtainable save at second hand. The modern microscope ob-
jective is a marvel in its performance, yet it is limited to the study
of mounted materials covered with a standard cover glass if over
a moderate power is required for the examination; but, unfor-
tunately, we chemists must work with uncovered preparations
and we must sacrifice resolving power for penetrating power and
for stereoscopic effects. We need instruments of moderate cost,
substantially built, and which will withstand the corrosive atmos-
phere of most of our industrial laboratories. Thus the third
reason for the backwardness of chemists to use the microscope has
been the lack of suitable models and accessories. Even our good
friends and near chemists, the petrographers, have never gone out
of their narrow way to try and impress the chemist with the fact
that the polarizing microscope is an indispensable adjunct of the
research laboratory. The modern petrographic microscope is a
measuring instrument of great precision. By its means alone
a vast number of chemical compounds can be positively identi-
fied. The manufacturer of organic compounds, especially, can-
not afford to ignore it as a means of increasing the ease of control
work. In the hands of a skilled worker this type of instrument
offers untold advantages.
The application of microscopic methods to analytical prob-
lems should appeal to every chemist. Not only can he perform
qualitative chemical analyses easier, but he can measure refrac-
tive indices of both solids and liquids, determine melting and
boiling points with exceptional accuracy and upon minute
amounts of material which cannot be isolated, determine molec-
ular weights and can study the structure of most of our com-
mercial materials. Dr. Harvey W. Wiley, in one of his happy
moods, once defined chemistry as "the astronomy of things in-
finitely small." Our telescope is the microscope. To make suit-
able progress we must, like astronomers, construct special instru-
ments for special purposes, and like the astronomers we must be-
come specialists in narrow fields within our vast science. We
chemists must have analogues to the students of double stars,
to the investigators of nebulae, to the seekers for comets, etc.
When this day comes the results reported will be comparable to
the discoveries of our astronomical friends. Americans make the
finest telescopes in the world. Why not microscopes as well?
Unfortunately the scientific world in the United States has
been obsessed with the idea that no microscopes were worth
using, unless made in Europe, We are all to blame for t fa a1
difficulties. Can you obtain an ultramicroscope, a lumincscense
microscope or even a polarization microscope in Wn ! ttited
States this 20th day of April? Not one, nor can you obtain con-
densers, lenses and eye-pieces of quartz suitable for photography
with ultra-violet rays, nor spectroscopic oculars; nor can we pur-
chase a really satisfactory moderate priced metallograph, although
in this line there is hope that instruments will soon be on the
market.
AMERICANS MUST STAND BY AMERICAN-MADE INSTRUMENTS
If each one of us here to-night will agree hereafter to stand by
American manufacturers and buy American-made instruments,
we will soon have special microscopes and accessories ranking with
the best obtainable. Our artisans have no superiors and few
equals, but in order that we may persuade them to undertake the
construction of the apparatus we require, it is essential that we
must support them with advice and hard dollars and not with
empty applause. It is easy to find fault and refuse to cooperate ;
but it takes time and tact to call attention to defects and suggest
improvements.
If those using special microscopes would stop and consider the
care and labor involved in their manufacture and would be a trifle
more tolerant toward mistakes in construction, far greater prog-
ress would be made than at present. Let us all agree to try and
stimulate the development of American types of microscopes
which will do our work better and easier, and cease being mere
copyists. Let us become "boosters" instead of "knockers."
I have already asserted this evening that the chemical micro-
scope will do more for the chemist than any other instrument or
group of instruments, and it behooves me to prove my contention.
In the first place, microscopic methods are the simplest and
shortest for the identification of a compound. Let us assume that
the analyst has in his hands a crystalline salt, and by qualitative
analysis in the usual manner he decides after about an hour's
examination that it contains sodium and phosphoric acid — noth-
ing else. It is manifestly a sodium phosphate, but which one?
Mono, di or tri? This he can answer satisfactorily only by quan-
titative analysis, and actually only by a determination of Na and
P04. If, however, he possesses a polarizing microscope, the
problem is quite simple. The mono-sodium salt is orthorhombic,
the di-sodium, monoclinic, while the tri-sodium phosphate is
hexagonal. He can clinch his opinion with one or more simple
optical measurements and prove his case by refractive index
determinations by the immersion method. Why is it that the
chemist never uses refractive index determinations by means of
the microscope as an aid in qualitative analysis? It is incon-
ceivable that we have had these methods used for years by min-
eralogists and petrographers, yet never had sense enough to ap-
ply them to our own ends and thereby save ourselves hours of
time.
But to go back to our phosphate ; had we made the qualitative
analysis by microscopic means it would not have taken us an
hour, but say not over half that time. We would have been seated
comfortably at a table and would have satisfied ourselves in a
very few minutes that the salt was di-sodium phosphate badly
effloresced and of commercial, not C. P., quality. This case is
actually a typical one and very simple. I have selected it be-
cause it illustrates quite clearly the way in which a simple salt
may be identified. But I hear some of you say this requires a
knowledge of crystallography. What of it? If this knowledge
will save us time and labor let us by all means do a little reading.
EASE, CHEAPNESS AND QUICKNESS OF MICROSCOPIC QUALITATIVE
ANALYSES
Of all the inorganic salts we will meet with in industrial work
only a very few belong to the isometric system and have no effect
upon polarized light. Very few are tetragonal and triclinic and
fewer still hexagonal. There is rarely need for expert (raining to
enable the analyst to properly place the compound under exam-
ination in one of these systems. Suppose again the analyst has
an inorganic crystalline salt, and under the microscope it separates
62
THE JOURNAL Of INDUSTRIAL A X D ENGINEERING CEEMI. TRY Vol. 10, Xo. i
from water in what appears to be large colorless octahedra which
are isotropic. The salt must be an alum, or strontium, barium,
or lead nitrate, or one of several chlorostannates. The addition
of a tiny drop of nitron sulfate gives no crystalline precipitate,
therefore it cannot be Sr, Ba or Pb, or other nitrate. A little
calcium acetate gives crystals of calcium sulfate. The salt pre-
sumably, therefore, is an alum. A refractive index determination
will show which alum, or we can go ahead and test qualitatively
for the bases present.
Fig. 1 X 50
The point I wish to emphasize is that in the identification of
many substances a systematic time-consuming analysis is un-
necessary. Note well also that all the work is done upon an ob-
ject slide, that only low powers are employed and the amount of
reagent required is negligible. Five grams of practically any
reagent used should last an analyst, even in daily examination,
almost a lifetime.
I find that the prevailing idea among chemists is that quali-
tative analysis, by means of the microscope, has for its purpose
the detection of such infinitesimal traces of material that all
other methods fail. Although it is true that microscopic methods
can be thus employed, by far the greatest points in their favor are
the rapidity of obtaining results and the certainty of the reaction.
Actually tin relative proportion of material to solvent is very
great; we .or apt to be working with high concentrations. We
take a fragment of the unknown material, not quite as large as a
pin-head, and dissolve it in a minute drop of water or acid. The
his drop ol solution until it appears to have
the diameter of a ten cent piece. This is almost equivalent to
taking a handful of the unknown and dissolving it in a liter of
solvent. The identity test is made by adding a reagent which
will lead to the formation and separation of a crystalline phase.
VALUE OF MICROSCOPE IN" ORGANIC ANALYSIS
It is in the field of organic analysis that the microscope stands
without any possible competitor. Differentiation of isomeric
compounds, recognition of different degrees of sulfonation,
nitration, etc., is so simple in most cases as to be mere child's
Fig. 2 X 50— Cu(CNS)i.Hg(C.VS)..HjO
play. 'Take the case of the phenolsulfonic acids. Recognition
of the different acids, mono or di, ortho, meta or para, or mixtures,
was a stumbling block for years until Pratt showed that the
barium salts were easily differentiated under the microscope.
The di-acid salt forms stout monoclinic prisms, the mono-ortho
acid long slender rods, and the para acid tufts of fine needles.
Quite recently the microscope was called upon to aid a large
plant in controlling the completion of a certain process. It was
found that the manganese salt of a certain organic compound
crystallized jin plates with vivid polarization colors; the other
■
product which it was desirable to eliminate en stallized only with
difficulty in sphaero crystals polarizing feel l\ A glance under the
polarizing microscope showed at ono he transforma-
tion of one form into the other. The older met hod of control took
not less than twenty four hours; the new no- over twenty minutes.
By far the majority of organic compounds cannot be differenti-
ated and identified without time-consuming quantitative deter-
minations. Judicious application of the methods of what I.ch-
inann years ago called cr\ stal anal) sis j Ids the necessary infor-
mation at once.
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
65
By means of an electrically heated stage not only can we de-
termine melting points with greater ease than by the usual
methods, but the accuracy of our observations is considerably
increased. Amounts of material so small as to be practically in-
visible to the naked eye can be employed. A further advantage
lies in the fact that the melting points of several different sub-
stances existing in a mixture may be ascertained without having
recourse to long and arduous separations, involving loss of
material and time.
Very reliable melting points of fats may also be obtained as
well as the boiling and subliming points of small quantities of
material
MELTING-POINT DETERMINATIONS BY MICROSCOPE
The advantages of microscopic melting-point determinations
will become more apparent when we recall that when we separate
one compound from another at our laboratory work table, we so
proceed that the final products stand upon our table a few inches
apart in suitable containers. If we spread a small quantity of the
original mixture upon a bit of cover glass and examine the prepara-
tion with a magnification of say 50 diameters, a decided space
will be seen to exist between most of the different components.
Gentle tapping will usually increase this space. To all intents
and purposes the magnification has done exactly what we ac-
pound and its subsequent separation as a solid crystalline phase.
These crystals are easily recognized and are so characteristic
that there is little danger of mistaking those given by one element
or compound for those of another. Add to the distinctive mor-
phology the fact that color also enters into the identification
scheme, and it will be even more apparent why microscopic
methods offer such ready means of identification.
In a large number of cases one and the same reagent will
cause distinctive crystal separations with a number of sub-
stances. One of the best examples of this is potassium (or sodium)
mercuric sulfocyanate, K2Hg(CNS)< [or 2KCNS.Hg(.CNS)2],
which gives characteristic crystals with copper, yellowish green
(Fig. 2) , cobalt, deep blue (Fig. 3) ; zinc, white (Fig. 4) ; cadmium,
colorless (Fig. 5); lead, colorless (Fig. 6) ; manganese, colorless
(Fig. 7); gold, yellow; silver colorless; and a red color with
iron. Thus the addition of a single reagent will show at once
the presence or absence of a number of elements, and at the same
time produce an identity test for each, thereby saving an enor-
mous amount of time and material. There are a number of such
reagents available, and by carefully choosing them we can com-
plete in a few minutes a qualitative analysis, intricate though it
may be.
Time will not permit me to show slides1 of more than one
5 X 50— Cd(CNS)!.Hg(CNS)2
6 X 50— Pb(CNS)s.Hg(CNSl2
complished in our long chemical separation; i.e., removed the
components from apparent contact with one another, and inter-
posed space between them. In most instances even very rapid
crystallization of two or more salts upon a slide by quick evapora-
tion of their solution will yield a preparation in which the salts
will be found to have separated without intermixture, and with a
sufficient space between them to allow a melting-point deter-
mination being made.
This fact is clearly shown in Fig. 1. Evaporation has been
poshed SO fast as to force the saltsto crystallize in dendritic forms,
yet each group of dendrites is clear and distinct. Were such a
preparation heated carefully and watched with the microscope,
I think you will all agree that as one of the components begins to
melt it will easily lie discerned and will not interfere with the
"ill' t When, however, the temperature is raised to the melting
point of the second component, the chances are that the two
liquids will flow together. Nevertheless the moment of fusion is
easily ascertained. If in melting-point observations, as 1 pointed
out some years ago, we make use of Hie polarization microscope,
D it ion from a solid anisotropic body to a completely
fused isotropic body is instantly recognized.
Doubtless thai branch of chemical microscopy of greatest
ipplii ability is in qualitative analysis. The addition of
a suitable reagent induces the formation of a distinctive coin-
more of these multiple test reagents. I have selected cesium'
chloride, which gives us reactions for bismuth, antimony, tin,
copper, silver and lead, and occasionally, aluminum and mag-
nesium. You will note that the crystals obtained are just as
different from each other and just as easily recognized as those
formed by the mercuric sulfocyanates. Furthermore, in the
characteristic reactions for the common acids the crystal forms
are so different and so easily remembered that there can result no
confusion when the tests are properly applied.
SMALL AMOUNTS USED IN TESTS
The amount of material required for our tests is shown by the
tiny fragment clinging to an ordinary No. 7 sewing needle (equiva-
lent to a fragment whose diameter is approximately that of a
period(.). The manner in which a test is performed I have
tried to show in this lantern slide (Fig. 8.) An ordinary ,3-in. X
1 in object slide with the steps in the analysis of an alloy has been
photographed natural size in order that the relative sizes of the
tlrops iini 1 e better judged. The tiny black spot (0.8 mm. Xo. 1 X
0.1 mm.) is a piece of the alloy of the exact size of that employed
for the analysis. The large spot at the corner is the space occu-
pied by the solution of the alloy after repeated evaporation with
tiny drops of nitric acid to render insoluble any tin present. The
nitric acid soluble portion lias been decanted to the second spot.
1 Not shown here,
64
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. i
The residue has been tested and found to contain tin, antimony
and copper. The nitric acid solution has been divided into three
drops as seen in the slide: the first shows the dry residue after
finding lead, copper and antimony present; the third spot is
what remains on the slide after testing for other elements and
finding zinc and iron in traces, in addition to those already found.
The fourth spot has been used for testing for the remaining pos-
sible metals which were not disclosed in the other tests.
We have thus carried out upon an object slide the entire quali-
tative analysis of a bearing metal containing tin, antimony, lead,
and a small amount of copper, and having traces of iron and zinc
present. Actually it took little more time to perform the anal-
ysis than it has taken to tell it. The worker has been seated
at a small table and has used less than five cents worth of reagents
and gas. Instead of cutting off a small portion of the alloy we
could just as well have rubbed it over a piece of ground glass or
unglazed porcelain, dissolved off portions of the streak with acid
and made our analysis as just outlined. The next lantern slide1
shows this method together with the results obtained and the
time required for the analysis. These cases are fair illustrations
of what is possible in the saving of time, money and labor,
through the employment of microscopic methods.
Other valuable applications of qualitative tests are those in-
volving testing for the purity of precipitates in gravimetric an-
U- ' - • f ;
Fig. 7 X 50— Mn(CXS)i.Hg(CXS)i
alyses in order to avoid the time and trouble involved in reso-
lution and reprecipitation, in testing for complete precipitation,
especially in electrolytic analysis and also in testing for com-
plete washing.
Another valuable application of microscopic chemical methods
is in the analysis of the total solid residue in water analyses. We
generally speak of the hypothetical combinations present. I
do not wish to raise the question of reporting ions or combina-
it I do desire to lay emphasis upon the fact that it is
possible and practicable, in most cases, to identify the salts
present in the solid residue through their habit and optical prop-
erties, providing the work is properly done. I know of several
instances wh< re identification of the principal compounds present
threw much light upon obscure problems. Traces or more of
the he.i\ v met. lis. such as lead, copper, etc., are Far more readily
detected by microscopic qualitative analysis methods than by
any other means at OUl disposal.
Watt i altOgethel too little attention to micro-
scopic examinations of sediments and suspended matters, and to
the deposits at the bottom of springs, wells and cisterns. Much
valuable information is also to be derived from the examination
of the muddy ooze at the bottom of streams, ponds and reser-
1 Not shown here.
voirs, and from the study of the coated sands from rapid filter
beds to learn the extent and character of the adsorption of
aluminum hydroxide by the sand grains. When we speak of the
"microscopy of drinking water," we generally mean researches
upon the flora and fauna giving rise to disagreeable odors and
tastes, but this is in reality only a very narrow portion of a
huge field which is by no means restricted to biological problems
or even to investigations made with the ordinary' microscope,
since it comprises problems soluble only by means of such special-
ized instruments as the ultramicroscope and the luminescence
microscope.
EXAMPLES OF RANGE OP APPLICATIONS
The remaining lantern slides' have been chosen to illustrate
the application of microscopic methods to the solution of prob-
lems in some of the great industries. I can do no more than
touch upon them. Permit me, therefore, merely to outline the
nature of the information given
abrasives — Proper grinding requires adequate speed without
undue heating; cutting of uniform depth; wheels which wear well.
In other words, the selection of the proper sort of wheel and speed
for the specific purpose. There enters, in addition, the size of
particles of abrasive and the nature of the bonding material giving
a hard or soft wheel. Much of the manufacturing has been done
upon a purely empirical basis and by rule of thumb methods.
Microscopic examinations of particles torn off show how the
wheels have acted, while a similar examination of the abraded
surface shows the character of the cutting done.
It is surprising how much information may be gained in this
way, and how it may be used to guide one in making proper selec-
tions.
I will be able to demonstrate that a grinding wheel of a certain
kind will tear off the surface of tool steel in such a manner as to
heat the steel and draw its temper to such a degree that the
particles you will see under the microscope have been fused into
tiny spheres. Another wheel rotating with the same surface
velocity will cut off the material in ribbons. You will note how
few melted fragments are present as shown by the absence of
tiny spherical masses. Such a wheel can be employed for purposes
for which the other is obviously unsuited.
CEMBNT, concrete, ceramics, ETC. — By microscopic examina-
tion it is possible to determine the character of the final product,
its component parts and their volume per cent : the prevalence of
an undue proportion of air and water voids; the thoroughness of
wetting of the cement mixtures, etc.
Xot less important is the recognition of improper bonding and
valuable information is obtainable as to the actual strength of the
concrete or its liability to failure. There is here a huge field for
the investigator offering untold possibilities.
The whole field of ceramics, both clay products and porcelains,
needs intensive microscopic research. Even our ordinary bricks
offer a most attractive subject for the investigator.
The thickness of glaze and the thoroughness of its bond with
the body-making material can readily be determined. I have
prepared slides of two high-grade porcelains; in one of these (Fig.
9) you will note the glaze is thick and between it and the porcelain
St number of tiny gas voids. In some cases these gas
voids penetrate the glaze as infinitely fine capillary tubes. The
other porcelain of far higher quality has a much thinner glaze
and as you see (Fig. 10) has almost no gas voids — the bonding is
almost perfect Examinations of this sort, employed in the
industry go a lone way to improve the products turned out.
foods and beverages — Doubtless the earliest application of
microscopic methods by the chemist was in the examination of
foods, food accessories and drugs for adulteration or deterioration.
Examinations of this sort are based largelj upon vegetable and
animal histology, and differ but little, if any from the ordinary
technique of histology. No other methods are available to ac-
1 Only two figured.
Jan., 1918
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
6S
complish the ends in view, and we can therefore assume that in
this line at least the microscope is indispensable, training in the
necessary technique imperative, and every food analyst and ex-
pert must perforce train himself to undertake studies of this
sort.
This field of activity is so well understood and so firmly estab-
lished that we can dismiss it without further comment. But there
is in this whole question of the microscopy of foods and drugs,
another phase, which chemists have greatly neglected — that of
the amazing possibilities of microscopic qualitative and quanti-
tative analysis. To even enumerate the list of substances whose
detection becomes simpler, more certain and much more rapid
than by our ordinary routine tests, would require more than the
remaining time at my disposal. These "micro" tests are applicable
to organic, as well as inorganic substances, as I have already
pointed out. We have nothing better than microscopic methods
for the detection of the poisonous metals, for the recognition of
the organic acids, for the detection of preservatives, for the
vegetable alkaloids, glucosides, and other active principles of
plants; nor can we find other methods available for the quanti-
tative analysis of starch mixtures and for similar analyses of
mixed powders and meals of vegetable origin.
The recognition of our commercial synthetic drugs also is con-
siderably simplified. In fact it is no exaggeration to say that
proper analyses of this sort cannot be conducted unless the
microscope is employed.
In the canning industry, especially that employing tin cans and
other containers, the microscope gives information of untold
value. Soldered and crimped joints yield up their secrets, as also
the tinned surface or other protective coating which may have been
applied to metal or paper surfaces. The possibilities are, in fact,
without end.
metallurgical industries — The microscopic study of metals
and alloys has been so firmly established within the last few years,
and the close relation between structure and physical properties
so generally recognized and its importance proved in practice,
that I need not spend time upon this question. Although these
methods have been placed upon a firm foundation in the iron and
steel industries, there is much work to be done in the great field
of commercial alloys. We generally think of heat treatments in
terms of steel only. As a matter of fact many alloys may be
greatly improved by carefully conducted heat treatments. In
order that such work may be properly done, microscopic studies
of structure are imperative. This is well shown in the photographs
of a copper-zinc, and of a copper-aluminum alloy.
Often the microscopic appearance of a roughly polished and
etched specimen taken in conjunction with a hasty qualitative
analysis will give the investigator all the information he may re-
quire to deduce the quantitative composition and to make a
shrewd guess at the physical properties.
A most fruitful field leading to improved practices is the study
of welds and brazes under the microscope. At least one expert
in welding by means of oxyacetylene owes much of his remark-
able success to microscopic studies of welded materials.
Not infrequently the microscope shows that a poor product is
due to improper temperatures of casting or coating, and not to
bad raw materials or wrong percentage composition. This is
especially the case in babbitts and in tinned goods. In these photo-
graphs showing the great difference in the structure of a babbitt
cast at too high a temperature and the same one poured just right,
it is obvious that in the one case friction will be considerably
greater than in the other, particularly if in a high-speed bearing.
paints, pigments, protective coatings — The microscopic
studies of materials falling in this group of commercial products
may be classed under three heads: (1) The examination of the
raw materials, (2) that of the coated surfaces and (3) studies of
the methods and results of applying the coatings to the objects
to be protected.
Briefly stated, the raw materials under the microscope (chiefly
pigments, etc.) reveal their source and nature, often the process
of manufacture and their suitability for the purposes for which
they have been purchased. Take for example the mere question
of size in the selection of the pigments for a mixed color paint.
It is a simple matter to obtain a whole series of different shades
by using, say two pigments and having them vary in the ultimate
size of their particles, although the per cent by weight of each
remains constant. The actual shape of the particles also probably
seriously affects the length of time the paint really acts as an
efficient protector, especially in paints containing silica, graphite,
or both. The microscope also throws light upon the nature of
the changes taking place in the pigments of paints exposed to
air, light and the weather. A good illustration is to be found in
the study of the cause of the darkening lithopones.
Examination of the weathered, coated objects, both of the
surface and of sections cut through the thin films of coatings, not
infrequently will permit the formation of an immediate opinion
as to the quality of the paints or coatings, and the skill of the work-
men who applied them.
Too little attention has been paid in the past to the study of
sections. I believe all of you will be interested in the prepara-
tions1 I have to show you. I have selected them because they
exhibit in a striking manner the differences between good and bad
paints, and between good and bad workmanship in their applica-
tion. You will also note that the appearance under the micro-
scope of these samples of japanned steel show very clearly the
superiority of the one method of baking over the other; in actual
1 Not shown here.
•66
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. i
practice the superior surface costs less to apply than the inferior
and wears longer and better.
The microscope in the hands of the chemist dealing with this
class of commercial mated il enables him to evaluate rapidly the
products handled by his 6rm, to improve faulty products and to
determine whether the materials supplied to the trade are being
properly applied.
Nor must we omit from mention the valuable information we
may obtain from the microscopic study of woods to which fire-
•or decay-proofing substances have been applied.
PAPER — I have thus far failed to mention one great industry-
based largely upon microscopical control -- the paper industry.
Practically, an analysis of paper without reference to its ultimate
composition as shown by the microscope is of little or no value.
Actually, much paper is manufactured and employed for various
purposes without studies under this instrument. As a necessary
consequence we frequently meet with paper-fiber goods manu-
factured with little regard for the ends to be attained other than
to sell at a profit. A fair criticism of our American paper products
are that they are too good; that is to say, the quality is higher
than need be, and the cost to the consumer is greater than it
should be for many of the objects to be attained. By that I
mean that a less expensive product would serve equally well and
not infrequently better. This is poor business and poorer con-
servation. Let me cite a case in point:
A few years ago a firm manufacturing a product (which must
be nameless, since the investigation was conducted in confidence)
appealed to the laboratory for advice. Their product, and that
of their competitors also, was failing to stand up under new con-
ditions of use. In desperation the chemist of the firm wanted to
know whether the microscope would reveal the source of the
trouble. A day or two's critical study of new and failed material
showed that changes made by the paper firms were probably the
•cause of the trouble. A commercially better grade of paper was
being supplied. The matter was taken up with the paper firm.
The answer was quick and to the point. The paper supplied was
the highest grade that could be produced at that price and further
they didn't propose to have any nun. mere analysts, tell them,
their business. They had been manufacturing papers before
the questioning men were born, etc., etc. In fact the same old
story, and the same old trouble with many well-meaning American
firms. All you industrial men have had similar experiences.
I need not go further.
A small firm was prevailed upon to make a paper of the kind
which, it was believed, would eliminate certain features which the
microscope seemed to indicate to be the cause, or at least one of
the causes of the trouble. This new paper was then treated in the
ptopci in, inner and tested out. The results were so satisfactory
that a contract was placed to take almost the entire output of the
paper linn with specifications as to the kind of paper needed. The
ml result was that a product was obtained in which, not only
were the old defects eliminated, but the cost of production was
ed, the final profit greatly increased, and the stability of
this industry assured. But I am not sure that the paper firm
which lost a large contract is even to day convinced that the new
methods of microscopic investigations are of value.
There is tittle doubt that similar conditions obtain in many of
the othei varied paper-fiber industries Microscopic methods
are the only ones which enable the analyst to identify the nature
Ol tin papei and to indicate its fitness and adaptability for the
specific u-e- to which it will be put.
'I'll, technique for the recognition of the nature of the fibers
and for their quantitative determinations arc fairly well
established and are on the whole quite satisfactory Hut a phase
investigation has been neglected, dm . > stu.lv of
the liui si ie.l sin face " illi i. I. i em is to the uses to which the paper
is loin applied A tUi ices with vertical illu-
minator and with oblique light yields most interesting results.
Were these methods more often employed there would be in
many cases a decided modification in certain papers on the
market.
the TEXTILE INDUSTRIES — Like paper, the analyses of textiles
and the recognition of the fibers of commerce are dependent
entirely upon the proper application of microscopic methods.
At the present time no other satisfactory methods are available
for differentiating between the species of fibers employed, the
specific treatment they have received, or the loom arrangement
by which the yarns have been woven into fabrics. In not a few
instances the information thus obtainable may go even further
and disclose the nature of the method used in dyeing the yarn or
the fabric. Uneven adsorption, variable penetration, etc., are
easily recognized. The skilled investigator may go even further
and discriminate between different qualities of the same species.
The technical microscopy of the textile fibers is still in its in-
fancy: its literature teems with inaccuracies and contradictions.
Too little attention has been devoted to the investigation of the
reactions of reagents and the selection of proper differentiating
stains, and the potential possibilities of dark field condensers
having very' oblique ray illumination (ultramicroscope) and of
luminescence illumination (ultra-violet rays) have not yet re-
ceived the attention they deserve.
By way of illustration of what the microscope reveals, I call
your attention to several lantern slides' selected to show how
neglect to employ this instrument led to the failure of a manu-
facturer to reproduce a fabric which the firm was called upon to
manufacture because of war conditions. The reproduction in-
volved producing a similar yarn from like fibers, a similar weave
in the fabric, and a similar colored printed pattern. The slides
show that in no case was he successful and that his different at-
tempts were a waste of time, material and energy, since he ap-
parently lacked the fundamental microscopic information
necessary for success.
I trust that in these rambling remarks I may have converted
some skeptics to a belief in the importance of chemical micros-
copy in our industries, and may stimulate a wider interest in a
branch of chemical analysis whose value has been greatly under-
estimated and whose development has been sadly neglected.
Department of Chemistry
Cornell University. Ithaca. X. V.
THE BUREAU OF MARKETS IN ITS RELATION TO THE
CONSERVATION OF FOODS-
By Charles J. Beaks
Recently. I noted a peculiar typographical error in one of the
western newspapers. An editorial, a half column in length,
seriously discussed the need of food conservation, but through
the carelessness of the t] pesettei the article was entitled "Food
Conversation." Much of the matter that is going the rounds
of the press in these days may be called not improperly "food
conversation." Your section of the American Chemical Society
and the Bureau of Markets arc. I hope, not interested in, nor in-
dulging in. careless and uninformed talk about food problems, but
arc taking serious steps to save the food of the country and to
effect its more economical use
Before proceeding to outline the relation of the Bureau of Mar-
kets to food conservation, let us first determine why the saving
of food is so unusually important at this time. Roughly speak-
ing, the diet of the average person in llie I : is obtained
from the following sources
39 per cent Animal
31 per cent v
2S per cent Fruits and \
5 per cent Sugar. Condiments, and Miscellaneous
1 Not shown here.
ited before the Division of Agricultur.il .ind Food Chemistry.
.s.sili Meeting ..f the American Chemical Society, Boston, September 10
to 13, 19
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
67
Therefore, if we examine into the world situation as to the
consumptive requirement and supply of animal and grain food
products, which total 70 per cent of the whole, the need of con-
servation will become apparent immediately.
As we have associated ourselves with the Allies across the
water in a grim determination to win the war, we cannot think
in terms of our own needs only, but must have in mind, in ad-
dition, those of our allies and those of deserving neutrals depend-
ent upon us. The problem of the neutrals is intricate and delicate.
Recent developments force the consideration seriously of a most
severe extension of the embargoes on foodstuffs and other im-
portant materials.
As stated above, food animals and meats constitute 39 per
cent of the average diet. On account of the inroads that war has
made upon the herds and flocks of the world, it is estimated that
there has been a decrease of over 115,000,000 head of cattle,
hogs and sheep. Although our own animal production has been
increasing slightly during recent years after a long period of
serious decline, it has not kept pace with our increase in popula-
tion, to say nothing of our growth in meat exports. The average
exportation of American meats during the three years preceding
the war was something over 493,000,000 lbs. During the war
year extending from July 1, 19 15, to June 30, 1916, the total
exportation was almost 1,000,000,000 lbs. It is, of course, im-
possible to increase animal production quickly enough to produce
this requirement, hence conservation must be called upon in
order to provide what is needed.
In the case of the cereals, the crop situation in the allied coun-
tries, while fairly satisfactory in view of the vast amounts of
labor diverted to war, still leaves an enormous total requirement
that must be supplied largely by North America. The pre-war
consumption and current import needs of wheat of Great Britain,
France and Italy, our most important allies, expressed in terms
of bushels, are as follows :
Pre-war Current
Consumption Import Needs
Great Britain 268.000,000 203,280.000
France 360.000,000 118.400,000
Italy 236.000,000 59,800,000
Total 864,000,000 381,480,000
The normal needs beyond their own production of the neutral
nations dependent upon us are about 192,000,000 bu. Hence,
the total import needs of our allies and the neutrals for wheat
alone are in the neighborhood of 570,000,000 bu. On the basis
of existing crop prospects, the United States, Canada, Argen-
tine, Australia, North Africa, India and Russia will be able to
supply about 500,000,000 bu. The long haul from Australia,
requiring three times the tonnage that shipments from North
America require, the uncertainty of being able to move any con-
siderable quantities from India, and the almost impossible
transportation situation in Russia, leave the burden upon the
wheat fields of North and South America. The crop in the River
Plate territory has not proven as large as usual, hence an added
responsibility for us.
The normal consumption requirement of the United States is
about 575,000,000 bu. The Bureau of Crop Estimates antici-
pates a crop this year of about 678,000,000 bu., hence our ex-
portable surplus will be about 100,000,000 bu. By conservation
it i, nf the highest importance that this quantity be increased to
the greatest possible extent in order that the foreign deficit of
70,000,000 bu. may in some way be covered. The extent of this
shortage will be more quickly grasped if we remember that it
requires 4Y2 bu. of wheat to make a barrel of flour, and that a
barrel of flour under average conditions of efficiency in modern
bakeries produces 275 loaves of bread. Our 71 >.< .<» 1,0. n bu.
shortage, therefore, converted into barrels of flour would amount
roughly i>> 15,500,000 bids, or a shortage of over 4,000,000,000
loaves of bread. As there are about 103,000,000 people in the
United States, this would represent a little less than 32 loaves for
each person.
I have cited these two important food sources to indicate the
amount and character of our needs.
In the case of two of our great food crops, the prospect is for
a large increase. The corn crop will probably exceed 3,000,000,-
000 bu. as compared with a five-year average of 2,600,000,000.
The potato prospect is for a crop of considerably over 400,000,000
bu. while last year's crop totaled only 285,000,000.
From this general review, let us proceed to a brief examination
of what the Bureau of Markets is undertaking to do to improve
conditions, not only as a war measure, but for peace times.
In the first place, we are trying to get the facts. An impor-
tant desideratum in all work on food problems has been
authoritative information regarding food habits, supplies, con-
sumption, ownership, location and the like. This lack of authori-
tative information has been due primarily to lack of authority to
obtain it. It seems incredible, but up to August 10 no branch
of the Government had the legal power to force the divulging of
information regarding food stocks held in any hands whatsoever.
On the recommendation of the Bureau of Markets, there was
included in the so-called Food Production and Food Survey Bill
(Public No. 40, 65th Congress) a section delegating quite com-
prehensive information-getting powers. This section, which is
Section 2, and that part of Section 8 making appropriations are
of sufficient interest in this connection to be read in their entirety:
Sec. 2. That the Secretary of Agriculture, with the approval
of the President, is authorized to investigate and ascertain the
demand for, the supply, consumption, costs, and prices of, and
the basic facts relating to the ownership, production, transporta-
tion, manufacture, storage, and distribution of, foods, food ma-
terials, feeds, seeds, fertilizers, agricultural implements and
machinery, and any article required in connection with the
production, distribution, or utilization of food. It shall be the
duty of any person, when requested by the Secretary of Agricul-
ture, or any agent acting under his instructions, to answer cor-
rectly, to the best of his knowledge, under oath or otherwise, all
questions touching his knowledge of any matter authorized to
be investigated under this section, or to produce all books, letters,
papers or documents in his possession, or under his control, re-
lating to such matter. Any person who shall, within a reasonable
time to be prescribed by the Secretary of Agriculture, not ex-
ceeding thirty days from the date of the receipt of the request,
willfully fail or refuse to answer such questions or to produce such
books, letters, papers, or documents, or who shall willfully give
any answer that is false or misleading, shall be guilty of a mis-
demeanor, and upon conviction thereof, shall be punished by a
fine not exceeding $1,000 or by imprisonment not exceeding one
year, or both.
Sec. 8. ****** For gathering authoritative information
in connection with the demand for, and the production, supply,
distribution, and utilization of food, and otherwise carrying out
the purpose of section two of this Act; extending and enlarging
the market news service; and preventing waste of food in storage,
in transit, or held for sale; advise concerning the market move-
ment or distribution of perishable products: for enabling the
Secretary of Agriculture to investigate and certify to shippers the
condition as to soundness of fruits, vegetables and other food
products, when received at such important central markets as
the Secretary of Agriculture may from time to time designate
and under such rules and regulations as he may prescribe ; pro-
vided, That certificates issued by the authorized agents of the
department shall be received in all courts as prima facie evidence
of the truth of the statements therein contained; and otherwise
carrying out the purposes of this Act, $2,522,000; provided
FURTHER. That the Secretary of Agriculture shall, so far as
practicable, engage the services of women for the work herein
provided for.
food surveys of the united statics
The plans which are now in operation contemplate a prelim-
inary survey as of August 31 . monthly reports on the important
food commodities and a fat more detailed survey about the first
of December when all of the crops of the year have been gathered
6:-;
1 III: JOURNAL OF INDUSTRIAL AND ENGINEERING CHEM1 >TRY Vol. 10 Xo. i
and threshed. The preliminary inventory is now in progress and
up to Monday noon 135,000 schedules had been returned from
the enterprises called upon for reports. The August 31st survey
requires the reporting of stocks on hand and in transit for eighteen
of the most important commodities or classes of commodities.
Included are the following:
I — Wheat
2 — Corn
3 — Beans, navy (pea beans), medium white and large white
4 — Wheat flour, all kinds (bbls. of 196 lbs.)
5 — Corn food-products
6 — Rice, cleaned or milled
7 — Rolled oats and oatmeal
8 — Salted and cured beef
9 — Cured hams, bacon, and shoulders
10 — Other cured and salted pork
1 1 — Lard, lard compounds, and lard substitutes
12 — Salt fish, dry and in brine
13 — Vegetable oils suitable for food, cottonseed, olive, peanut, etc.
14 — Solid vegetable cooking fats (labels state whether vegetable or not)
15 — Sugar, all kinds
16 — Sirup and molasses, excluding any unsuitable for human food
17 — Condensed and evaporated milk
18 — Canned salmon.
Reports are also requested for purposes of comparison of stocks
on hand one year ago on the same date. The eighteen items in-
cluded in the preliminary survey will be used as the basis of the
monthly reports already mentioned. Both the preliminary sur-
vey and the more comprehensive one to be made after the crops
are harvested contemplate the obtaining of four classes of infor-
mation:
I — Stocks on hand on farms.
II — Stocks in wholesale, jobbing, storing, manufacturing and
other commercial establishments.
Ill — Stocks in retail establishments.
IV — Consumers' stocks, consumption records and dietary
study.
I — STOCKS ON HAND ON FARMS
The determination of the quantities of the various classes of
food products on farms, necessarily involving principally the
quantity of cereals and the numbers of live stock and poultry,
is being made by the Bureau of Crop Estimates through its exist-
ing machinery and usual methods. Their inquiry includes all of
the grains, buckwheat, flaxseed, the sorghums, peanuts, beans of
all kinds, peas, cottonseed, forage crops, milch cows, calves,
beef cattle, sheep and lambs, swine, and poultry. The Bureau's
figures for the total will, of course, be based on estimates, but the
estimates will be somewhat more inclusive than those customarily
made. Reports will be received for the preliminary survey from
over 30,000 of the Bureau's regular township reporters. For the
more comprehensive survey after the crops have been g
returns will be requested not only from the state, county and
30,000 regular township reporters, but also from 10 farmers in
the vicinity of each such reporter.
II — STOCKS IN WHOLESALE, JOBBING, STORING, MANUFACTUR-
ING, AND OTHER COMMERCIAL ESTABLISHMENTS
Information regarding holdings in manufacturing, storing,
jobbing, wholesale and other commercial establishments', is ob-
tained by requesting from each such concern a statement of the
exact amount, as nearly as possible, .if each commodity on hand.
In the distribution of the schedules for the A.ugus1 ,;i^t survey,
tin 11 was included a list of the more than one hundred separate
items upon which reports will be requested in the later inventory.
Approximately, 384,000 schedule-, were sent out to the various
food handling and distributing enterprises, As an indication of
then charactei and number, I will cite some of the more important
groups:
Grain elevators, mills, and wholesale dealers 38.000
Grain, flour and feed dealers and proprietary feed manufacturers. . . 18,000
Breweries 1.200
Distilleries 800
Rice mills and storages 800
Canners of fruits, vegetables, meats and sea food: . . 6.500
Mills, refineries and exclusive dealers of eoible oils 1.400
Sugar and sirup mills and refineries 1.300
Wholesale and retail bakers 32.000
Manufacturing and wholesale confectioners 1,800
Fish freezing plants, and dry and salt fish packers 1,040
ten and meat packers 3,700
Lard compound and oleomargarine manufacturers 169
Wholesale poultry, butter, egg and cheese dealers 5,000
Poultry packing and fattening plants, and five poultry shippers. . 5,000
Wholesale fruit and vegetable dealers. . . 1.500
Wholesale grocers and merchandise brokers with stocks 7.500
Creameries and milk conuenscries (condensenes 393j 7,000
Cheese factories 5.000
III — STOCKS IN RETAIL ESTABLISHMENTS
On account of the great difficulty, in fact, practical impossi-
bility of making a complete inventory of the stocks of the smaller
retail concerns, the retail survey has been confined to retail
grocers carrying stocks of Siooo and over and to general stores
selling foodstuffs carrying total stocks of S3000 and up. In ad-
dition to this, the work already under way includes a detailed
survey of the stocks of smaller retail concerns in a number of
representative cities and rural districts. The figures thus secured
will be used as a basis for estimating the total stocks for the
entire country. In the general survey, schedules have been sent
to 64,000 retail grocers, 63,000 retail meat markets, 60,000 general
stores carrying foodstuffs, 100 chain store companies (a single chain
store company operates as many as 3400 retail stores) , 1 200 depart-
ment stores handling groceries, and 1200 hotels and restaurants.
For the purpose of estimating the stocks of the entire country
the counties of the United States have been divided into groups
according to the population of the largest city, town or village
in each county. This classification includes as a separate class 44
large metropolitan districts. 43 counties have been selected for a
detailed or intensive survey, which is being conducted by personal
canvass. With the careful classification of all counties, and ap-
plying the returns obtained from the 43 counties selected, we hope
to determine with a valuable degree of accuracy the retail holdings
of the entire country.
A similar detailed canvass has been made of New York City
with the cooperation of Dr. L. P. Brown, of the Bureau of Food
and Drugs of the Department of Health and of the Police De-
partment. New York City. The great importance of New York
as a consuming center and the problem involved in supplying its
foodstuffs from great distances give the canvass of that city
especial importance.
iv — consumers' stocks, consumption records and dietary
STUDY
For determining consumers' stocks a detailed survey has been
made of the amounts held by a large number of r< presentative
families. 10,000 families in all parts of the United States were
visited and a record was made of all food materials found in their
possession. From this an estimate is to be mule of the house-
hold stocks of the country. This is admittedly unsatisfactory
but represented the best compromise which for the immediate
purpose could be found between ignoring household stocks en-
tirely or attempting to get returns from the 20,000,000 families
in the United States, a manifest impossibility.
In passing, it should be said with refereni •. to the preliminary
survey as a whole that while it will yield information of un-
questionable value, one of its greatest u> :s will be the organization
of an efficient machine and the elabora tii a of; factory methods
for malring the more accurate survey in Nov. ml ei or 1 lecember.
In connection with the determination of . ■: -outers' stocks, a
careful estimate of the weekly consumption nore important
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
60
articles of food is being made among 3.5°° typical families. A
carefully prepared schedule for a week's consumption of 54 items
of table food is being used and the cooperation of a suitable num-
ber of families has been enlisted in filling it out. Each was asked
to keep a daily record of the food used by her family for 7 days.
In case of food purchased, the cost was also recorded. If home-
produced, that fact was set forth. All of these facts are, of
course, held in confidence except so far as their use in general
statements of totals and conditions are to be made.
A supplementary dietary study is being made in connection
with the determination of consumers' stocks in which informa-
tion was also collected as to the occupation, age, sex, health,
racial stock, income and general economic condition of the
families. While 3,500 families may seem a small number upon
which to base any statement regarding the dietary of 100,000,000
people, it should be borne in mind that Atwater's American figures
supplemented by some secured by Langworthy a number of years
ago based upon a total of 400 families are the most satisfactory
now available. In addition, it should be borne in mind that these
figures have been used as the basis of the British Royal Commis-
sion's food supply investigations and in part also by Eltzbacher's
commission which investigated Germany's food supply.
In the dietary study, all food on hand at the beginning, all
procured during the course of the study, and all remaining at the
end, are carefully weighed and recorded. Waste and refuse are
taken into account, and from these figures the amounts actually
used are determined. Over 400 institutions of learning scattered
throughout all of the States are assisting through their teaching
staffs and through their graduates in home economics. In ad-
dition, about 700 families, mostly members of the American Home
Economics Association, are furnishing schedules either for their
own homes or for families cooperating in the study1.
When the comprehensive survey of the early winter has been
finished it is believed that the food information of the United States.
will be more complete, detailed and accurate than any in the world.
In passing, may I say in correction of many statements that
have run the course of the press that only $600,000 of the $2,500,-
000 appropriated for all marketing and distribution investiga-
tions are to be used in the conduct of the food surveys of the
United States throughout the year.
I have described the food survey work in some slight detail as
1 believe it to be a subject of especial interest to your member-
ship, whether engaged in physiological or other chemical lines.
With thoroughgoing information, far more can be accomplished
than without it. Nevertheless, we have in the past four years pro-
ceeded upori many lines of conservation work, which will be greatly
emphasized during the coming year. A description of the chief
lines with some examples of their operation and utility follows.*
The following titles describe to a degree those activities of the
Bureau of Markets which most specifically relate to the conserva-
tion of foods.
(1) — The promotion of equitable distribution through the dissemination
of market information by telegraph, telephone and mail.
(2) — Investigations and demonstrations in the conservation of food
products in transportation and storage.
(3) — Market inspection of perishable foods.
(4) — City market service for the distribution and utilization of the
home and commercial garden surplus.
(5)— Conservation of grain food supplies through the work in grain
marketing, standardization and the supervision of grain inspection.
(6) — Reports on cold storage holdings of food products, available sup-
ply of space, and cold storage management.
(7) — Miscellaneous publicity activities designed to bring about con-
sumption of products especially plentiful at certain
Bureau op Markets
Washington, D. C.
1 As a working hypothesis, a daily requirement of from 90 to 100 g.
of protein for a 150-pound man at full vigor with 3.000 calorics of energy if
he does a moderate amount of muscular work, has been generally adopted.
'On account of lack of space we are forced to o
matter. — Kditor.
THE CANNING INDUSTRY— SOME ACCOMPLISHMENTS
AND OPPORTUNITIES ALONG TECHNICAL LINES1
By H. A. Baker
There are produced in the United States at the present time
about thirty-two million base boxes of tin plate per annum.
About five million base boxes are exported, and approximately
one-half the balance is used in making containers for canned
food; that is, the equivalent of nearly five billion No. 2 or i1/*
lb. cans are being packed this year.
The canning industry is nothing more nor less than kitchen
activity carried out on a large scale, with mechanical labor-
saving devices. Food laws and evolved trade custom and ethics
define canned food as natural products, with or without added
salt and sugar, plus water when desirable or necessary, steril-
ized and preserved by heat alone. The point that naturally
arises is, Why should any chemists be needed in an industry
that is so simple as this? Some developments and work in this
connection might therefore prove interesting, because more
chemists are needed than are engaged in the industry at the
present time.
Up to about nine years ago chemists exerted very little in-
fluence in the development of this industry. Of course, every
one is familiar with the fact that the industry was founded on a
basic scientific discovery, but it was developed largely by shrewd
experimenters, usually without technical education. It is
true that valuable assistance was rendered from time to time
by technical men, usually associated with colleges, but the in-
dustry, until lately, did not have on its own pay-rolls men with
technical training.
The Department of Agriculture gave some attention to canned
foods, which was helpful, but for considerable time their help
was along critical and not constructive lines, which is in sharp
contrast to their present activities.
In 19 1 2 the canning industry had become sufficiently pro-
gressive to have developed a strong national organization for
self-development, education, dissemination of statistics, and
activities along many lines other than marketing. It was then
prepared to go one step further and establish a National Associa-
tion Technical and Research Laboratory. This was accom-
plished through the assistance of generous donations from
some of the allied industries. This development opened the
opportunities for much experimental work on a large scale of a
cooperative nature, that hitherto had been difficult, if not im-
possible. The Department of Agriculture has looked very
favorably on the Association Laboratory, and has cooperated
with it on several large investigations in connection with various
industrial manufacturing concerns, supplying the tin plate,
steel and cans for the trade. This machinery for cooperation
is so complete and safeguarded from bias that investigations of
national scope can be carried out and the results accepted,
both by the trade and the technical men of the country.
It might be well at this point to give an outline of some of the
problems that are studied, as well as those yet to be worked
on. In doing this we will not attempt to make any individual
mention of technical men or laboratories, the main point being
to disclose somewhat the nature of the work, and the field for
technical men in the canning and allied industries.
To begin with, we would point out that it has been found
the work involves two sets 01 technical men: those who are
straight technical men with superficial knowledge of the prac-
tical end of the work, and technical men with a broad and ade-
quate knowledge of laboratory work, who are primarily luisi
men with some executive ability. It will be readily seen
that this arrangement is much more satisfactory than the
usual one where purely practical and business men have tin re
sponsibility for the direction of technical activities. While
1 Address presented before the New York Section of the American
Chemical Society, November 9, 1917.
I III: JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, Xo. i
canning work is merely kitchen work on a large scale, it involves
the use of high-speed machinery, concentrating and cooking de-
vices, elimination of air and gas in the product, proper sealing
temperatures and exhaust, proper closure, proper cooking
temperature, as well as proper preparation of the food for can-
ning.
Innumerable problems arise connected with spoilage, quality,
appearance, discoloration, consistency, etc. Many of them can
hardly be answered from the laboratory, and must be worked
out by practical experimentation in a factory. For instance, a
few parts per million of copper in canned corn from cooking
utensils will turn it a dark gray. A very minute amount of
copper will turn canned shrimp black. If evaporated milk
does not receive the proper heat treatment after condensing, it
will not stand sufficient processing to sterilize it without causing
coagulation of casein and separation of cream. If condensed
milk is not properly prepared in regard to the proportions of
milk solids, sugar and water, and if the cans are not properly
sterilized before filling, and aseptic methods of fillin g are not
used, yellow discoloration of the product and spoilage will
occur. If corn is not properly preheated before canning, the
resultant product is watery, and separates. If string beans are
not properly blanched, the product is either too tough, or is
slimy. If red cherries are held in cold water too long, they will
turn brown after canning. If cherries are packed in too
heavy a syrup they will become very tough. If clam juice is
extracted at too high a temperature it will turn black in the can.
It will be seen that any of these problems, if carried to a con-
sulting chemist outside of the industry, would cause him endless
trouble, and could not be solved by analytical work.
A curious difficulty arose some time ago in connection with
canned apples from a certain section of the country. These
apples perforated tin containers very badly, spoilage was enor-
mous, and there seemed no way of stopping the trouble. A peculiar
thing was that these apples which caused trouble only contained
about one-half as much acid as apples packed in neighboring
states that caused no trouble. A certain chemist figured out
from observing the drop in the water line of the cans that there
must have been more air in these apples than in those that did
not perforate. Actual tests showed this to be the case. It
was found practicable to vacuumize these apples under water,
in which case the exhausted air cells became filled with water
when the vacuum was released, and it was found that apples
packed after this treatment, on a large commercial scale, had not
the slightest tendency to perforate the containers. Because
■bf the urgency and extremely heavy losses, it was necessary to
jump directly from a small laboratory' experiment in glass to a
factory installation capable of handling millions of pounds of
apples in a season. Peculiarly enough, the installation worked
perfectly from the outset.
About three-quarters of all the Hawaiian pineapple that is
packed is vacuumized for quite another reason. It was found if
the sliced pineapple was vacuumized that on the releasing of
the vacuum the free juice on the outside of the slice, entering into
the emptied an a Us of the fruit, would change the color instantly
from a rather unattractive white color to a rather standard
yellowish color, which gives the appearance of perfectly ripened
fruit.
For a long time the waste of tin- trimmings and the small pine-
apples was a dead loss. Some chemists want to work anil now
small pineapples and trimmings are crushed, thi
acid removed, and the syrup concentrated and used in ..iiiiMii..
in plan of cane sugar. There is approximately a pound to a
pound ami one half of cane sugar in one gallon of fresh pine-
apple juice. This is now being used, and has lowered the cost
to tlie consumei of cann< d pineapple
Great changes have taken place in the methods of meat
packing m tin- last few years, and have saved over half the labor
cost of canning. It was considered for a long time necessary to
seal meat products in cans under vacuum on account of the
sensitiveness of meat products to discoloration when cooked in
the presence of air. It was pointed out and demonstrated by
chemists that by changing the type of can, filling it so full
that very little air space is left in it, and by merely steam-heat-
ing the product before scaling, that better results could be ob-
tained than was possible with the vacuum system. The labor
cost was cut in half, and an enormous saving resulted.
Cooking large cans of approximately gallon size had always
been an expensive matter, and involved much loss on account
of the internal strain on a can of large area. Extremely heavy
weights of tin plate were demanded and still buckles occurred,
tin plate was broken, and spoilage resulted in cooking retorts
when the surrounding counterbalancing steam pressure on the
outside of the cans was released. Simple pressure cooling de-
vices were evolved, which eliminate all trouble and loss on this
score, besides reducing the cost of the container.
Methods of analyzing tin plate have been developed in a
certain laboratory which designed a machine that enables four
nu n in an 8-hr. day to turn out one thousand analyses of tin
plate.
Much technical work has been done on tomato products.
Sanitary' methods of handling, sorting and cleansing have been
devised so that it is possible to make tomato pulp, puree, ketchup,
etc., with a minimum count of yeasts, mold and spores. Meth-
ods have been worked out that are simple enough to be applied
by the average factory to control the finishing point, or density,
of tomato concentrated products. Chaos previously reigned in
this manufacture, and the loss and miscalculations were sur-
prisingly large. Some canners boiled their product, allowed it to
stand, drained off the liquor which settled at the bottom, little
dreaming that in this way they were losing most of the sugar
and flavor, and a very high percentage of solids. Much more
profitable manufacture and elimination of waste resulted from
concentrating the liquor as well as the pulp.
A great deal of work has been done on the cause of bacterial
spoilage in canned food. This trouble is always occasioned
by one of two things: either a minute defect in the can, or under-
sterilization. All of the arts of the can maker, all the devices
for testing, and the cunning of the bacteriologist is necessary
in arriving at the cause of spoilage in many instances. It will
be readily understood that successful work along these lines
means the elimination of loss; that is. conservation of food ma-
terials and reduction in the cost of food to the consumer. It is
not necessary to cite innumerable examples along these lines,
for enough has been given to indicate the nature of the problem
and possibilities of their solution. We should, however, mention
es of work that were done cooperatively through the
organization previously described in connection with the National
Canners Association Laboratory.
A general survey was made of the absorbed tin in all types of
canned food in all types of containers, with various weights, or
thicknesses of tin coating, both plain and enameled. It can be
predicted at the present time approximately how many milli-
grams of tin per kilogram of food there will be in any tin can,
with any product, in a given space of tune, and whether or not
the can should be ;>lain or enameled.
Another extremely lar.L;e experiment was carried out on de-
termining the relative value of different weights of tin coatings
on tin containers, and it was found that for all general purposes,
except one, there was practically no difference in the protective
in coating running between one pound and two pounds
of tin per base box. Approximately the same number of breaks,
or minute defective spot-, m tin •■ md, irrespective
of the weight of tin coating, and if discoloration trouble develops,
it cannot be taken care of by extra weight of tin coating. The
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
7'
product itself must be so prepared and handled that it will not
attack the container in such a way as to cause discoloration.
Consider for a moment the element of conservation involved
in this. Supposing tin plate were to be manufactured which
-carried half a pound of tin coating more per base box than was
. -of value, the industry would be carrying a burden of 20 to 25
' -cents per base box, which, of course, would be passed on to the
■consumer. On thirty million base boxes of tin plate this would
be fifteen million pounds of tin a year, or approximately seven
million dollars. Not only would there be the burden of un-
necessary cost, but the actual waste of the world's mineral re-
sources which should be conserved. The experiment itself
cost only about fifty thousand dollars.
When one speaks of conservation in food industry the usual
thought is merely the saving of some waste or by-product; the
question narrows down in people's minds to some such question
as taking care of potato peelings. Conservation on its broader
side is mostly concerned with developing new and better ways
•of doing things, involving a saving of labor, money and ma-
terials, together with the enhancement of quality, and benefit
to the public. It is true that there are plenty of waste products
to work up in the canning industry, but it is also true that the
more promising field is new developments. At the present time
only 50 per cent of tomatoes delivered at the factory are turned
out in the canned fruit product. Thousands of tons of pear
peelings are wasted because they do not make a vinegar that
tastes like vinegar. Thousands of tons of fish scrap, particu-
larly on the Pacific Coast and Alaska, are wasted because easy
and profitable methods of getting the values out of them have
not been devised. Enormous quantities of green corn cobs are
allowed to ferment and are used for fertilizer and cattle food,
when it is well known that there is more sugar left in the cob
than was taken off in the corn. Probably many kinds of bac-
teria which at present only destroy food could be made to do
useful work, producing useful substances and chemicals, if they
were thoroughly studied and put to work. Enormous quantities
of sea food, which cost nothing to grow, are at present unused by
the human family because no one has prepared them in a way
that would make them palatable and attractive. Enormous
quantities of shark and gray fish are not used because they hap-
pen to contain a small quantity of urea which in cooking turns
into ammonia. The Department of Agriculture is giving this
matter attention, and they, or other chemists, shall probably
succeed in making this sea food as palatable and popular as
Tuna fish, which for a long time was absolutely ignored. It
was a huge, slimy, soft, unattractive looking fish that was so
repulsive in its natural state that no housewife or cook would
buy it and prepare it for the table. Somebody found out
that if it was properly heated the soft flesh coagulated into firm
flesh of attractive appearance. When it was cut up into small
portions and canned, it became very popular, and millions of
cases of this fish are now consumed.
It is not necessary to point out specifically a lot of things
that lie waiting for chemists to do in the food industry and allied
industries, because specific definitions tend to paralyze the im-
agination, and it is much better for individuals to hammer out
their work a'ong their own lines than to assign them definite
and limited tasks
It is ill r, ,111 -,. ] mil,, , t,, 1, 11 tli. A m.i 1. ,111 ] ml .in that it should
not neglect its chemists, and that if it will give the chemists a
chance they will show how to save waste, reduce costs, and make
life more comfortable and easy. Tin 1 one end of the problem,
the other end being the chemist himself . He has to go out and
dig up things for himself to do, and then ai I I ill man and
sell himself to do them. After all, is that not fair, provided
the chemist is fully warned and told by his teachers that that
is what the Kanu- is, ami that is the waj he shall have to play it?
The canning field is broadening every day, and inviting some
men of technical training to its assistance. Many other technical
men should invite themselves because the work is there, and the
results are to be obtained, and the public is waiting for the re-
sults.
. American Can Company
120 Broadway
New York City
EDIBLE FATS, IN WAR AND LAW1
By David Wesson
With our country starting to take an active part in the World
War, the food question becomes of vital importance. It is
estimated at the present time that the United States has 1,600,-
000 men in its Army and Navy. Great Britain has nearly
7,000,000 and France 3,000,000. Our country is only begin-
ning to build the Army which will be needed before the war is
over.
No matter how well our Army is equipped with artillery,
ammunition, and other tools of warfare, it will not be able to
do its work properly unless it is well fed. We might as well
expect the Empire State Express to make schedule time running
on slack coal as to expect our armies and those of our allies
to achieve great victories on improper or insufficient food.
The great advances made in the science of nutrition during
the last 25 years have given us means to measure the amount
of food required for men doing various kinds of work. When
Atwater was making his painstaking investigations it did not
seem probable to any of us that the results obtained with the
calorimeter bomb were going to help decide the battle of to-
day. Atwater has shown that persons engaged in very active
work require far more food than when doing ordinary work.
Some of his figures are very instructive. Without going too
much into detail, the following will prove interesting as show-
ing the different requirements:
Calories
Rowing Clubs in New England 3 , 955
Bicyclists in New York 5 , 005
Football Teams, Connecticut and California 6,500
Prussian Machinists 4,270
Swedish Mechanics 4 . 500
Farmers' Families, United States 3,415
Mechanics' Families, United States 3,335
Laborers' Families, large cities 2,925
Lawyers, Teachers, etc., United States 3 ,220
College Clubs, United States 3.580
Judging from the intensive training our men are receiving
in the several camps, and the active work they will have to
perform on the battlefield in the cold, damp European climate,
it is quite evident they belong in the football class, and will
need about 6,000 calories per day per man.
Atwater gives in his table the following make-up of the foot-
ball players' diet:
Actually Eaten Digested
Protein 226 208
Fat 354 336
Carbohydrates 634 615
Fuel Value, calories 6500
The fat in this diet would furnish 2,536 calories, or 39 per
cent of the total, while in weight it amounts to one-third of the
food elements.
When we consider the enormous demands on the world sup-
ply of fats by the warring nations, and the terrible curtailments
which have taken place in production, due to the decrease in
fat-yielding animals, the shortage of crops and the difficulties
in transportation, it can readily be seen that the edible fat
problem is a vital one, not only for the proper supply of our
armies and those of our allies, but for the workers at home who
have to supply the armies with lighting materials, and last but
not least, the large civilian population.
1 Address presented before the New York Section of the American
Chi mlcal S01 iety, Novi mbi 1 9, 1917.
7-'
THE JOURNAL OF INDUSTRIAL AND ENGINEERING ill I. : io, Xo. i
No attempt can be made to go into statistics, which had bet-
ter be left in the hands of our able food administrator, Mr.
Hoover. It is sufficient to say that the edible fat supply in
this country is now being greatly augmented by the increased
production of peanut oil, which largely offsets the decrease in
cotton-oil production due to the relatively small crops of the
last two years. The country is also importing large quantities
of copra and cocoanut oils, which formerly went to F.urope
Soya beans and bean oil are also used in large quantities, but
there is not enough to supply our needs here and those
abroad, unless the strictest economy is enforced.
Attention need only be called in passing to the fact that large
quantities of perfectly good edible oils are used in soapmaking
and metal cutting, and also in mixing illuminating and signal
oils. The use of edible oils should be rigidly controlled and sub-
stitutes prescribed for use in the arts, wherever possible. Waste
should be cut down in the use of soap, which should be made
of inedible materials to the greatest extent.
Where the housekeeper most feels the shortage of edible fat
is in the high price of butter. Butter is high because it is scarce;
substitutes, however, can be found to take its place, but be-
cause the manufacture and sale of them are so hampered by
legal restrictions the public has but little opportunity to become
acquainted with their merits.
You all remember the Bible story of how the children of Israel
during the absence of Moses on Mount Sinai persuaded Aaron
to make a golden calf, which they all fell down and worshiped,
and when Moses came down with the ten commandments
and saw what was happening he was so overcome with wrath
that he broke all the commandments on the spot. Many of
us engaged in the production of edible fat sympathize with
Moses, because in the year 1886 our great American Congress,
not to be outdone by the Israelites in worshiping a calf, deified
the great American cow, and have been worshiping her ever
since. I refer to the oleomargarine law which, wTith its amend-
ments and regulations, covers over 90 pages of an octavo vol-
ume. It imposes a tax of $600 on every person who manufac-
tures oleomargarine. It says expressly that any person who
sells, vends, or furnishes oleomargarine for the use and consump-
tion of others, except to his own family table without com-
pensation, who shall add to or mix with such oleomargarine any
artificial coloration that causes it to look like butter of any
shade of yellow, shall also be held to be a manufacturer of oleo-
margarine within the meaning of the act.
Wholesale dealers are taxed $400 a year; retail dealers who
sell less than 10 pounds at one time are taxed $6 a year. Any-
one who manufactures oleomargarine without paying the tax
is liable to a fine of not less than Si, 000 nor more than $5,000,
while wholesale dealers are subject to a fine of $500 to $2,000
and retailers from S50 to $500. The law provides for two
kinds of oleomargarine: colored, paying a tax of 10 cents per
pound; uncolored, paying ■ ( cent per pound. The law has
worked out somewhat as follows
For the fiscal year ending June 30, 191 7, the tax receipts on
oleomargarine were Si. 995, 720, of which $792,838 came from
special taxes on dealers and manufacturers in addition to those
on the product.
The quantities made were:
Colored 6,327,000 lbs., paying 10 cents per lb.
Uncolored 228.066.000 lbs., paying '/. cent per lb.
Total 234 . 393 , 000 lbs.
The year previous the consumption was 152.124.cxx> lbs.
The figures show the increased demand in spite of restrictions.
When the oleomargarine laws were passed in 18S6 the only
.it the command of the manufacturers were oleo oil,
neutral lard ami imperfectly refined cottonseed oil, with small
quantities of imported peanut and sesame oils.
At the present time, with improved refining methods, the
whole field of vegetable oils is open to us, and several choice
brands of vegetable oleomargarine are being made of cocoanut,
peanut and other oils which are sold at about 30 cents per pound
as against butter at 50 cents, and, except in the case of growing
children, are every bit as satisfactory from a food standpoint
as the more expensive products of the cow.
Under reasonable laws, the average consumption of oleo-
margarine in Great Britain is 8 lbs., against 17 lbs. of
butter. Denmark, one of the greatest butter-making and
consuming countries of the world, has an annual consump-
tion of 43 lbs. of oleomargarine per inhabitant, Norway 331/*
lbs., and Holland 20 lbs. The United States consumed last
year 2.34 lbs. of oleomargarine and 18 lbs. of butter per in-
habitant.
While practically nearly all the oleomargarine in this country
is sold uncolored. color is furnished with it and the consumer
can color the material to suit his state.
Congress did so well with the oleomargarine law that in 1888
it tried to deify the hog in like manner by passing similar
legislation against compound lard which, in those days, was a
mixture of lard, oleostearine and cottonseed oil. Fortunately,
the cottonseed oil product was able to present a better bill of
health than the hog product and as a result the lard-compound
industry grew.
Thanks to the chemist, a flavorless, odorless and almost
colorless cotton oil was placed on the market in 1900, which,
combined with oleostearine, made a lard substitute preferred
by its users to the hog product.
Now with the hydrogenation process, lard substitutes, better
than lard, are made without the use of any animal fat what-
ever. The lard supply of the country receives a much needed
assistance, and the Southern farmer is obtaining about 8 times
as much as he did for his cottonseed, at the time Congress
tried to strangle the industry.
The oleomargarine law is not our only grievance against our
statute books. About 1872, dairymen became very much con-
cerned about the manufacture of cheese from skimmed milk
and oleomargarine, which ten years later was superseded by
the use of lard under patents issued in 1873 and 1881. The
cheese was made by emulsifying skimmed milk with the melted
fat, using two or three parts milk to one of fat. then treating
the emulsion in the cheese factory in the usual way. Very good
cheese was the result; it was not injurious to health, but it com-
mitted a sacrilege against the products of the sacred cow, whose
high priests in Congress June 6, 1S96, passed the filled cheese
law promulgating regulations as onerous as those of the oleo-
margarine laws. Manufacturers are taxed $400 per annum;
wholesale dealers $250; retailers $12. with lines and regulations
galore, besides a tax of 1 cent a pound on the product. Natur-
ally the industry languished, and though the bill was passed as a
revenue measure, the last report of the Collector of Internal
Revenue shows there is no longer an; cheese made.
If there was any good excuse for the passage of the bill at the
time, there is none now. There is no a compound
cheese made from skimmed milk and carefully refined vegetable
oils should not be perfectly wholesome as a rticle of diet, and
with proper methods of manufacture .-.\ many of
the cheeses now on the market It won'.,! uitely better
than skim-milk cheese, for example, t fall under
the ban of the law.
When the war started I immediate'.'. to look for
available fat and protein. I knew the value f the various
ible oils as food and realized that in ord - I utilize them
to the best advantage they should I rith protein.
Such a combination spells cheese, one of our most concentrated
forms of food, and skimmed milk at one I :tself as the
best available material. The first thing encountered in the
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
73
literature was the filled cheese law. This put a bar against
experimenting on a suitable scale, otherwise I would have had
some products here to-night. It will not, however, prevent us
from contemplating some figures which in the present food crisis
are worth considering.
The census of 19 14 shows that the creamery production of
butter in this country was 769,810,000 lbs., which would call
for not much less than 20 times that much of skimmed milk
and buttermilk, amounting in round numbers to say 15,400,000,-
000 lbs. of material containing about 3 per cent of casein, say.
460,000,000,000 lbs. If this were worked up into a standard
cheese of 28 per cent casein and 36 per cent fat, it would pro-
duce 1,650,000,000 lbs. of cheese and require 594,000,000 lbs. of
oil, equal to 1,485,000 bbls. This amount of cheese would
furnish our present Army and Navy with 1,000 lbs. per man
per year, or, if divided with the armies of Great Britain, France,
England, and Italy, 13,000,000 men, each man would have
127 lbs. a year, or 0.35 lb. per day, furnishing 719 calories or
about 12 per cent of his daily ration.
Even if only half the skimmed milk from the creameries could
be worked up in this way, the figures are well worth considering.
When we think of the oleomargarine and filled cheese laws
which allow any farmer working under unsanitary conditions
to color the white butter from winter-fed cows and foist his
product on the public as "golden June butter," and at the same
time subject the makers and sellers of wholesome food products
to more taxes, fines and restrictions than are imposed on whiskey
dealers and saloon-keepers, we cannot help hoping that the day
may soon come when the members of Congress will be guided
by patriotism rather than politics and wipe these iniquitous
laws from our statute books.
Southern Cotton On, Company
25 Broad Street
New York City
CURRENT INDUSTRIAL NEWS
PERFUMERY FOR SIAM
Perfumery and cosmetics were imported into Siam during the
year 1915-16 to the value of over $105,000, the United Kingdom
being the chief supplier to the value of $30,000, followed by Japan
with $26,000. Under this classification are included all kinds of
perfumes and scented toilet waters, face powders, talc powders,
tooth pastes and powders, shaving soaps and creams, cosmetics
and lotions for the hair and face. American toilet requisites,
according to the Times Trade Supplement, seem to be taking well
on the market. The import duty on goods of this class is 3 per
cent ad valorem. — A. McMillan.
DESULFURATION OF HYDROCARBONS
The removal of sulfur from petroleum is a problem of first
importance and the following method adopted by La Fresnaye
et Suchy and for which a patent has been taken, is of interest.
The process hitherto adopted involving the use of ozone and
sulfur dioxide is only effective up to a certain point.
According to a report in the Chemical Trade Journal, 61 (1917),
331, it has been found that the sulfur can be removed by a simple
process of precipitation and without any decomposition, by
treating the oils to be purified with a metallic compound under
certain conditions after the addition of certain organic com-
pounds, such as ether and phenol compounds, trioxy benzoic
acid and trioxybenzole. The sulfur combines with the metal
and may be removed by filtration. Suitable metallic com-
pounds for this purpose are zinc carbonate, lead oxide and other
compounds of the heavy metals having great affinity for sulfur.
The amount of the metallic compound to be added depends,
of course, on the percentage of sulfur in the oil, and it is advisable
to use the metallic compound in excess.
One example of the process is as follows: 20 liters of oil having
sulfur content of approximately 0.5 to 1 per cent arc mixed with
300 cc. acetic ethyl ether in which are dissolved 5 to 7 g. tri-
oxybenzoic acid or trioxybenzole. To this are added 50 to 70 g.
lead carbonate or other suitable metallic compound, and the
mixture heated to a few degrees above the boiling point using a
reflux condenser or a closed vessel until a black precipitate is
f< .1 in. -.1 r 11 until tin liquid, at first turbid, becomes dear. If the
end point is too yellow, the liquid is ozonized to saturation
and then washed with caustic soda until the pyrogallol is removed.
\n ml containing ;i high percentage of sulfur should be converted
into a liquid oil by addition of ether and, if necessary, slightly
befon adding the metallic salts corresponding to the
sulfur content, At the conclusion of the process the ether added
is removed by distillation and the black residue is filtered off. — M.
LAMPBLACK MANUFACTURE
A process for the manufacture of lampblack from hydrocarbons
is the subject of a recent German patent, says Chemical Trade
Journal, 61 (191 7), 348. According to this invention a vessel
is charged with an inflammable mixture of gaseous hydrocarbons
and oxygen under pressure, the bottom of the vessel containing
a layer of liquid hydrocarbon in which a slow tension arc is set
up between two electrodes and decomposes the liquid with the
formation of lampblack, while at the same time the overlying
mixture is ignited. A tension of 200 volts is generally used and
must not in any case exceed 1,000 volts. By modifying the com-
position of the mixture, the decomposition can be retarded so as
to prevent excessive pressure and temperature. As an example,
a vessel with a capacity of 2 cm. is charged with 2/a gas and
Va liquid hydrocarbon, the first-named constituent being acety-
lene and the hydrocarbon consisting of high fractions from the
distillate of brown coal tar or crude petroleum. In addition
to lampblack, hydrogen, methane, carbon monoxide, ethylene
and heavy hydrocarbons are produced, the carbon remaining
in the liquid while the gases pass into the acetylene mixture.
Air is blown into the vessel and decomposes the acetylene, the
resulting hydrocarbons splitting up into carbon and hydrogen.
As the liquid charge thickens from the deposited carbon, it is
drawn off, filtered and returned with a fresh portion of charge.
Such of the carbon as is not deposited passes off with the effluent
vapors and is collected in a second vessel. — M.
BORIC ACLD AND BORAX
In the September issue of La Science et la Vie, an interesting
account is given of the utilization of the natural steam from the
volcanic area of Tuscany and of the manufacture of boric
acid and borax. The highly saturated steam issues from the
ground often at fairly high pressures, but, for purposes of con-
version, it is utilized for heating a scries of tubes containing
water, the steam pressure in these tubes being two atmospheres
(30 lbs. per sq. in.). The steam drives low-pressure turbines
which, in turn, are coupled to alternators. The steam and water
of these "soffioni," as they are termed, contain quantities of
boric acid which is concentrated in a special apparatus and gives
a product of about 99 per cent purity. The acid, treated with
sodium carbonate, gives borax, which is produced in the form of
crystals and powder. Ammonium carbonate is also manufac-
tured, the carbonic acid necessary for the p being also ob-
tained from the "soffioni." Investii ng carried
out on the radioactivity of the gases of the td on the
Separation of the lu'littit! whicli is fiiunil tn In pn .cut M.
74
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. i
POWER FROM REFUSE
In a circular illustrating some of their standard types of refuse
destructors, Messrs. Meldrums, Manchester, state that, although
with small amounts of refuse up to, say i or 2 cwt. daily, it is
not usually worth while to use the heat produced for raising steam,
a water heater can be combined even with the smallest de-
structor where a need for hot water exists, while with the larger
sizes burning a ton an hour or more it almost invariably pays
to install a boiler for purposes of steam raising, power, or heat-
ing. A portion of the steam is advantageously employed in
providing forced draught for the destructor, since, in this way,
the burning capacity is increased at least 50 per cent for a given
grate area. Several typical examples of the utilization of refuse
are given. At a large tannery in the Midlands a destructor,
placed in front of a Lancashire boiler and dealing with 150 tons
of spent tan a week, provides the whole of the steam required
for drying without any other fuel. By means of a three-grate
plant in conjunction with a Babcock and Wilcox water-tube
boiler, all the steam required for running a textile mill at Roch-
dale is generated from shoddy waste. — M.
MINERAL PRODUCTION IN CANADA
The following statistics of the mineral production in Canada
during 1916 are taken from the report recently issued by the
Canadian Department of Mines.
1916 1915
Quantity Value Quantity Value
Nickel 82,958,564 lbs. $29,035,497 68,308,657 lbs. $20,492,397
Lead 41,593,680 lbs. 3.540,870 46,316.450 !bs. 2,593,721
Asbestos 136,016 tons 5,133,332 111,142 tons 3,553,166
(1 ton = 2000 lbs.)
Natural Gas. . . 25,238,568 3,924,632 20,124,162 3,706,035
(1000 ft. unit)
Pyrites 309,411 tons 1,084,019 286,038 tons 985,190
Gypsum 341,618 tons 730,831 474,815 tons 854,929
Salt 124,033 tons 668,627 119,900 tons 600,226
Petroleum 198,123 bbls. 392,284 215,464 bbls. 300,572
Zinc (from zinc
ores) 23,515,030 lbs. 3,010,864
According to the report of the British Columbian Minister of
Mines, the output of zinc from the smelter at Trail in 1915 was
approximately 1,500,000 lbs. At the beginning of 191 7 the
output of the smelter was from 25 to 30 tons per day. — M.
COPPER AMALGAM AS METAL CEMENT
The Vienna metal cement, which is sometimes mentioned
in description of apparatus, is a copper amalgam. The Giesserei
Zeitung recommends the following method for the preparation
of this cement:
A strip of zinc is placed in a solution of copper sulfate and the
powdery copper which is precipitated is put into a mortar and
kneaded with mercurous nitrate, mercury and water into a plastic
paste; three parts copper are used to seven parts mercury. When
metals are to be cemented with this amalgam which is brought
into the market in small cylinders, the parts are polished and
heated up. The amalgam is heated up also to 80 or 900 C.
and the parts are pressed together, The amalgam, itself can be
hammered, rolled and put under a die; it takes a good polish.
Placed in boiling water it softens sufficiently to use it as a ma-
terial for taking casts. It is rolled into a thin strip which is
applied t<> the heated object; the replica obtained is afterwards
backed with type metal M
JUTE SACKS FOR ARGENTINA
It is estimated that the stocks of jute sacks available in the
Argentine Republic for carrying this season's crop of wheat,
oais, and linseed amount to 50,000,000, which are sufficient to
contain 3,000,000 tons of grain. As, however, the total crop is
expected to be more than don!. I, thai amount, a further 50,000,-
000 sacks or containers of some description will be wanted. — M.
JAPAN PEPPERMINT CULTIVATION
We hear, says the Monthly Trade Journal, that steps will
soon be taken at Hokkaido, where the chief peppermint cultiva-
tion of Japan is carried on, to systematize the cultivation of the
planting and the manufacture of menthol. In the past the sun-
drying process especially has left much to be desired and, while
the peppermint in the shape of crude oil has so far been shipped
to Yokohama and Kobe where it is distilled in the factories, it
is now proposed to erect factories in the chief farming districts
on a cooperative basis.
Peppermint oil derived from the residue of oil after being
properly refined is finding every year a larger demand abroad.
Before the war the largest customer of Japanese menthol crystal
was Germany, while to-day America is taking at least 88 per cent
of the total output. The average price has been between Si
and $1.50 per lb., while several factories at the end of 1916 sent
circulars to their chief customers announcing that, owing to cir-
cumstances, prices were likely to go up during 1917. This did
not happen owing to improved factor)' conditions. During 1916
about 525,000 lbs., valued at $1,031,250, were produced. — M.
NON-INFLAMMABLE PLASTIC MATERIAL
A recent French patent, says the Chemical Trade Journal,
61 (191 7), 365, describes a new plastic material which is non-
inflammable and inodorous. The material is produced by trans-
forming gelatines, glues and such substances of animal origin
by suitable chemical reagents giving them plastic and malleable
properties which allow them to be used industrially in a manner
similar to natural products.
The gelatine or glues are first melted in a water bath at a tem-
perature of 90 ° C. A decoction of hop-flowers is then prepared
and mixed with dilute oxalic acid or any dibasic acid of that
series and the solution is added to the melted gelatines or glues
in varying proportions according to the quality of the materials
used. The addition of this solution causes the gelatine to be-
come more supple and also causes the impurities to deposit at
the bottom of the vessel. When the gelatines are liquefied,
they are poured out in the form of thin sheets or sticks of the de-
sired thickness and left to dry in the cold air.
The coloring of the material is then proceeded with, natural
or artificial dyes being employed The sheets, when colored,
arc plunged into a bath of approximately the following composi-
tion: 25 to 35 percent formaldehyde, 25 to 35 per cent water,
25 to 35 per cent alcohol and the rest composed of oxalic acid,
tannin and glycerine. The oxalic acid may he replaced by any
acid of that series. In the case of rich gelatines, a larger per-
centage of alcohol is used.
The substances may serve for the manufacture of combs,
buttons, etc., and as imitation of tortoise, horn amber or ivory
and is unlike cellulose products in being absolutely non-in-
flammable and odorless M
ELECTRIC LAMP TRADE IN JAPAN
lap. in. v.ivs the Electrician, appears likely to be a serious com-
petitor in the incandescent lamp trade. In 1 y 1 (1, the Japanese
exports of incandescent lamps were value I at $335,000 and in
the first four months of the current year at 5440,000 or at the
OO per year These figures are to be compared
with no exports and with exports of the value of Siso.ooo in
tin yeai prior to the u.ir The one difficulty the Japanese lamp
manufacturers have had. was in the supply of filaments, prac-
tically all of which used to be imported. Now. however, only
a small fraction of the filaments usi ' are imported. Large
factories have been constructed and th J se manufacturers
are now in a position to supply their own filaments. — -M.
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
7S
IMITATION LEATHER FOR SWITZERLAND
Supplies of imitation leather on the Swiss market and the
scarcity of real leather have produced an exceptional demand
in that country. French manufacturers are supplying an ac-
ceptable quality with a waterproof lining of rubber but are not
now in a position to give good deliveries. Their total output
comes far short of Switzerland's present needs in imitation leather.
Some of the uses to which imitation leather is put are drivers'
seats and upholstering of motor cars, upholstering of furniture,
cabinets and in making school satchels, while heavier qualities
are employed in book-binding.
Manufacturers are recommended to equip agents with the
necessary catalogs, price-lists and samples. Light but strbng
packing material is essential, this being important on account
of tariff treatment. Motor-car upholsterers ask for antique or
Moorish designs. A favorable dimension is 36 ft. long by 4 ft.
to 4 ft. 9 in. wide. The price paid per piece varies from $2 to
$8. It is not thought likely that the Swiss boot manufacturers
will as yet adopt artificial leather. — M.
NEW MAGNESIUM ALLOY
The new magnesium alloy which the Chemische Fabrik Griesham
Elektron is introducing under the name of Elektron Light Metal
seems to be a war substitute only likely to subsist under war
conditions. It is described as a silvery white metal, density
1.8, which melts at 620° C, and will burn only in shape of thin
foil. It resists the action of caustic alkalies which would attack
aluminum, and is said to be sufficiently strong and otherwise
suitable to serve in the place of aluminum, copper and brass,
also as an electric> conductor. It is, however, acknowledged
that the alloy is corroded by dilute acids and oxidizes in the air,
though not superficially. — M.
ELECTRO-STEEL WORKS IN GERMANY
During the past two years, says Engineering, 104 (1917),
469, ten electro-steel works of the Lindenberg type have been
built and put into operation in Germany and Austria, their
aggregate capacity being 125,000 tons annually. Another
eleven works are in course of construction with an aggregate
capacity of 220,000 tons per annum and they will be started
in the course of the next few months.
The Lindenberg Steel Works of Remscheid-Hasten showed a
surplus for last year of $606,261 against $337,081 for the previous
year. The dividend is given as 25 per cent in addition to a bonus
of 10 per cent.
The German Electro-Steel Company has raised its capital
to $200,000 and a further increase of $400,000 is contemplated,
the domicile of the company being removed from Berlin to
Saxony. — M.
FATS AND OILS
According to a recent German patent, the greases recovered
from technical processes dealing with such substances as wool,
leather, faeces, etc., by extraction, mostly contain saponifiable
and unsaponifiable matters which can be separated by a treat-
ment based on the fact that the latter can be volatilized by the
vapors of inert liquids. For example, crude sewage fat is first
saponified as completely as possible by the treatment with an
alkaline earth or a metallic oxide, and the dry, anhydrous mass
of soap is subjected to the action of superheated steam in a
suitable still at a temperature above 200° C. The unsaponi-
fiable oil passes over with the steam, leaving behind in the still
a soap which, when decomposed with acid, yields fatty acids
free from unsaponifiable fats and oils. The steam may be re-
placed by highly heated vapors of benzine, carbon tetrachloride,
• ■ 1 1 ■ . M
NEW BRITISH DYE
The announcement has been made by the British Dyes, Ltd.,
Huddersfield, that they are now placing on the market two
brands of a yellow vat dyestuff of the anthracene series under th e
name of chloranthrene yellow D. & G. This yellow, it is said,
will be of great value to the textile trade as a self-color on ac-
count of its fastness to light, milling, washing and bleaching.
It may also be used with great advantage in conjunction with
chloranthrene blue for the production of various shades of fast
green on vegetable fibers. The investigation of other dyes
of the same class is being pursued successfully and these will
shortly be available to the dyeing industry. — M.
WATER-PROOF GOODS FOR SOUTH AMERICA
Fully 70 per cent of the water-proof goods imported into Argen-
tina are of British origin, but in come of the other states, such
as Chile, Colombia and Venezuela, the last few years have wit-
nessed a not inconsiderable increase of German and French
made goods of this description. This market, says the Times
Trade Supplement, is well worth attention and now that the com-
petition from Germany is, for the moment, out of the way, it
seems an opportune time for manufacturers to press their wares.
The duty payable on water-proof coats — ponchos — large square-
shaped sheets of water-proofed material provided with a hole in
the centre for the reception of the head, with neck capes, etc.,
for men and women, is 42 per cent upon an arbitrary value of
$6, and one-half of that rate for children's garments. The
growth of the import trade has been notable, since in five years
it has doubled itself. Thus, in 1909, the number of water-proof
articles did not exceed 12,179, worth $70,377; while, by the end
of 1913, the total was 24,328 articles valued at $137,313. Of,
these, the United Kingdom provided 70 per cent, Germany 10
per cent and France 15 per cent. Only the cheapest grades
are manufactured locally. Silky materials are not much in de-
mand, as the heavy rains of the country usually penetrate any
but the thickest materials. Those with a proportion of wool
are sometimes asked for. — M.
JAPANESE GLYCERINE
The British Commercial Attache at Yokohama reports that
the manufacture of glycerine was first commenced in Japan in
19 16, when new plants were established by Government subsidies.
The output of glycerine from these works is increasing, but is
not sufficient for home demands, and refined glycerine is still
imported from the United States. One Japanese company
produces 70 tons glycerine monthly. The imports of glycerine
to Japan in 1916 were 800,830 Kin (1 Kin = 1V3 lb.), com-
pared with 1,712,912 Kin in 1914 and 1,430,922 Kin in 1913.
Until recently Japanese fish oil was used as the basis for the manu-
facture of glycerine, but, with the expansion of the industry,
animal fat from Australia and cocoanut oil from the South Seas
are being used. The use of bean oil for this purpose is also under
investigation, but the stability of the product for use as a con-
stituent of dynamite has not yet been determined. — M.
WATER-PROOF AND DUST-PROOF FABRICS
The skin which forms on the surface of some oil paints and
varnishes is practically air-tight. Engineering, 104 (1917), 340,
quoting from a German contemporary, says that such a skin,
which seems to be water-proof and dust-proof, can be formed on
sacks of jute and on bags of cardboard, etc., for the transport
of lime, chalk, cement and dextrine as well as for packing greasy
and oily materials. The process is described as the Pltiss-
Staufier process, but there are no further particulars. It is
merely stated that the skin is pressed upon the material, which
deed not be a texture, by special machinery. — M.
76
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. i
RECOVERY OF PLATINUM METALS FROM CANADIAN
NICKEL
The Report of the Royal Ontario Commission on Nickel,
issued recently, states that although the presence of gold and
silver and of metals of the platinum group in practically all
nickeliferous pyrrhotites has long been known, their importance
in connection with the Ontario nickel industry is not recognized
except by those who recover and sell them. The nickel-copper
ores of Sudbury are said to be capable of producing more pal-
ladium than the whole of the present world supply together
with a large proportion of platinum, iridium and other metals
of this group. The quantity of palladium present is much in
excess of the platinum, but iridium, rhodium, ruthenium and
osmium are also found. Although it is not possible to state
exactly the actual quantity of the platinum metals present in
the ores, the quantity recovered can be ascertained from the
atsay of the matte, provided the number of tons of ore smelted
per ton of matte is known. In the year ending Dec. 31, 1916,
the total ore smelted at Sudbury amounted to 1,521,689 tons
with a production of 80,010 tons of matte. One company,
which produced 63,567 tons of the total given above, states that
the average content of precious metals per ton of matte for the
three years ending 1 9 1 5 was as follows: Gold, 0.050 oz. troy;
silver, 1.75 oz. troy; platinum, 0.10 oz. troy; palladium,
0.15 oz. The report also discusses the advisability of utilizing
the large quantity of sulfur at present expelled as sulfurous
anhydride (S02) in roasting, it being estimated at not less than
300,000 tons of sulfur which would produce 1,000,000 tons
sulfuric acid. — M.
GUTTA-PERCHA FROM THE SHEA BUTTER TREE
A supplement to the official Nigeria Gazette for August pub-
lishes a note to the effect that a trade in what is known locally
as gutta-percha — a substance prepared from the latex of the Shea
butter tree — has sprung up during the last two years in the Prov-
ince of Bornu. The local price of the product at Nafada is
8 cents per lb. The method of collecting and preparing the
product is given as follows: Small pieces of the bark are chipped
out of the tree with a narrow native axe. The latex that slowly
exudes from these cuts is scraped off as it contains impurities
such as dirt, bark, etc. It is then boiled until the impurities
float to the top when they are removed. The latex then coag-
ulates and, in this form, is known as gutta-percha. It is not
advisable to tap trees of less girth than 30 inches. The Shea
butter tree is abundant in many parts of the Northern Provinces,
and especially so in Meko, Shaki and Oyo districts of the Southern
Provinces and in Ilorin. When collecting this product, the tap-
pers could with advantage collect the Shea nuts and thus help
to stimulate the trade in Shea butter. — M.
BRITISH PAPER EXPORTS
Since the war started, the export trade in paper from Britain
has been seriously affected. The total quantity exported last
year amounted to 2,556,621 cwt., a decline of 198,063 cwt.
compared with 1915, 567,685 cwt. compared with 1914, 942,-
293 cwt. compared with 1913, and 772,840 cwt compared with
1912. hi the year's total ;.' 70 pei cenj represented the ship
ments to British Possessions, and 27 j pel cent to foreign coun-
tries. Taking the figures for 191 ■. the trade with British
Possessions represented 70.7 per cent of the total exports and
that with foreign countries 29.3 pei cent. 01 course, some
markets have suffered more than others in regard to reduced
supplies, c. g., a subsianti.il shrinkage in shipments to India is
shown, while the position of S Africa and Australia appears to
ibli France rea ived 1 p ipi 1 from Britain last
year than in the pre war period. M.
LOW-GRADE ORE UTILIZATION
According to a report in Stahl und Eisen of July, 1917, we see
that the war, the stopping of imports and the rise in prices have
forced German metallurgists to make use of raw materials which
were considered too poor in peace times. In several cases,
sufficient success has been obtained by new methods to justify
the working of low-grade ores even in normal times. Thus
copper schists were hardly utilized when they contained only
2.5 per cent copper. Now ores of 1 per cent and even 0.7 per
cent find utilization. As regards iron and steel, there has not
been much change, but poor pyrites and phosphatic ores are no
longer rejected. The vanadium for steel is found in sufficient
bulk in slags which do not contain more than 0.7 percent vana-
dium; the wolframite of old waste heaps is a raw material for
tungsten; chrome ore of 24 per cent is welcome — half the per-
centage formerly deemed worth mining — and sources of nickel
are worked if they contain 1 .5 per cent of nickel ; bauxite of
40 per cent aluminum is considered sufficiently rich. It is also
stated that the aluminum can, after all, be got out of clay. There
is no change as to arsenic and antimony Sulfur, no longer
obtainable as such, is gained from gypsum and anhydrite and
phosphates of 20 per cent are converted into manure. — -M.
SWEDISH INDUSTRIAL DEVELOPMENTS
The Helsungborg Copper Works, among other extensions,
are about to begin the manufacture of electrolytic copper on a
large scale. Detailed plans have been prepared and the work
will be proceeded with as fast as the necessary raw materials
can be obtained. One of the most important departures is the
formation of a large chemical company with plenty of capital
and excellent men at its back, in addition to which a large number
of chemical engineers have been connected with the undertaking
which will boast the largest laboratory in Sweden. The pro-
gram is a very comprehensive one and is based not only upon
home consumption but also to some degree at least upon exports.
So far the preliminary labors have principally been confined to
dyestuffs of which Sweden formerly imported 1,000 tons from
Germany. Benzole is the principal raw material; but this, as
well as most of the chemical substances required, can be produced
within the country, as is also the case with most of the plants.
The work is intended to commence in 191s — M
BRITISH BOARD OF TRADE
During the month of October, the British Board of Trade
received inquiries from firms in the United Kingdom and abroad
regarding sources of supply for the following articles. Firms
which might be able to give information regarding these things
are requested to communicate with the Director of the Com-
mercial Intelligence Branch, Board of Trade, 73 Basinghall St.,
London, E. C.
MACHlNb'KV AND PLANT FOR:
Guillotine. 30 in. for cutting
paper for dice cups
Handlin. peat
Producing small wire articles such
Chemicals:
Arsenious oxide, pure, snow-white
Carbonate of lime, granulated
Carbonate of sodium
Sulfate of sodium
Vanadate of lead or mottramite
Borate of m.ikncsium
Tartaric acid substitute
Bone pitch (* tons)
Composition fittings for glass
Compositiaa (with shellac base) for
■ phone records
Davy thermometers
Kbony goods, toilet brushes, trays,
mirrors
Hair-slides, metal fittings for
Jcttoline asphaltum
! .nikins and paper piercer?
Leather, suede
. cones
for making small
wood for mending
Metal u
ceJlulo
fish-nc
Novelty .
ointment
Perforate
- of synthetic
Steanne |te saponified,
solid
Studs and links cheap, gilt carded
ip briar, plated
for punching papers for
mounts
\
Africa
tlet, eheap, for West
M.
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
77
SCIENTIFIC SOCIETIES
DECENNIAL INDEX PATRONS
In order to print the Decennial Index to Chemical Abstracts
it became necessary to ask the friends of the American Chemical
Society among the chemical corporations to assist in the work
of donating $10,000 toward the fund required. This was done
after $25,000 had been subscribed by members of the Society
and others directly interested in purchasing the publication.
The donations were asked for first through the local sections.
The Philadelphia Section secured donations in the amount of
$1,510.00; the Indiana Section, $50.00; the Pittsburgh Section,
$50.00; the Detroit Section. $25 .00; and the New York Section,
$25 .00, from local firms. A general request was then sent from
the Secretary's office to fhe chemical industries of the country,
asking for help on this important publication. The response
was immediate. The Society desires to acknowledge with
thanks the help of its friends listed below:
Alberene Stone Company $ 10.00
Aluminum Castings Company 50 . 00
Aluminum Company of America 100.00
American Can Company 150.00
American Cotton Oil Company 50 . 00
American Glyco Metal Company 25 . 00
American High Explosives Company 25 .00
American Smelting & Refining Company 250.00
American Zinc Lead & Smelting Company 100.00
Anaconda Copper Mining Company 250.00
Arlington Mills 100.00
Atlantic Refining Company 50.00
Ault & Wiborg Company 100. 00
Badger & Sons, E. B 100.00
Baker & Company, Incorporated 100.00
Barrett Company, The 250.00
Bausch & Lomb Optical Company 100.00
Berlin Mills Company 100.00
Buffalo Foundry & Machine Company 100.00
Butterworth Judson Corporation 50 . 00
Castner Electrolytic Alkali Company 25 . 00
Celluloid Zapon Company 25 . 00
Columbia Chemical Company 25 . 00
Commonwealth Edison Company 100.00
Detroit Testing Laboratory 1 0 . 00
i Devine Company, J. P 100.00
Digestive Ferments Company 5 . 00
Dow Chemical Company 50.00
Du Pont de Nemours Company, E. 1 1 , 000 . 00
Duriron Castings Company 25 .00
Eastern Manufacturing Company 100.00
Eastman Kodak Company 50.00
Edison, Thos. A., Inc 100.00
Eimer & Amend 100.00
Elyria Enameled Products Company 50 . 00
Fels & Company 25.00
Fisk Rubber Company 100.00
General Bakelite Company 100.00
General Chemical Company 500.00
General Electric Company 250.00
Grasselli Chemical Company 50.00
Harshaw Fuller-Goodwin Company 1 00 . 00
Heinz Company, H.J 100.00
Heyden Chemical Works 250.00
Hurlburt. E. B 25.00
Interocean Oil Company 25.00
Jeffery-Dewitt Company 25.00
Knight, Maurice A 100.00
Lennig Company, Charles 25 .00
Lillv & Company, Eli 50.00
Lindsay Light Company 100.00
Mallinckrodt Chemical Works 50.00
Marden, Orth & Hastings 25.00
Mathieson Alkali Works 250.00
McElwain Company, W. H 100.00
Merck & Company 250.00
Monsanto Chemical Works 50.00
Morgan & Wright 25.00
National Aniline & Chemical Company 200.00
National Carbon Company 70.00
National Lamp Works of the General Electric
Company 50.00
National Lead Company 100.00
NisiK.ira Alkali Company 50.00
' I ompany 100.00
Oakland Chemical Company 50.00
Pacific Coast Horax Company 100.00
Pennsylvania Rubber Company 50.00
Pennsylvania Salt Company 100.00
Pfaudicr Company 25.00
Philadelphia Quartz Company 1 5 . 00
Pittsburgh Plate Glass Company 100.00
Powers-Weightman-Rosengarten Company 50.00
Primos Chemical Company 25.00
Procter & Gamble Company. 1 In- 250.00
Raymond Bros. Impact Pulverizer Company ... 25.00
Republic Chemical Company. Inc 25.00
Roessler & Ilasslacher Chemical Company 100.00
Rohm & Haas 25.00
Rome Soap Manufacturing Company 25.00
Rosenwald, Julius
Sargent & Company, E. H
Schaar & Company
Schoellkopf. J F
Scoville Manufacturing Company
Sellner, Albert
Smith, Kline & French Company
Sowers Manufacturing Company
Sprague, Warner & Company
Squibb & Sons^ E. R
Standard Oil Company of New Jersey
Swenson Evaporator Company
Textor, Oscar
Thomas. Arthur H., Company
Thorkildsen Mather Company
Toch Brothers
Union Oil Company of California
Union Sulfur Company
United Engineering & Foundry Company
United States Smelting & Refining Company. . , .
Victor Talking Machine Company
Virginia-Carolina Chemical Company
Washington Steel & Ordnance Company
Weston, Edward
Whitall Tatum Company
Anonymous
100.00
100.00
10.00
200.00
100.00
5.00
20.00
25.00
25.00
50.00
250.00
25.00
5.00
100.00
100.00
25.00
100.00
100.00
25.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
TENTH ANNUAL MEETING
AMERICAN INSTITUTE OF CHEMICAL ENGINEERS
ST. LOUIS, MO., DECEMBER 5-8, 1917
The tenth annual meeting of the American Institute of Chemical
Engineers was called to order at Hotel Statler, St. Louis, at 9.45
a.m., by President G. W. Thompson. As the local section of
the American Chemical Society participated in the meeting,
the Chairman of the Section, Mr. A. C. Boylston, assisted Presi-
dent Thompson in conducting this and other sessions of the
meeting.
The address of welcome was delivered by Mr. Wm. T. Findly,
representing Hon. Henry W. Kiel, Mayor of St. Louis. Pres-
ident Thompson responded to the address of welcome.
The ballots for officers were canvassed by a committee con-
sisting of F. E. Dodge, R. S. Bicknell and S. F. Grove. The
following officers were elected: G. W. Thompson, President,
J. C. Olsen, Secretary, F. W. Frerichs, Treasurer, M. Toch,
Auditor, and A. W. Smith, T. B. Wagner, D. Wesson, Directors.
The Council reported the appointment of a committee to con-
sider the advisability of appointing a representative of the
Institute on the joint committee of the Engineering Societies in
cooperation with the United States Government in its war activi-
ties. The committee consists of: G. W. Thompson, Chairman,
Chas. F. McKenna, M. H. Ittner, J. C. Olsen.
The Council has also authorized the purchase of $750.00 of
Bonds of the second U. S. Liberty Loan.
The membership of the Institute at present is 283, consisting
of 1 honorary member, 241 active and 41 junior members.
The membership during the past six months has been increased
by 1 2 active and 3 junior members. During the past year the in-
crease has been 28 active and 5 junior members, making a net
increase of 33 members, which is a larger increase than during
any previous year.
The Secretary reported that six members had received com-
missions in the United States Government service as follows:
Edward Bartow, Major in Sanitary Corps in National Army.
Hardee Chambliss, Major. Ordnance Sec, Officers' Reserve Corps.
A. R. Chandler, Captain, Ordnance Dept., U. S. R., Rock Island Arsenal,
Rock Island. 111.
A. S. Cushman, Major, Ordnance Dept., U. S. R., Frankford Arsenal.
R. M. Gage, First Lieutenant, Sanitary Corps, U. S. Army.
A. H. White, Captain, Ordnance Dept., U. S. R.
The Treasurer reported a balance on hand of $1616.00.
The Committee on Meetings reported the following localities
under consideration for the summer meeting to be held the latter
part of June: Chicago, 111., Syracuse, N. Y., Providence, R. I.,
and Newark, N. J. After sonic discussion the matter was re-
ferred t<> tin- Council for decision.
78
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. i
The first paper on the program was "The Relation
Efficiency of Refrigerating Plants and the Purity of Then Am-
monia Charge," by Dr. F. W. Frerichs of St. Louis, In a
preliminary statement Dr. Frerichs stated that a large amount
of ammonium nitrate is required for the manufacture of ex-
plosives and that most of the ammonia obtained from the by-
product coke-oven plants is in the form of ammonium sulfate.
There is only one plant in the United States, viz., that of
Herf and Frerichs in St. Louis in which aqua ammonia can be
made from ammonium sulfate, and this plant is engaged in
producing liquid ammonia for the refrigerating industry. Upon
request of the Food Administration of the United States, the
capacity of this plant is being increased 50 per cent in order to
secure an ample supply of liquid ammonia for tin cold stora^i
warehouses and the ice plants so as to conserve the food supply.
In order to obtain an adequate supply of aqua ammonia
for the manufacture of ammonium nitrate, in the manufac-
ture of explosives, Dr. Frerichs has been requested by the
United States Government to erect eight new plants, the
size of the St. Louis plant, at various points. Dr. Frerichs
has generously offered the Government complete plans
and specifications and the use of his patents for the duration of
the war, the plants to be dismantled at the close of the war.
In the paper presented, the results of tests made by the Bureau
of Standards were given which showed that the ammonia made
by Dr. Frerichs contained only one-thousandth of one per cent
of organic impurities and that other samples of commercial
liquid ammonia contained as high as 450 thousandths of one
per cent of such impurities. Impurities of this kind produce
permanent gases in ice machines which greatly reduce the effi-
ciency of the process. This was shown in a practical test with
two identical ice machines. With pure ammonia 57 tons of
ice were made while with impure ammonia only 42-44 tons were
made daily. During the entire test period 16,862 tons of ice
were made in the first machine, while only 1 1,308 tons were made
in the second. A very much greater amount of the impure
ammonia was required so that the cost of ammonia per ton of
ice using pure ammonia was only 1 .27 cents per ton while the cost
was 15.16 cents with impure ammonia. The coal consumption
was one ton for eight tons of ice with pure ammonia, and only
5V2 tons of ice per ton of coal with impure ammonia,
Serious leaks due to corrosion were observed in the machine
using impure ammonia, while there was no trouble of this kind in
the machine using pure ammonia.
A paper by Wm. M. Booth of Syracuse, N. Y., on "Distilled
Water" was then read. The author presented the results of
many analyses of distilled water, rain and snow water, and also
the requirements for purity in various industries. This was
supplemented by a large number of letters from users and pro-
ducers of distilled water. Various types of apparatus for the
production of distilled water were then presented.
Wednesday afternoon members of the Institute and St.
Louis Section of the American Chemical Society went by
automobile to the very large ice plant of the Anheuser-Busch
Brewing Association. This plant has a capacity of [2O0 tons 01
ice pel day and is the largest plant of its kind in the world
The party then proceeded to the plant of the Herf and Frerichs
Chemical Works. Construction work was here going on both on
the extension of the ammonium sulfate plant and on a new plant
designed to use ammonia liquors from gas works. Large circular
reinforced concrete tanks were being Constructed for the storage
of ammonia gas liquors, To prevent leak 1 e thesi 1 inks were
placed within a larger rectangulai concrete tank which is
kept full of water.
The liquid anhydrous ammonia wis being produced from am-
monium sidfate. This salt is treated with lime and tin eon
ammonia absorbed in water. From this it is distilled, dried by
lime and compressed to 250 lbs. The gas is washed by means of
liquid ammonia, then cooled and charged into s teel cylinders.
Tin purity of the liquid ammonia is assured by testing a sample
drawn from each cylinder.
The party then visited the By Product Coking Plant of the
Laclede Gas Light Company. The rich portion of the gas from
the coke ovens is sold as illuminating gas, while the leaner portion
is used for heating the by-product coke ovens. The illuminating
gas for St. Louis is sold on the B. t. u. standard of 650 per 1000
cu. ft.
The gas is first cooled which removes the tar and about one-
fifth of the ammonia, the remainder being absorbed in dilute
sulfuric acid. The gas is then passed through a tower containing
parafiine oil which removes the benzine and toluene. The light
oil is distilled out of the parafiine oil which is used again for
scrubbing the gas.
The party was very much interested in inspecting the stills
in which the light oil is fractionated to separate the benzene
from the toluene.
( m Wednesday evening the members of the Institute and of the
local section of the American Chemical Society took dinner at
the St. Louis Club as the guests of Dr. F. W. Frerichs. The
very handsome club house was much admired. The dinner was
held in the spacious dining-room on the second floor, which was
beautifully decorated with flags. Covers were spread for about
eighty. After dinner. Dr. Frerichs gave a cordial welcome to
his guests in a few well-chosen remarks. President Thompson
and Mr. A. C. Boylston, chairman of the local section of the
American Chemical Society, responded
President Thompson then delivered an address on "Our
Resources." Attention was called to not only the natural
products in which the United States abounds but also to de-
ficiencies, and suggestions were made as to measures which
should be taken to render the United States independent of
foreign sources of supply. The achievements of the American
chemists during the war period were especially emphasized with
reference to platinum supplies. President Thompson suggested
that there were large quantities of platinum in the form of
jewelry wdiich should be made available for the war needs of
our country.
The Secretary, Dr. J. C. Olsen, expressed the appreciation
of the members of the Institute and of the American Chemical
Society for the very delightful dinner which had been provided
by Dr. Frerichs, affording such an opportunity for making the
acquaintance of the local chemists; of Dr. Frerichs' courtesy in
showing his ammonia plant, at which the purest ammonia made
in the United States is manufactured; and of the patriotism of
Dr. Frerichs, who, although born and educated in Germany,
offered his services so freely to the Government. Vigorous
applause indicated hearty endorsement of the sentiments ex-
pressed.
Mr ( 1. F. Soule, of the Merrill-Soule Co. of Syracuse, then ex-
plained briefly the process of evaporating milk by atomizing it
under high pressure into a chamber, through which a current of
warm air was passing. The entire proce; ■. is illustrated by
moving pictures Samples were shown of evaporated skimmed
milk, and also evaporated cream containing 74 per cent
of butter fat. The remainder of the e\ ening was spent in getting
acquainted, the occasion being voted by all as a highly enjoyable
one.
Thursday morning the pum proceed' i by automobile from
Hotel Statlcr to the City Water Works Mr. E. E. Wall, water
commissioner of the City ol St ned the history of
the development of water purification in St. I.ouis and gave an
outline of the process employed for purifying water. This
consists of pumping the water ti ■ tmber where
about .-s per cent of the solids, consisting 1 inlj of sand, settles
out. The water is then treated with lime which reduces the
hardness from over 300 to slightly over per million.
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
7 9
Sulfate of iron is then added which produces flocks of hydrate
of iron which remove the finely suspended impurities. A
charge of aluminum sulfate is also given to remove coloring
matter. The water is then pumped into large settling basins
where most of the sludge settles out. The remainder of the
suspended matter is removed by filtering through sand filters,
after which the water is treated with liquid chlorine to remove
the remainder of the bacteria.
The party then inspected the plant. The washing of one of
the sand niters was watched with the greatest of interest. The
automatic devices for adding the lime, ferrous sulfate and alu-
minum sulfate were carefully examined. The lime is added as
milk of lime, the ferrous sulfate automatically fed in powdered
form, while the aluminum sulfate is added as a solution of
standard strength. The excellent condition of the entire plant
and its simple operation were greatly admired.
The party was then taken to the Riverside Club where luncheon
was served in the spacious and beautifully decorated dancing
pavilion of the Club.
After luncheon the party drove to Granite City where the
plant of the National Enameling & Stamping Company was
visited. Here the production of the enamel, grinding and dipping
of the enamel ware were shown, as well as the furnaces in which
the material is baked. The stamping machines were also in-
spected with great interest, as well as the electric welding of
handles and other parts of the enamel ware.
On Thursday evening, a joint meeting with the local section
was held at Hotel Statler. A paper by Gaston Du Bois of the
local section on "Engineering and Chemical Works" was first
read. Dr. Du Bois called attention to the deficiency of many
chemists in knowledge of engineering problems met with in the
construction or operation of chemical works, and pointed out
the deficiency of the preparatory education of many chemists in
this respect. A very lively discussion followed the paper as to
the amount of chemical engineering training which should be
given in the schools and the amount which could only be learned
by experience in the chemical industry.
A paper on "Organization of Chemical Companies" was read
by Mr. Frank Hemingway. The author showed that the lack
of cooperation between the business interests and the technical
staff of corporations lead to lack of efficiency and in many cases
to failure of companies which otherwise had every prospect for
success.
On Friday morning the members and their guests left the
Hotel Statler by automobile for the plant of the Commercial Acid
Company. At this plant the sulfuric acid chambers were in-
spected. Louisiana sulfur was used as the raw material. The
capacity of the chamber plant was 240 tons of 66 Be. acid. The
nitric acid plant was then inspected, special interest being shown
in the horizontal cast iron retorts and in the sewer pipe conden-
sers. The manufacture of hydrochloric acid was then shown,
shallow iron pans being used for the salt and acid. The phenol
plant was also inspected. In this plant benzene is treated with
sulfuric acid. The resulting product is neutralized with lime
and sodium carbonate and is then added to fused caustic soda.
After neutralization, the phenol is distilled olT into iron drums.
Some of the members then visited the plant of the Laclede
Christy Fire Clay Company.
During the forenoon, three papers were read on the general
subject of Evaporation and Drying. Mr. Hugh K. Moore, of
Berlin Mills, X. II., read the first paper on "Some General
Aspects of Evaporation and Drying." Mr. Moore gave an out-
line of all methods of evaporation and drying which are possible
or available, and he gave the conditions under which each method
could be used to advantage. He discussed at greater length
heat conductivity phenomena in evaporator tubes and more
particularly forward and backward flow in multiple effect
evaporation, and showed the great advantages to be derived
from backward flow operation. This phase of his paper was dis-
cussed at considerable length.
Mr. F. M. deBeers read the paper on "Some Problems in
Evaporation and Drying" presented by Mr. P. B. Sadtler and
F. M. deBeers. Mr. deBeers presented the practical difficulties
which are met with in designing evaporators and especially
methods of overcoming such difficultieswhen very viscous liquids
must be evaporated.
Mr. H. McCormack, of Chicago, read a paper on "Evaporation
and Drying of Tannin Extracts by the Carden Process." In
this process the tannin extract is atomized and the spray evap-
orated by a stream of warm air. The product produced is
superior in every respect to the extract produced by other methods
of evaporation.
Friday evening the subscription dinner was held at Hotel
Statler. The attendance of sixty-three was about equally
divided between members of the Institute and of the American
Chemical Society. Music was furnished by Mr. F. W. Saltan,
violinist and Miss Elsa Diemer soloist accompanied by Miss
Mina Neaman.
President Thompson acted as toastmaster and presented
Alex. S. Landsdorf, Professor of Electrical Engineering and Dean
of the School of Engineering of Washington University. Pro-
fessor Landsdorf described the work carried on by the University
and exhibited a considerable number of lantern slides showing
the buildings, grounds and laboratories of the University.
Dr. B. M. Duggar of Shaws Garden explained the founding of
this remarkable botanical collection, and the work which is
being done at present at the Garden.
Secretary Olsen gave a toast to the ladies, and pointed out
that the attendance of the ladies at this meeting was the largest
in the history of the organization and that much of the pleasure
at the meeting was due to their presence.
Dr. Chas. E. Caspari, of the St. Louis College of Pharmacy,
was introduced as the recently elected Chairman of the local
section of Lhe American Chemical Society, and spoke of the
work being carried on by this section, and also of his high opinion
of the influence of the American Institute of Chemical Engineers
on the chemical profession.
On Saturday, the plant of the National Lead Company at
Collinsville, Mo., was visited, the mechanical furnace being of
special interest to those who made the trip.
A special program had been arranged by the local Ladies' Com-
mittee under the chairmanship of Mrs. A. A. L. Veillon for the
entertainment of the visiting ladies. This program included on
Wednesday a luncheon with members of the Institute at Hotel
Statler; a sight-seeing trip of St. Louis by automobile;
a dinner at the Hotel in the evening, followed by a
theatre party. On Thursday the ladies accompanied the
men during the visit and inspection of the City Water Works as
well as at the complimentary luncheon at the Riverside Club.
During the afternoon the ladies were entertained at tea by Mrs.
Queeny at her residence, 3453 Hawthorne Boulevard. On
Thursday evening the ladies attended a theatre party at the
Jefferson Theatre. On Friday morning Mrs. Veillon gave a
musicale at her residence, 4222 Flora Boulevard. During the
afternoon, Shaws Garden was visited, and in the evening the
subscription banquet was attended.
Although a considerable number of members could not attend
the meeting on account of urgent war duties, the usual number
were present at most of the meetings and functions, the attend-
ance ranging from 50 to 100.
The St. Louis members proved to be very royal hosts, and
the members of the Institute were interested to find so many
important chemical industries in this locality.
Coopbr Union J. C. OlsEN, Secretary
December 15, 1917
8o
THE JOURNAL OF INDUSTRIAL AND ENGINEERING I II i RY Vol. 10, Xo. i
AMERICAN CHEMICAL SOCIETY PIN
Arrangements have been made for obtaining the Society pin
at a cheaper price, one of 14 kt. gold of the same quality as the
one now used, and one in rolled-gold which will have- the same
appearance, but will be cheaper. The pin will have a safety catch
and will In- of such length that the wearers will not be subject
to being scratched. Members will please note the following:
1 — The pins are ready for delivery.
2 — The solid 14 kt. pin will be carried in stock at $3.00. plus 3 per
cent war tax— totol. 5
3 — The rolled-gold pin will be carried in stock at $1.00. plus 3 per
cent war tax — total. SI. 0.1.
4 — To obtain pins members must be in good standing and obtain an
order from the Secretary of the Society, to whom no money should be sent.
5 — Orders obtained from the Secretary should be sent or delivered to
the C. G. Braxmar Company. 10 Maiden Lane. New York City, together
with cash, check or money order in payment of the pin, whereupon the
pin will be delivered post-free.
The pin adopted by the Society is an unusually attractive
emblem, and the Society's colors, cobalt-blue and gold, are now
being worn by many of our members. It serves as a means of
introduction and will frequently enable you to meet fellow chem-
ists whom you might not otherwise know are in the same profes-
sion. It is important that the members of the American Chem-
ical Society wear this insignia as regularly as the members of
the engineering societies display their distinguishing emblem.
Show that you are proud of your Society and its work. Write
to the Secretary for an order. Chas. L. Parsons, Secretary
THE NICHOLS MEDAL AWARD
The Nichols Medal for 1917 will be conferred on Dr. Treat B.
Johnson of the Sheffield Scientific School of Vale University.
The Medal, founded by Dr. William H. Nichols in 1902, is
awarded annually by the New York Section of the American
Chemical Society on the merit of tin- original communications
published in the journals of the Society.
The formal presentation to Dr. Johnson will be made on March
8, 1918, in Rumford Hall, Chemists' Club. New York City.
THE PERKIN MEDAL AWARD
The Perkin Medal for 1918 has been awarded to Dr. Auguste
J. Rossi, Ph.D., of Niagara Falls, N. Y., for his work on
titanium.
The Medal will be presented by Dr. W. H. Nichols at
the regular meeting of the New York Section of the Society of
Chemical Industry to be held at the Chemists' Club, January
18, 1918. Mr. F. A. J. FitzGerald, past-president of the American
Electrochemical Society, will deliver an address on Dr. Rossi
and his work. Owing to illness. Dr. C. F. Chandler will not be
able to participate in the program.
WASHINGTON LLTTLR
By Paul Wooton, Metropolitan Bank Building. Washington, D. C.
Centralization of activities pertaining to chemicals, the lack
of which has been so glaringly apparent for many months, is
now being accomplished by the formation of a chemical section
of the Raw Materials Division of the War Industries Board.
This board, which consists of L. L. Summers, M. F. Chase, C.
H. MacDowell and M. T. Bogert, is acting as a clearing house
for all matters of chemical interest related to the war. This
applies to the purchases of the allied governments as well as
to domestic matters having a bearing on chemical supplies.
The chemical specialists attached to the War Industries Board
are making no effort to occupy the anomalous position of repre-
senting the government and the industry at the same time.
That such a plan is not feasible was shown in the collapse of the
cooperative committee section of the Council of National De-
fense. Out of this experience, however, has grown the plan for
war service committees representing each industry. These
committees will form the point of contact with the government
and will be representative of nearly 100 separate industries.
The war service committees now are being formed through the
medium of the Chamber of Commerce of the United States
Every effort is being made to complete their organization, as the
War Industries Board now is working at a considerable disad-
vantage through the lack of a unit organized to act fur an industry.
The formation of a chemical section of the War Industries
Board will in no way effect the research activities of the National
Research Council. Dr. Bogert continues at the head of its
Committee mi Chemistry and will divide his time between his
duties with that committee and with the War Industries Board.
Mr. MacDowell severed his connection with Armour and Com
pany. where he was in charge of fertilizers and other by-products,
to aid the government. Mr. MacDowell refers to himself as a
"layman" chemist. For many years he has specialized in
potash. He was closely in touch witli the development of the
alunitc deposits at Marvsvale, Utah. Prior to the war, he made
a careful study of tin German potash deposits.
Organizations of various industries interested in commodities
which require import licenses have been called upon by the War
Trade Board to select committees to co&perate v, ith it in secui ing
an equitable distribution of certain imported commodities,
committees are given no authority in the granting or
refusing of import licinsis ,,r in detennining "ho shall import
the commoditii - requiring licenses. The representatives of the
industry are to act as consignees and will release commodities as
instructed by the Wai Trade Board. Thecommittei is to obtain
from importers such guarantees and agi eementsas the War Trade
Board may require. Each committee will keep itself informed
as to the use and disposition of the imports and will keep full
records of all the shipments received. A few of these committees
have been announced already, but the majority of them are still
to be selected. Two of the most important committees will be
those which will cooperate with the War Trade Board in the
importation of manganese ores and iron pyrites. Other im-
ports of chemical interest which require license are antimony,
asbestos, chrome, cobalt, all ferro-alloys, iridium, molybdenum,
emery, sodium, potassium and calcium nitrates, platinum,
schcclite, titanium, tungsten and vanadium.
Exports of sulfuric acid during 19 17 will not fall as far behind
those of 1916 as had been anticipated earlier in the year. An
increase of more than 1,000,000 lbs. took place in the exports of
October. November figures are not available but even a more
substantial gain is known to have taken place during that
month. According to the Department of Commerce, there
were exported in October 4,492.200 lbs. of sulfuric acid, as
compared with 3,466,818 lbs. in October of 1916. During the
first ten months of 1917, 53,487,786 lbs. of sulfuric acid were
sent out of the country. This compares with 57,386,036 lbs.
for the first ten months of 1916. That such a good showing is
being made this year with the tremendous increase of domestic
requirements is a source of much favorable comment among
chemists here.
I'i C. L. Parsons, chief chemist of the Bureau of Mines,
called together the chemical advisory committee of that bureau
on December 17th and went carefulh ovei t!u war work under his
direction. Pr. Parsons, owing to the increased amount of war
ing done by the Bur< - been forced to
turn over to others the direction of the work being done on other
matters. Di Parson nitted his report on
the method used in the oxi Ja which was
developed at the Semet Solvaj 1 lant at Syracuse, N. V. This
work v.. is done under a coopei ; between the
Ivay Company and the Bun of Mines.
An important and timely report on the sulfuric acid situation
has been picp.u .1 Mines staff.
Mr. Wells is working in clost 1 Parsons and
M. F. Chase, of the War [ndusb I is survey of the
sulfuric acid situation
important developments in th< pyrite situa-
tions, which will have a bearing | minerals, are
expected within the very neai futur -been reached
where unusual steps must be t.ikt -.. mestic produc-
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Si
tion of manganese, pyrite and other products. Precedents will
be broken, in all probability, in the legislation which will be
proposed to provide means to secure increased domestic produc-
tion, so as to save shipping.
Changes which will alter permanently conditions of interna-
tional competition in the chemical industries and which will
have a direct bearing on the volume of foreign trade in chemicals
are to be the subjects of a special investigation just begun by
the United States Tariff Commission. The developments that
have taken place in the chemical industries since the passage of
the tariff act in 1913 are to be studied closely. The scope of the
inquiry is set forth by the Tariff Commission as follows:
1 — The manufacture within the United States of articles formerly-
unavailable or obtained exclusively by importation ; for example, phos-
gene.
2 — In the case of industries previously established in the United States,
the erection of new plants or increase in capacity of existing plants; for
example, the increase in capacity of existing plants for making caustic soda
and chlorine and the installation of such plants at textile and paper
a ills.
vhich
3 — The future of industries or establishments newly created,
productive capacity has been greatly increased to meet a direct war demand.
How can these plants be utilized when the war demand disappears? For
example, the acetone industry.
4 — Any general or significant differences in the prevailing method of
manufacture in the United States and abroad, such as the relatively small
use of the carbureted water-gas process in England compared to its use in
the United States.
5 — Differences in the organization of the industry in the United States
and abroad.
6 — The development or invention in the United States or abroad of new
or improved processes which are likely to influence the conditions of inter-
national competition; for example, the hydrogenation of fatty oils or the
flotation process for concentrating ores.
7 — Significant changes in the conditions of international competition
caused by the recent law-making patents owned by citizens of enemy coun-
tries available to American manufacturers; for example, the patents on
salvarsan.
8 — Industries which have been seriously hampered in their normal
operations or in their development by difficulty in securing materials or
supplies formerly imported; for example, the lack of potash for fertilizer
or glass. If these difficulties have been met by the introduction of substi-
tutes, is it expected that there will be a return to the old materials and
methods when foreign supplies again become available, or will the changes
be permanent?
9 — Developments or changes in other industries which have created
a new or greatly increased demand for chemical products; for example,
the manufacture of new varieties of glass in the United States.
10 — The discovery of new uses of materials, creating a new demand or
furnishing a market for materials formerly wasted; for example, the use of
aniline as an accelerator in the vulcanization of rubber.
tal hindrances in the United States or abroad,
rommerce; such as the export duty on nitrate from
The Commission will publish only general statements or sum-
maries, which will not reveal the operation or plans of individual
companies.
The Tariff Commission is preparing for a systematic census
of the production of the following coal-tar products: interme-
diates, dyes, medicinals, flavors, photographic chemicals and syn-
thetic phenolic resins.
Issuance of licenses for the manufacture and sale of salvarsan
has been begun by the Federal Trade Commission. It is ex-
pected that the price per dose will be lowered to $1.50, as a
result of this action.
11-
—Any govt
either ii
manufact
Chile.
Without the necessity of roll call, the House of Representatives
on December 15th passed a joint resolution "for the purpose of
promoting efficiency, for the utilization of the resources and
industries of the United States, for lessening the expenses of the
war, and restoring the loss caused by the war by providing for
the employment of a discovery or invention called the 'Garabed,'
claiming to make possible the utilization of free energy." It
required a special rule to get the matter before the House but
the Committee on Rules promptly supplied this deficiency.
Practically the entire day was taken up in the discussion of
cosmic forces and other matters related to the device of Garabed
T. K. Giragossian, interspersed with parliamentary wrangles and
squabbles over amendments. Despite the fact that Mr. Gira-
gossian refused to show his device or its operation to any mem-
ber of the Committee on Patents or to any committee that would
be appointed by the House, most of the members of that body
were dissuaded from voting against the resolution by the idea
expressed in this question put by Representative Garrett: "Why
is it that gentlemen so much fear to ascertain whether we really
have some new blessing for mankind?"
PERSONAL NOTES
Mr. R. S. Banks, instructor in analytical chemistry at Iowa
State College, has been appointed a member of the Inspecting
Department of the Picatinny Arsenal, Dover, New Jersey.
Mr. L. A. Rumsey, former instructor in organic chemistry at
Iowa State College, has been appointed head of the department
of chemistry at Denison University, Granville, Ohio.
Mr. A. J. Wuertz, former research chemist of the Experiment
Station of the agricultural and biological department of the
University of Minnesota, is at present instructor in organic chem-
istry at Iowa State College.
Mr. William H. Kerr, assistant treasurer of the General Chem-
ical Company, and manager of the Philadelphia offices of the
company, has been elected a director to succeed Mr. Edward
H. Rising, deceased.
Mr. Frederick Pope, of Moses, Pope and Messer, Inc., con-
sulting engineers of New York, has been commissioned a captain
in the Engineer Officers' Reserve Corps, Gas and Flame Division
(Thirtieth Engineers).
Mr. A. Gordon Spencer, formerly chief chemist of the Canadian
Inspection and Testing Laboratories of Montreal, has severed
his connection with that company and is opening an office at
617 Transportation Building, Montreal, Canada, as a consulting
chemist and metallurgist.
oited States Bureau of Mines has broadened the scope
of its station at Urbana, 111., to include work in coal and metal
mining and the metallurgical industries of the Middle West.
Tin present safety work will be continued and all work will be
conducted under a cooperative agreement with the mining de-
partment of the University of Illinois. The Bureau staff is
under the superintendence of E. A. Holbrook, supen ising mining
engineer and metallurgist. Other members are W. B. Plank,
in charge of mine safety, and F. K. Ovitz, chemist.
Mr. Lester Yoder has been appointed as assistant chemist
for the chemical section of the Agricultural Experiment Station
at Iowa State College.
Mr. H. B. Underwood has severed his connection with the
Buffalo Foundry and Machine Company and has identified
himself with the Hewitt Rubber Company, Buffalo, N. Y.
Rensselaer Polytechnic Institute, in March, 191 8, will start
work on extensive additions to be made to the laboratories of
the department of chemistry. Entirely new and complete lab-
oratories will be constructed for quantitative analysis, or-
ganic chemistry, and physical chemistry. The food analysis
and gas analysis laboratories will be materially enlarged, and new
space will be assigned for lecture and recitation rooms. The
great increase in the number of students entering for the course
of chemical engineering has made these changes imperative.
Dr. J. Stieglitz has appointed the following Committee on
the supply of organic chemicals for research during the war:
E. Emmet Reid, Chairman, Roger Adams, II. L. Fisher, J. W.
E. Glattfeld, W. J. Hale.
Mr. James H. Ellis, research associate in physical chemistry
at Throop College of Technology, Pasadena, Cal., has become a
member of the physics department of the college as instructor in
electrical measurements.
Mr I Inward B. Hishop has severed his connection witli the
Genera] Chemical Co., at Easton, to accept a position with the
National Aniline and Chemical Co.
Mr. C. A. Mace has been appointed head of the textile de-
partment of Marden, Orth and Hastings Corporation, succeed-
ing Mr. H. Gardner McKcrrow. Mr. Mace has been for eight
years with the Badische organization at the head of their Chicago
offices. He is a graduate of the Massachusetts Institute of
Technology.
82
THE JOURNAL OF INDUSTRIAL AND ENGINEER! NC CHI UIS1 RY Vol. 10, Xo. i
Mr. R. J. Quinn has left the Wahl-Henius Institute and ac-
cepted a position with the Midland Chemical Company.
Dr. J.W. Turrentine is directing the work of the Government's
experimental kelp-potash plant at Summerland, near Santa
Barbara, Cal. The plant is in operation and is producing crude
potash. Apparatus is now being installed which will make pos-
sible the production of refined potash and by-products, particu-
larly iodine, for both of which chemicals there is a large demand
for industrial and military purposes.
Professor Charles H. LaW'all of the Philadelphia Section has
been elected president of the American Pharmaceutical As-
sociation.
Major S. J. M. Auld, of the British Army, addressed the
Northeastern Section of the A. C. S., at Boston, on December 8,
on "Gas Warfare."
The United States Civil Service Commission announces an
open competitive examination for junior chemist, for both men
and women. Until further notice, applications will be received
at any time. Salaries range from $1020 to $1800. There is
special need of eligibles who are qualified as physical, biological
or metallurgical chemists. The Commission also announces an
examination for assistant petroleum chemist, for men only, to be
held on January 15. Salaries range from $1680 to $1920. For
further information apply for Form 131 2, Civil Service Com-
mission, Washington, D. C., stating the title of the examination
desired.
Mi Guy R. McDole, Assistant in Soils, in the University of
Minnesota, and formerly Research Assistant in Agricultural
Chemistry in the University of Nebraska, has enlisted in the
Gas and Flame Regiment (Thirtieth Engineers).
Mr. H. Gardner McKerrow, for the last two years associated
with the Marden, Orth and Hastings Corporation in the estab-
lishment and management of their textile department, is now
connected with K. F. Drew and Co., Inc., 50 Broad Street, New
York City. Mr. McKerrow will have the management of the
textile department, and it is proposed to go into dyestuffs as
well as the mill chemicals and industrial oils. Special attention
will be given to American dyestuffs. Through the efforts of Mr.
McKerrow and others a convention will be held in New York
City, January 22 and 23 at the Chemists' Club, at which
it is hoped all the manufacturers of American dyestuffs will be
represented, for the consideration of a proper means of standard-
izing American colors. Mr. McKerrow will have associated
with him, Mr. T. F. O'Keefe.
Mr. Carl F. Speh, secretary of the Turpentine and Rosin
Producers Association, has been appointed on the sub-committee
of the National Paint, Oil and Varnish Association to look after
legislative matters of interest to naval stores, producers and manu-
facturers, and distributors of paints, oils and varnish.
Mr. Charles H. McDowel, president of the Armour Fertilizer
Company of Chicago, has been called by the government to
aid in chemical research work and development.
Dr. R. K. Strong, of the University of Chicago, has been
engaged as professor of industrial chemistry at the Oregon
Agricultural College.
Twenty-five members of the Southern California Section of
the A. C. S. accepted the invitation to the Technical Societies
of Los Angeles to inspect the wonderful one hundred inch re-
flector of the Mount Wilson Solar Observatory, on November 24
and 25. This was the first occasion in its history' where the
rigid schedule of the Observatory was broken for any reason.
The Michigan Smelting & Refining Co., announces that Charles
T. Bragg takes the position of Works Manager of its Detroit
plant, January 1, 191 S. Mr. Bragg had been Chemical Engi-
neer of The Ohio Brass Co. for six years and was for over four
years Technical Director of Perry Bros, of Detroit.
Canada recently appointed Sir Henry Drayton royal commis-
sioner to investigate exportation of Canadian Niagara power and
controller of the distribution and production of electrical energy
in Ontario.
The University of Illinois will givt a Short Course in Ceramic
Engineering January 7-19, 1917. The Course will be under
the direction of Professor E. W. Washburn, Head of the De-
partment of Ceramic Engineering, and Mr. A. V. Bleininger,
Ceramic Chemist of thi Bureau of Standards, assisted
t.v Professors C. W. Parmelee and R. K. Hursh, of Illinois,
and a corps of lecturers on special topics. The two-weeks'
course is intended to cover in an elementary and practical
manner the scientific principles underlying the practice of clay-
working. A common school education will suffice for the work
of the course and no tuition fees will be charged. The course
is open to all who are interested.
Prof. John Charles Clark, of James Millikin University, has
been elected to the presidency of the Illinois Academy of
Science.
The 276th meeting of the Washington Section of the A. C. S.
was held on December 13 at the Cosmos Club. Mr. Atherton
Seidell spoke on "Utilization of the Adsorptive Power of Fuller's
Earth for Chemical Separations and Mr. Oswald Schreiner
spoke on "Potash Situation in Relation to Food Crops." A
special meeting was held at the same place on December 18, at
which time Prof. Wilder D. Bancroft of Cornell University spoke
on the subject of "Contact Catalysis."
Mr I. M Larsen has accepted a position in the research
laboratory of Ault and Wiborg of Cincinnati.
On Saturday, December 8, Professor Grignard and Lieut.
Engel of the visiting French Commission gave addresses before
the Robert Kennedy Duncan Club of the Mellon Institute of
Industrial Research at Pittsburgh. Professor Grignard was
made the first honorary member of the club. The two dis-
tinguished guests were entertained at the University Club at
luncheon. After luncheon, Prof. Grignard Live a short informal
address in French which was translated in substance by Lieut.
Engel.
The 101st regular meeting of the California Section of the A.
C. S. was held on 1 lecembi r 15, in San Francisco, in conjunction
with the annual banquet. Among the after dinner speakers were
Prof. Edmund < >'Ncill of the University of California, Prof. John
M. Stillman of Stanford University, and Dr. Harry East Miller
of the International Precipitation Company.
INDUSTRIAL NOTL5
To help out in the use of sugar, Italian scientists have de-
veloped a process for obtaining a large yield of sugar resembling
honey from grapes. This product isvci\ suitable for preserving
fruits ami marmalades and for use in soda fountain syrups. If
this industry attains any magnitude it will affect the trade in
half rciiued tartar which is obtained from grapes, which will in
its turn affect the woolen dyers who use tins substance as one
of the ingredients in the production of olive drab.
The Ideal Laboratories Company has been incorporated under
the laws of Delaware with a capital stock of (2,000,000 In-
corporators. T. W. Cole. Chicago. 111.; K. S. Wilson and Marion
I. ucc of Oak Park, ill
A shipment of platinum received December 12 at a Pacific
Coast port from Russia was the cause of much satisfaction to
Government officials. The shipment weighed 21,000 ounces
and was valued at more than $2,000,000 It was consigned to
the Secretary of Commerce who will supervise its distribution.
Because of the internal conditions in Russia it is feared that the
shipment will be the last exported from that country for some
time to come.
Announcement has been made that the Consolidated Gas
Company of New York has reached an agreement with
Washington officials to manufacture toluol to help meet the
which exists in this wai 1 Qti il The Government
is to pay foi the erection of the stills at the Company's plants
and the Consolidated Gas Companx is to furnish the labor
for the actual manufacture of the toluol from its gas The
product is to be furnished the government at the actual cost of
its manufacture. It is understood that contracts have already
been let for the erect:.: : that work has
already been started at the Company's plant in Long Island City.
We Karn from the i.Yi.v.:.' c ■ • .it the discovery
of platinum in Alaska has led the Government to assign experts
to study the situation there and report whether the discoveries
can replenish the platinum supply cut off by the cessation of
activity in the Ural Mountain mi
The T. N. T. plant of the Aetna Chemical Company at Heidel-
berg, a sul>uil> of Pittsburgh, Pa W : | . the extent of
DJ an explosion on I ig the death of
eight men and seriously injuring man]
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
83
American sulfur production will be augmented by the de-
velopment of New Mexico deposits, which are claimed to be of
high grade and extensive in quantity. To undertake this develop-
ment the United Sulfur Development Company has been in-
corporated with S3, 000,000 capital by J. J. and M. de Praslin
of Lake Charles, La., and J. B. Bailey of Wilmington, Del.
Perchlorate Explosives Company of Poughkeepsie has been
formed with a capital stock of $2,100,000. Incorporators:
L. Bedell, C. W. H. Arnold, H. B. Vosburgh, Poughkeepsie.
The Amalgamated Dyestuff and Chemical Works of New
York has increased its capital stock from $50,000 to $500,000.
Aluminum, antimony, arsenic, bismuth, magnesium, phos-
phorus and potassium are all found in the state of Queensland,
Australia. Platinum is found but in small quantities.
Wyoming Sulfur and Refining Company, dealers in sulfur and
chemical products, has been incorporated under the laws of
Delaware with a capital stock of $2,000,000.
Exports of cinchona bark and alkaloids and their salts from
the United Kingdom have been prohibited to all destinations,
according to a cablegram from the American consulate at London.
Advices received from Havana, Cuba, state that planters in
Cuba are turning their attention to the growing of castor beans.
The shortage of castor beans in this country has turned
attention towards the possibilities of bean cultivation in the
island of Cuba. Plantings have been made and the reports from
the growers are encouraging. Soil and climatic conditions are
declared to be entirely adapted to the cultivation of the castor
bean, and it seems assured that the new industry will be given
a real test on the island.
The salicylic acid plant of E. I. duPont de Nemours and Co.,
at Newark, Delaware, was burned recently, entailing a loss of
approximately $100,000. The fire apparently was the result of
an explosion.
The Commonwealth Silica Co., Chicago, 111., has been in-
corporated with a capital of $1,500,000, to mine silica, lime and
other substances. The incorporators are L. L. and B. P. Cowan
and P. Zak.
According to British Imperial Institute reports, a consider-
able amount of attention has been given in recent years to the
recovery of wax from the waste produced in the extraction of
sugar from the sugar-cane, and this industry has now been
started on a small scale in Natal. Samples of the first consign-
ment of Natal sugar-cane wax shipped to England have been
examined at the Institute and have been found to be of good
quality, quite equal to that of the first trial samples made and
examined. Sugar-cane wax is now becoming better known on
the market, and could be used as a substitute for the better-
known carnauba wax in the manufacture of gramaphone records,
polishes, candles, etc.
In a paper read before the New York Section of the American
Chemical Society on November 23, E. D. Boyer called attention
to a new use for Portland cement brought about by the war,
namely, the construction of ships and barges of concrete. He
states that ships of this character have recently been successfully
built in Norway, and a 5000-ton ship is at present being con-
structed in San Francisco, while on November 21, a 250-ton
ship was successfully launched at Montreal. The American
Concrete Institute and the Portland Cement Association have
organized committees who are making a study of the construc-
tion of vessels of this type, and these committees have designed
a reinforced concrete barge of 2000-ton carrying capacity, with
every reason to believe it will be successful.
The Federal Trade Commission has entered order for licenses
to three firms to manufacture and sell the product heretofore
known as "Salvarsan," "606," "Arsenobenzol," "Arsaminol,"
patent rights which have been held by German subjects. Here-
after this important drug will be manufactured and sold under
the name of "Arsphenamine." The three firms designated
are Dermatological Research Laboratories of Philadelphia,
Takamine Laboratory, Inc., New York, and Farbwerke Hoechst
Company (Herman A. Metz Laboratory), New York. The
supply of the drug was heretofore almost exclusively obtained
by importation from Germany. The enormous shortage of
supply on this important product will immediately be relieved,
and the article placed in the hands of the Government, the
hospitals and the medical profession at a much lower price.
It is reported that the Spreckles interests of California have
purchased extensive deposits of soda salts in southern Oregon
and will start development work in the near future.
Further data have been received by the United States Bureau
of Foreign and Domestic Commerce on the successful incom-
bustible substitute for celluloid. Announcement of this in-
vention by a professor in one of the Japanese universities was
made about a year ago and aroused considerable interest in the
United States. The new product has been given the trade name
of "Satolite" derived from the name of the inventor, Prof. S.
Sato, and a company for its manufacture has been started with
a capital of $1,000,000. Satolite is a galolith made of the glucine
of soya bean, coagulated by formaline. It is said to be produced
much more cheaply than celluloid, and to have several advantages
for industrial use not possessed by the latter. The factory is
to be built in the Mukojima district in Tokyo, and the actual
production will soon begin.
At the annual meeting of the National Academy of Sciences,
held at the University of Pennsylvania, Philadelphia, November
20 and 21, Dr. Simon Flexner of the Rockefeller Institute,
announced that two American physicians, Doctors Jacobs and
Heidelberger, of the Rockefeller Institute, have evolved a new
remedy to replace salvarsan. Dr. Flexner stated that it has
many advantages over salvarsan, one being its cheapness. It
is stated that it is less injurious to the human tissues and more
readily manufactured than salvarsan. Like salvarsan it is an
arsenic compound.
The cottonseed oil refinery being erected by Swift and Company
in Houston Heights, Texas, is near completion. The approxi-
mate cost of the plant is about $250,000. The plant as a whole
will include three buildings, the power house, packing house,
in which the oil is refined and the acidulating building. Three
large storage tanks have been built with a capacity of 27,000
barrels of cottonseed oil. This company is also planning the con-
struction of a large fertilizer plant, to cost about $500,000, at
Hammond, 111.
The United States Industrial Chemical Company, which was
chartered recently under the laws of Maryland with a capital
stock of $24,000,000, is reported to have secured land for the
erection of a plant near Curtis Bay to manufacture chemicals,
fertilizers and hydrocarbons. It is also reported that the new
company will take over the entire plant of the Curtis Bay Chem-
ical Company, subsidiary of the United States Industrial Alco-
hol Company of New York. The new company's incorporators
are Patrick H. Loftus and Francis C. Nickerson of Brooklyn
and Stewart M. Seymour of New York. Directors for the
first year are George S. Brewster, William R. Coe, Edward W.
Harden, William S. Kies, Adrian H. Larkin, Percival J. Mcintosh^
Horatio S. Rubens, Richard P. Tinsley and Milton C. Whitaker
Nineteen schools of technology are now maintained by the
Japanese government at various sections of the island empire.
So far as is possible each school is specialized to meet the general
agricultural, mining and industrial needs of that portion of the
country in which it is located. At Tokyo and Osaka, dyeing,
bleaching and printing, the tanning of leather, industrial design-
ing and the manufacture of oils, soaps, and colors are among the
courses offered, and the faculty of the Tokyo school alone num-
bers eighty-eight, including two foreign instructors.
A training school for the higher technical education of women
was recently opened in Lyons, France, the centre of the silk
industry in that country. So severe a drain has been made on
French manhood of all classes that it was deemed imperative
that women should be offered an opportunity in the more im-
portant fields. The courses of study offered cover most of the
technical courses hitherto confined to men.
A school of industrial chemistry, the first in Italy, is being
organized at the L'niversity of Pavia.
Restrictions are being placed upon copra exports to France,
apparently with a view of assuring a greater supply for the
domestic production of edible cocoanut oil.
Platinum production in Colombia is increasing. Prospecting
has shown that the metal occurs in the steam gravels and in the
high gravels for long distances on the Arato and San Juan River.
A thorough and scientific investigation of the dyestuffs in-
dustry in the United States is being undertaken by the United
States Tariff Commission for the purpose of ascertaining the
need of further tariff protection and also in relation to the pro-
duction of explosives.
Brazilian manganese is now being imported in large quantities
by the United States, owing to the closing of other sources of
supply.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. i
GOVERNMENT PUBLICATION
By R. S. McBride, Bureau of Standards, Washingto
NOTICE — Publications for which price is indicated can be
purchased from the Superintendent of Documents, Government
Printing Office, Washington, D. C. Other publications can
usually be supplied from the Bureau or Department from which
they originate. Commerce Reports are received by all large
libraries and may be consulted there, or single numbers can be
secured by application to the Bureau of Foreign and Domestic
Commerce, Department of Commerce, Washington. The regu-
lar subscription rate for these Commerce Reports mailed daily is
$2.50 per year, payable in advance, to the Superintendent of
Documents.
NATIONAL MUSEUM
Mineral Industries of the United States; Interpretation of
Fertilizer Situation in the United States. J E. POCUB. Bulletin
102. 22 pp. Issued October 10, 1917. Paper, 5 cents.
PUBLIC HEALTH SERVICE
Trinitrotoluol. Practical Points in its Safe Handling. J. W.
ScherEschewsky. Public Health Reports, 32, 1919-26 (No-
vember 16).
The Bacteriological Examination of Water. Comparative
Studies of Media Used. H. E. Hasseltine. Public Health
Reports, 32, 1878-87 (November 9). "The results of this
work indicate that if the new Standard Methods (1917) be ad-
hered to in the bacteriological examination of water, time, labor,
and material will be unnecessarily expended and misleading re-
sults may be obtained."
GEOLOGICAL SURVEY
Chromite in 1916. J. S. DillEr. Separate from Mineral
Resources of the United States, 1916, Part I. 18 pp. Published
October 26. "The greatly increased trade in steel and the
consequently larger demand for ferroehrome have stimulated
the search for chromite in the United States, as is shown by the
fourteenfold increase in production in 19 16 as compared with
1915. * * * * The total yield for the United States was
47,035 long tons, valued at $726,243.
"The price of chromite in California on the basis of a content
of 40 per cent of chromic oxide ranged in 1916 from $14 a ton
f. o. b. at points of shipment early in the season, to $20 toward
the end of the year. To this must be added for the eastern buyer
a freight rate for carload lots ranging from Sio a ton to Chicago
to nearly $15 a ton to the eastern seaboard and making the
California 40 per cent ore cost on the eastern seaboard from
$29 to $35 a ton. A premium of 50 cents a unit for chromium
oxide is usually allowed and a penalty of 50 cents a unit is ex-
acted for chromium oxide under 40 per cent and silica over 6
per cent. At the Atlantic seaboard the ore from the Pacific
coast meets the imported ore, which is sold on the basis of a
content of 50 per cent of chromic oxide. Prices "of imported
high-grade ore are reported as ranging in 1916 from $35 to $45
a ton f. o. b. eastern seaports. Low-grade Canadian ore con-
taining 30 to 40 per cent chromic oxide sold for $25 to J30 B
ton f. o. b. at the same points. Tw< nty five pel cent ore sold
as low as $18 a ton.
Embargoes were placed on the shipment of chrome ore from
some of the principal sources, and it was feared that the supply
for the United States would bi cul off, but after the producers
received a guaranty that the ore would not be reshipped to
enemj belligerents the imports greatly huh, it, I. compared
with 1914, especially those from Rhodesia, New Caledonia,
and Canada, though imports from Greece have declined slightly
and those from Turkey have entirelj Ct
Silver, Copper, Lead and Zinc in the Central States in 1016.
Mines Report J. P. DUNLOP AND B. S. Hitler Separate
from Mineral Resources of the United States, 1916, Part I.
105 pp. Published October 27.
Bauxite and Aluminum in 1916. J. M. Hill. Separate
from Mineral Resources of the United States, 1916, Part I.
12 pp. Published November 2. The production of bauxite
in the United States in 1916 was 425,100 long tons, having a
value at the mines of $2,296,400, an increase over the produc-
tion in 1915 of 43 per cent in quantity and 52 per cent in value.
The production from the Georgia, Alabama, and Tennessee
field in 1916 was 49,190 long tons, an increase of about 74 per
cent, and the Arkansas production of 375,910 long tons showed
an increase of approximately 40 per cent.
Apparently the producers of aluminum consumed about
300,000 tons, makers of chemicals about So.ooo tons, and makers
of abrasives and refractories about 45.000 tons of bauxite in 1916.
As will be seen by the tables, though the domestic consump-
tion of bauxite in 1916 also increased 43 per cent over the con-
sumption in 1915, domestic deposits were apparently able to
supply the whole demand and still leave some bauxite for ex-
port. The larger exports were apparently to Canadian aluminum
and abrasive makers.
The prices received for bauxite in 1916, as reported by pro-
ducers, ranged from a low of S4.25 to a high of $6.25 a long ton,
the average price for the whole production in 1916 being S5.40
a long ton. During the latter part of the year and early in
1 91 7 higher prices were offered for good grade bauxite from the
central Georgia field.
Owing to the freight embargoes placed by various railroads
in the last half of 19 16 and also to the shortage of cars the pro-
ducers of bauxite had considerable difficulty in meeting their
orders. The exceptionally wet winter was also a handicap to
regular production and shipping and, at a few pits in the central
Georgia field, work had to be stopped on account of difficult
mining or hauling conditions.
"The value of primary aluminum produced in the United
States in 1916 was $33,900,000, an increase of 108 per cent over
the value of the output in 1915. This increase is, in part, due
to the increased price, but is also due in a considerable degree
to the greater output of primary aluminum in 1916 than in
1915. It will also be noticed, as shown in the tables, that the
value of aluminum produced from scrap in the United States
in 1 9 16 increased more than 300 per cent over the value of the
production in 1915, owing in part to the greatly increased price
in the open market, but also to greater recoveries of aluminum
from scrap. The value of the total domestic production of new
metal and metal produced from scrap in -,-.330,200,
as compared with (22,082,100 in 1915. The value of imports
of aluminum has continued to decline, but the value of exports
has increased greatly ."
In tin United States the quoted pi n;ary or "virgin"
aluminum ranged from a low of 5 iund in January
to a high of 65.12 cents a pound in Nov, 1 : the average for
the year being 60.71 cents a pound, as comp d with 33.98 cents
in 1915. These prices are for small lot> and immediate delivery,
offered in the open market, and 1 1 10 represent
the price received by the single produce] ry aluminum
in this country. It is reported, a- ,1 authority,
that the contract prices of the Alumiuun iy of America
tuners ranged from 31 pound in 19x6
as compared with 2e> to 31 cents a pound • - The demand
for aluminum was very large during 191 darly for war
materials of various sorts, and it i- ., that the de-
mands in the near future will be inci • ably.
Jan., 1018 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY 85
Prices of Aluminum, 1912-1916 in Cents per Pound(o) accuracy for use in specifications for the purchase of coke by the
Average _ ....
Open Market Price Contract Government, by industrial concerns, or by private individuals.
X"^ SmaUi'0t5 2^\ "Moisture can be determined quickly and with adequate ac-
\9\i.V... ....'.'.'.'..'. .'.'.'.'. .'.'.'.'.'.'. 23 '64 (6) curacy, ±0.5 per cent, by simply heating to constant weight a
191| "; " 33.98 20-31 large sample of lump coke, in any convenient oven, or on a stove,
1916 60.71 31-37 hot plate, or steam coil at a temperature of 100 to 200° C.
{$ N&^UMJX^^uFS^^iZ&Z-** con- "Because of its simplicity and flexibility this method may be
tracts were made on approximately the same basis as for 1912. used advantageously at points when coke shipments are
Nearly 70 per cent of the domestic output of bauxite in 1916 sampled."
went into aluminum, but manufacturers of aluminum salts Effect of Low-Temperature Oxidation on the Hydrogen in
used nearly 19 per cent; apparently 8 per cent was consumed Coal and the Change in Weight of Coal on Drying. S. H.
in the manufacture of bauxite abrasives; and 3 per cent was KaTz and H. C. Porter. Technical Paper 98, 10 pp. Paper,
used by makers of "high-alumina refractories," sometimes 5 cents. In order to gain information regarding the possible
called bauxite brick. changes of the hydrogen of the coal substance during the altera-
The Palestine Salt Dome, Anderson County, Texas. The tion of coaI by the air. the work described in this paper was under-
Brenham Dome, Washington and Austin Counties, Texas. taken.
O. B. Hopkins. Bulletin 661-G, from Contributions to Economic "The following conclusions are reached:
Geology, 1917, Part II. 28 pp. Published October, 1917. "1— There is a lack of agreement between the weight of water
The highly folded, faulted, and eroded condition of the Pales- evolved by coal and the loss of weight when dried in an inert at-
tine dome and the general absence of oil and gas as surface mosphere. The excess weight of the coal may be due to absorp-
seepages and in shallow wells in this area detract from its oil *ion °> Sas-
prospects. The tilting and faulting of the rocks probably pro- "2— A study of the vapor tension of water in coal, as indicated.
vided outlets for the escape of oil, and as no evidence of oil ex- hV ihe water removed by a regulated current of dry nitrogen and
ists the conclusion is suggested that no large amount remains air used alternately, shows no production of water by the oxida-
here, even if it ever accumulated. It is possible, however, that tion of coal at ordinary temperatures.
the soft and dominantly impervious nature of the formations BUREAU OF STANDARDS
involved in this fold closed up any possible lines of escape for Durability of Cement Draintile and Concrete in Alkali Soils
the oil, as its absence at the surface may be interpreted to in- (Containing Results of Third Year's Tests). R. J. Wig, G. M.
dicate. The eroded condition of the dome, as shown by the WnxlAMS> a. N. Finn in cooperation with S. H. McCrory,
presence of Cretaceous rocks at the surface, and the presence chief of Dramage Investigations of Department of Agriculture,
of the salt core within 140 ft. of the surface over a large area 3 c BebBj Engineer of U. S. Reclamation Service, and L. R.
are also unfavorable conditions, as they eliminate the possi- Ferguson, Engineer, Portland Cement Association. Tech-
bility that oil may be found on the crest of the dome, which noiogic Paper 95, 91 pp. Issued November 15.
might otherwise be the most favorable area for its occurrence. „ „, ., T . ... ,, .... . _ T „... . ..
6 ..... . Gas-Mantle Lighting Conditions m Ten Large Cities m the
Oil in commercial quantities has not yet been found in a salt ,-, .. , „, . „ „ •.»_■„ „ z^t^t.- t-,
* , . United States. R. S. McBride and C. E. Reinicker. Tech-
dome so far removed from the coast as this one. . . „ r- ... . . n. . Iir.
„ , . , , , .„. noiogic Paper 99, 35 pp. Published October 29. From an
In the Brenham dome, as in most other salt domes, drilling r , ., , . . . ...
, , . , . . , . , , inspection of about 4500 gas mantle lamps in service m 10 cities
is attended with many uncertainties and should not be under- r .. .... r ., , .,_. ,. . .
. „ , , „ . _, . ..... a summary 01 the condition 01 mantles, glassware, pilot light,
taken without full knowledge of them. Failure to find oil in . .. .. , , . , . , . . .
.... ,. , ,, and other particulars was made in order to determine to what
commercial quantities in the porous limestone, the cap rock, ... . _. , .. , ...
, , , , . , . , , extent the customer benefited through periodic maintenance
and the sands overlying the crest of the dome makes deeper
service,
drilling necessary, with its increased costs and risks. frn .- . - , , .. . , .
By these observations it is found that a lamp not on regular
bub AU or mines maintenance is likely to be defective five and one-half times as
Approved Electric Lamps for Miners. H. H. Clark and frequently as a lamp which is regularly maintained. Also it is
L. C. Ilslev. Bulletin 131. 47 pp. Paper, 20 cents. shown that on the average 1 in 3 of the lamps on regular main-
Yearbook of the Bureau of Mines, 1016. V. H. Manning. tenance was not in good condition, whereas the defects noted in
Bulletin 141, 165 pp. Paper, 30 cents. This bulletin describes the lamps not so maintained, average more than one for every
in some detail the more important work done by the Bureau of lamp.
Mines during 1916 in efforts to increase safety and efficiency in "One satisfactory system of estimating the expenses for main-
the mineral industries. The purpose and organization of the tenance work together with a set of unit costs is presented, based
bureau and a review of its work for each fiscal year are presented upon the analysis of the operation of 10 gas companies. A
in the annual reports of the director. Those reports are neces- suggested table of costs for each type of unit is given."
sarily summarized; they cannot give full details of noteworthy Determination of Absolute Viscosity by Short-Tube Vis-
experiments nor describe at length new and improved equip- cosimeters. W. H. Herschel. Technologic Paper 100, 53
ment, apparatus, and devices that are being used by the bureau pp. Issued November 9. Paper, 10 cents. "The conclusions
or have been devised by its engineers and chemists. This bulle- from this investigation for short tubes, such as are used in the
tin gives descriptions of some noteworthy safety devices and dis- Engler and the Saybolt Universal viscosimeters, are as
cusses in fuller detail than the annual reports the relation of the follows:
bureau's work to the general problems of safety and efficiency "1— The value of the product of the velocity of flow and diam-
in the mineral industries and the significance of the results that eter of tube, divided by the kinematic viscosity, must not be
the bureau has been able to achieve. greater than 800 if the flow is to be viscous rather than turbulent.
The Determination of Moisture in Coke. A. C. Fiki.dner "2 — Consequently water is not a suitable liquid for use in find-
and W. A. Selvig. Technical Paper 148, 8 pp. Paper, 5 cents. ing the relation between viscosity and time of discharge, and
"The experiments described in this i>:i]nr were undertaken; in Ubbelohde's equation and all others based upon it are seriously
the course of fuel investigations made by the Bureau of Mines, in error.
with the purpose of ascertaining the most rapid and simple "3 — A small but positive amount must be added to the
method for determining the moisture in coke with sufficient measured length of lube lo grt the effective length.
;-,(,
THE JOURNAL OF INDUSTRIAL AND ENGINEERING < III ' RY Vol. 10, No. r
"4 — Boussinesq's value of 1.12 for the coefficient of the kinetic-
energy correction would be approximately applicable if the av-
erage head could be correctly determined.
"5 — If the average head is determined by Meissner's formula,
which is the best available, although unsatisfactory and far from
accurate, a lower value must be used for the coefficient."
A Method for Testing Current Transformers. F. B. Silsbee.
Scientific Paper 309, 13 pp. Issued November 3. Paper, 5 cents.
Some Electrical Properties of Silver Sulfide. G. \Y. Yi.val.
Scientific Paper 310. 9 pp. "Silver sulfide may be prepared in
the form of short wires or thin strips like a metal. The wire,
which must be drawn hot, was found to conduct electricity like
a metal of high specific resistance and approximately zero tem-
perature coefficient. A strip of sulfide rolled at room tem-
perature has a large temperature coefficient and shows both
metallic and electrolytic conduction. It has a volt-ampere
curve characteristic of a pyroelectric conductor. The strips
are sensitive to small alternating currents, which increase the
resistance enormously, while small direct currents have the op-
posite effect. The specific resistance has been measured and ex-
periments made on the electrochemical decomposition."
Axial Aberrations of Lenses. K. D. Tillyer and H. I.
Siiultz. Scientific Paper 311, 24 pp. Issued November 3.
Paper, 5 cents.
COMMERCE REPORTS OCTOBER, 1917
The iron and steel output of Japan is expanding greatly,
especially in the shipbuilding, pipe and rail industries. (P. 10)
Among recently reported German discoveries or practice arc
the following: Formation of a viscous yellow mineral oil
by treating coal with liquid sulfurous acid; production of il-
luminating oil by heating naphthalene with aluminum chloride;
production of ozokerite from lignite; increase of 80 per cent in
the output of atmospheric nitrate plants; use of new lead and zinc
alloys to replace copper and brass; smelting of copper schists
with 0.7 per cent copper and of low-grade lead-sandstone ores;
production of aluminum from clay; smelting of low-grade nickel
ores; new methods for regeneration of rubber; and increased
use of nettles as a cotton substitute. (P. 50)
Steps are being taken to increase the production of candelilla
wax in Mexico. (P. 55)
A new petroleum refinery is in operation in Venezuela. (P.
57)
Large areas of mangrove are found in the Philippines with
21 varieties, the bark of which contains from 12 to 35 per cent
tannin. (P. 118)
Use of nettle fiber for textiles is increasing in Denmark. The
nettle "Urtica dioca" is about 30 in. high. It is dried, stripped,
and retted like flax, except that the water must be changed to
prevent fermentation of the sugar present. (P. 119)
Production of salt from sea water is proposed in New Zealand.
(P. 153)
Experiments in Scotland to increase the use of straw have
shown that it can be rendered more digestible for cattle food
by superheating with dilute caustic soda. Its use for paper pulp
is also increasing. Experiments on the use of straw as fertilizer
have shown that it stimulates the growth of "azotobacter,"
ami Other nitrogen organisms This effect is most marked with
straw containing 1 part of arsenic per 100,000. (P. 164)
Efforts arc being made to locate petroleum in Australia, which
is now entirely dependent on foreign countries for its oil supply.
(P. 168)
Gas is being used extensively in Birmingham, England, as a
substitute for gasoline in motor vehicles. 250 to 300 cu. ft.
of gas arc equivalent to 1 gal. of gasoline. No change in the
engine is required, and the only objection is the great bulk of
the gas containers. (P. 170)
The vegetable wax produced in Japan is extracted from the
fruit kernels of a native tree, by crushing, steaming and pressing.
It is refined by crude methods, which are, however, being im-
proved. It is used for polishes, pomades and soaps, and in dressing
leather. 'P. 227)
The Malay Peninsula is now the largest rubber-producing and
exporting country in the world. Exports to the United States
are now greater than to any other country. Pp. 232-6)
Exports of dyestuffs from the United States in July amounted
to $1,278,709, distributed to over 12 countries. 1 P. 271)
Additions to the "conservation" list of articles, export of which
from the United States is practically prohibited, include: phos-
phorus, babbitt metal, bichromate, bismuth salts, brass, bronze,
caustic potash, china-wood oil, ores, alloc, or compounds of
chromium, cobalt, copper, manganese, molybdenum, nickel,
tin, tungsten, and vanadium; crucibles, industrial diamonds,
electrodes, hydrofluoric acid, mercury, emery, graphite, solder,
type metal. The complete revised list is published. A complete
revised list of articles requiring a license for export is also in-
cluded. (Pp. 292-9)
A systematic prospecting of the placer deposits in the Ronda
Mountains in Spain have shown the presence of workable plat-
inum deposits, with extensive deposits of chromium, nickel and
magnetite ores. The nickel is present as garnierite, with 16-
20 per cent nickel, i. e., equal Canadian and New Caledonian
deposits. (P 311
Increased prices for antimony have caused the re-opening of
mines in Italy. (P
Exports of mineral oils from the United States in 1916-17
were greater than ever before. (P. 354)
A marked improvement is observed in the quality of dyestuffs
made in England. Many new dyes are available, but there is
still a lack of certain dyes, e. g., diamond black, B H direct cotton
black, patent blue, and rhodamin 6 G. (P. 360)
Production of iron and steel in Canada in 191 7 shows a de-
cided increase. (P
Canada has removed the prohibition on the manufacture and
sale of oleomargarine, which can now be sold under strict regu-
lations. (P. 417
The use of chromium in steel except for war purposes has been
prohibited in England, thus stopping the manufacture of "stain-
less" steel cutlery, etc. Chrome steel is being used for naval,
ordnance, and airplane part
A new zinc smelter is being erected in Mexico, to use petroleum
for fuel. 1'
Special, Supplements Issced in October
British Wl'st [ndkss — 22a British Guiana — t4a
Brazil — 40a Philippine Islands — 80a
Statistics op Exports to the I'nited States
1 i .<; — 156
Hr\zii.— Sup. 40a
Antimony
1
Hides
Earthenware
Diamonds
Hides
Ipecacuanha
Leather
Rubber
Peanut oil
Carnaaba wax
Aniseed oil
Jamaica — Sup. 22a
Cassia oil
Logwood
Peanuts
Logwood extract
Paper
Sugar
Rum
Tin
Fustic
Cumato
COMMERCE REPORTS. NOVEMBER, 1917
The mineral exports of New Zealand include gold, silver, tung-
sten, ore. coal, and kauri gum. "Kauri-gum oil," obtained by
distillation of peat found in kauri-gum swamps, is being used
with gasoline, as motor fuel. (P,
Efforts are being made to develop the production of winter-
green oil in Assain. India, when the leaves and stems of the
"gaultheria" plant yield, upon distillation, about 0.68 per cent
oil, as compared with as little as 0.12 per cent in other regions
of India. (P. 440)
Plans have been m.nlc in France for courses of instruction
for apprentices in metallurgical industries, to be conducted by
Jan., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
87
the employers; attendance is compulsory, but apprentices are
to be paid for the period of instruction. (P. 455)
All the London milk dairies have been consolidated into a
$20,000,000 corporation in order to effect economies in labor and
operation. (P. 456)
Export duties on manganese ore from Brazil have been in-
creased from $0.85 to $3.00 per ton. (P. 472)
Experiments are being conducted in Mexico upon the produc-
tion from bananas of flour, starch, vinegar, alcohol, fiber, paper
and cardboard. (P. 478)
A large detinning plant has been erected near Dundee, Scotland.
(P. 486)
To avoid exportation of raw hides and tanning materials from
India, efforts are being made to develop a local tanning in-
dustry. (P. 507)
Exports of wattle bark and extract for tanning purposes from
South Africa, show a marked increase. The trees are cultivated
from seed, and are cut down for stripping the bark, after five or
six years. (P. 508)
Cultivation of the wild geranium for the production of geranium
oil is being urged in India. (P. 516)
Wolframite is being mined extensively in South China. (Pp.
522 and 546)
A new law in Uruguay requires a chemical analysis of all
drugs and chemicals to be imported. Owing to lack of labora-
tory facilities much delay has arisen. (P. 539)
Mineral exports from Spanish Morocco include hematite,
galena and calamine. (P. 563)
A large part of the output of castor oil in England is now being
used as a lubricant for airplane engines. (P. 586)
The zinc industry of Russian Poland has been revived, with
an output nearly equal to that before the war. (P. 631)
Soap is now being made in Sweden from sewer fat, the oils of
beechnuts and horse-chestnuts. (P. 641)
A company has been organized in Sweden for the manufacture
of dyes. (P. 653)
Among the mineral products of Japan are antimony, chromite,
copper, gold, iron, lead, manganese, platinum, mercury, silver,
tin, tungsten, molybdenum, zinc, asphalt, coal, petroleum,
graphite, phosphate rock, pyrite, and sulfur. (P. 668)
Although Italy has rich zinc deposits, the output of zinc is
limited by the shortage of fuel. (P. 669)
Attempts are being made in Italy to briquette rice hulls for use
as fuel. (P. 678)
Mineral products of South Africa include gold, diamonds, coal,
copper, tin, antimony, asbestos, corundum, and lime. (P. 692)
There has been a great increase in the vegetable oil industry
in Sao Paulo, Brazil, including cottonseed, castor oil, linseed,
peanut, and cashew nut. (P. 710)
New Zealand has offered a bonus for the production of mer-
cury. (P. 718)
As a sugar substitute, "honey of grapes" is used in Italy. It
is obtained from unfermented grape juice by evaporation fol-
lowed by freezing (removing water and tartaric acid), and by
further evaporation under reduced pressure. (P. 756)
A large blast furnace, rolling mill, etc., are to be erected in
Holland to prepare, from foreign ores, steel for the shipbuilding
industry. (P. 771 J
The business of the British dye syndicate has been very suc-
cessful thus far. The list of colors has been greatly extended,
and the manufacture of intermediates has been increased. Re-
search is being conducted at the Universities of Oxford, Leeds
and Liverpool, and a main research laboratory is being erected
at Huddcrsfield. (P. 776)
A non-combustible substitute for celluloid, known as "Sato-
lite," has been introduced in Japan. It is made from the glucine
of Boya bean, coagulated by formaldehyde. (P. 779)
The mineral products of Burma include petroleum, salt, and
ores of tungsten, lead, silver, tin, gold, zinc, iron, antimony,
molybdenum, platinum, and copper. (P. 780)
The methods of making and coloring glass beads in Venice
are described in great detail. (Pp. 789-98)
The glycerine now being recovered in England from waste
fat, etc., from the army camps, is sufficient to provide propellant
ammunition for 17,000,000 shells per annum. (P. 811)
Owing to decreased demand for natural indigo, the production
in Madras is considerably below that of last year. (P. 820)
Investigation of vegetable fibers in Brazil has shown some
suitable for paper, but not for textiles. The latter are in great
demand for bagging, etc., owing to scarcity of jute. (P. 831)
Special Supplements Issued in November
France: — 5a, 6, c Scotland — 19d
Italy— 80 Ecuador— 43a
Netherlands — 96
Spain— 15e Peru— 46a
England — 196 Spain — 58a
Wales — 19c Egypt — 68a
Statistics of Exports to the United States
Hankow, China — 492
Antimony
Soya beans
Camphor
Albumen
Gall nuts
Hemp
Hides
Bean oil
Cottonseed oil
Rape seed oil
Soya bean oil
Nut oil
Sesamum seed
Tallow
Turmeric
Malaga — 580
Fusel oil
Tartar
Thymol
Hides
Juniper oil
-Sup. 5a
Lav
oil
Pennyroyal oil
Origanum oil
Rosemary oil
Thyme oil
Almond oil
Olive oil
Copper ore
Iron ore
Licorice
Glasgow — 598
Acids
Corundum
Creosote
Sodium cyanide
Hides
Magnesite
Paper stock
Ammonium sulfate
Marseilles — Sup. 5c
Benzoic acid
Citric acid
Belladonna
Cochineal
Glycerine
Hides
Nickel matte
Ocher
Copra oil
Olive oil
Palm oil
Papes stock
Graphite
Soap
Tin
Zinc oxide
Italy — Sup. 8a
Hides
Mercury
Fusel oil
Mr
ail
Parchment paper
Zinc ore
Citrate of lime
Pumice
Sulfur
Tartar
Artificial silk
Citric acid
Bergatnot
Sesame oil
Sumac
Senna
Zinc ore
Glassware
Bones
Carbon
Alizarin
Casein
Hides
I Hi-
oil
Peanut oil
Essential oils
Platinum
Saffron
Zinc ore
Havre — Sup. 56
Copper matte
Fertilizer
Optical glass
Hides
Colza oil
Flint pebbles
Prussiate of potash
Rubber
Lyon — Sup. 56
Calcium tartrate
Orchil extract
Gum arabic
Tartar
Copper matte
Hides
Enameled iron
Photographic plates
Artificial silk
Netherlanc
96
Beeswax
Chemicals
Drugs
Dyes
Cocoa butter
Fertilizers
Fibers
Hides
Ink
Leather
Matches
Paper stock
Paraffin
Rubber
Stearine
Formic acid
Spain — Sup. \he
Antimony
Argols
Fusel oil
Glycerine
Calcium tartrate
Potash
Hides
Lithopone
Barytes
Paper stock
Mercury
-Sup.
Olr
:oU
Peanut oil
Soap
Scotland — 1
Asphalt
Glassware
Leather
Paper stock
Guano
Hides
Gelatin
Acids
Hone char
( ,,.,1,1,1,1,,,
( Ireosote oil
Magnealte
Manganese o
England — Sup. 19&
Animal charcoal
Ammonia
Hides
Iron oxide
Alum
Barium carbonate
Carbolic acid
Creosote
Cresol
Fertilizer
Gum copal
Castor oil
Palm oil
Rape oil
Paris white
Ultramarine
Rubber
Bones
Copper
Grease
Ferro manganese
Coconut oil
Whale oil
Paper stock
Ammonium sulfate
Ammonium chloride
Bleaching powder
Cochineal
Cutch
Gum tragasol
Soda ash
Sodium silicate
Leather
Artificial silk
Tin
Ecuador — Sup. 43a
Gold
Hides
Indigo
Kapok
Ivory nuts
Rubber
Peru — Sup. 46a
Aluminum
Antimony
Copper matte
Silver
Guano
Hides
Molybdenum
Mercury
Rubber
Gold
Sugar
Tungsten ores
Vanadium ores
Zinc ores
Kerosene
Naphtha
Crude oil
Cocaine
Potassium sulfate
Siam — Sup. 58a
Gum benzoin
links
Slick lac
Tungsten ore
Gill!
abic
link-
Iron ore
Paper stock
Senna
Ivory nuts
77//. JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. i
BOOK RHVIE.W5
Standard Table of Electrochemical Equivalents and Their De-
rivatives. By Carl Hering and Frederick H. Gbtman.
130 pp. D. Van Nostrand Co., New York, 191 7. Price,
$2 .00 net
This little book should serve a useful purpose to the electro-
chemist or any one engaged in electrochemical work. The
tables, which are four in number, include electrochemical equiva-
lents by weight, grams per ampere hour in the order of magni-
tude, electrophysical equivalents by volume and the valences
of the elements in their combinations. The principal table is
that of the electrochemical equivalents by weight, and is very
complete. On eight pages are given the element, symbol,
atomic weight, valence, milligrams per coulomb, coulombs
per milligram, grams ampere per hour, ampere hours per gram,
pounds per 1000 ampere hour, and ampere hours per pound.
Calculations are taken up, giving by a well chosen set of
examples, the method best adapted for solving such problems
as are liable to arise in electrochemical work.
Part II deals with electrolysis, theory of electrolytic dissocia-
tions, Faraday law and coulometers, and a section is given to
the electronic theory-
An Appendix includes a chapter on valence, chemical reac-
tions and calculations, conversion factors used in electrochem-
ical calculations which is taken from Mr. Hering's "Conversion
Tables," and finally a glossary of terms
It will be seen that all of this information is to be found in
other books, but it is convenient to have it brought together
in one volume, and it is presented in a clear and logical manner
that should recommend it as a reference book.
Samuel A Ticker
A Short Manual of Analytical Chemistry, Qualitative and
Quantitative — Inorganic and Organic. Ry John Miter.
Ph.D., F.R.S.H., F.I.C., F.C.S., Analyst to the Metropolitan
Asylums Board, Late Editor of The Analyst, etc. 6th Amer-
ican Edition, Illustrated, xiii + 237 pp. Edited by J.
Thomas, Sc.D. P. Blakiston's Son & Co., Philadelphia,
191 7. Price, $2 .00 net.
This manual, which is prepared primarily for the use of
pharmacists, has previously passed through ten English and five
American editions, indicating its acceptability to the pharma-
ceutical profession. The notable characteristics of the present
edition is the revision of the procedures for the assaying of
drugs and the inclusion of the legal standards for drugs, as laid
down 111 the ninth decennial revision of the United States Pharma-
copoeia.
It is obvious that any attempt to cover so wide a field within
the compass of a short niiinu.it must involve extreme brevity
of treatment of main topii lures It is also true
that many of the procedures for the estimation of inorganic
nts will scarcer} appeal to the practicing analyst
outside of pharmacy, and it may be deplored that pharmacists
are disposed to accept such procedures without adequate criti-
cism. The fact remains, however, that the continued popu-
larity of this manual indicates that it satisfies a demand in the
field for which it is prepared, and the present edition is doubt-
less at least as satisfactory as those which have preceded it.
H. P. Talbot
The Chemical Engineering Catalog— 1917 Edition. 517 pp.
Illustrated. Obtained by special arrangement with the
Publishers, The Chemical Catalog Co., Inc New York City.
A need was felt, even before the recent new and increased
capacities in our chemical industry, on the part of the chemical
engineer, superintendent and buyer for a compilation containing
the fullest knowledge relative to chemical-technical data, plant
equipment and products and imparting information regarding
the source of supply of the manifold needs of laboratory' and
works. This information, so essentia] to the successful de-
velopment of the industry, was not only lacking in coordination
but also extremely meager, and the little that was obtainable
was scattered in periodicals, pamphlets and individual catalogs.
To supply this necessity, a joint supervisory committee was
appointed by the American Institute of Chemical Engineers,
the American Chemical Society and the New York Section
of the Society of Chemical Industry, with the result that the
first edition of the Chemical Engineering Catalog was published
in 1916 by the Chemical Engineering Catalog Co., Inc. This
first edition was of 288 pages of the size of This Journal, listed
136 manufactures of chemical plant equipment, products and
material, and contained in addition a number of illustrations of
apparatus and machinery. If the first edition was an experiment,
the edition of 1917 proves the success of the experiment. The
1 91 7 edition comprises 517 pages, 277 being devoted to illustra-
tions, descriptions and uses of a variety of plant equipment.
Such rapid strides must have exceeded the expectations of the
most optimistic sponsors of the Catalog and the editors of the
volume are to be congratulated on their accomplishment. An
improvement worthy of note is the division of the book into two
sections, one devoted to chemical plant equipment, data of in-
terest to the engineer and superintendent, while the other pertains
to materials and supplies peculiar to the province of the buyer.
Although the Catalog has doubled in size since last year,
it must be realized that it is not yet complete and represents
only part of that completeness contemplated by the editors
"to produce such an encyclopedia of trade information that the
engineer or buyer will be able to obtain from it the data neces-
sary to enable him to specify or purchase the equipment or
material required to take a plant from a mere idea to the point
where it is successfully turning out a finished product"
This has not yet been attained, but cooperation on the part
of those who unquestionably will benefit by such a work, will
assist so materially that it will not be long before the ideal
condition will be consummated.
There is ample assurance therefore that the Catalog will then
become the inseparable companion of the several classes opera-
tive in the Chemical Industry and. moreover, others who are not
yet interested will eventually find in it valuable information for
their respective fields of activity. With the improvements and
advances noted, it is only another convincing index of the prog-
ress and achievements of the American Chemical Industry.
Geo. D. Rosengarten
The Leather Specimen Book. B> Frederic \Y. LaCroix,
of the Blister & Vogel Leather C .. Wis. Price,
This book, as the author claims, has been prepared especially
for the use of those interested in a general ay in the manufac-
ture of leather. The descn; t processes em-
made brief, but at the same time it con-
ood idea of some of the numerous st iges through which
a hide or skin must pass before it becomes .1 iinished product.
The eighty tour specimens 1 ,wn, together
with the text accompanying each, are most interesting. Those
engaged in leather manufacture or in allit : lines will find this
volume both helpful and instructive.
Allen Rogers
Jan., 1918
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RECENT JOURNAL ARTICLES
Acid Open Hearth Process. Iv Rogers Blast Furnace and Steel Plant,
Vol S (1917), No. 12, pp. SI
Agriculture and National Defense. D. P. Houston. The
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Blast Furnace Gas: A New Blast Furnace Gas-Cleaning Machine. John
Ruddiman. Metallurgical mil • inuring, Vol. 17 (1917),
No. 10, pp. 608-611.
British National Physical Laboratory. I. W. Chubb. Industrial Manage-
ment, Vol. 57 (1917), No. 3, pp. 420-426.
British Welders and the World War. Frank Mynott. Journal of Acetylene
Welding, Vol. 1 (1917). No 6, pp. 254-256.
Caffetannic Acid a Bugaboo. C W. Trigg. Tea and Coffee Trade Journal,
Vol 33 (1917), No. 5, pp. 437-439.
Cement Floors: Protective Treatment for Cement Floors Subject to
Injurious Liquids. W. P. Anderson. Metallurgical and Chemical
Engineering, Vol. 17 (1917), No. 11, pp. 667-668.
Coal: Using Coal to the Best Advantage. E. H. Hinckley. Textile
World Journal, Vol. 53 (1917), No. 22, pp. 41-45.
Color: The Physical Basis of Color Technology. M. Luckiesh. Metal-
lurgical and Chemical Engineering, Vol. 17 (1917), No 11, pp. 631-637.
Cotton: Use of Cotton as a Wool Substitute. Textile World Journal,
Vol. 53 (1917), No. 23, pp. 25-27.
Crude Oil: A New Method of Burning Crude Oil. W. K. Janssen. Blast
Furnace and Steel Plant. Vol. 5 (1917), No. 12, pp. 569-570.
Dezincification of Brass Pipe. E. B. Story. Metallurgical and Chemical
Engineering, Vol. 17 (1917), No 11. pp. 653-659.
Engineering Advice in Making Electric Power Contracts. A. L. Johnston,
Jr Industrial Management, Vol. 54 (1917), No. 3, pp. 366-369.
Ferro-Manganese: Bibliography of the Manufacture of Ferro-Manganese.
E. C. Buck. Metallurgical and Chemical Engineering, Vol. 17 (1917),
No II, pp. 638-642.
Fertilizer Industry and the Potato Situation. H. G. Bell. The American
Fertilizer. Vol. 47 (1917), No. 11, pp. 28-31.
Fertilizers — An Interpretation of the Situation in the U. S. J E. Pogub.
The American Fertilizer, Vol. 47 (1917), No. 10, pp. 25-35.
Flotation: Status of the Flotation-Patent Litigation. R. C. Canby.
Engineering and Mining Journal, Vol. 104 (1917), No. 22, pp. 951-959.
Flotation Tests with Hardwood Oils. R. E. Gilmour and C. S. Parsons
Mining and Scientific Press, Vol. 115 (1917), No. 21, pp. 763-764.
Fuel: Methods for More Efficiency in Utilizing Our Fuel Resources.
H G. Barnhurst. General Electric Review, Vol. 20 (1917), No. 12,
pp. 924-931.
Fuel Oil: Practical Details in Burning Fuel Oil under Boilers. H. J.
Kennedy. Industrial Management, Vol. 54 (1917), No. 3, pp. 370-383.
Furnace Refining of Copper. Lawkence Addicks. Metallurgical and
Chemical Engineering, Vol. 17 (1917), No. 10, pp. 579-584.
Grinding Wheels: Economical Use of Grinding Wheels. W. T. Mon-
tague. The Iron Trade Review, Vol. 61 (1917), No. 22, pp. 1 153-1 159.
Heap-Leaching of Copper-Sulfide Ore. C. DeKalb. Mining and Scientific
Press, Vol. 115 (1917), No. 21. pp. 749-757.
Industrial Power on the Pacific Coast. H. J. Kennedy. Industrial
Management, Vol. 54 (1917). No. 2, pp. 214-224.
Industrial Waste — A Tax Paid to Ignorance. W. N. Berkeley. In-
dustrial Management, Vol. 54 (1917), No. 3, pp. 321-322.
Manganese: Utilizing Domestic Manganese Supplies. Edmund Newton.
The Iron Age, Vol. 100 (1917), No. 22, pp. 1290-1292.
Miami: The Smelting of Ore. T. A. Rickard. Mining and Scientific
Press, Vol 115 (1917), No. 22, pp. 784-796
Mill Pumping Stations. A. W. Allen. Metallurgical and Chemical
Engineering, Vol. 17 (1917), No. II, 629-631.
Oxide of Zinc. G E. Stonb. Mining and Scientific Press, Vol. 115 (1917),
No. 21, pp. 759-762.
Peat Production in 1916. J. S. Turp. The American Fertilizer, Vol.
47 (1917), No. 11. pp. 35-36.
Photographic Research Laboratory. C. E. K Mees. The Scientific
Monthly, Vol. 5 (1917), No. 6, pp. 481-496.
Physical Analysis of Refractory Material. Cosmo Johns. Blast Furnace
and Steel Plant, Vol. 5 (1917), No. 12, pp. 563-566.
Power Plant: Improving Power-Plant Operation through Instruction.
H. A. Fisher. Industrial Management, Vol. 54 (1917), No. 3, pp. 393-395.
Pyrite in Northern New York. D H. Newland. Engineering and Mining
Journal, Vol. 104 (1917), No. 22, pp. 947-948.
Refractories: Industrial Uses of Refractories. H. C Arnold. The
Iron Trade Review, Vol. 61 (1917), No. 23, pp 1212-1217
Rosin Size: The Cooking Process in the Manufacture of Rosin Size.
J. A. DeCew. Pulp and Paper Magazine. Vol. 15 (1917), No. 46, p. 1072.
Slide Rules: Design of Special Slide-Rules. A. L. Jenkins. Industrial
Management, Vol. 54 (1917), No. 2, pp. 241-248.
Sulfur: Recovery of Sulfur from Illinois Coals. J. E. Pogub. Metal-
lurgical u»d Chemical Engineering, Vol. 17 (1917), No. 10, pp. 584-585.
Tungsten: New Derivatives of Tungsten. J B Hill. Chemical News,
Vol 116 (1917), No 3225, pp. 235-238.
War Work of the Technical Societies. C. W. Rice The Iron Trade
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Wood: Economic Importance of Wood Preservation. K. C. Bartii.
Engineering and Mining Journal, Vol 104 (1917), No 23, pp 985-990
go
MARKET REPORT— DECEMBER, 1917
WHOLESALE PRICES PREVAILING tN THE NEW YORK MARKET ON DEC. 20
INORGANIC CHEMICALS
Acetate of Lime 100 Lbs.
Alum, ammonia, lump 100 Lbs.
Aluminum Sulfate, high-grade Ton
Ammonium Carbonate, domestic Lb.
Ammonium Chloride, white Lb.
Aqua Ammonia, 26°. drums Lb.
Arsenic, white Lb.
Barium Chloride Ton
Barium Nitrate Lb.
Barytes. prime white, foreign Ton
Bleaching Powder, 35 per cent 100 Lbs.
Blue Vitriol Lb.
Borax, crystals, in bags Lb.
Boric Acid, powdered crystals Lb.
Brimstone, crude, domestic Long Ton
Bromine, technical, bulk Lb.
Calcium Chloride, lump. 70 to 75% fused Ton
Caustic Soda. 76 per cent 100 Lbs.
Chalk, light precipitated Lb.
China Clay imported Ton
Feldspar Ton
Fuller's Earth, foreign, powdered Ton
Fuller's Earth, domestic Ton
Glauber's Salt, in bbls 100 Lbs.
Green Vitriol, bulk 100 Lbs.
Hydrochloric Acid commercial 20° Lb.
Hydrochloric Acid. C. P.. cone. 22° Lb
Iodine, resublimed Lb
Lead Acetate, white crystals Ltv
Lead Nitrate Lh
Litharge, American Lb
Lithium Carbonate Lb
Magnesium Carbonate. U. S P Lb
Magnesit:. "Calcined" Tod
Nitric Acid 40° Lb.
Nitric Acid. 42° Lb.
Phosphoric Acid. 48/50% Lb
Phosphorus, yellow Lb.
Plaster of Paris Bbl.
Potassium
Potassium
Potassium
Potassium
Potassium
Potassium
Potassium
Potassium
Potassium
Quicksilvt
Red Lead
Salt Cake
6.00
0
6. OS
4.00
0
4.50
60.00
0
80.00
11
<4
11V
15
g
17
18
®
19
15
0
16
65.00
@
70.00
9>/
0
11
28.00
e
30.00
2.00
(4
2.25
9»/i
a
9'/
7 V.
0
8
12»A
0
14
DOminal
5Vi
18.00
30.00
15.00
8.50
1.00
1.00
@ 15.00
2'/»
17 @
19
nominal
9>/>@
10
1 .50
18 @
20
60.00 @ 65
00
8>/i @
9
9 @
10
7>/i @
8
1.90 @ 2
00
1 50 @ 1
70
Bichromate, casks Lb.
Bromide, granular Lb
Carbonate, calcined. 80 O 85% Lb.
Chlorate, crystals, spot Lb.
Cyanide, bulk. 98-99 per cent Lb.
Hydroxide, 88 @ 92% Lb.
Iodine, bulk Lb.
Nitrate Lb.
Permanganate, bulk Lb.
r. flask 75 Lbs.
American, dry Lb.
glass makers' Ton
Stiver Nitrate Or.
Soapstone, in bags Ton
Soda Ash. 58%, in bags 100 Lbs.
Sodium Acetate Lb.
Sodium Bicarbonate, domestic 100 Lbs.
Sodium Bichromate Lb.
Sodium Chlorate Lb.
Sodium Fluoride, commercial Lb.
Sodium Hyposulflte 100 Lbs.
Sodium Nitrate. 95 per cent, spot 100 Lbs.
Sodium Silicate, liquid, 40° Be 100 Lbs.
Sodium Sulflde . 60%. fused. In bbls Lb.
Sodium Bisulfite, powdered Lb.
Strontium Nitrate Lb.
Sulfur. Sowers, sublimed 100 Lbs.
Sulfur, roll 100 Lbs.
Sulfuric Acid, chamber 66° 3i Ton
Sulfuric Acid, oleum (fuming) Ton
Talc, American white Ton
Terra Alba. American. No. 1 100 Lbs
Tin Bichloride. 50° 100 Lbs.
Tin Oxide Lb.
White Lead. American, dry Lb.
Zinc Carbonate Lb.
Zinc Chloride, commercial Lb
Zinc Oxide. American process XX Lb.
ORGANIC CHEMICALS
Acetanllid. C. P . In bbls Lb.
Acetic Acid. 56 pot cent. In bbls Lb.
Acetic Acid, glad 1. 99>/t%. in carb oys Lb
Acetone, drums Lb.
AloaboL denatured. 1 80 proof i '. • 1.
.1 45 @ 1.46
lominal
82
e 84
2.90
28
@ 30
4. 10
@ 4.15
15.00
@ 120.00
10
@ 10'/
30.00
@ 35.00
S3
& 56
10.00
@ 12 50
2 90
@ 3.00
24'/.
60.00
15.00
2.00
4.75
2.00
© 65 00
@ 18 00
9./,
10'/.
Alcohol, sugar cane. 188 proof Gal
Alcohol, wood. 95 per cent, refined GaL
Amyl Acetate Gal.
Aniline Oil, drums extra Lb.
Benzoic Acid, ex-toluol Lb.
Benzol. Pure Gal.
Camphor, refined in bulk. bbls. Lb.
Carbolic Acid, U. S. P.. crystals, drains Lb.
Carbon Bisulfide Lb.
Carbon Tetrachloride, drums. 100 gals Lb.
Chloroform Lb.
Citric Acid domestic, crystals Lb.
Creosote, beech wood Lb
Cresol. U. S. P..
Lb.
Dextrine, corn (carloads, bags) Lb.
Dextrine, imported potato Lb.
Ether. U. S. P 1900 Lb
Formaldehyde. 40 per cent Lb
Glycerine, dynamite, drums included Lb.
Oxalic A.id in casks Lb.
Pyrogallic Acid, resublimed . bulk Lb.
Salicylic Acid, U. S. P Lb.
Starch, cassava Lb .
Starch, corn (carloads, bags) pearl 100 Lbs.
Starch, potato. Japanese Lb.
Starch, rice Lb.
Starch : sago flour Lb
Starch, wheat Lt.
Tannic Acid, commercial Lt.
Tartaric Acid, crystals Lr.
OILS, WAXES, ETC.
Beeswax, pure, white Lb.
Black Mineral Oil. 29 gravity Gal.
Castor OU No. 3 Lb.
Ceresin. yellow Lb.
Corn Oil, crude Lb.
Cottonseed Oil. crude, f o. b. roUl Gal.
Cottonseed Oil. p. 8. y Lb.
Menhaden OU. crude (southern) Gal.
Neat's-foot Oil. 20° Gal.
Paraffin, crude 118 to 120 m. p Lb.
Paraffin Oil, high viscosity Gal.
Rosin. "F" Grade. 280 lbs Bb".
Rosin Oil first ran Gal
Shellac, T. N Lb.
Spermaceti, cake Lb.
Sperm Oil. bleached i winter. 38* Gal.
Spindle Oil. No 200 Gal.
Stearic Acid, double-pressed Lb.
Tallow, acidless Gal.
Tar OU. distilled Gal.
Turpentine, spirits of Gal.
METALS
Aluminum. No. 1. ingots Lb.
Antimony, ordinary Lb.
Bismuth. NY Lb.
Copper, electrolytic Lb.
Copper, lake Lb.
Lead. NY Lb.
Nickel, electroly tic Lb.
Platinum, refined, soft Ox.
SUver Ox.
Tin. Straits Lb.
Tungsten (WO.) Per Unit
Zinc. N. Y Lb.
FERTILIZER MATERIALS
Ammonium Sulfate 100 Lbs.
Blood, dried, f. o. b Chicago Unit
Bone. 3 and 50. ground raw Ton
Calcium Cyanamid Unit of Ammonia
Calcium Nitrate. Norwegian 100 Lbs.
Castor Meal Unit
Fish Scrap, domestic, dried, f. o. b works Unit
Phosphate, acid. 16 per cent Too
Phosphate rock. f. o. b. mine
Florida land pebble. 68 per cent Ton
Tennessee. 78-80 per cent Ton
Potassium "muriate." basis 80 per cent Ton
Pyrites, lurnacc sixe, imported Unit
Tankage, high-grade, f o. b. Chicago. .
5.05
•
3.25
1.35
0
1.40
5.2S
0
5.50
26
a
27
3.20
0
3.30
43
0
45
76 '/i
*
77>
53
0
54
7 V
0
8
14
0
16
63
0
65
75
0
78
1.90
<4
2.00
18
0
20
7
<s
8
18
0
20
27
0
30
19
0
20
62
g
64
45
0
46
3.15
0
3.25
1.2S
&
1.30
6.30
0
6.45
10V»
0
11
10
0
12
6'/.
0
7>
5'/.
■
6>
50
0
60
78>/s
0
79
32
@ 33
nominal
—
@ —
1.30
@ 1.35
18.60
@ 18.70
—
@ -
2.50
@ 2.60
lO'/i
@ 11
2.85
23 V.
23 Vt
lSVs
2.90
nominal
25.00 @ 25.00
7.30
0
7.35
6.60
0
6.65
32.00
9
35.00
norair
al
6.50
@
10
16.00
0
16.50
5.50
0
6. SO
9
2. SO
5.50
6
6.00
350.00
0
355.00
lomin
al
The Journal of Industrial
and Engineering Chemistry
Published by THE AMERICAN CHEMICAL SOGIETY
AT EASTON, PA.
Volume X
FEBRUARY 1, 1918
No. 2
Editor: CHARLES H. HERTY
Assistant Editor: Grace MacLeod
Advertising Manager: G. W. Nott
ADVISORY BOARD
H. E. Barnard, H. K. Benson, F. K. Cameron, B. C. Hesse, A. D. Little, A. V. H. Mory, M. C. Whitaker
Published monthly. Subscription price to non-members of the American Chemical Society, $6.00 yearly; single copy, 60 cents
Price per single copy to American Chemical Society members, 50 cents. Foreign postage, seventy-five cents, Canada, Cuba and Mexico excepted
Entered as Second-class Matter December 19, 1908, at the Post-Office at Easton, Pa., under the Act of March 3, 1879
All communications should be sent to The Journal of Industrial and Engineering Chemistry.
Telephone: Vanderbilt 1930 35 East 41st Street, New York City
Subscriptions and claims for lost copies should be referred to Charles L. Parsons, Box 505, Washington, D. C.
ESCHENBACH PRINTING COMPANY, EASTON, PA.
TABLE OF CONTENTS
Officers for 19 18:
Dr. Nichols — Leader in Chemical Industry 92
Editorials :
On with the Investigation 93
Somebody, Please Cut the Tape 94
Platinum Oscillations 95
An Appreciation and a Greeting 95
Chemistry Insignia 95
Original Papers:
The Extraction of Potash and Other Constituents from
Sea Water Bittern. Joel H. Hildebrand 96
The Direct Heat Treatment of Cement Mill Dust to
Increase Its Water-Soluble Potash Content. Albert
R. Merz 106
Effect of Coal Ash on the Liberation and Nature of
Cement Mill Potash. N. S. Potter, Jr., and R. D.
Cheesman 109
Toluol Recovery and Standards for Gas Quality. R. S.
McBride 1 1 1
Catalysts in Vulcanization. D. Spence 115
Vulcanization of Rubber by Selenium. Charles R.
Boggs "7
The Pigments of the Tomb of Perneb. Maximilian
Toch 118
The Preparation of N/100 Permanganate Solutions. J.
O. Halverson and Olaf Bergeim 119
The Use of Microorganisms to Determine the Preserva-
tive Value of Different Brands of Spices. Freda M.
Bachmann 121
Disinfection with Formaldehyde. A Substitute for the
Permanganate-Formalin Method. C. G. Storm. . . . 123
Effect of Fertilizers on Hydrogen-Ion Concentration in
Soils. F. W. Morse 125
The Seeds of the Echinocystis Oregana. Milo Reason
Daughters 126
Variation in the Ether Extract of Silage. L. D. Haigh . 127
Laboratory and Plant:
Some Methods of Analysis for Nebraska Potash Salts
and Brines. A. H. McDowell 128
Suggestions on Some Common Precipitations. George
H. Brother 129
A New Portable Hydrogen .Sulfide Generator. W.
Faitoute Munn 13°
An Automatic Hydrogen Sulfide .Stopcock. Carl H.
Classen 1 3 '
A Simple and Efficient Filtering Tube. William M.
Thornton, Jr 132
Addresses:
The Automatic Control and Measurement of High
Temperatures, Kichard P. Brown 133
Airplane Dopes. Gustavus J. Esselen, Jr 135
The Collaboration of Science and Industry. V. Grig-
nard 137
Perkin Medal Award:
Introductory Address. Jerome Alexander 138
Mr. A. J. Rossi and His Work. F. A. J. FitzGerald ... 138
Presentation Address. William H. Nichols 140
Address of Acceptance. Auguste J. Rossi 141
British Progress in Dyestuff Manufacture:
British Dyes Limited. James Falconer, M. P 145
Levenstein Limited 149
Current Industrial News:
Platinum in Spain; Tungsten in Malaya; Tubular Cycle
Components; Magneto Machines for Pocket Torches;
Thermit Welding; Refractory Properties of Magnesia
Bricks; Prevention of Scale in Boilers; Electric Heat
Storage in Boilers; British Board of Trade; Mineral
Production of Victoria; Manufacture of Electrodes;
Recovery of Potash and Magnesia from Canadian
Lake; Fluxes; Waterproof Varnish from Oil; Shellac
Derivatives; Cellulose Turpentine; Substitute for Oil
in Paint; Dye from Sulfite Lyes; Electric Arc Weld-
ing 150
Scientific Societies:
Reduction of Waste; Seventy-Fifth Annual Meeting
American Association for the Advancement of
Science, Pittsburgh, Pa., December 28, 1917 —
January 2, 191 8; American Metric Association;
Annual Meeting Technical Association of the Pulp
and Paper Industry, New York City, February 5-7,
1918; New York Section of the Societe De Chimie
Industrielle 153
Notes and Correspondence:
Two Letters on the Chemical Control of Ammonia
Oxidation; Avoidable Waste in the Production of
Sulfuric Acid by the Chamber Process; Bromine Pro-
cess Decision; United States Tariff Commission In-
quiry in Regard to Chemical Industries; Special
Chemicals and Apparatus Available through the
Chemistry Committee of the National Research
Council; As to Platinum; Platinum Resolutions;
Fuel for Manufacture of Chemicals; A Study of the
Estimation of Fat in Condensed Milk, Etc. — Correc-
tion; Composition of Loganberry Juice and Pulp — ■
Correction; Chemists and the Draft 155
Washington Letter l6°
Personal Notes ' ° '
Industrial Notes io2
Gcivkknment Publications l65
Book Reviews l67
New Publications ,69
Market Report '7°
TUE JOURXAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 2
OFFICLR5 FOR 1918
The following officers have been elected by the
American Chemical Society for the year 1918:
President: William H. Nichols, General Chemical
Company, New York City.
Directors: H. E. Barnard, State Laboratory of
Hygiene, Indianapolis, Ind.; and G. D. Rosengarten,
Powers -Weightman - Rosengarten Co., Philadelphia,
Pa.
Councilors -at- Large: H. E. Howe, A. D. Little,
Inc., Cambridge, Mass.; G. A. Hulett, Princeton
University, Princeton, N. J.; W. A. Noycs. University
of Illinois, Urbana, 111.; and Allen Rogers, Pratt
Institute, Brooklyn
X. Y.
DR. NICHOLS-LEADER
IN CHEMICAL
INDUSTRY
By C. F. Chandler
Dr. William H.
Nichols was one of the
small group of New
York chemists who, in
1876, originated this by
far the largest chemical
society in the world. It
now has 5 1 local sections
and appr oximately
11,000 members, and
publishes three distinct
chemical journals.
Dr. Nichols was born
January 9, 1852, in
Brooklyn, N. Y. He
graduated from the
Brooklyn Polytechnic
Institute in 1868 and
then entered New York
University, where he
had the good fortune to
study chemistry under
Dr. John W. Draper, the
first President of the
American Chemical So-
ciety. He received his
B.S. in 1870. In 1S73 he received his M.S. from
the same institution; in 1904, LL.D. from Lafayette and
Sc.D. from Columbia. In 191 2 he was decorated by
the King of Italy with the Order of Commendatore of
the Crown of Italy. He was president of the English
Society of Chemical Industry 1904-1905 and of the
Eighth International Congress of Applied Chemistry
held in Washington and New York in 191 2.
In 1870. when only eighteen years old. he founded
his own chemical business under the title G. H.
Nichols and Company, using his father's name be-
cause he was not yet of age. Later the business was
incorporated as the Nichols Chemical Company.
William H. Nichols. President American Chemical Soclety
The instincts of the pioneer in Dr. Nichols led to the
origin in his plant of many ideas and appliances used in
chemical industry to-day, for example, the well-known
practice of storing and transporting sulfuric acid in steel.
The manufacture of sulfuric acid from pyrites was
first carried out profitably in the Nichols Chemical
Works at Laurel Hill. The pyrites used contained
some copper and the search for the proper metallurgical
treatment of it led to the invention of methods still
employed for smelting such ores and also to the devis-
ing of a method for analyzing copper by electrolysis,
which was the foundation of the industry of the elec-
trolytic refining of cop-
per. These processes
for smelting and refining
copper ores were so suc-
cessful that the business
grew rapidly to such di-
mensions that in 1898
it was transferred to a
special company, the
Nichols Copper Com-
pany, of which Dr. Nich-
ols is president. The
works, located on New-
town Creek, Brooklyn,
constitute one of the
most extensive copper
plants in the world. In
1899, the chemical
branch of the business
went into the General
Chemical Company.
The superior execu-
tive ability of Dr.
Nichols shows in the
success he has had in
such enterprises as the
rehabilitating of the
Granby Consolidated
Mining. Smelting and
Power Company, Ltd.,
ing it into one of
the best-managed cop-
per companies in the
world: the recent or-
ganizing of the National Aniline and Chemical Company,
Inc., looking to the permanent relief of American textile
manufacturers and others; the bringing of a new lease
of life to his Alma Mater, the Polytechnic Institute of
Brooklyn, which seemed to be on the decline but is to-
day a school of engineering of high mark, due largely
to the good work of Dr. Nichols.
With all these business activities Dr. Nichols has
is chairman of the Committee on Chemicals for
the government and just recently has been appointed
by Secretary Lane chairman of the Committee of
Chemists advisory to the Bureau of Mines.
New York Otv
Feb.. 101S
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
93
EDITORIALS
ON WITH THE INVESTIGATION
The massing of German reinforcements from the
East on the western front led Winston Churchill,
British Minister of Munitions, in an address at the
American Luncheon Club recently, to exclaim:
"America! Come and aid us with all your might and
speed, for this is a matter for action on the largest
scale ever planned. * * We are sure to win the
whole of President Wilson's program if we will utilize
all our resources fully." Such an appeal, coming
from a member of a race strong in self-reliance and
bull-dog tenacity, must sink deep into the heart of
every American.
That we have lacked speed in many of our prepara-
tions has been shown clearly by the investigations of
the Senate Committee on Military Affairs. The re-
ports show that the Committee felt fully capable of
probing deep into the supply of cannon, machine guns
and rifles, but when the subject of ammunition for
such arms, and particularly of the basic chemicals
needed in its manufacture, was approached, the in-
vestigation seemed at once to veer from so technical
a subject. This is not difficult to understand, and
yet we feel that the Committee can perform further
public service if it will extend its investigations to
cover thoroughly this field, particularly as to acetic
acid for aeroplane dope and toluol for high explosives.
Enormous quantities of acetic acid are needed
immediately, and until this is supplied the aviation
program will be held up. The present total output
of this product is already engaged for the Navy and our
Allies. New factories must be built for further output.
With the liberty motor completed, with all arrange-
ments made for the supply of spruce wood in abun-
dance, the startling fact remains that, unless action has
been taken within the twenty-four hours previous to
this writing, not even the method of manufacture of
the necessary acetic acid has been decided upon, much
less has the erection of any plant begun. In view of the
tremendous difficulties of plant construction in these
times, it is appalling to think of the delays ahead in
this work which even in peace times and under normal
conditions would prove an extremely formidable under-
taking. It looks as if someone has blundered seriously,
•especially when we reflect upon the unprecedented
speed with which Congress at the outset appropriated
$650,000,000 for the aviation service.
The fundamental importance of toluol, the great
need for it in the production of high explosives, and
the method of its manufacture by stripping gas
are well understood at the present time. Appro-
priations have been available since the adjourn-
ment of the previous session of Congress. Nearly
six months have elapsed since the conference was held
in Washington between representatives of the War
Department, the gas producers, and the public service
commissions. Yet to-day there are many gas plants
with which no final arrangements have been made by
the War Department for the erection of scrubbers to
strip the gas. That this condition is not due to lack
of cooperation by the companies is indicated in a let-
ter to us from Brig. -Gen. William H. Crozier. Under
date of October 17, 1017, he states: "We have re-
ceived a ready response to cooperate with us from
every company that we have written to so far." We
have been informed by the Ordnance Department that
for the present at least negotiations for the installation
of apparatus for the recovery of toluol will not be
conducted with gas plants whose capacity would be
less than 40,000 gallons per year. It would be interest-
ing to learn through a public investigation how far
these negotiations have resulted in actual contracts
and inauguration of construction work, and what
dates such contracts bear. Unfortunately we are
not in position to give much detailed information on
this point, but we know of one contract which has
been shifting forward and backward for months, and
is not yet signed. Whether the delay in settling
the petty features of the contract is due to the attitude
of the manufacturer or to the methods of the War
Department it is not for us to judge; but we do
know that the construction firm in question would
not be at all adverse to an investigation of the reasons
for this delay. When all is said, it is not a ques-
tion of this or that manufacturer; if any such firm
delays the prompt execution of government plans, turn
aside from him and get a contractor who will start the
work promptly It is toluol that is needed, and not the
saving of a few cents per gallon in its production. It
would seem that officials of the War Department are
still following the leisurely ways of contract making
characteristic of peace times, while material which may
be of the utmost importance at a critical moment is
now being burned, and can never be recovered.
Of course the decision to use mixtures of toluol and
ammonium nitrate for high explosives relieves the
situation somewhat, nevertheless the ammonia plants
are not yet completed. We have upon us the
responsibility of supplying not only the needs of our
own Army, but of aiding in every way possible those of
our Allies. This applies particularly to Italy, fighting
so resolutely to-day, its very existence immediately
threatened.
If it be held that toluol recovery must not exceed
nitration capacity because of lack of storage tanks,
will not the War Department contemplate the many
cases of seemingly autocratic procedure adopted by
government officials during the last few weeks, acts
which have been accepted cheerfully by the country
because they were war measures? In the light of such
procedure the storage question can readily be solved
by commandeering some of the many storage tanks
scattered throughout the country and now filled with
petroleum products. Can anyone doubt the relative
value to ourselves and our Allies of a half dozen such
storage tanks filled on the one hand with kerosene,
or on the other hand with toluol? Then too, is the
94
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 2
War Department certain that the nitration capacity
of the country is not in excess of toluol recovery,
or that it will not be so by the time the recovery plants
are installed? Already the coal shortage has seriously
diminished the production of toluol from the by-
product coke ovens, until now the chief source of
supply.
This country can possess no more valuable reserve
than ample quantities of stored toluol. Another Hali-
fax disaster, the bombing of a few munitions stations,
the sinking of a few supply ships stored with this
material might at any moment make a serious shortage,
a shortage which would be criminal with all the lives
at stake, if the possibility of such can be avoided.
Cn with the investigation! Senator Chamberlain can
perform a distinct service if through his Committee he
can speed up matters in the supply of such materials.
The country will hereafter crucify with its scorn any
manufacturer who now seeks to profiteer at its expense
in this its hour of trial. So, too, will the country hold
accountable those of its public servants who dilly-dally
over minor details in fundamental matters.
SOMEBODY, PLEASE CUT THE TAPE
If the National Retail Merchants' Association should
arbitrarily rule that all would-be purchasers of hats
must be supplied with the hat most convenient to the
reach of the clerk in attendance, without regard to the
shape, color or size of the hat, what manner of Easter
parade would result from males and females thus
adorned! Or suppose the Amalgamated Employment
Bureau should decree that seekers of help could secure
only "the next on the list," regardless of qualifications.
What would eventually result to the regular processes
of commercial life if, seeking a stenographer, one should
draw a cook! These suggestions are not intended to
reflect on the good qualities of the number six hat on
the seven and a half head or on the abilities of the do-
mestic in her proper sphere. Wait a minute — these
cogitations are not trivial.
Burns was all right when he wrote "A Man's a Man
for a' That," but there are all kinds of men and there
are all kinds of chemists: analytical and research chem-
ists, organics and inorganics, chemists fresh from the
universities and chemists who have been able to add
to their university training valuable plant experience.
Some have specialized in explosives, others in metal
alloys. Some are accurate in analytical work, others excel
in planning research. If, however, a government depart-
ment, bureau or division wishes to increase its chemical
force by securing the transfer of a specially qualified
chemist from a cantonment to a government labora-
tory, such coordinate branch of the government ser-
vice must send out to the camps and simply ask for
a chemist. Chemists must not be sought by name.
To request a specially qualified man, designating the
man you want, is no longer permitted. Such is the
ruling of the General Staff of the Army, to which ruling
the War Department has strictly adhered for some
weeks past. Shades of common-sense America, what
an absurd situation! Is this the final outworking of the
spirit of the selective draft which President Wilson
assured us was to fashion this nation into the most
efficient fighting machine, which law, the record of these
columns will testify, we have striven steadfastly to
uphold? Is Secretary Baker aware of this ruling,
a ruling which was not brought into being three thou-
sand miles away, but right in the city of Washington
in his own Department?
The results of such procedure are not only disaster
to government chemical work but serious demoraliza-
tion of the staffs of the chemical industries, which are
supplying the very sinews of war. This can be illus-
trated best by two specific cases. A colonel in the
Ordnance Department wrote recently to a prominent
chemical manufacturing company stating that the
Department was desirous of securing the services of
a number of chemists and factory foremen for use as
inspectors at munitions plants. He specified that they
should have had such experience as would enable them
to carry out intelligent inspection of explosives manu-
factured for the government in this emergency. The
manufacturer was asked to go over his organization and
advise as to any men who might be available and whom
he could recommend. That is all right from one point
of view. Of course the government must have compe-
tent inspectors, and chemical manufacturers are just
as patriotic as other men and will gladly sacrifice their
staffs if need be. That is the real question, "if need
be." There are more than three hundred chemists
in cantonments to-day, practically inaccessible for
government chemical work because of this remarkable
ruling of the General Staff. One of these is a graduate
of two leading American universities, in each of which
he specialized in chemistry. Furthermore he has had
three and a half years of experience in research and
in the manufacture of explosives, dyestuffs and pharma-
ceuticals, and is familiar with the installation and
operation of chemical machinery. Yet his daily duties
consist of scrubbing floors, shoveling coal or cinders,
chopping wood, digging ditches (not trenches) and
general work around the stable or kitchen.
We do not seek to arouse sympathy for this young
soldier chemist. He is having a good experience
and loyally doing his duty as any other young Amer-
ican would; his clear eye and soldierly bearing show,
too, that he has made good as a soldier. He makes not
the slightest complaint. But we do feel that the gov-
ernment is not getting from him the most efficient
service he could perform; and it is a shame for a simi-
larly qualified man to be taken at this time from the
industries for government work while such a man could
be made available in a few hours were it not for the
weird ruling of the General Staff.
Sixteen thousand chemists at the outbreak of the
war filed with the Bureau of Mines complete data
concerning their training and specialization in order
that their services might be promptly and intelligently
availed of as need arose. Alas, these cards of volun-
tary information are now bound tightly together by
the red tape of this rule-beyond-understanding promul-
gated by the General Staff.
Somebody, please cut the tapel
Feb., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
95
PLATINUM OSCILLATIONS
At the recent meeting of Section C (Chemistry)
of the American Association for the Advancement of
Science at Pittsburgh the platinum resolution (page
159, this issue), introduced by Mr. George P. Kunz,
of Tiffany & Co., New York City, was unanimously
passed. To present this matter to the proper authori-
ties a committee was appointed consisting of Dr. W.
A. Noyes, Chairman, and Dr. W. F. Hillebrand.
The admirable suggestions contained in the resolu-
tion will appeal immediately to every chemist in uni-
versity or technical laboratories. Unfortunately for
the ray of hope held out by this movement, Dr. Hille-
brand, of the Bureau of Standards, in declining to
serve upon the committee, felt compelled to take this
step because of his knowledge that all of this platinum
supply is needed immediately by the government,
and has indeed already been turned over to the Nitrate
Committee for catalyzer purposes in the oxidation of
ammonia. There seems, at least for the present, no
hope that the use of residues for research on the platinum
group of minerals can be undertaken, as the question of
government ownership of this material is undetermined.
The accounts of the energy, resourcefulness, and
peregrinative ability of Mr. Draper, who safely trans-
ported from Russia 21,000 ounces of platinum and
platinum ore and delivered it to the Department of
Commerce, furnish very interesting reading and com-
mand unquestioned appreciation of his achievement.
The necessity for such a journey, however, suggests
further thought as to the accuracy of judgment of
the Secretary of Commerce, who last Spring, evidently
while this material was being collected, gave ample
assurances to the jewelers of the country that the
government had an abundance of platinum, either on
hand or available from stocks known to be existing
abroad, which statement was heralded very widely by
the Jewelers' Committee. We tremble to think of
the fix the government might have been in if Mr.
Draper had stubbed his toe in going aboard ship and
spilled the precious metal into the sea, or had lost
his trunk in the mazes of the Union Station baggage
room in Washington, or had met with the same delay
in express shipments which the average citizen en-
counters nowadays. Seriously, we have been running
very close to the danger line in government supplies
of this material for munitions manufacture, while the
advertising campaign for platinum jewelry has gone
merrily on. Meanwhile, the university and industrial
chemist cannot hope for relief from the present high
prices of platinum ware from the source contemplated
by the resolution of Mr. Kunz.
The communication from Dr. Jas. Lewis Howe,
printed in this issue, views the platinum situation solely
from the standpoint of "business as usual," an anti-
quated slogan whose pernicious effect upon war pro-
grams has already made itself plainly evidi
Two new tn< thods of attacking the problem of plat-
inum conservation have developed. Individuals and
local Sections can use their influence with the local
press to persuade them to refuse advertisements of
platinum jewelry. The New York Times and the
New York World have adopted such a policy, and it
it is a pleasure to state that this has been done on the
urgent appeal of Mr. Kunz, who is endeavoring to
bring all of the New York newspapers into line.
The second interesting development is the recent
organization of the Women's National League for the
Conservation of Platinum. May the good work of
this new organization prosper in every way. It is
for women that this platinum jewelry is designed;
it is through women that its use can be most effectually
discountenanced. Perhaps through this League the
real punch will be put into the platinum conservation
movement.
AN APPRECIATION AND A GREETING
The appearance of the January number of the
Journal of the American Chemical Society marks the
retirement of Dr. W. A. Noyes from its editorship
and the entrance upon his duties of the newly elected
editor, Dr. A. B. Lamb.
After fifteen years of splendid service, Dr. Noyes
carries with him on retirement universal grateful ap-
preciation of the devotion he has shown to the upbuild-
ing of that Journal. To its list of contributors he has
called all of the research workers in pure chemistry
in this country. As a result of his accurate and con-
scientious editorial work the publication stands to-day
as one of the great chemical journals of the world.
In assuming his new task, Dr. Lamb may feel con-
fident of the continuation of that spirit of cooperation
which in the past has proved so potent a factor in the
success of the Journal. He has, moreover, the solid
satisfaction of knowing that not only was he the
unanimous choice of the Council, but that such choice
was based upon the unanimous report of a committee
of our ablest men who canvassed the field with closest
scrutiny. The fact that Dr. Lamb begins his editor-
ship while devoting much of his time to government
service constitutes an additional reason for loyal
support.
CHEMISTRY INSIGNIA
For the first time in the history of the United States
an Army group will wear a design typifying chemistry
as a recognized branch of war service. Through the
courtesy of the manufacturers we are the proud pos-
sessors of the first insignia and collar design struck from
the dies.
Officer Enlisted Man
Insignia for Chemical Service
From the record of attainments of the first men
selected to wear such insignia it can be predicted with
certainty that they will be worthily worn.
Good luck to the Chemical Service Section of the
National Army!
96
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10 No. 2
ORIGINAL PAPERS
THE EXTRACTION OF POTASH AND OTHER
CONSTITUENTS FROM SEA WATER
BITTERN1
By Joel H. Hildkbrand
Received December 5, 1917
COMPOSITION OF SEA WATER
The main constituents of sea water, besides sodium
chloride, are magnesium sulfate, magnesium chloride
and potassium chloride, together with a small quantity
of magnesium bromide and calcium salts. During
the evaporation of the sea water to secure sodium
chloride, the calcium present is almost completely
deposited as calcium sulfate, so that calcium salts are
practically absent from the mother liquor. By con-
sidering the various analyses of sea water we may calcu-
late the relative amounts of the solid salts that might
be obtained by evaporation. The salt works around
San Francisco Bay, with which we are primarily con-
cerned, produce something over 100,000 tons of sodium
chloride per annum; the amounts of the other salts
associated with this amount of sodium chloride would
be as follows:
Tons
Sodium chloride (NaCl) 100,000
Potassium chloride (KC1) 2,800
Magnesium chloride (MgCh.6H>0) 27,300
Epsom salts (MgSOi.7H«0) 16,000
Bromine (Br) extracted from the bromides 240
At this time, when the country is suffering from an
acute shortage of potassium salts, the amount of
potassium chloride indicated above is of considerable
importance. During the first half of 191 7 the total
potash production of the country, calculated on
the basis of K2O, was 14,000 tons, which amount was
but 10 per cent of the normal amount used before the
war. It is evident that the amount of potash that
could be extracted from the bitterns of the salt works
on San Francisco Bay alone would add about 10 per
cent to the country's present annual production of
potash. The amount of salt actually produced in
this region is nearly 140,000 tons per annum, so that
a liberal allowance for losses in working up the bittern
should leave still 3000 tons of potassium chloride.
By utilizing the bitterns from other regions on the
Pacific Coast, notably San Diego, this amount would
be very greatly increased.
The other materials mentioned in the above table
also represent very considerable values, although they
have less relation to the present national emergency.
After the removal of most of the common salt in the
salt ponds, the other salts would be contained in ap-
proximately 100,000 tons of bittern, having a volume
of approximately 100,000 cubic yards.
The values represented by these materials, and their
importance both as a natural resource of California
and in supplying the country with potash in the present
acute emergency, made the study of this problem seem
a proper one to undertake at this time.
' This work has been supported by the Council of Defense of the State
of California.
SCIENTIFIC BASIS OF METHODS FOR RECOVERY OF THE
CONSTITUENTS OF BITTERN
We are very fortunate to possess a vast fund of
information upon the solubility relationships of the
various salts obtainable from sea water through the
classic work of van't Hoff and his co-workers. This
work is described in great detail in "Uber die Bildungs-
verhaltnisse der ozeanischen Salzablagerungen" (Leip-
zig Verlagsgesellschaft, 1912). During the progress
of the work two smaller volumes were published in
1905 and 1909 by van't Hoff, entitled "Zur Bildung
der ozeanischen Salzablagerungen" (Braunschweig,
Vieweg).
Inasmuch as very little of this work has been trans-
lated into English, and in view of the difficulty of
interpreting it in its formidable complexity, it seems
desirable to give a general outline of its nature.
The solubility of a single salt in its relation to
changes in temperature may be represented by simple
diagrams of the type familiar to all trained chemists.
100
Temperature, degrees Centigrade
Fig. I
In Fig. I are represented the solubility curves for the
main salts with which we have to deal, vis., sodium
chloride, potassium chloride, potassium sulfate, mag-
nesium sulfate and magnesium chloride. In this figure
solubility is expressed as the number of mols of an-
hydrous salt per 1000 mols of water. Of course,
other units may be used, such as mols or grams of salt
in a certain number of grams of water or of solution,
or in a certain number of cubic centimeters in solution.
If we know the solubility expressed in any of these
terms it is possible to calculate it in any other terms,
the density of the solution being required where the
conversion is between a weight and volume basis.
The laws of dilute solutions may frequently be ex-
tended to give an approximate idea of the behavior of
concentrated solutions. The solubility of a given
Feb., 191S
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
97
salt is varied by the introduction into the solution of
another salt. The effect of the second salt can be
predicted qualitatively by remembering that where the
salts possess a common ion the solubility of each is
usually decreased by the presence of the other. If,
however, there is a strong tendency to form a complex
salt the solubility of one may be increased by the
presence of the other. Again, where there is no com-
mon ion the solubility of one is increased by the pres-
ence of the other owing to the interaction of the two
salts.
There are various ways of representing graphically
the solubility relationships of salt pairs. The method
adopted by van't Hoff is to represent the amount of
each salt in the solution in terms of mols of anhydrous
salt per 1000 mols of water, measured along two axes
at right angles to each other, as illustrated in Fig. II.
Each curve here represents the composition of a solu-
tion saturated with one component. The intersec-
tions of the curves represent the composition of a solu-
tion saturated with both components. A point be-
tween these curves and the origin denotes the composi-
tion of an unsaturated solution. A point outside of
the curves would represent a mixture of a saturated
at so-c.
Mols /VaC/ per /ooo
Fig. II
solution with one or both solid salts, depending upon
its position. On evaporation of an unsaturated solu-
tion the relative amounts of the two salts would re-
main the same until the solution becomes saturated,
so that, for example, a solution having the composition
represented by the point a in Fig. II would, on evapora-
tion, change in composition as represented by the mo-
tion along the line ab. As soon as the curve AB is
reached, representing in this case the composition of
a solution saturated with potassium chloride, solid
potassium chloride will separate and the solution must
become relatively richer in sodium chloride, so that as
the evaporation proceeds from b the solution will
change in composition along the solubility curve to-
wards B. Similarly, an unsaturated solution having
the composition represented by c would, on evapora-
tion, change in composition as represented by move-
ment along the line td. At d sodium chloride would
begin to crystallize, whereupon the solution would
become richer in potassium chloride, its composition
changing along the line dB. It is evident that the
final result in the evaporation of any solution of these
two salts would be a saturated solution having the
composition represented by B, changing into a mixture
of the two solid salts.
The effect of temperature may be indicated on a
third axis at right angles to the others, giving a solid
figure, as represented in perspective in Fig. III.
Where a double salt may be formed, the solubility
relationships at a given temperature would be repre-
sented by a diagram such as that in Fig. IV. This
diagram represents the solubility at 30 ° of mixtures of
sodium sulfate decahydrate, and magnesium sulfate
heptahydrate, which form the double salt, astra-
kanite, Na2Mg(S04)2.4H20. The middle portion of
the curve seen in this figure represents the composition
of solutions saturated with astrakanite. Solid astra-
kanite, which contains equivalent quantities of the
two salts, has a composition lying upon a line bisecting
the angle between the two axes. The composition of
the solid salt is represented by a point on this line at
E, expressing the number of mols per 1000 mols of
water in the solid salt. The composition of solid
sodium sulfate, Na2SO.(.ioH20, which lies along the
line OA, is at a distance from the origin corresponding
to its water content at F. Similarly, solid magnesium
sulfate has the composition represented by the point
■'",
G. When an unsaturated solution containing these
salts is evaporated, its composition will, as in the
previous case, move along a line away from the origin
until one of the curves representing the composition
of the saturated solution is reached, when the solution
will change in composition along this line in the direc-
tion away from the line representing the composition
of the solid which is separating. Thus a solution having
the composition represented by a would, on evapora-
tion, change in composition along the line ab, when,
on further evaporation, sodium sulfate would separate,
and finally, at B, both sodium sulfate and the double
salt would separate, the solution remaining constant
in composition until it had all disappeared. Similarly
an unsaturated solution of composition represented by
c would change in composition in the direction cdB,
the solids separating being first pure astrakanite and
then a mixture of astrakanite and sodium sulfate.
The point B represents, therefore, the end-point of
crystallization for solutions which contain more sodium
sulfate than magnesium sulfate.
Fig. V represents the solubility of mixtures of
magnesium chloride and potassium chloride, from which
THE JOURNAL OF INDUSTRIAL AND ENGINEERING < EEMISTRY Vol. io, Xo. 2
100'
F
NotSOflOHaO
T
1
/
1 60
/
250
I
A
6m B
/
X
$40
/
4
1 »
a Cf /
1
c
;
D
MgSO*
e
20 40 60 80 100 120 140
Afo/s Mg S04 per woo mo/s H20
Fig. IV
it is possible to crystallize the double salt carnallite,
KMgCl3.6H20. Unlike the previous instance, how-
ever, the line OE, somewhere upon which lies the point
representing the composition of solid carnallite, does
not intersect the curve BC which expresses the compo-
sition of solutions saturated with carnallite. This
fact makes the path of crystallization, during the
evaporation of solutions of these two salts, somewhat
different from that considered above. A solution
having the composition represented by a will, on
evaporation, change in composition till 6 has been
reached, whereupon potassium chloride begins to
crystallize out, and the solution, becoming richer in
magnesium chloride, will move along bC. When the
solution has reached the composition represented by
C, carnallite will begin to separate, but since carnallite
contains more potassium chloride than does the sat-
urated solution at C, it is evident that while carnallite
crystallizes, the solution will tend to move along the
line CB instead of remaining at C. The phase rule,
however, requires that while both potassium chloride
and carnallite are present, the solution must remain
constant in composition at C. Therefore, instead of
the liquid phase disappearing at this point, as was the
case in the former salt pair, it is one of the solid phases,
potassium chloride, which will now disappear, being
changed over into carnallite. It is not until all of the
mi chloride lias been so changed that the solu-
tion can move from (.' to B. B will thus repn
end-point of crystallization, while C will not. It is
that in order to prepare crystals of
carnallite it is necessary to use a solution containing
; ian the equivalent amount of magnesium chlo-
ride, the relative amounts of the two salts being such
that, mi evaporation, the line BC will be intersected
slightly above C. Similar considerations show us that
on treating solid carnallite with water, instead of dis-
solving as such, it would tend to change into solid
potassium chloride and a solution whose composition
is that represented by C. It is obvious, therefore, that
20 40 60
Afo/s KCt per woo mo/s
Fig. V
80
r/,0
it is not difficult to obtain potassium chloride from
carnallite, a point of importance in the treatment of
salt bitterns, as will be discussed later. After the
removal of the potassium chloride the solution can be
evaporated, carnallite separating, while the composi-
tion of the solution changes from C to B. This car-
nallite can be treated with water, leaving solid potas-
sium chloride, etc.
Solutions containing magnesium and potassium
chlorides and sulfates are in equilibrium with solid
phases at 2 5 ° according to the data in Table 1 , and are
Table 1
System, KCl-MgClr-KjSO.-MgS04. at 25°
Composition op Solution
Mots of constituents
per 1000 mols HiO
KiClj MgCU MgSO. KjSO(
10S
72.5
105
104
Solid Phases
A KC1
B MgCU.6H,0
C M>;SO,.7H,0
D KiSOj
E KC1 and KMgCli.6HtO 5.5
K MgC'l:'.ll i) and KMgCU.6HiO 1
G MgCU.6HjO and MgS0..6H:0
H MgSOi. 7II.-0 and MgS0..6H,0
I(o) MgSO<7H,0 and K-M^i SO,),.6HiO 58.5 S.5
K KjSO, and KiMg(SO,)i.6H!0 22 16
L K,SO, ond KC1 42 1.5
M KCI; KiS04 and K!Mg(SO.)i.6H:0 25 21 11
N KCl.MgSO. 7II:Oand K:Mg(SO,)..6HiO 9 55 16
P KC1; MgSO«.7HiOand MgSd, 6H.O ... 8 62 15
Q KC1 nd KMgCU.6HjO... 4.5 70 15.5
R MgCI II" EMgCh.6HiO and
-D.6HJO 2 99 12
(a) The composition of the solution at this point is given by different
figures in van't Hod's earlier and later hooks. The latter are doubUess
incorrect, as the former agree with those of H. S ran Klooster, /. Phys.
Chem.. »1 (.1917), 513.
represented by van't Hoff along four axes, as in Fig.
VI, each pair of axes representing solutions containing
a common ion. The boundary lines correspond to
solutions saturated with the two constituents repre-
sented by the end re salt pairs con-
taining no common ion are present it is impossible to
represent the composition by a point in the plane of
this figure. A mixture of equiv. u unities of
potassium sulfate and magnesium chloride would evi-
dently lie at the origin 0 and would be indistinguish-
able from pure water by its position in the plane. In
order to make this distinction il is necessary to intro-
Feb., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
99
duce a vertical axis representing the sum of the con-
stituents of the solution. Again, since equivalent
quantities of potassium sulfate and magnesium chlo-
ride in solution may be represented equally well as
equivalent amounts of magnesium stilfate and potas-
sium chloride, by plotting along the potassium chloride
axis not mols of potassium chloride, but double mols,
namely, K2C12, it is possible to construct a solid model
expressing the composition of solutions containing any
amounts of these ions. Such a model, a perspective
drawing of which is seen in Fig. VII, may be constructed
by inserting needles at the intersections of the lines in
the plane figure, the heights of the needles being equal
to the total number of mols of dissolved salt in the solu-
tion at this point, always remembering to consider the
mol of potassium chloride to be K2C12. The tops of
these needles may be connected by threads which mark
off surface within which a saturated solution is in
equilibrium with a single salt. Along the threads
tion would move along the line in space away from the
origin 0 until one of the fields is reached representing
the separation of a solid salt. Further evaporation
would then result in a change in composition of the
solution equivalent to the removal of a saturated solu-
tion of the solid which is separated, since both this
solid and water are being removed simultaneously.
The composition of the solution would thus move
along one of the faces of the model until one of the
boundary lines has been reached, when a second salt
would begin to separate along with the first. The
solution would then change in composition as repre-
sented by motion along this line. By drawing lines
on these surfaces it is possible to represent in the
projection of the solid model such crystallization
paths, so that the projection may be used in many
cases instead of the solid model.
It is possible to calculate in this way the amounts of
the various solid salts and the amount of water which
have separated from any solution when a certain point
on a crystallization path has been reached. Thus,
separating two fields the solution is saturated with two
salts, while at the intersections three salts are present.
The composition of unsaturated solutions is repre-
sented by points within the model. For example,
a solution containing 2 mols of K2C12, 8 mols of MgS04
and 10 mols of MgCl2 will be represented by a point
found by counting 2 divisions along the potassium
chloride axis, 8 divisions to the left in the direction of
magnesium sulfate, which would then be 6 divisions
to the left of the magnesium chloride axis, 10 divisions
along the magnesium chloride axis, and then upwards
20 divisions, representing the total number of mols.
This solution could also be represented as containing
6 mols of magnesium sulfate, 12 mols of magnesium
chloride, and 2 mols of potassium sulfate, which would
give the same locus to the point. On the removal of
water from this solution all of the solid constituents
will increase in the same proportion, so that the solu-
in the case of the solution considered above, the di-
agonal which joins the origin with the point repre-
senting the composition of this solution will be found
to intersect the schonite face, showing that this would
be the first salt to separate on evaporation. As
evaporation proceeds the crystallization path would
meet the boundary line of this face with the mag-
nesium sulfate face, after which these two salts would
separate together. Suppose, for example, we wish to
calculate the actual amounts of these two salts sep-
arating and the amount of water that must be removed
when the point N has just been reached, at which
potassium chloride just begins to separate. The solu-
tion at N has the following composition: ioooH20 +
qK2C12 + i6MgS04 + ssMgCl2. The amount of this
solution we may represent as an unknown quantity
by p, the amount of schonite separating we may repre-
sent by g, the magnesium sulfate by r, and the amount
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. Xo *
of water removed by j. We may then represent what
has become of the original solution during evaporation
by means of the following equation:
ioooHjO + 8MgSO, + ioMgCl, + 2K2C12 = />(ioooH20 +
i6MgS04 + 55MgCl, + qK2C12) + 8(K,Mg(S04),.6H,0) +
r(MgSO,.7H20) + sH20
By equating coefficients of the various substances
present, it is possible to set up the following equations:
Coefficients of H20: iooo = iooo/> + 6g + -jr + s
Coefficients of Mg: 18 = yip + q 4- r
Coefficients of K2: 2 = gp + q
Coefficients of Cl2: 12 = 64/)
The solution of these equations gives the following
values:
p = 0.188; q = 0.31; r = 4.38; s = 779
These values of q, r and s represent the amounts
of the respective substances which have separated
by evaporating the original solution and p represents
the amount of solution left. If, instead of taking the
Table 2
System, NaCl-KCl-MgClr-MgSO.-Na,S04. at 25°
Mols per 1000 Mols HjO
Saturation with NaCl and NaiClj KiClj MgCh' MgSC>4 NaiSO.
0 5S.5
A MgCIi.6HsO 2.5 ... 103
B KC1 44.5 19.5
C NaiSCfc 51
D MgCli.6HiO. Carnallite 1 0.5 103.5
E KC1, Carnallite 2 5.5 70.5
F KC1, Glaserite 44 20
G NatSO(, Glaserite 44 10.5
H NajSO«, Astrakanite 46 16.5
1 MgSOi.7HiO, Astrakanite 26 ... 7 34
J MgS04.7HiO, MgS0..6H-0 4 ... 67.5 12
K MgSOi.6H:0, Kieserite 2.5 ... 79 9.5
L Kieserite, MgCli 6HsO 1 ... 102 5
M KC1, Glaserite, Schonite 23 14 21.5 14
N KC1, Schonite, Leonite 19.5 14.5 25.5 14.5
P KC1, Leonite, Kainite 9.5 9.5 47 14.5
Q KC1, Kainite. Carnallite 2.5 6 68 5
R Carnallite. Kainite, Kieserite 0.5 1 85.5 8
S NaiSO«, Glaserite, Astrakanite 26 8 16
T Glaserite, Astrakanite, Schonite. . . 27.5 10.5 16.5 18.5
U Leonite, Astrakanite, Schonite 22 10.5 23 19
V Leonite, Astrakanite, MgS0..7HjO 10.5 7.5 42 19
W Leonite. Kainite, MgS0..7H:0 9 7.5 45 19.5
X. MgS0.6H,0, Kainite, MgS04.7HiO 3.5 4 65.5 13
Y MgSO«.6H,0, Kainite, Kieserite. . . 1.5 2 77 10
Z Carnallite. MgClt.6HiO, Kieserite. 0 0.5 100 5
No. Field
1 ALZD
2 BFMNI'QK
3 CGSH
4 DZRQE
5 FMTSG
6 SHIVUT
7 VIJXW
8 JXVK
9 KVRZL
10 Tl'NM
11 NUVWP
12 PWXYRQ
FORMULA
MgCl!.6HiO
KC1
NatSOi
KMgClj.6HiO
( 1 33K 0.67Na)SO«
Na.Mg,SO.)t.4H»0
MgSO(.6HiO
MgSOt.HjO
KsMg(SO()i.6HiO
Mg(1.52K 0.48Na)(SO.)!.4H,O
MgSO..KC1.3HiO
Mineral ogical
Designation
Bischonte
Sylvite
Thenardite
Carnallite
Glaserite
Astrakanite
Epsom salts
Not found
Kieserite
Sch6nite
Leonite ,
Kainite
amount of the original solution represented by iooo
mols of water, a different amount is taken, propor-
tionate amounts of the solids and water are obtained
from the solution on evaporation to the same point.
When we come to consider the evaporation of sea water,
we have in addition to the above components large
amounts of sodium salts. Since during evaporation
sodium chloride is always present, it is possible to
represent saturated solutions such as are obtained on
evaporating sea water by solid models similar to the
one considered above. By introducing sodium chlo-
ride as another component no new degrees of freedom
are introduced, provided it is stipulated that solid
sodium chloride shall always be present. Van't Hoff
and his co-workers have determined the solubility
relationships at 250 and S30. Fig. VIII represents the
results for 25 ° contained in Table 2; results for 83*
are found in Table 3 and Fig. IX. The amount of
sodium chloride present is not considered in the pro-
jection, but is counted in the total number of dissolved
mols which would be represented in a solid model.
Sodium sulfate may be expressed in terms of the other
salts present, since Xa2S04 = Xa2Clj + MgS04 —
MgCl2, or, = Na.Cl, + K2S04 — K2C12. Thus point
C, Table 2, is represented in Fig. VIII by counting
12V1 divisions to the left of the origin and 12V1 di-
visions along the K2S04 axis. Its position in a space
model would be 6}l/t divisions vertically above the
point so obtained. Such a model may be constructed
in a way similar to that previously described.
The composition of sea water which has been evap-
orated until it is saturated with sodium chloride is as
follows, expressed in mols of each constituent:
Table 3
System, NaCl-KCl-MgClr-MgSCV-NaiSOV at 83°
Mols per 1000 Mols HtO
Saturation with NaCl and NaiCli KiCli MgClj MgSO( NatSO.
0 59
A MgCli.6HsO 1 .121
B KC1 39 37
C NajSO( 56.5 8
D MgCli.6H,0, Carnallite 1 2 117
E KC1. Carnallite 1.5 10 92
F KC1. Glaserite 39.5 39 4.5
G Na,SO<, Glaserite 43.5 21 11.5
H NatSO., Vanthoffite 51 4.5 10.5
1 Vanthoffite, Loeweite 35 .. 22 12.5
K Loeweite. Kieserite 12.5 61.5 5.5
L Kieserite. MgClj.6H:0 1 .120 1
P KC1, Glaserite, Langbeinite 29.5 33.5 13 10
Q KC1, Carnallite. Kieserite 2 12 86.5 5
R KC1, Langbeinite. Kieserite 11 15 76 5
S Glaserite, NasSO,. Vanthoffite... 43 22.5 ... 7.5 5.5
V Loeweite, Glaserite, Vanthoffite. . 34.5 26.5 8.5 17.5
W Loeweite, Glaserite, Langbeinite.. 30 24.5 12 16.5
Y Loeweite, Kieserite. Langbeinite. . 16 10 5 42 14
Z Carnallite, MgCl:.6H,0. Kieserite 1 2 116 1
MlNERALOGICAL
No. Fibld Formct-a Designation
1 ALZD MgCli.6HiO Bishcofite
2 BFPRQE KU1 Svlvite
3 CGSH NaiSO< Thenardite
4 DZQE KMgCU.6HiO Carnallite
5 FPWVSG (K, Na)»S04 Glaserite
6 HSVI MgNai(SO<)< Vanthoffite
7 IVWYK Mg:Na1(SO«)4.5H:0 Loeweite
8 KYRQZL MgSO.H.O Kieserite
9 WPRY Mg2Ki(SO.)i Langbeinite
ioooHjO, 47Xa2Cl:, i.o3K:Cl2, ;.36MgCl2, 3o7MgS04
By the use of a solid model it is possible to determine
that this solution, on further evaporation, would inter-
sect the surface at the point a, where Epsom salts
would begin to separate. The composition of the
solution at this point is approximately ioooH-0,
iiNa»Cl», 6K2C1;. 2oMgS04. 4iMgCl2. Further evap-
oration would lead to the boundary between this
field and the kainite field II'A, after which these two
salts would separate together. It is possible to calcu-
late as before the amounts of each substance removed
from the solution when the latter has the composition
indicated, say, by X. Suppose that 10,000 g. of the
original solution are used. The number of grams corre-
sponding to the number of mols of each substance in
the original solution is 24,790. so that 10,000 g. of solu-
tion would contain, instead of the previous number of
mols of each constituent, only 0.404 of these quanti-
ties, namely, 404HJO, igNajCl., o.42K2Cls, 3MgCl»
and i.44MgS04. On evaporation this solution would
yield p mols of the solution saturated at X, containing
its constituents in the proportions indicated in Table 2,
together with t7MgS04.7H:0 + rXa.Cl, + sKCl.-
Feb., 1918
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
MgS04.3H20 + «H20. We can, therefore, write the
following equation:
404H20 + i9Na2Cl2 + o.42K2Cl2 + 3MgCl2 + i.44MgS04 =
p(ioooH20 + 3-5Na2Cl2 + 4K2C12 + 6s.5MgCl2 + i3MgS0,)
+ gMgS04.7H20 + rNa2Cl2 + sKCl.MgSO4.3H2O + <H20
By equating corresponding coefficients and solving
the resulting equations, we obtain the following values:
p = 0.0458; q = 0.37; r = 18.9; 5 = 0.47; I = 354
BISCHOFITE
KZESERITE
CABNALLITE
B KzC/z
G
Fig. VIII
Hence we conclude that 354 mols of water have been
evaporated, and 0.37 mol of Epsom salts, 18.9 mols
of Na2Cl2 and 0.47 mol of kainite are in the solid
portion. Similar calculations may be made to de-
termine what will happen during all sorts of changes.
For example, instead of removing water, a certain salt
may be added to a solution saturated with other salts,
and by the aid of geometric and algebraic considera-
tions it will be possible to determine what will take
place.
It is evident from the position of point a in the
diagram for 25° that only a small amount of Epsom
salts will have been crystallized by evaporation of the
mother liquor from sea water before kainite will begin
to separate. It is true that kainite shows a great
tendency to supersaturation, and unless suitable nuclei
MgC/z
A^ BISCHOFITE
.CARWALLITE
flbeS04
KzSO^
are present this field might not be present, which will
allow the evaporation and separation of Epsom salts
to continue somewhat further until the potassium
chloride field is reached. The conditions obtaining
in solar evaporation are, however, very favorable to
the crystallization of such a substance because of the
presence of many impurities. In order to get a good
separation of the potassium salts from the magnesium
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 2
salts in the bittern of sea water it is not desirable to
carry on the evaporation so as to separate more than
a small amount of Epsom salts at 25 °. On comparing
Figs. VIII and IX it will be seen that at the higher
temperatures it is possible to continue the evaporation
much farther before any salt containing potassium will
crystallize from the hot solution. At this tempera-
ture and in the presence of the magnesium chloride
which exerts a dehydrating effect, instead of Epsom
salts crystallizing, kieserite, MgSO<.H20, is obtained.
The fact that the solubility of magnesium sulfate tends
to decrease at higher temperatures, while the solu-
bilities of potassium chloride and magnesium chloride,
and hence, carnallite, increase, causes the kieserite
field at 83 ° to become large at the expense of the
fields of potassium chloride and carnallite. It is evi-
dent, therefore, that most of the sulfate present in the
solution could be removed as kieserite by evaporating
the bittern at higher temperatures until the carnallite
boundary is approached. During this evaporation,
the solids which separate would be sodium chloride and
kieserite. By removing these from the hot solution
they could be obtained relatively uncontaminated
with potassium. If, now, the mother liquor from these
crystals is cooled, the growth of the carnallite field
as lower temperatures are reached indicates that 'this
salt would separate as the solution cools, while the
mother liquor from the carnallite would consist largely
of a solution of magnesium chloride. These considera-
tions seem to indicate the possibility of a satisfactory
process for the separation of the bittern into three main
constituents: magnesium sulfate, carnallite, and a
solution of magnesium chloride. There would remain
the necessity, first, of separating magnesium sulfate
from the sodium chloride accompanying it, second,
of treating the carnallite for the recovery of potassium
chloride, according to the principles discussed earlier,
and, third, the evaporation and cooling of the magne-
sium chloride liquor to obtain MgCl2.6H20.
EVAPORATION EXPERIMENTS
The process outlined above, on the basis of the equi-
librium diagrams, was first tested on a laboratory
scale by evaporating weighed quantities of bittern.
In one set of experiments the evaporation was carried
on at the boiling point of the solution. Crops of crys-
tals were removed from the solution from time to time
by centrifuging the liquid through a muslin bag. The
density of the solution was read by the aid of a hydrom-
eter made of pyrex glass, the small coefficient of ex-
pansion of which made its readings nearly cor
Spite of changes of temperature. The boiling point
was read with a thermometer graduated to one-tenth
of a degree. The amount of water, when each reading
ad boiling point was made, was determined
by weighing the vessel containing the hot solution.
It will be seen from the results, plotted in Fig. X.
that the density and boiling point rise gradually until
water has bei Qj to about
cent of the weight of the original bittern. The density
and boiling point from lure on increase more rapidly
with the further removal of water. This more rapid
increase is caused by encountering the boundary of
the carnallite field shown in Fig. IX, and the subse-
quent separation of carnallite. The crystals which are
deposited from the solution after this point is reached
contain a considerable amount of potassium in the
form of carnallite. A calculation of the amount of
water which should be removed in order to reach the
carnallite boundary at 83 ° gave a figure corresponding
very closely with that indicated by the above curve.
The original mother liquor at 25 ° is saturated both
with sodium chloride and magnesium sulfate, but since
the solubility of sodium chloride does not materially
change with the temperature, whereas that of magne-
sium sulfate does increase during the first part of the
evaporation, the solution is saturated with sodium
chloride but not with magnesium sulfate, hence the
first crystals to separate consist largely of sodium
chloride, which was found to be the case with the aid
both of the microscope and of a chemical analysis.
It is possible, therefore, to remove an additional amount
of sodium chloride from the magnesium sulfate by
filtering the hot solution by the aid of the centrifuge
during the early stages of the evaporation. This
procedure simplifies the further purification of the
Fig. X — Water Evaporated in Per Cbnt of Bittern Taken
magnesium sulfate which separates as evaporation
proceeds. Table 4 gives the results of the analysis of
the crystals removed from the solution by the aid of the
centrifuge at the stages of evaporation indicated in
Fig. X.
Table 4
Crop from
cooled
mother Crop
liquor from final
Crop 1 Crop 2 Crop 3 Crop 4 from 4 evaporation
MgSO. 15.1 ■*' 24.6 20 1 24.1 1.3 3.5
MgCls 12.0 It 12.3 • 9 39.2 38.2
KC1 4.8 6.3 44 17.1 3.6 1.1
..20.3 20.3 13.3 17 0 1.3
HiO 52.8 36.4 40 5 24 9 54.7 57.5
The centrifuge employed was not very efficient,
and some cooling took place during the process, so
that the respectiv. ted with the
salts that should remain in the mother liquor. It
is evident from the results of this analysis, together
with the course of the density and boiling-point curves,
that the process contemplated furnishes the desired
>n. In a second experii :sed upon the
results of the first . the solution was evaporated until
the density had reached a v.. ,. at the boiling
point of the solution, 121 °. The crystals separating
up to this point were removed and the mother liquor
Feb., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
103
allowed to cool. The crystals separating on cooling
should be carnallite, and it will be seen from the anal-
ysis of these crystals in Table 5 that their composition
approximates closely to that of carnallite. The mother
liquor from the carnallite consists principally of a
solution of magnesium chloride, as is confirmed by its
analysis. The potassium content of the first two frac-
tions may be attributed to the cooling in the centrifuge
inevitable in working on such a small scale. As is to
be expected, the proportion of MgS04.H20 to NaCl
is greater in the second crop of crystals than in the first.
Table 5 — Composition op Material Obtained at Various Stages in
Per cent
Removed at Removed Theoretical Final
b. p. 121°, from for mother
B. p. 116° d. 1.35 cooled liquor carnallite liquor
K 3.1 5.7 10.0 14.1 0.4
CI 23.5 19.1 36.6 38.4 23.4
SOi 16.9 32.2 trace 0.0 2.7
Mg 3.9 9.2 7.6 8.7 7.9
The curve given in Fig. XI was obtained by an
evaporation in which no crystals were removed, thus
avoiding the inevitable losses occurring through at-
tempts to remove crystals from the hot solution.
The break in the boiling-point curve in Fig. XI is at
a higher temperature than that in Fig. X. This is
doubtless due to the use of different samples of bittern
in the two experiments, so that the carnallite field is
encountered at different points in the two cases. It
may be noticed that the break is more pronounced in
the case where it occurs at the lower temperature which
is just what would be expected on the basis of the solu-
bility diagram in Fig. IX. The composition of the two
samples of bittern used in the above experiments is
given in Table 6. The sodium content is not given.
Table 6
Bittern used in getting curves
in Fig. X in Fig. XI
K 1.48 1.76
CI 15.82 18.22
SO« 5.81 3.88
Mg 5.38 6.32
OUTLINE OF PROPOSED PROCESS
i. evaporation of the bittern — The bitterns
from various sources will vary somewhat depending
on the temperature of the liquid in the last salt pond,
and whether or not any Epsom salts are allowed to
separate. There is, in fact, no reason apparent why
a crop of Epsom salts should not be removed by cooling,
either artificially or by storage till winter, before the
subsequent process of separation is applied. The
process of solar evaporation should not, however, be
carried far enough to cause any potassium salts to
crystallize, as it is probably not desirable to separate
the potassium content into two portions. The varia-
tions in the composition of the bittern caused by any
of the above factors would not cause any serious diffi-
culty, as during the later evaporation the separation
of NaCl and MgS04.H20, kieserite, would take place
in such proportion as to make the resulting liquid
converge towards a fairly uniform composition.
It is more important, under present conditions, to
recover all of the potassium salts, and hence to pre-
vent their contaminating the NaCl and kieserite frac-
tion, than it is to recover all of the Epsom salts, or to
obtain pure magnesium chloride from the final liquor.
Such contamination would result, if the evaporation
were continued as far as the carnallite boundary,
for some cooling during the separation of the kieserite
from the mother liquor is inevitable, and if the solu-
tion is saturated with carnallite before this separation
begins, some of it will crystallize along with the kieser-
ite. On the other hand, if the evaporation is not con-
tinued so far, a little of the sulfate will remain in the
solution, and will probably pass through the succeeding
operations and come down with the magnesium chlo-
ride at the final stage of the process. Since very pure
magnesium chloride will probably not be desired, the
presence of this sulfate can do no harm.
Instead, therefore, of continuing the evaporation
as far as the break in the boiling-point curves, as in
Figs. X and XI, it will doubtless be better to evaporate
till the boiling point is about 120° C. This will re-
sult in the recovery of practically all of the carnallite
and still allow leeway for variations in the bitterns
used.
Fio. XI — Water Evaporated in Per cent op Bittern Taken
The best type of evaporator for this operation will
doubtless be of the film type, where a given part of
the liquid is not boiling for a very long time. There
is a tendency for magnesium chloride to hydrolyze,
giving magnesium hydroxide and hydrochloric acid,
which escapes with the steam. If the liquid is evap-
orated in a kettle it is boiling for such a length of time
that a considerable amount of magnesium hydroxide
is formed. If, on the other hand, the liquid is allowed
to flow over a heated surface, the evaporation taking
place very quickly, there is little time for this hydrolysis
to take place. This liquid may then be kept in a
settling tank without further loss of hydrochloric
acid, even near the boiling temperature, provided
actual boiling does not take place.
In principle, then, the process indicated is as follows:
Evaporate until the boiling point of the liquid is
raised to about 120° C. and the density is approxi-
mately 1.35. The liquid running off from the evap-
orator should be caught in a steam-jacketed tank
104
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. a
where it is allowed to settle. The clear liquor is al-
lowed to run off to a cooling tank, in which the car-
nallite will separate. The sludge of XaCl and kieserite
is run into centrifuges, previously heated, where it is
separated from the adhering mother liquor, which is
run into the cooling tank mentioned above. The
separation of the NaCl from the material remaining
in the centrifuges and the recovery of Epsom salts will
be discussed later.
2. THE RECOVERY OF THE CARNALLITE The liquor
containing the carnallite may be cooled by the fresh
bittern going to the evaporator, in order to utilize the
heat content of the latter. After it has been thor-
oughly cooled, the carnallite which has separated is
removed and freed from its mother liquor by centri-
fuging. The recovery of the potassium chloride from
this carnallite will be discussed later.
3. THE RECOVERY OF BROMINE AND MAGNESIUM
chloride — The mother liquor from the carnallite con-
tains a very little potassium, a little sulfate, a consider-
able amount of colloidal organic matter, the bromine
content of the sea water, and a large amount of mag-
nesium chloride. The liquid must be evaporated fur-
ther in order to recover MgCl2.6H20. During this
evaporation, however, the temperature rises con-
siderably, unless vacuum evaporation is employed,
charring the organic matter, and strongly darkening
the magnesium chloride which separates on cooling.
To destroy this organic matter, therefore, as well as
to recover the bromine, preliminary treatment with
chlorine is desirable. The details of this treatment
are now the subject of investigation in this labora-
tory. We can only say at the present time that there
seems to be good prospect of success.
The disposal of the large quantities of magnesium
chloride that would be obtained from these bitterns
presents an economic problem. The possible outlets
seem to be as follows: magnesium oxychloride cement,
magnesium oxide and hydrochloric acid, and metallic
magnesium. The use of magnesium oxychloride ce-
ments might be greatly increased by skilful advertising,
hydrochloric acid might be substituted for sulfuric
acid, for certain purposes, and there seems to be good
reason to anticipate a large production of magnesium
in the future.
4. the separation of sodium chloride and
magnesium sulfate — The separation of the sodium
chloride and the kieserite obtained in the first part of
the process is complicated by the possibility of forming
astrakanite, Xa2Mg(S04)2.4H20, at ordinary tem-
peratures and of loeweite, XaiMg^SCM-i-sHiO, or
vanthoffite, Na6Mg(S04)4, at higher temperatures.
In order to put the separation of the magnesium from
the sodium salts on an exact basis' it is desirable to
have a knowledge of the solubility relationships of the
chlorides and sulfates of these two metals. It has
been found possible, by using data given by van't
Hoff, Seidell1 and Roozeboom,1 to construct the equi-
librium diagram for all but two points which are un-
* Am. Chem. J..Vt (1902), 52; see also Schreinemakers and Baat, Z.
physik. Chem., 67 (1909). 533.
• Z. physik. Chem.. 2 (1888), 518.
important for the present purpose. The data used
are given in Table 7, and are represented graphically
in Fig. XII, giving a diagram similar to that in Fig.
VI, where potassium chloride is considered instead of
sodium chloride. The two undetermined points have
been added more or less at random, for the sake of
completing the fields, and are denoted by interrogation
marks on the figure.
Now the material obtained from the first stage of
our process contains MgSO« and XaCl in nearly equiva-
lent amounts, and hence, if dissolved in water, would
be represented by a point lying nearly vertically above
the origin, at a distance increasing as the solution is
evaporated. It might, therefore, cut the surface of
the solid model in the astrakanite face, which would
prevent the separation of the sodium from the mag-
nesium. A little magnesium chloride, however, would,
if added, raise the solution away from the astrakanite
field, so that we would have only XaCl and MgS04.-
7H2O to deal with.
The solubilities of these two salts are affected so
differently by the temperature that we may anticipate
their separation by first cooling, removing Epsom salts,
then evaporating partly at higher temperatures, re-
moving sodium chloride, then cooling again, etc. The
portion of the equilibrium diagram that can be con-
structed for 83 ° from van't Hoff's data shows that at
that temperature loeweite and vanthoffite intrude
themselves between the magnesium sulfate and sodium
chloride fields, even when a considerable amount of
magnesium chloride is added, so that it may not be
advisable to evaporate the solution for the removal
of sodium chloride at too high a temperature. The
great tendency of these double salts towards super-
saturation might allow the evaporation to proceed
without their formation.
Feb., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
105
Not determined
9.5
Table 7
System, NaCI-MgClr-MgSO.-Na2SO«, at 25°
Solid phases NajCh MgCh MgSO, Na2SOi
UaiCh 55. 5
NajSO<.10H2O
MgSOi.7H20
MgCl2.6H20
MgCl2.6H20; Na2Cl2 2.5
Na2Cl2; Na2SO. 51
Na2SO«; Na2SO<.10H2O(*) 30
.Na2SO<.I0H2O; Na2Mg(S0.)2.4H2O
MgSO«.7H20; NajMg(Sr>0».4H:O
MgSO(.7HjO; MgS0(.6H2O
MgS0<.6H2O; MgSO<H20
MgSO(.6H20; MgCI2.6H20
NaiCh; Na2SO«; Na2Mg(SO.)2.4H20 46
Na2SO<; Na2SO,.10H2O; Na2Mg(SO«)2.4H20. .
Na2Cl2; MgS0..7H20; Na2Mg(S04)2.4H20 26
Na2Cij; MgS0..7H20; MgSO,.6H20 4
NajCls; MgSO,.6H20; MgSO..H20 2.5
Na2Cl2; MgSO,.H20; MgCl2.6H20 1 102 5
(*) From the experimental work of Professor W. C. Blasdale, which is
still in progress in this laboratory, this point may be considerably in error.
In order to have the desired data it is very important
that the equilibria here involved should be determined
for temperatures both lower and higher than 25°.
Work on the solubilities at o° is now in progress in
this laboratory and will be published as soon as possi-
ble. It is planned, also, to include potassium salts
in this work, so that a diagram for o° similar to that
in Fig. VIII can be constructed, and which might sug-
gest a modification of the first treatment of the bittern.
S. THE RECOVERY OF POTASSIUM CHLORIDE FROM
carnallite — The recovery of potassium chloride
from the carnallite was discussed earlier in connec-
tion with Fig. V. We may ask whether hot or cold
water should be used for this purpose. A reference to
the tables shows that the proportion of potassium
chloride to magnesium chloride in the solution at equi-
librium with potassium chloride and carnallite is much
less at 25° than at 83°. This makes it obvious that
a much smaller proportion of potassium chloride goes
into solution at the lower temperature. The composi-
tion of the solution in equilibrium with potassium
chloride and carnallite at 25° is as follows: 1000H2O +
5.5K2CI2 + 7 2.5MgCl2. From this it is possible to
calculate the amount of water to be used in extracting
the magnesium chloride from the carnallite at this
temperature. If 1 mol of carnallite is used we can
write the following equation:
KMgCU6H20 + xH20 = yK2Cl2 + z(ioooH,0 + 5SK2CI2 +
72.5MgCl2)
From this we find x = 7.8; y = 0.425; 2 = 0.0138.
That is, 1 mol, or 277.5 %■ of carnallite, requires 7.8
mols, or 140.4 g. of water, or, the weight of water re-
quired is approximately half the weight of the car-
nallite. At the lower temperatures that would natur-
ally be used somewhat more water would be required,
but relatively less KC1 would be dissolved.
The liquor used in extracting the carnallite may
then be partly evaporated and cooled, whereupon
another crop of carnallite crystals will be obtained.
To obtain the maximum amount of carnallite but no
magnesium chloride the solution should be evaporated
to such an extent that on cooling with separation of
carnallite its composition will correspond to point B
in Fig. V, which is ioooH20 + iosMgCl2 + K2C12.
The amount of evaporation necessary is calculated
from the following equation:
ioooHjO + 72.5MgCI, + 5.5K1CI, = xH20 + yKMgCl,.6H20 +
s(ioooH20 + io5MgCl, + K2C12)
This gives x = 340; y = 9.8; 2 = 0.6; hence 25720 g.
of solution should lose 6120 g. of water, giving 2720 g.
of carnallite on cooling; or, 1 ton of solution should
lose 0.238 ton of water, and deposit 0.107 ton of car-
nallite.
It will probably not pay, here or in stage 2 of the
process, to recover the small amount of potassium
chloride remaining in the mother liquor from the car-
nallite.
Condensed summary of the above process:
Evaporate bittern till boiling point becomes about 120°, and density (hot)
1.35. Separate solid and liquid while hot (settling tank and centrifuge).
A. Solid. NaCl and MgSOi.H20. Dissolve out NaCl with cold
water (containing some MgCli?) ; dissolve residue in hot water
and cool with ice machine, getting MgS04.7HjO.
B. Liquid. Cool.
I. Solid carnallite. Extract with minimum amount cold water,
leaving
1. Solid KC1.
2. Solution. Evaporate partly, cool.
a. Solid 'carnallite, add to I.
b. Solution of MgCl2, add to II.
II. Solution, mainly MgCl2. Bleach with CI2 and remove Br2.
Evaporate, cool, recover solid MgCl2.6H20.
The above process is being tested in this laboratory
on a semi-commercial scale under the direction of
Professor Merle Randall, and will be described in a
later publication. It may be mentioned, however,
that an excellent separation of actual bittern has been
obtained into one lot of material consisting of kieserite
and sodium chloride, another consisting of carnallite
of a high degree of purity and whiteness, and a mother
liquor consisting of magnesium chloride solution con-
taining but very small amounts of sulfate and of potas-
sium. . For example, using 1 50 lbs. of bittern, and evapo-
rating till the boiling point was 1180, the three fractions
of material obtained had the following composition:
NaCl, Kieserite Carnallite Fraction Mother
Fraction Found Theoretical Liquor
K 1.6 11.0 14.1 Trace
CI 21.1 37.4 38.4 23.4
SO« 22.2 0.4 0.0 1.25
Mg 10.0 8.1 8.7
The writer wishes, in conclusion, to express great
appreciation for the cordial cooperation of the Oliver
Salt Company, which has given information and has
furnished samples of material and bittern.
Generous credit should be given to Messrs. A. H.
Foster, W. D. Coughlan, Carl Iddings and W. D.
Ramage for much of the experimental work herein
described, and to Mr. Iddings for drawing the illus-
trations. Professor W. C. Bray has given considerable
time to the final criticism of the manuscript and the
checking of the figures necessitated by the absence of
the author from Berkeley due to his acceptance of a
commission in the army.
Since concluding the above work there has appeared in
Chemical Abstracts, Vol. 11 (1917), 2719, a brief outline
of a process by T. Nishimura, J. Chcm. Ind. Tokyo, Vol.
20 (1917), 587, for extracting potassium from bittern
which, apart from certain serious errors in translation,
seems to be fundamentally similar to that herein de-
scribed, and which we may welcome, therefore, as
additional evidence of the feasibility of working up
these bitterns instead of allowing them to be largely
wasted, as at present.
Iu;rki:lf:y, Cai..
io6
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 2
THE DIRECT HEAT TREATMENT OF CEMENT MILL
DUST TO INCREASE ITS WATER-SOLUBLE
POTASH CONTENT
By Albert R. Mbbz
Received November 9, 1917
When a potash-containing silicate mixed with lime
is ignited at temperatures above iooo°, the lime dis-
places more or less potash which is volatilized. This
fact suggests a possible procedure for the immediate
commercial production of potash from potash silicates.
Since, however, commercial grades of any insoluble
potash silicate in quantity contain comparatively small
percentages of potash no process for recovering potash
from such material can offer much promise of profitable
application unless there is also produced some other
product of value in addition to the potash. Fortu-
nately, and by strange coincidence, the two manu-
facturing industries of this country which have the
largest outputs are industries wherein raw materials
which contain potash silicates are heated with lime-
stone to temperatures so high that the potash is more
or less displaced and volatilized. These two indus-
tries, vis., the blast-furnace and Portland cement in-
dustries, are already firmly established and for them
the problem becomes merely one of the successful
recovery of the volatilized potash as a by-product.
It may be stated that the chief potential source of
potash in this country is the raw material which is or
may be used in these industries.
Some potash is contained in all cement materials.
In a recent publication by this Bureau1 it was shown
that in the raw mix as fed into the kiln the potash varies
from 0.20 to 1.16 per cent in the various cement mills
of the United States and Canada, and that the 'per-
centage of this potash driven from the kilns in the differ-
ent plants varies from 24.5 to 95.9. From the results of
the analysis of samples of raw mix and of cement from 102
plants it has been calculated that the potash escaping
from the kilns of these plants ranges from 0.35 to 5.14
lbs. per barrel of cement produced with an average
for the plants of this country of 1.93 lbs. On the basis
of an average production of 90,000,000 bbls., the total
potash escaping from the cement plants of this country,
as at present operated, amounts to about 87,000 tons
annually. The profitable recovery of this potash is
not dependent upon successful collection alone, but it
must be obtained in a form so concentrated as to be
merchantable and at a cost sufficiently low to permit
of a profit under normal market conditions. Three
factors determine such profitable recovery and must
be considered in any attempt advantageously to ob-
tain potash as a by-product in the cement industry:
liberation of the potash, recombination and collection.
A full discussion of the various conditions which
affect the liberation of potash from the raw mix in the
kiln and of the methods which have been devised to
increase the percentage of potash volatilized is to be
found in the publication already mentioned. Similarly
the methods of collection of the potash that escapes
from the kilns have received ample treatment in this
' W. H. Ross, A. R. Men and C. R. Wagner, U. S. Department of
Agriculture, Hull. 671.
bulletin. The work presented here deals with a method
for making water-soluble the "recombined" potash of
cement dust.
The recovery of the potash which escapes from the
kilns of cement mills was first made by the Riverside
Portland Cement Co., at Riverside, Cal., using the
Cottrell process of electrical precipitation. The ce-
ment dust recovered at this plant was found to contain
upward of 90 per cent of its potash in the water-soluble
form. A sample of precipitator dust secured from this
mill was analyzed by the author and found to give a total
potash content of 10.7 per cent, and a water-soluble
potash content of 9.8 per cent. The water-soluble
potash of this particular dust was 92 per cent of the
total potash present in the dust. It was natural to
expect that the dust which would be recovered by a
similar method at other plants would have a water-
soluble potash content approximating the same per-
centage of the total potash present. It was found,
however, when the Cottrell process was installed at
the mill of the Security Cement and Lime Company,
at Hagerstown, MrL, that the dust collected contained
a considerable portion of its potash content in a form
which was not readily soluble in water. A sample of
dust obtained from this plant was found to contain
1 1.4 per cent total potash, whereas the water-soluble
potash content was but 6.8 per cent. Instead of the
anticipated 90 per cent or over, this particular sample
of dust contained but 60 per cent of its potash in
water-soluble form. It has been found at another
plant, the Alpha Portland Cement Company at Cemen-
ton, N. Y., where installation of the Cottrell process
for the recovery of dust has been made, that the water-
soluble potash in the dust recovered constitutes a con-
siderably lower proportion of the total potash present
than at the Security plant. A sample of the dust re-
covered at this mill was found by the author to contain
7.0 per cent total potash and only 2.9 per cent water-
soluble potash This sample of dust, therefore, had
but 41 per cent of its potash present in the water-
soluble form.
The term "water-soluble potash" as used above
refers to that potash which is obtained in solution by
the procedure given in the "Methods of the Associa-
tion of Official Agricultural Chemists," in accordance
with which 10 g. of the sample are boiled with 300 cc.
of water for 30 min. and the volume subsequently
brought to 500 cc. As it is customary in the fertilizer
trade to make payment for none other than this potash
it becomes a matter of vital importance to the cement
manufacturer who recovers his dust for sale to the
fertilizer trade on the basis of its water-soluble potash
content to ascertain the cause of the failure to secure
the maximum amount of his potash in this form, to
devise methods, it possible, to obtain most of the potash
in his dust directly as water-soluble potash, to adopt
some procedure which will profitably increase the
water-soluble potash of his dust as at present obtained
or. finally, to endeavor to secure from the fertilizer trade
credit for that available potash of his dust which is
but slowly water-soluble and for which at present
he receives no compensation.
Feb., 191S
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
107
As stated in a previous publication,1 the potassium
compounds occurring in cement dust may be divided
into three groups: (1) those which are readily water-
soluble; (2) those which are slowly soluble; and (3)
those which are insoluble.
The insoluble potash represents the combinations
occurring in the original silicates of the raw mix carried
over mechanically in the dust before being subjected
to a temperature sufficiently high to bring about de-
composition. The form of combination which is
slowly soluble in water has been attributed to the
recombination of the volatilized potash with the finely
divided incandescent particles of siliceous coal ash
carried over in the dust2 and it is claimed3 to be pro-
portional to the amount of coal ash present in the gases
from the kiln. Where oil or gas is used for fuel this com-
bination of the potash occurs in comparatively small
amount but, where coal is used for burning, the extent to
which the potash occurs in this 'recombined" form may
be considerable. Of the three cement p'ants mentioned
above, the Riverside Portland Cement Company
uses oil for fuel while the Security Cement and Lime
Company and the Alpha Portland Cement Company
use coal in their operation. The insoluble potash is
assumed to be that portion of the total potash which
remains undissolved after the dust is boiled in a 5 per
cent solution of hydrochloric acid. The difference
between the total potash and the sum of the water-
soluble and insoluble portions is taken as the slowly
soluble or recombined potash. It has been shown by
Nestell and Anderson4 that continued extraction of
cement dust with boiling water for 10 hrs. is sufficient
to dissolve practically all this slowly soluble potash.
Various methods have been tried to prevent the re-
combination of potash and it is reported by J. J.
Porter,4 of the Security Cement and Lime Company,
that the use of salt has been found beneficial in this
connection.
In a publication by W. H. Ross5 it was shown that
when feldspar and lime are digested with water under
a steam pressure of 10 to 5 atmospheres about 90
per cent of the potash in the feldspar passes into solu-
tion. In cement dust as it escapes from the kilns,
the slowly soluble and insoluble potash are already
associated with a considerable percentage of free lime
and consequently he concluded that the greater part
of the constituents might be recovered in water-soluble
form by digesting the dust with steam under pressure.
Experimental work has shown this to be the case and
the results obtained by this procedure will be pub-
lished separately.
Since ignition of a potash-containing silicate in the
presence of lime liberates potash and since the cement
dust, as has already been stated, contains a considerable
proportion of free lime, it occurred to the author that
the recombined potash might be rendered water-
soluble by simple ignition of the dust. A preliminary
1 W. H. Ross and A. R. Mere, Tins Journal, 9 (1917), 1035.
' K. J Nestdl ami B. Anderson, Ibid., 9 (1917), 646
'J. J. Porter, paper presented at the meeting of the Portland '
Association. Chll . 1917.
* Loc. cit.
• This Journal, 9 (1917), 467.
experiment was carried out in which a sample of the
above-mentioned treater dust from the Security Cement
and Lime Company was ignited with an equal weight
of calcium carbonate in a J. Lawrence Smith crucible
at about iooo° for a period of 40 minutes. The water-
soluble potash was found to have been increased by
this treatment from 6.8 to 10.4 per cent on the basis
of the original sample. In other words, the water-
soluble potash had been increased from 60 per cent to
91 per cent of the total potash content. The addition
of calcium carbonate served, however, to considerably
12
Is
s:
-Untreated Security -Dyjtj^
JJrlreatedJll^haJJjJsr^^
600 700 BOO 900 /OOP //0t>
Fig. I — Percentages
Temperature °C-
\9 Water-Soluble Potash in
Treated Dusts
lower the percentage of \\ itcr-soluble potash in the
resultant product so that the latter contained 7.1 per
cent of water-solublt potash. It is possible that a
procedure somewhat similar to this on a large scale
should prove profitable to the cement manuf;
who at presenl receives nothing for his recombined
potash, for although he has not appreciably in
the percentage of water-soluble potash in the material
he sells, he has increased the quantity of his prodt
40 per '
io8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, Xo. 2
Similar experiments were carried out without the controlled by use of a thermo-electric pyrometer and
addition of calcium carbonate, using the same dust a rheostat in the circuit of the electrically heated muffle,
and also the dust from the Alpha Portland Cement and it was decided to make ignitions of the two cement
Company already referred to. The results obtained dusts through a range of temperatures to ascertain
were unexpected — with the former dust there was a the influence of differences of the temperature of ignition
decided increase of the water-soluble potash of the on the conversion of "recombined" potash into water-
original sample, whereas with the latter there was an soluble potash or on the further recombination of water-
actual decrease. Table I gives the percentages of soluble potash. As interest was centered on the be-
total potash in the dusts before treatment and the per- havior of the Alpha dust an initial experiment was
centages of water-soluble potash before and after run with this dust subjected for 40 min. to a tempera-
treatment at about 10000 in a closed crucible all ex- ture of 6oo°. This experiment showed that instead
pressed on the basis of the original sample. of a diminution of water-soluble potash as obtained
Table i previously there was an increase thereof when the car-
SecUri^ECemTe„?UAiphRa°Portiand bonaceous matter was removed by combustion. It is
OrfginaTbust C <?rig?nai0Du)satny questionable that the recombination of potash can be
Per cent Per cent attributed solely to the siliceous ash of the coal in the
w.?i52hSiSu»h before 'treatment.:; "I 2.° light of the above results. The writer hesitates to
water soluble potash after treatment... 9.4 2.1 ascribe this effect to the carbon, however, because the
From Table I it may be seen that ignition of the Alpha dust also contains sulfides in some quantity,
Security dust in this manner has caused an increase a fact forcibly presented when the dust was treated
of water soluble potash from 60 to 82 per cent of the with hydrochloric acid. These sulfides no doubt
total potash in the un-ignited dust, while an identical also undergo change when the dust is ignited in an
procedure with the Alpha dust has brought about an oxidizing atmosphere and it may be that they have
actual decrease of water-soluble potash from 41 to 30 an influence on the recombination of potash in the
per cent. The method of ignition which was carried absence of air.
out as in the J. Lawrence Smith method precluded the Table II contains the results of this series of experi-
loss of this potash by volatilization and the only con- ments with the two dusts.
elusion to be drawn was that a further "recombination" The readings of the pyrometer are probably not ex-
of water-soluble potash takes place in the dust. act indications of the actual temperatures obtaining
Table II — Effects of Ignition for 40 Minutes in an Open Dish on Precipitator Dust Expressed in Percentages
, Security Dust . > Alpha Dust ;
Untreated Temperature of Ignition Untreated Temperature of Ignition
On Basis of Original Dust Dust 600° 700° 800° 900° 1000° 1 100° Dust 600° 700° 800° 900* 1000° 1 100°
Loss in weieht 5.69 6.05 6.40 6.64 7.32 8.70 12.91 13.21 13.48 14.55 15.52 17.84
Total potash K,b 11.40 11.37 11.42 11.42 11.27 11.19 10.99 7.02 6.98 6.97 7.00 6.48 5.97 5.38
Water-soluble potash'.'.'.' 6.79 9.36 9.95 10.18 10.55 10.62 10.82 2.93 4.16 4.69 5.06 4.96 5.15 5.01
TotalADOtash RODUCT 11.40 12.06 12.15 12.20 12.07 12.07 12.04 7.02 8.02 8.03 8.09 7.58 7.07 6.55
Water-soluble potash 6.79 9.93 10.59 10.88 11.30 11.46 11.85 2.93 4.78 5.40 5.85 5.81 6.10 6.10
Table III — Water-Soluble Potash in Ignited Cement Dusts Expressed in Percentages of Total Potash Content
. Security Dust * , Alpha Dust »
Untreated Temperature of Ignition Untreated Temperature of Ignition
Dust 600° 700° 800° 900° 1000° 1100° Dust 600° 700° 800° 900° 1000° 1100°
On basis of total potash in original dust.... 60 82 87 89 93 93 95 42 59 67 72 71 73 71
On basis of total potash in ignited dust 82 87 89 94 95 98 .. 60 67 72 71 86 93
A glance at the dusts in their original condition be- in the dishes. In the first place, it was evident that
fore ignition would be sufficient to enable anyone to all parts of the muffle were not at a uniformly high
distinguish between them. The Security dust is ash- temperature and, again, the temperatures locally pro-
gray in color while the Alpha dust is black, evidently duced by the combustion of the carbon in the Alpha
containing unburnt carbonaceous matter. A sample cement dust may have been considerably in excess of
of the latter dust was boiled with concentrated hydro- the recorded temperatures. In consequence of this
chloric acid for 30 minutes, filtered on an alundum carbon content the manner of distribution of the sample
plate and a carbon determination was made on the in the dish may also have had an influence on the local
residue. The carbon was found to form 9.26 per cent temperatures of the samples. These same conditions,
of the dust. Assuming the dust lost from the kiln however, would obtain in large s :ale operations.
to be 4 per cent of the raw mix, and 600 lbs. of raw Table III shows that the igniti at icmperatures of
mix as necessary to yield a barrel of cement, then the 6oo° or over in an oxidizing atmosphere of treater dust
loss of carbon per barrel of cement produced amounts from cement mills results in a liberation of the recom-
to 2.2 lbs. The view that this carbonaceous matter bined potash of the dust and that this released potash
may have an influence on the behavior of the cement (at 900 °) amounts to 33 per cent of the total potash of
dust suggested the ignition of a sample of Alpha dust the original dust in the one case and to 29 per cent in
in an open dish placed in a muffle so that the carbon- the other. In view of this fact it is considered possible
aceous matter might be burned up, combustion of this that a procedure similar to this may find successful
material not occurring to any great extent in the closed application on a manufacturing scale. The use of a
J. Lawrence Smith crucible. The temperature at kiln using oil or gas as a fuel is to be cons '.red necessary
which such ignition occurred could be approximately for such operations, or if coal is used some arrange-
Feb., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
ment whereby heat is supplied without contact of the
fuel with the dust to be treated.
In case the dust is to be sold directly to the fertilizer
trade such a process would have the advantage of yield-
ing a product with its water-soluble potash more con-
centrated than in the original dust, for not only is the
recombined potash liberated by this procedure but
the total weight of the material is diminished. This
diminution of weight may be attributed to loss of water,
of carbon dioxide, and of any carbonaceous matter
in the dust. If, however, the preparation of potash
salts is aimed at, it is possible that for dusts behaving
like the Alpha dust digestion under steam pressure, as
mentioned above, would be the preferable method of
treatment since in the latter method there is no vola-
tilization of potash and the yield of water-soluble potash
on the basis of the total original potash is consequently
greater. This volatilization apparently commences at
about 900 °. As stated before, the temperatures of the
Alpha dust very likely were considerably above those
indicated by the pyrometer and relatively greater
volatilization of potash in this dust at a given tempera-
ture may be easily explained on this assumption.
To ascertain the effect of time of heating on the two
dusts, samples were ignited at 1000 ° for 20, 40 and 60
minutes. The results obtained are shown in Table IV.
Table IV — The Effect on Water-Soluble and Total Potash Content
of Variations in Duration of Ignition. Temperature 1000°
. Security Dust . . Alpha Dust ,
20 min. 40 min. 60 min. 20 min. 40 min. 60 min.
On Basis of Original Dust
Loss in weight 7.06 7.32 7.37 15.15 15.52 15.80
Total potash 11.33 11.19 11.06 6.12 5.97 5.89
Water-soluble potash . . 10.60 10.62 10.58 5.02 5.15 4.89
On Basis of Product
Totalpotash 12.19 12.07 11.94 7.21 7.07 7.00
Water-soluble potash .. . 11.41 11.46 11.42 5.92 6.10 5.81
It is apparent from inspection of this table that for
the periods considered ignition of the dust for a longer
period than 20 minutes has no decided effect on the
ratio of water-soluble to total potash in the material.
SUMMARY
I — Dusts from cement mills using coal as fuel have
considerable proportions of their potash content in a
form not readily water-soluble.
II — Ignition of such dusts in an oxidizing atmosphere
at temperatures of 600-noo0 converts the recom-
bined'" potash into a readily water-soluble form.
Ill — For the periods considered (20 to 60 minutes)
' time of ignition apparently has little effect on the water-
soluble potash content of the resultant product.
Department of Agriculture
Bureau of Soils. Washington. D. C.
EFFECT OF COAL ASH ON THE LIBERATION AND
NATURE OF CEMENT MILL POTASH
By N. S. Potter, Jr., and R. D. Chessman
Received December 6, 1917
In all articles thus far published relating to potash
as a by-product in the manufacture of cement, no
consideration has been given to the potash content
of the coal used in burning and its attendant effects.
It is the purpose of this paper to point out the effect
the coal ash has upon the liberation of potash in the
kilns and upon the nature of the so-called "treater
dust" collected.
The potash collected from the kiln stack gases where
coal is used for burning appears in practically two forms,
water-soluble potash and the insoluble or slowly soluble
potash. The insoluble potash has been attributed
to two causes: the potash in the unburned or partly
calcined raw material carried over mechanically
in the gases and to a recombination of the volatilized
potash with the finely divided ash particles of the coal.
R. J. Nestell and E. Anderson in their paper, "The
Nature of Cement Mill Potash,"1 state that "the most
important differences in the potash material from coal-
fired and oil-fired kilns, as shown by the analyses given,
lie in the relative amounts of soluble and insoluble
K20, and in the wide variation in potash concentra-
tion in the lighter fractions of dust obtained from
kilns using these two different forms of fuel. In the
dust from the oil-fired and coal-fired kilns previously
referred to, where in the first case the per cent of in-
soluble K20 was 0.56 and in the second case 4.55 per
cent, it seems safe to assume that the amount of me-
chanically carried-over raw material was practically
the same, consequently the difference noted in the
amount of siliceous material shown cannot be due to
a greater amount of calcined raw mix in one case. The
only other source of siliceous material is the ash from
the coal used as fuel. Since this ash, coming as it
does from finely powdered coal, must be in a state of
extremely fine subdivisions, approaching that of a
true fume, it is reasonable to suppose that part of this
ash would be collected among the lighter portions of
dust. Since approximately 9 lbs. of coal ash are in-
troduced into the kiln per barrel of clinker burned,
if only one-half this amount is carried out with the
gases, it would still be sufficient to effect appreciably
the composition of the collected dust, as the amount
of dust caught per barrel of clinker produced is only
about 20 lbs. Consequently it is probable that the
considerable amount of insoluble potash shown to be
present in the dust from the coal-fired kilns is in reality
due to a combination of the volatilized potash with
the finely divided incandescent particles of siliceous
coal ash."
Wm. H. Ross, in his paper on "The Extraction of
Potash from Silicate Rocks — II,"2 also states that "the
slowly soluble combination is explained on the ground
that during the burning of the cement part of the vola-
tilized potash undergoes a recombination with the
silicates in the dust."
The following is taken from an article on "The
Recovery of Water-Soluble Potash as a By-product
in the Cement Industry:"3 "The insoluble potash
represents the combinations occurring in the original
silicates of the raw mix which is carried over mechan-
ically in the dust before being subjected to a sufficiently
high temperature to bring about decomposition.
The form of combination which is slowly soluble in
water is supposed to be due to a recombination of the
volatilized potash with the silicates in the dust. In
1 This Journal, 9 (1917), 646.
« Ibid.. 9 (1917), 467.
* Ibid., 9 (1917), 1035.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHE MIS I HY Vol. 10, Xo. 2
some plants where coal is used for burning, the extent
to which the potash occurs in the "recombined" form
may b( considerable, while in certain other plants
>:.l is used for fuel this combination of the potash
is present in compa nt." Thus it
is evident that the potash content of the coal
ash has been quite neg1<
coal burned in the kiln,
Table I, bring out the fact that the potash content
of the ash is considerable and to such an extent that
it must be taken seriously into consideration in figuring
liberal inn and potash balances. The samples taken
for analyses represent a week's composite 1
daily a oing into the kiln. Being com-
pelled to buy coal upon the open market due to the
coal situation, it was impossible to differentiate the
sources relative to the mines furnishing the coal.
Work ah iotash content
of the ash of coal from different mines throughout the
country is now in progress and the results obtained will
be published in due time.
Tabu i i st of Kiln Coai. Ash
Sample Per cent K:0
Week ending Oct !9 1917 5.22
Week ending Nov 5,1917 4.54
Week ending Nov 12, 1917 4.85
Week ending Nov. 17, 1917 4.75
The average potash content figures close to 5 per cent.
As the coal consun n cement plants
throughout the country varies greatly, ranging from
80 lbs. coal per barrel to 250 lbs., it is apparent that
the potash entering with the coal is considerable.
Assuming the ash content to average 10 per cent and
using the above figures, it is evident that the potash
introduced by the coal lies between 0.4 lb. an
lbs. per barrel of clinker. Due to the very finely
divided state of these ash particles and the velocity of
the gases in the kiln, but a very small percentage of
the ash is deposited in the kilns, nearly all passing out
with the gases. The per rent being deposited in the
kiln is undoubtedly higher in mills using the v.
cess where the ash particles have a tendi
to the wet slurry. In order to observe this effect of
the asli upon the nature of the materials in the kiln,
samples of I In- ma; 1 vals of 10 ft.
ngth of the kiln t upon
the K 0 CO materials is shown graphically
in Fig. I.
Curve I takes LI 1 .ration the actual K.( >
■mined by analyses assuming the original ma-
(slurry) to be previously calcined.
Cur\ I ' 1 1 ii.il !\ 1 1 in 1 hese different
sampi
Curve III attempts to show the KjO conteril of the
samples as it woul< 1 ntent of
slurry entering the kiln and taking into COnsidi
ual loss attained at the different intervals as
tiemical analyses, disregarding any addi-
1 if K 1 1 I nun 1 il her sources.
Curve IV shows the KjO 'he different
intervals calculated on the assumption that the material
ly calcined ami no volatilizt
the kiln or addition of KjO from other Si
Comparing Curves II and III it is dearly shown that
the KjO content of the slurry is effected appreciably
from some other source. This source is either the
K;0 in the ash from the coal or the IvO as fume in
the gases. Due to the very physical nature of the
om these two causes it is safe to assume that
the K ' h is the principal contaminator.
The appreciable rise in the K.O content of the slurry
at 115 ft. as shown in Curve II is probably only a
local condition due to the peculiar construction in our
kilns at this point. I-beams aboui 1 5 ft. in length
Fig. I — Distance from Burning End of Kiln
I — Actual KjO. supposing no loss on ignition.
II -Actual EiO in samples.
Ill — Theoretical K:0, supposing no contamination from ash on volatiliza-
tion of K;< >
IV — Theoretical KjO figured to no loss on ignition basis, non-volatiliza-
tion of KiO and no adulteration from ash.
are attached to the interior wall of the kiln. These
are spaced at intervals of .? ft. and lie parallel to the
axis of the kiln. The kiln in rotating lifts the slurry
at this point to approximately the top of the kiln where
it drops back through the gases to the floor of the kiln.
This very readily acts as a filter causing considerable
of the fine dust particles to deposit with the wet slurry.
Table II -Chemical Analyses
Distance from Loss
Front of Kiln on
Ft. SOi S Ignition
5 If, 0.05
15 22.4! 1.54 1.14 0.06 4.90
25 1.41 0.07 12 05
35 19 4 ) ^. .. 99 S3. 9 i 21 1.04 0. 17 19.11
45 05 0.04 32.10
2.62 4.14 40.17 2.66 0.76 0.32 57 15
57.40
0.19 0.58 38.56
85 14.34 16 0.10
95 0 29 0.22 38.80 -
105 14 ii .. Jl 0.30
0 43 39 01
> 59 38.96
Ash 41.63 8.77 55.09 15.23 I (.7
The ash deposit with the slurry is further demon-
by chemical analyses.
Table II shows the chemical -lie different
samples as taken throughout the kiln and also the ash
analyses of the coal used a: thai lime.
As the velocity of the kill; ,■ high these
ash particles will b( .-. of the
me of the kiln but a a minute, possibly
not more than a few seconds. Further, the very nature
of combustion being exother
• a very high temperatun tained by
the ash particles. Such being lsi -.here should
ih in the
ashes from the coal in the kilns.
Feb., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY in
Table III — Solubility Tests on Coal Ash for KiO ™„c.+; + „„„ + „ t„ t-\.;~ -i. ■ • * j j £ .
■ tt . j * r.1 ivt 1 t> . , ., constituents. In this paper it is intended, first,
Sample Heated to Glow over Meker Burner for 1 Hour f f 1 j j">
Total k2o in Ash, 4.47 Per cent to present a summary of the more important condi-
How Treated Sol. K2O Per cent H»0 in Sample +;„„„ „c „ „ +■ 1.'* -u j ± .1 <. 11 a .
washed on filter paper o. io tlons of °Peratlon which detertmne the probable effect
>A hour boil 0.16 of toluol recovery upon the quality of the gas supplied ;
1 hour boil 0.23 . ., J & rr >
2 hours boil 0.23 second, to illustrate the method of estimating the
4 hours boil 0.23 , ■,, ~ . . ... ,
7 hours boil o.25 probable effect in any particular case; and third, to
i5hcursb~ii o >8 summarize certain general recommendations as to
24 hours boil 0.25 changes in standards that must be made in order that
Samples of kiln coal ash containing 4.47 per cent recovery of toluol can be carried out effectively in a
K20 were heated to a glow for approximately one hour lar2e number of localities. In this memorandum,
over the Meker burner. This showed no volatiliza- char>ges of standards are considered only from the
tion. Two gram samples of this ash were then boiled standpoint of toluol recovery. No consideration is
vigorously for different periods up to 24 hrs. to de- 8iven to any other factors which might properly in
termine whether this could be made water-soluble many cases make desirable a change of standards,
upon boiling. Table III shows that after 1 hour's Such matters would depend upon a number of factors,
boiling there is no increase in water-soluble KaO. not within the sc0Pe of the present discussions.
This water-soluble is so small as to be negligible. While SUMmary of present standards of gas quality and
this does not reproduce the kiln condition exactly it GAS company operating conditions
is quite evident that at the temperature attained by
., , • .1 , ,, , -, , c 4-u -j Both the heating value and the candle-power of
the ash in passing through the kiln and for the period . 6 H
to which it is subjected to this temperature, no potash gf are used. m this country as a measure of the c'ua,U>'
of the ash will be volatilized. ot the product suPPhed- Usually only one of these
,,.,., two characteristics is prescribed by ordinance or ad-
Assuming that 00 per cent of this ash in a dry process ministratlve ruUngj but in some cases both are fixed_
plant and 7S per cent in a wet plant passes up the flue In cases whefe guch standards have not been ad ted
with the gases the effect of the insoluble K«0 in the „„,, ., ,.. c *i r j • j ^ 1 i_
& and the quality of the gas supplied is determined by
ashes will affect the nature of the treater dust very ., , , _ .. ■ c ■ . . , , .
3 the local gas company, it is of interest to know what
apprecia y. quality of gas is being supplied. This information
Due to observations made while assisting in the re- js presented below; for convenience of consideration
search work at the Security Cement & Lime Company trie companies are classified according to the standard
and to data showing potash balances at different plants in force_ rjata are included for all American gas com-
at hand, but which we are not at liberty to publish panies making 500,000,000 cu. ft. or more of coal,
at this time, it is quite evident that the insoluble potash water, or oil gas per year and for such other companies
content of the dust collected from the kiln gases is of as have been recommended to the Ordnance Depart-
two sources, that which passes over with the raw ma- ment for consideration by the Sub-Committee on Coal-
terial, or partially calcined dust, and that which passes Tar By-Products.
over with the ash from the coal used in burning. T_Gag companies in the foUowing cities are ex-
conclusions pected to supply gas in compliance with the candle-
I- K2( ) content of coal ash is considerable. Power requirement as follows:
II- K-i ) content of coal ash must not be disregarded (*) Requirements of 20 candles or higher:
in calculating the liberation in kilns. New York City (deluding the New York Consolidated
III— K.0 content of coal ash appears in "treater System, the Brooklyn Union Gas Company, and the King's
dust" as insoluble K2( >. ,C°Unty L'f t,ng Co™^ « c-f' (Permission has recently
, . ... -. been given to change to a heating value ol 650 B. t. u. at the same
IV- I aking into consideration the K20 content of pdce or tQ any lower heating_value standard if a proportiollate
ash and the K-..0 in raw mix carried over mechanically reduction in price of gas is made.)
there is apparently no "recombination" of the vola- „, ■, , , , • T) c .. , ,. ...
^' ■" Philadelphia, la., 22 C.-p., tixed by a franchise contract with
tilized IvO with the siliceous ash particles. the city
Michioan Portland Cement Company rjes Moines, Iowa -J c.-p.
C,,E,-SI!V M,C1 Sioux City, Iowa, 21 c.-p.
Omaha, Neb., 2.? c.-p. measured at the gas works, or 21.2 c.-p.
TOLUOL RECOVERY AND STANDARDS FOR GAS "",1 " "" "u testin8 5tation- a'"' ',0° B- t u- neatin«
QUALITY' ' '''"'■
Charleston. S. C . 20 c.-p. and 600 B. t. u.
B i' S Mcliium:
, ]917 Kast St. Louis, 111., 20 c.-p. (an old city ordinance require-
i" azol and toluol Erom gas neces- """' ""' '"' B< ' ,L
sarily reduces the heating vain.- and candle-power of Northern Illinois cities supplied by Public Service Company
iUa nao. ik„ „„. 4- „<■ 1 .• 1 1 a of Northern Illinois, 22 c.-p. (ordinance) and s/'S H. t. u
the gas; the amount ol reduction depends upon the > r v 00
originally in the gas, -,. _ , ,. ., ,,
' ° ' th) Kii/i<in'iiiiiil\ nl /.S Kin/lies:
the thoroughness of washing, and l charac lH,rniu NIl(.h [g ,, p , , „ , „
flighting Lansing, Mich., 18 c.-p. and 600 B. t. u. cheating value
1 Pub!.-.!...! v.hI, pcrmi ..... .,1 Hi,- Director, Bureau ol Standard!, Los Angeles, Cal . [8 c, p and 600 B. t. u, (most of the Kas
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHE " V Vol. 10, No. ?
supply of this city is natural gas which is not limited by these
requirements).
(c) Requirements of 16 candles:
All cities of Massachusetts, 16 c.-p. (fixed by State statute
but subject to some waiver for purposes of investigation by
the State Board of Gas and Electric Light Commissioners.
This Board has very recently recommended to the State legisla-
ture a standard of 528 B. t. u.). The following Massachusetts
cities are of interest in this connection: Boston, Brockton,
Cambridge, Fall Kiver, Haverhill, Lawrence, Lowell, Lynn,
Maiden, New Bedford, Pittsfield, Springfield, Worcester.
Nashville, Tenn., 16 c.-p. and 600 B. t. u.
Jackson, Mich., 16 c.-p. (20 c.-p. for water gas) and 600 B. t. u.
Grand Rapids, Mich., 16 c.-p. and 600 B. t. u.
Peoria, 111., 16 c.-p. and 565 B. t. u.
(d) Requirements of candle-power less than 16:
Minneapolis, Minn., 15 c.-p. and 600 B. t. u.
Birmingham, Ala., 15 c.-p. and 575 B. t. u.
St. Paul, Mian., 14 c.-p. and 600 B. t. u.
II — Gas companies in the following localities supply
gas in compliance with heating-value requirements
as follows:
(a) Total heating value, 600 B. t. u.:
St. Louis, Mo. (This is a municipal requirement; the State
requirement is 570 B. t. u.)
Baltimore, Md. Tacoma, Wash
Indianapolis, Ind. Milwaukee, Wis.
Hammond, Ind. Madison, Wis.
Peru, Ind. Atlantic City, N. J.
South Bend, Ind. Elizabeth, N. J.
Cedar Rapids, Iowa. Jersey City, N. J.
Washington, D. C. Newark, N. J.
Wilmington, Del. Paterson, N. J.
Seattle, Wash. Trenton, N. J.
(b) Total heating values, 585 and belcnv:
Denver, Colo., 575 San Diego, 550
Bridgeport, Conn., 575 AUentown, Pa., 570
Hartford, Conn., 575 Chester, Pa., 570
New Haven, Conn., 575 Reading, Pa., 570
Waterbury, Conn., 575 Wukes-Barre, Pa., 570
Portland, Ore., 570 Manchester, N. 1 1., 565
Ardmore, Pa., 570 Chicago, 111., 565
San Francisco, Cal., 550 Oakland, Cal., 550
Cities of New York State, 585. (Of these cities the following
are of interest in this connection: Albany, Biughamton, Buffalo,
Poughkeepsie, Rochester, Schenectady, Syracuse, Troy, Ctica.)
Ill — The gas companies in the following cities have
no requirements limiting the candle-power or heating
value of the gas which they supply but are reported to
be supplying gas of candle-power and heating value
as given below:
New Orleans, La., 22 c.-p. and 600 B. t. u.
Jacksonville, Fla., 20 c.-p. and 580 B. t. u.
Atlanta, C,a., 10 c.-p. and 600 B. t. u.
Richmond, Va., 18 c.-p. and 590 B. t. u.
Pawtucket, R. I., 17 c.-p. and 600 B. t. u.
Providence, R. I., 17 c.-p. and 600 B. t. u.
Salt Lake City, Utah, 17 c.-p. and 600 B. t II.
Houston, Tex , 17 c.-p, and 585 B. t. u.
Mobile, Ala., 15 c.-p. and 600 B. t. u.
Portland, Me., 15 c.-p. and 570 B. t. u.
Savannah, Ga., 575 B. t. u.
Battle Creek, Mich., quality not reported.
San Antonio, Tex., quality not reported.
METHOD OF ESTIMATING INFLUENCE OF TOLUOL
RECOVERY UPON GAS QUALITY
As previously stated the quantity of toluol or benzol
in the gas initially is a large factor in determining the
quality of the gas both before and after removal of the
toluol, since the conditions which make for the pres-
ence of large quantities of these aromatic hydrocarbons
are the conditions prevailing during the production of
high-candle-power and high-heating-value gases. In
general the quantity of toluol and other light oils pres-
ent in water gas depends upon the amount of gas oil
used in the production of thi; gas. Approximately
10 per cent of the volume of gas oil used can be re-
covered as crude light oil and of this amount from '/»
to Ve can be recovered as pure toluol. Coal gas made
by any of the usual horizontal retort processes, which
are the only processes of coal-gas manufacture re-
quiring particular consideration in this report, usually
contains about one-fourth to one-third of a gallon of
light oil per 1000 cu. ft., depending upon the character
and treatment of the coal and the quality of the gas.
From one-eighth to one-tenth of this light oil is re-
coverable as pure toluol.
For each one-tenth gallon of light oil removed per
1000 cu. ft. of gas the total heating value is reduced
by approximately 10 to 14 B. t. u. per cu. ft. and the
candle-power by 2V2 to 3 candles. However, re-
storing part of the. light oil removed, for example,
enriching with the benzol fraction, may in some measure
compensate for the loss in heating value and candle-
power brought about by the initial washing. In fact,
if a sufficient amount of additional benzol is available
the candle-power and heating value can be restored
substantially to the original values. (The increase in
quality is about the same per unit of volume of benzol
returned as was the loss on removal of the light oil.)
However, this practice would not generally be prac-
ticable since it demands the purchase of benzol or other
enriching constituents to take the place of those con-
stituents which are permanently removed from the
gas. In estimating the loss of candle-power and heating
value, the figures here presented are probably slightly
higher than would correspond to the change in quality
of gas at the customers since in distributing unwashed
gas there is usually considerable loss due to condensa-
tion.
From these two generalizations and a knowledge of
the initial candle-power and heating value of the gas
it is readily possible to estimate approximately the in-
fluence upon the quality of the gas of recovering differ-
ent amounts of toluol or of toluol and benzol. Such
estimates are, of course, not exact, but they furnish
an excellent guide for readjustment of standards in
any case where this is necessary or for approximating
the quantity of materials which can be obtained by
washing the gas. The following examples will make
clear the application of the data:
(1) Assume water gas made from 4 gallons of oil
per 1000 cu. ft., having an open-flame candle-power
of 20 and a heating value of 625 B. t. u. About 0.4
gallon of light oils per 1000 cu. ft. could be re-
covered from such gas with practically complete wash-
Feb., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
ing. If none of the benzol was returned to the gas the
result would be a gas of about 575 B. t. u. and 10 candle-
power. If the light oil were distilled and the benzol
fraction were returned to the gas the loss in heating
value and candle-power would be, perhaps, one-half
as great, and the result a gas of about 600 B. t. u. and
15 candles. In order to restore the heating value and
candle-power to substantially their original figures it
would be necessary to add benzol to the extent of ap-
proximately 0.2 gallon per 1000 cu. ft. of gas manu-
factured. From the 0.4 gallon of light oil originally
obtained, some 0.07 to 0.08 gallon of toluol would
probably be obtainable on refining.
(2) Assume carburetted water gas with 3 gallons
of gas oil per 1000 cu. ft. and assume a very high oil-
efficiency so that the candle-power was 18 and the
heating value 570 B. t. u. From this gas about 0.3
gallon of light oil, equivalent to, perhaps, 0.05 to 0.06
gallon toluol, would be obtained per 1000 cu. ft. with
commercially complete washing. The result of this
washing would be a gas approximately 530 B. t. u.
and 9 to 10 candles, which would be restored to 550
B. t. u. and about 12 candles if re-enriched with the
"benzol portion of the light oil.
(3) A mixture of coal gas and water gas in about
equal proportion may be assumed made from water gas
for which 3V2 gallons of gas oil were used to give 18
candles and 600 B. t. u. and coal gas of 580 B. t. u.
and 15 candles. Such mixed gas would yield, perhaps,
0.3 gallon light oil per 1000 cu. ft. and the average
candle-power would be reduced by washing from 16V2
to 8 or 9 candles and the heating value from 590 B. t. u.
to about 550 B. t. u. Restoration of the benzol
fraction would give a product of about 12 candles and
570 B. t. u.
(4) A coal gas made from ordinary grade of gas coal
to yield 10,000 cu. ft. of gas per ton is assumed to pro-
duce gas of about 14 candles in the open flame and of
585 B. t. u. From this approximately 0.3 gallon of
light oil per 1000 cu. ft. of gas could be recovered; and
from it 0.025 to 0.03 gallon of toluol per 1000 cu. ft.
would be available. The gas after washing would
have approximately 8 candles and 550 B. t. u. which
would be increased to, perhaps, 12 candles and 570
B. t. u. if the benzol fraction were restored.
In any of the above cases the net loss in heating
value and candle-power might readily be reduced if
some of the other constituents of the light oils, such as
the solvent naphtha fraction, were also restored to the
gas; or the loss in heating value and candle-power
could be made less by operating the washing equip-
ment in such a way as to accomplish only a partial
removal of the light oils. In the latter case if removal
of only 75 per cent of the quantity of light oil readily
obtainable were considered satisfactory this would
make the losses in heating value and candle-power of
only about 3/4 as great as above indicated, but, of course
it would also somewhat reduce the yield of toluol.
It is probable that complete washing of the gas with
restoration of the benzol in most cases will be con-
sidered advisable since the need for toluol is con-
siderable and very little sacrifice of toluol yield can be
allowed. But the demand for benzol is not so great
and the restoration of the benzol to the gas might give
results at first more satisfactory to the gas users than
would the sale of this benzol with the slight reduc-
tion in total costs for the gas which might possibly be
accomplished thereby. Especially might the restora-
tion of benzol be necessary where a high candle-power
standard has been in force, since otherwise the loss in
candle-power would be rather greater than would
be desirable at one time. In any computation, there-
fore, it is probably best to assume, unless other basis
is known to be correct, that commercially complete
washing of the gas would be necessary and that the
benzol fraction of the light oil amounting to approxi-
mately one-half the total volume of light oil removed,
will be restored to the gas.
RECOMMENDATIONS REGARDING STANDARDS FOR GAS
QUALITY
From the estimates in the preceding section it is
evident that much greater difficulty is met in complying
with a candle-power requirement after removal of
toluol or light oil than is encountered if a heating-value
standard is to be complied with. Because of this
fact it seems desirable that in any case where toluol
is to be removed the candle-power standard be al-
together eliminated or be made sufficiently low so that
it will not interfere seriously with the proposed opera-
tions. Many other factors independent of toluol
recovery make evident the desirability of eliminating
candle-power requirements and substituting heating-
value requirements as the primary basis of gas measure-
ment. Therefore, the war is only 'an added influence
tending to hasten an end otherwise desirable.
In all cases 'where the candle-power has previously
been below 18 it would seem that the elimination of
the candle-power requirement altogether would be
reasonable; although in any event it is expected that
the company would supply a gas of at least 8 or 10
candles, which would be sufficient to care for the need
of those customers who must use some portion of the
gas for open-flame lighting. In cases where 18 or 20
candles or higher have been maintained regularly in
the past, it might be undesirable to have the candle-
power go below 12 to 14, unless open-flame lights were
generally eliminated and a readjustment of the ap-
pliances of all customers were made wherever the
change in quality might make this necessary. For all
companies which have been complying with require-
ments of 18 candle-power or higher, an understanding
might be reached as to the maintenance of at least
12 to 14 candles for such a period as might be neces-
sary to accomplish a general adjustment to the new
conditions.
When coal gas is supplied either alone or mixed with
very small percentages of water gas it is impracticable
to make a very rich gas since the character of the coals
available in most instances would preclude economic
operation if a higher standard, either of heating value
or of candle-power, must be maintained. For cities
where only coal gas is supplied the standard could
scarcely be higher than about 570 B. 1. u. il practically
complete toluol recovery is expected. Higher heating-
114
THE JOURNAL OP INDUSTRIAL AND ENGINEERING ( SEMISTRY Vol. 10, No. 2
value standards than this would probably have to be
modified for such gas supplied.
II water gas is manufactured cither alone or as a
major constituent of the supply it is entirely prac-
ticable to make a gas of reasonably high heating value
and candle-power initially and have after removal of
the toluol a heating value of 585 to 600 B. t. u. In
each case it would be a question as to which pro-
cedure was the more economical; that is, whether i1
would be better to make the same quality of gas as
had previously been supplied and supply the customer
with a somewhat lower product than formerly after
the toluol had been removed from the gas. or to make
the gas initially somewhat richer than before by the
use of slightly more gas oil per 1000 cu. ft. so that the
product after washing would have substantially the
same healing value as had previously been supplied.
If the quality previously supplied was rather high,
approaching the maximum of the range of quality per-
missible for efficient operation, then any increase in
the initial quality would obviously be undesirable;
but otherwise an initial increase in quality with subse-
quent washing down to the original might be the best
practice. Since the quantity of toluol available is
largely dependent upon the initial richness of the gas
which has been washed there is considerable advantage
from the standpoint of the Government in having the
richest practicable gas made initially; but, of course,
in any case the limits of economical operation must
be clearly recognized, and conservation of oil might
also be an important factor.
As a summary of these points the following sug-
gestions are offered as desirable adjustments to facili-
tate the recovery of toluol:
I — Eliminate all candle-power requirements now in
force except for the cities where 18 candles or higher
has been supplied, in which localities reach an under-
standing that at least 12 candles will be maintained
for a period, say a year, during which time readjust
ments of appliances ami substitution of mantle lamps
would be accomplished to such an extent as to justify
complete elimination of candle-power regulations.
II — For plants making coal gas (or practically only
coal gas) let the heating value standard be from 550
to 570 B. t. u.
III for plants making water gas, either al
as a major constituent, Lei th( Hue standard
be 570 to 600 B. t. u. monthly average total heating
value, 1 hi ad iu I rm rrl being >":";< bi ese limits
according to the economic conditio! ion.
[n ordi the number of companies that would
ected by these several recc ions the
Eollowing t abulation of the compani
prepared. This tabulation doc-, Q0 0Un1 of
any unusual local conditions which might
of the 1 ase , material^ , The t ind ol gas manufactured
is also indicated: \Y. water gas; C. coal gas; O, oil
I'., by product coke
as; and \, natural gas.
1 — Localities in which no change ird will
probabh I" m no serious change in the quality
of gas supplied will probably result:
1 . Pa.
Reading, I
Wilki Barre, Pa.
re, Pa.
Ulentown, Pa.
Portland
Manchester, N. II.
Hartford, Conn.
Brii Igeport, Conn.
New Haven, Conn.
\\ aterbury, Conn.
Denver, Colo.
YV • B Schi necta ly, N. V. M
W Troy, N. V. W
YV Utica, N. V. W
W Poughkeepsie, N. V. W
W Syrai use, N. V. M
O Binghamton, X. V. W
M V M
M Chicago, ill. W+B+N
W Sat i Cal W+O
M San Francisco, Cal. O
W Oakland, Cal. O
M Houston, Texas W
Pawtucket, R. I. M
Providence, R. I. M
Battle Creek, Mich. M
Portland, Me. M
Salt Lake City, Utah M
MobHe, Ala. M
San Antonio, Texas W
Savannah, Ga. W
Jacksonville, Fla. M
Richmond, Va. M
Atlanta. Ga. M
New ( Irleans, La. W
Albany, X. Y. W
2 — Localities in which a candle power standard may
have to be abandoned, but with no serious change
in the heating value of the gas supplied:
Lynn, Mass. M Fall River, Mass. M
Boston, Mass. M Haverhill, Mass. W
Brockton, Mass. M Springfield, Mass. M
Lawrence, Mass. M Maiden, Mass. M
Lowell, Mass. M Birmingham, Ala. M
New Bedford, Mass. M Waterloo, Iowa. W
Pittsfield, Mass. M Peoria, 111. M
Worcester, Mass. M Nashville, Term. M
EastSt.Louis.il!. W+N Cambridge. Mass. M
3 — Localities in which slight change in heating-
value regulations may, perhaps, be required, but in
no case probably more than equivalent to 5 per cent
of the present value. (The six cities marked (*) have
candle-power standards which should be eliminated
also.)
Indianapolis. Ind. B+W Buffalo, N. Y. M
Tacoma, Wash. C+0 Milwaukee, Wis. M
Seattle Wash. B + M Madison. Wis. W
Trenton. X. J. B + M Cellar Rapids, Iowa. M
l'aterson, X. J. W St Louis, Mo M+B
Newark, N.J. M Baltimore, Md. W+B
Jersey City, X. J. W Hammond, Ind. M
Elizabeth, X. J. W South bend, Ind. M
Atlantic City, X. J. W Peru. Ind. M
Washington, D. C M Wilmington, Del. W
'ml. Minn. W *Grand Rapids, Mich. M
- apolis, Minn. M 'Jackson, Mich. M
"Detroit, Mich. Los Angeles, Cal. 0+N
4 — Localities in which high candle-power regula-
hould be changed or eliminated in order to
permit operation on a heating value basis; the reduc-
tion in heating value of the gas delivered would prob-
a considerable p.- present value.
of Lansing and Omaha a lower heating
value than now in force would also be necessary.)
New York City M Charleston, S. C. W
Omaha, Neb. W Des Moines, Iowa W
Lansing. Mich. M Sioux City, Iowa W
Philadelphia, Pa. M
Northern Illinois cities supplied bj Public Service Company
,.f Northern Illinois. M.
livKii.M' op Standards
Washington, D. C.
Feb., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
H5
CATALYSTS IN VULCANIZATION1
By D. Spence
When the Chairman of this Section wrote me asking
if I would read a paper on "Vulcanizing Catalysts,"
to me one of the most fascinating subjects of rubber
chemistry, it was with regret I advised him that I
would be unable to do so on account of lack of time to
prepare a paper. In the meantime, however, I
have found an article prepared by me in 191 1,
but never published, which, together with a few notes
prepared on my trip to Boston yesterday, with your
permission I will read, as they should clear up some
of the points raised in this discussion, and at the same
time serve to show the extent to which the investiga-
tion of this subject had been carried by some of us
prior to 191 1, and our knowledge of this subject in
America at that date.
This subject is one which is of particular interest
to me, as it has been, I may say, my main field of in-
vestigation for the past eight to ten years. During
that period many interesting discoveries have been
made, more than one hundred widely different vul-
canizing catalysts have been prepared, investigated
and put on record, and results of scientific as well as
of technical importance have been obtained.
By some of our good friends and allies across the
water, jealous of their claims to discoveries along this
line, I have been recently criticized, for not placing on
public record by patent or otherwise, the results of
these past years of investigation, but I am confident
that by the time they have carried their studies a
little further, they will appreciate the difficulties in-
volved in the problem, and my reasons for compara-
tive silence. These remarks will, I hope, serve to
answer some of their criticism and, at the same time,
outline the history of this subject as far as I am con-
cerned.
In the first place, I would point out that, as a matter
of fact, discreet mention will be found in some of my
earliest published work on vulcanization, of this basic
principle, the importance of which our European
friends, as well as enemies, have to-day begun to realize.
Thus in an article dealing with the theory of vulcaniza-
tion2 and in particular with Axelrod's theory of a vary-
ing velocity of reaction with the degree of polymeriza-
tion of the rubber, I took occasion to point out that
"what Weber, Axelrod, Ostwald and all investigators
had overlooked was the fact that the vulcanization of rubh r
with sulfur, as we know it. is essentially a catalytic reac-
tion." Even earlier; however, and in the controversy be-
tween Ostwald and myself in 1910- 1 1 . over the chemical
w. adsorption theories of vulcanization, which some of
you probably remember, it was the knowledge of the true
of the reaction, overlooked by Ostwald, which
led me to take the stand I did. In the Kolloid Zeit-
Vol. 13, pp. 270, 271, will be found further
e to this subject, together with figuri
curves showing the influence of varying amounts of
rful catalyst on the rate of vulcanization, as
determined by the amount of combined sulfur. That
1 Read before the Rubber Section, at the 55th Meeting of the
Chemical So id mbcr 12. 1917.
' KMoid-Z., 11 (1912). 275.
this basic discovery was not made the subject of a
patent as Peachey has suggested,1 may appear remark-
able at first thought, but its very breadth rendered
patent protection well-nigh impossible and disad-
vantageous to seek. The number of substances which
can be used in this connection with more or less success
is legion, so that patents such as those which have
been granted recently, can be readily overcome, and
are of no intrinsic value in any case. By the methods
of organic chemistry, all manner of substances can
be, and have been prepared, which will be found to
accelerate vulcanization, and to bring about the phys-
ical result to a greater or lesser extent; simple organic
substances widely different in constitution, such as
aniline oil, piperidine, diazobenzene, etc., metallo-
organic compounds such as alkyi derivatives of lead,
and the salts of the fatty acids or of aniline oil. with
the alkali metals; then there is the great group of sub-
stances which by decomposition, natural or induced
during vulcanization, produce some very active and
efficient catalysts to which class the thioureas belong.
Each of these various classes contains several dozen
different representatives, which I have already investi-
gated, and there are doubtless hundreds still to be
tested, so that I am sure you will agree with me that
the task of adequately protecting an invention of the
scope of this one is hard, to say the least . and of doubtful
value if attempted. It has certainly not been accom-
plished so far. In 191 1, in an effort to cover by patent
the results of past years of research in this line, I set
down a description of some of the discoveries made
by that time, together with four claims, from which,
with your permission, I will read the following extracts.
The article is entitled "Improvements in and Relating
to the Vulcanization of India Rubber" and is dated
August, 191 1. I was surprised, on referring to it
again the other day, to find how fully it deals with the
subject.
Since the publication of the classical researches of C. O.
Weber into the nature of the vulcanization process, this process
has been generally regarded as a simple addition of sulfur or
sidfur chloride to the rubber hydrocarbon and the practical
vulcanization of the rubber of commerce by sulfur has been
handled from the standpoint of a simple chemical reaction, as
generally understood, between the rubber and the sulfur at the
vulcanization temperature. In view of certain difficulties
experienced from the earliest of times even to the present day in
accepting the simple chemical theory of vulcanization2 it is
therefore the more surprising that what we believe to be the key
to successful vulcanization has not been discovered or made
known as far as published work shows The conception of a
simple chemical reaction between the rubber and the sulfur
at tin- vulcanization temperature has long been felt to fail to
account for certain practical results obtained in vulcanization
and only a- recently as last year the physico-chemical or ad-
sorption theory of vulcanization was put forward by an eminent
authority on the chemistry of rubber on the ground alone that
. i„ [ped to explain the practical facts of vulcanization better
than Hi'- simple chemical theors ol Weber.
I have cited Hi' se Fai ts is ordei to show that from Hi
days of the industry to the presi m time what we believe to be
note to the vulcanization process as determined by our
investigation has never once been sounded * * *.
0, (hem. h„t.. 36 (1917), 321.
raid, Kolloid-Z., 6 (1910), 136.
n6
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHUM! i RY Vol. 10, No. 2
For the better understanding of the facts leading up to and
bearing on the present invention, it is necessary to refer to the
following discoveries made by us:
That the vulcanization of pure rubber (by which is meant the
rubber of commerce divested of those impurities usually asso-
ciated with it in greater or lesser amount) by sulfur is an ex-
ceedingly slow reaction. The amount of sulfur which enters
into combination with the rubber in a given time is relatively
small, and even the best of the products obtained have very
poor physical properties, usually deteriorate rapidly and are of
little or no industrial value. It has been universally reported
that this inferiority of so purified rubber is due to the quality
of the rubber per se or to changes in the rubber per se brought
about by the purification process. That this is not correct we have
established by experiments in which, by returning to the purified
rubber, certain of the so-called impurities removed in the first
case, and investigated by us, or by adding to the rubber certain
substances having an analogous action in vulcanization, the
velocity of vulcanization of the original rubber and the superior
physical properties of the vulcanized product were restored.
For example, it is known that by dissolving Para rubber in
solvents and precipitating the rubber from its solution by acetone
or by simple extraction of the rubber by acetone, the vulcanizing
capacity of the rubber is greatly reduced, and products with
very poor physical properties are obtained. We have discovered,
however, that by returning to the rubber certain of the so-called
impurities removed in purification, the original vulcanizing
characteristics of this rubber are restored.
We have discovered in fact that :
I — The superior qualities of certain raw rubbers with respect
to vulcanization are not necessarily due to any superiority in
the quality of the rubber itself, but are determined far more
by the existence in these rubbers of commerce of certain sub-
stances, hitherto regarded as impurities, which are not present
in like degree or at all in the other rubbers. These so-called
impurities are soluble in acetone and can be extracted in this
way. When they are added to rubbers with inferior vulcanizing
properties, products which vulcanize rapidly and with superior
physical properties are obtained.
II — The acetone extract from Para rubber contains, in addi-
tion to the resinous impurities generally held to constitute the
acetone extract, organic substances, nitrogenous and feebly basic
in character, having all the reactions and characteristics of an
organic alkaloid.1 We have found, furthermore, that it is
these organic nitrogenous substances present in one form or
another in Para rubber that impart to this rubber its charac-
teristic vulcanizing properties and are capable of bringing about
substantial improvements in vulcanization when added to other
so-called low-grade rubbers. These substances which occur in
Para and in some other rubbers to a less extent we shall call hence-
forth the "active principle" of raw India rubber. To what
extent this active principle occurs in Para we have not yet
been able to determine, but from calculations made there is
probably less than 1/10 of 1 per cent.
Ill — The function of this active principle in effecting more
rapid and better vulcanization of rubber by sulfur is complex
but essentially that of a catalyst (as generally understood)
accelerating as it does enormously the rate of reaction between
the rubber and the sulfur. This has been established by us
beyond doubt by comparative curves of the combined sulfur of,
purified rubber, vulcanized with sulfur only, (<i) in absence of,
(6) in presence of the active principle of India rubber, (c) in
presence of substances having analogous properties,
IV — Organic substances having analogous reactions and
1 At the time this was written these nitrogenous bodies had not been
definitely identified; only their behavior towards the well-known tests for
alkaloids had been noted.
properties can be used as catalysts to replace the "active
principle" of Para rubber in the vulcanization of India rubber by
sulfur. Thus by adding 1 per cent of the well-known alkaloid
quinine to a mixture consisting of 100 parts purified rubber with
8 parts of sulfur, the reaction between the rubber and sulfur is
so hastened that the time required using 40 lbs. steam pressure
to effect proper vulcanization is reduced from 4 to 5 hrs. when
no quinine is present to 25 min. when quinine is present. The
physical properties of the product obtained are likewise im-
proved enormously by the use of this substance as catalyst.
V — The number of organic substances which can be used to
replace the "active principle" existing in higher-grade rubbers is
unlimited; derivatives of these and metallo-organic bodies may
be likewise employed and although the substances which
may be employed may differ widely in chemical composition,
they all have the common property of behaving as catalysts in
vulcanization, hastening the velocity of reaction by carrying
over the sulfur to the rubber at the temperature of vulcaniza-
tion. We have found, furthermore, that the power which these
substances possess as catalysts in vulcanization varies with their
constitution and with the nature and arrangement of their
reactive groups. We have discovered that it is possible, by
suitably modifying the structure of the substance or its reactive
groups by the well-known methods of organic chemistry or by
suitably modifying the amount of the substance or substances
used in vulcanization, to obtain any desired effect. Thus whereas
we have found para-phenetidine to be a very' powerful catalyst
in vulcanization, ortho-phenetidine is but feebly so and the
somewhat weak catalytic action of para-amido-phenol is wonder-
fully increased by converting it into the corresponding amido-
phenetol. Similarly diphenylthiourea is but feebly active
compared with the corresponding tetramethyldiaminodiphenyl-
thiourea.
As examples of organic substances having the power to act
directly as catalysts in the vulcanization of India rubber by
sulfur, we may mention aniline, para-phenetidine, piperidine, and
quinine.
As examples of derivatives of organic substances with in-
organic radicles and metallo-organic substances acting catalyti-
cally in the vulcanization of India rubber by sulfur, we may
mention the alkyl derivatives of lead and mercury and the salts
of oleic acid with sodium or lead.
As the third class of catalyst in vulcanization we have dis-
covered, furthermore, certain substances which are inactive in
themselves, but which at the temperature of vulcanization, it
may be alone or it may be in the presence of other substances,
break down into a substance or substances having the properties
of powerful catalysts. As an example of a substance of this
kind, we may mention sulfocarbanilide or diphenylthiourea.
What we claim to have discovered is the basic principle of
vulcanization of India rubber by sulfur; that the vulcanization
of India rubber by sulfur is not a simple chemical reaction as is
to-day assumed, but owes its whole success industrially to its
catalj tic nature.
We are aware of the well-known action of litharge in the
vulcanization of India rubber by sulfur. This inorganic sub-
Stance has been used from the earliest times in large quantities
in rubber compounds (up to 40 per cent and is known to hasten
vulcanization. Further, we are aware of the use of magnesium
oxide as an accelerator in vulcanization and of the work of
Weber and of Henriques in this connection. Henriques, as the
result of investigations into the inorganu >■;> the ash)
of different rubbers, came to the conclusion that it is the presence
of compounds of the alkaline earths (inor cnts, in other
word in quick-curing rubbers, that accounts for the ease with
which these rubbers vulcanize. This statement as far as the
literature shows is still generally accepted as correct, and gave rise,
Feb., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY 117
we believe, to the use of magnesium oxide as an accelerator in VULCANIZATION OF RUBBER BY SELENIUM
the vulcanization of rubber by sulfur. We have come to an By Charj.es R. Boggs
entirely' different conclusion, however, and, although we do not Received October 31 1917
deny the specific results to be obtained by the use of both Vulcanized rubber has been manufactured for some
litharge and magnesium oxide in the vulcanization of India , , ,, . „ , . . , ,
,,,.,. , . . . . .. , .„ years, but there has really been no essential change
rubber bv sulfur, we lay no claim here to the use of any of these , . .,,.,.. . .
inorganic ingredients in vulcanization. We claim, furthermore, fr0m the general methods of vulcanization as originally
that the results obtained by the use of any of these inorganic sPecified by the inventors. The two original meth-
accelerators in the vulcanization of rubber by sulfur are sub- ods> which are still in use, are the vulcanization with
stantially different from those obtained by the methods of our sulfur by heat and that by sulfur chloride in the cold.
invention; both these inorganic substances have to be used in. Variations in the processes have been introduced and
large amount to produce any marked result and neither of these innumerable mixtures made with other materials, but
inorganic accelerators gives the physical properties to the vul- no rubber article of practical importance has been put
canized rubber possessed by the products of our invention, on the market which has essentially deviated from the
which is best illustrated by comparative results and by the fact two or;ginal processes,
that the addition of the products of our invention to com- r^u . , . . ,. ,,
...•*, . . . ^ There have been made, however, manv slight vana-
pounds already containing these inorganic substances causes a . ,. , , .,,..,
.... , . . . j. ,<.<■■ • . tions in compounding rubber mixtures which have
still very pronounced improvement in the results of vulcanization. r °
produced vulcanized rubber products that are charac-
I will omit the claims at this present time. The terized by properties which fit them to special work
article also gives six examples which I have omitted, better than any previously known compounds. It
and defines in full the conditions under which the was with this idea that we thought rubber vulcanized
process may be carried out, and the pros and cons of with selenium might give a product of especial adapta-
various classes of reagents. Thus it points out, among bility to some of the many uses of rubber. At the
other things, that some agents are solids, difficult to time that we first tried to vulcanize rubber with
handle; others yield colored products on vulcaniza- selenium, 1913, we thought that we were the first,
tion (nitrosodimethylaniline, for example); others on although it is evident that anyone with a knowledge
account of their poisonous character or odor would of chemistry would expect selenium to act similarly
not be suitable for practical purposes; nor will the to sulfur. We have since noticed that Pearson in his
methods of application constitute a novelty in con- book, "Crude Rubber and Compounding Ingredients,"
nection with discoveries along this line as the descrip- mentions two methods, one by heating rubber with
tion sets forth in detail. equal parts of selenium and the other by dropping
TC , . , ., ... .. , ,, .... . , , liquid selenium into a CS2 solution of rubber at 3000
If our friends across the Atlantic should still doubt „ , T, . ., . ., . ^, ., .
... , ,. . ., . , . . , F. under pressure. It is evident that these methods
our claims to priority of discovery of this fundamental , . . , _ . ,.
, , . .. , . ., . .1 ,.... had nothing to recommend them and I believe could
principle of vulcanization let them test the validity , , , , . ,
, . _, ... »«.,.., j never have been developed because 01 the unsatisfac-
of their patents. They will find that the records
which I have just cited are a mere indication of the • , , . . ' , • , r ., . ,.
, . , ... , . ,,. , , Selenium is a metal in the same group of the periodic
volumes of evidence and facts which can be established , , „ . . ,
r , . ., . ,. , . table as oxygen, sulfur and tellurium, is much more
to dispose of any claim on their part to novelty of in- . ,,. . ,, , , ... ... . .
.. , . . . jAf metallic than sulfur and has a higher melting point
vention as far as America is concerned. As far o^x ^ • ^1 1 • , ^ j- e
.... .. . . .. .. (217 C), sufficiently high to discourage one from at-
as the specific claim to the use of *-nitrosodi- . ' .. , • r ■,. .. « .
, , .;. , , . * „ , tempting to use it as a vulcamzer for rubber which is
methylamlme is concerned, let me assure Mr. Peachey . , - ... . .. , Ti
^, , , . . T JAJ l not capable of withstanding such a temperature. Its
that when he is ready, I am prepared to demonstrate . r . ■ ■ . T° . . „.
. ,._ *, . ... . . , atomic weight is 79.2. It occurs in two crystalline
through several different sources that this material , ° ". . , , ,
. , . . i._ ., , . , A . ,, and one amorphous form and forms a complex mole-
was tried out both scientifically and industrially in , , , _ , . . ., . ., .
". cule when cold, bes being very similar to sulfur. A
this country so long ago as 1910, and was long . , , ' f , ,,
, , r, ... j short table of its properties follows:
since abandoned on account of tne serious disadvantages
to its extensive use. I recall indeed having used it in Crystai. Gravity Solubility Point8
one instance in the preparation of rubber stoppers for B1^in°r gray crys" octahedral insoluble in
laboratory use, but with unfortunate results. It is a Hexagonal 4. so cs* 217°
,. I _ , , , . , , . . . Red crystalline Monoclinic 4.46-4.51 Soluble in CS; 175°
Substance which I Should not think of employing induS- Red amorphous 4.26-4.28 1 soluble (and Softens
. . „ .. .. . .. 1 insoluble) at 102°
tnally now, as there are so many objections to its i„ csi
All modifications go over to the black crystalline
In conclusion, a good reagent must intensify not form wnen heated at ioo to 150° C. The black crys-
mcrely the chemical process of vulcanization, but also talline powder can be obtained on the market in small
the physical; it should toughen the rubber, whether raw quantities, but it should be procurable in fair amounts
or vulcanized; and should render it immune to deteriora- ;f there were a commercial demand for it. Black
tion. All this has been achieved in America, giving a selenium has the further peculiar property of being
Tubber superior to that from any natural source. A an electric conductor under the influence of light al-
"noble" rubber, similar to the "noble" alloys, is an ac- though the other forms are insulators. It might,
complished fact. therefore, cause rubber which has been vulcanized
«._-___„ with it to show some slightly unusual electrical charac-
NORWALK TlRB AND RuDBBR Co., INC. °
Norwalk, coNNBcncuT tenstics.
n8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 2
Our first attempts were with selenium in the form
of black powder used in a standard 50 per cent Para
compound in the equivalent proportion that sulfur
would be used. By heating at about 1500 C. for a
couple of hours a partial vulcanization resulted. The
physical tests showed a normal elongation, but a ten-
sile strength of only about 50 per cent of the similar
sulfur compound. The point to be noted is that partial
Vulcanization was obtained, although the temperature
ell below the melting point of Se. Increase in
the time did not improve the product. All of these
first samples have aged well and after nearly four
years give the same elongation and tensile-strength
values of about 70 per cent of the original.
Doubling the amount of selenium and using an or-
ganic accelerator, which we were then using with sulfur,
did not improve the product bu1 did make the samples
lieces with age, a normal characteristic of over-
vulcanized and under-vulcanized rubber. A peculiar
point about this, compound was that when it was re-
moved from the press hot it expanded 25 per cent of
its volume. Its volume became normal when cold.
This high coefficient of expansion indicated lack of
vulcanization.
Using amorphous selenium and an organic accelera-
tor we were able to increase the tensile strength some
without sacrificing the elongation. Some other ac-
celerators were tried without much success. The
amorphous selenium should go over the metallic form
at the temperature used.
The most promising compound we then had was put
on wire and has been tested regularly for the last
three years and the remarkable point is that it has
not deteriorated appreciably in that time. This com-
pound was below normal in its tensile strength. The
difficulty seemed to be that the long heating at the
relatively high temperature used to effect vulcaniza-
tion caused too great a depolymerization of the rub-
ber.
ial we have now found accelerators which en-
able us to satisfactorily vulcanize rubber with selenium
d at the ordinary vulcanizing tempera-
ture of 27SCF. i 135° C.) for only about twice the time
required with sulfur. The produd gives the normal
tensile 1 100 to 1. 'oo lbs.) and elongation (2 to
ioin.or 12 in.) of the same compound with sulfur. It is
This compound shows no deteriora-
tion under the short life test of 4 .lays' heating in air
at 7 o I
arried out on wire in-
with this compound and the insulation re-
strength are somewhat low.
as dielectric loss, etc., have
not >
Chemical analysis as applied to ordinary sulfur com-
pounds does not apply lounds vulcan-
ized with selenium, as the black selenium is practically
insoluble in acetone and itly the uncombined
Se is not separated by extraction with acetoni
it is only very slightly soluble in CHClj and CS;.
The acetone extract contains only the resins from the
rubber (provided oils, wax. not added).
The CHCh, extract contains some Se and a small amount
of unvulcanized rubber as with soft vulcanized rubber
when cured with sulfur. A determination of rubber
by the tetrabromide method gave 31.7 per cent rub-
ber plus resins, etc.. in a compound to which 31.7
per cent rubber had been added. This would indicate
that no correction should be made for combined Se,,
i. c. that the selenium was either not chemically com-
bined or more likely that it was so weakly combined
that it was displaced by Br. It is possible that a com-
plete chemical study of the vulcanization of rubber
with selenium may throw some additional light on the
theory of vulcanization. Also it may help in the
study of the nature of the catalytic effect of accelera-
tors as the vulcanization occurs so far below the melt-
ing point of the Se.
The product as we now have it has not yet shown
any unusual electrical properties, but the indications
are that its deterioration with age is much less than
with sulfur compounds. It can be brominized and
oxidized but the natural oxidation seems to have
been slowed up. As the deterioration of rubber goods
is the one disadvantage of rubber, especially in those
lines of work where permanency is desired, it may be
that the use of selenium may partially remove this
disadvantage.
Rubber Laboratory of the
Simplex Wire & Cable Company
Boston, Massachusetts
THE PIGMENTS OF THE TOMB OF PERNEB'
By Maximilian Toch
In 1013 Mr. Edward S. Harkness presented to the
Metropolitan Museum of Art of Xew York City, the
Tomb of Perneb. which originally stood in the ceme-
tery of the ancient Memphis. Mr. Harkness acquired
this tomb from the Egyptian Government and Dr.
Albert M. 1. I he tomb from Sakkara
and re-erected it in the main hall of the Metropolitan
Museum of
The tomb was built approximately 2650 B. C. and
is buried an Egyptian ' amed Perneb,
who held high office under the king at Memphis.
The tomb contains many figures in relief, particularly
the side wall in the main chamber. the carv-
ings are very profuse. The figures are all colored
with various |
The pigments used on the 1 neb are red,
yellow, blue. [ There is a popu-
lar belief that the red u . as was red
ochre. This is an error o\v naturally,
and only turns re urned or calcined.
Ochres all normally contain between ic and 20 per
cent of oxide of iron, whereas th r.^yptians
contain more than 50 per cenl oxide of iron, and
from their very color it red of the
ancients was hematite. This is n ry bright
1 Paper presented at the meeting of the New VorL Section of the
Society of Chemical Indostl ■'. 1917
* It is a great pleasure for me to acknowledge the assistance that I
have received Irom Dr. Albert M Lythgoc, through whose courtesy I was
given the pieces of limestone and the udhcrent pigments which were taken
from the Tomb of Perneb.
Feb., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
119
red, but is always one which we associate with brick
color.
yellow — All the yellows used were the native
ochre, which is clay stained with iron rust.
blue — The Egyptian blues are very beautiful and
range from a light sky-blue to a dark ultramarine. An
examination with a microscope of the dark Egyptian
blue shows it to be powdered glass or porcelain. This
material has been known as "frith" and has of itself
no hiding or obscuring power, nor does it seem to have
been put on with a binder. This powdered glass has
been rubbed into the surface and allowed to set with
the Nile clay or the Nile mud, which, on account of
its slightly alkaline nature, is cementitious of itself
and has both setting and binding power. The appear-
ance of this blue glass, which in modern times is called
"smalt," appears blue just the same as snowflakes
appear white, because the light is broken up on its
crystalline structure, yet a single snowflake is as
transparent as pure glass.
greenish blue is azurite, a hydrated carbonate
of copper.
green is malachite, azurite and clay.
black is carbon black composed of charred wood
or burnt wood or charred bones.
gray is limestone mixed with charcoal or carbon.
Mr. Lythgoe found two paint pots which had evi-
dently been thrown out by the workmen and an ex-
amination of these shows the pigment to be hematite
mixed with limestone and clay.
It is remarkable that in all investigations of his-
toric materials, many of the tools and implements
used have been either forgotten or in many cases not
found. I have, in times gone by, paid a great deal
of attention to the pigments used by the old masters,
beginning with the primitive painters of Italy and
going through the history of the Flemish materials
down to the English masters, and while I have had
abundant matter I have had hardly any historic data
concerning the implements used, such as brushes and
-palette knives. There are practically no brushes
left to show us how the wonderful technique of the
older painters has been carried out. The same may
be said of the musical instruments. The bows used
by the early violinists of Italy are not well known
and their history, method of manufacture and composi-
tion are very largely shrouded in mystery.
There is a brush in the Metropolitan Museum of Art,
from one of the excavations of the Palace of Amen-
hotep III at Thebes, that dates from the XVIIIth
dynasty. This brush is similar in size and shape
medium-sized sash tool used by the house paint-
oi tin present day. The bristles are not hair,
bul evidently ol a vegetable stalk similar to bamboo,
whii i n beaten until the longitudinal fibers
It is bound around with a twine
of lil up, just the same as a 1
era round paint brush is bi th wire or
Then .. no work done on 1
with the exception of the chapter by Dr.
ell, (ailed ., Colors," in the book
"Medum" by Flinders Petrie, compiled in 1892. Dr.
Russell was in error, however, when he stated that
the splendid rich blue was a silicate of copper, for the
samples that were submitted to me proved to be cobalt,
and upon investigation I found that A. W. Hoffman
demonstrated that the blue frits of the time of Rameses
III were painted with cobalt.
Nearly everyone has made the popular error of
assuming that the Egyptians used the white of egg
as a binder for their pigments. I cannot find any
trace of any albuminous binder in the pigments sub-
mitted to me, but they do show some evidence of the
use of glue or gelatine. It is well known that the
Egyptians manufactured very excellent grades of glue
either by boiling parchment or bones and hides of
animals. They were excellent cabinet makers and
used glue very largely in joining pieces of wood. In
the great museum at Cairo there are to-day many
samples of furniture glued together with Egyptian
glue, which are still in excellent condition. It is,
however, more than likely that little or no binder was
used when the pigments were applied on the various
tombs, even to those built about 1500 years later,
like the Temple of Karnak. We all know that the
climate of Egypt is exceedingly dry and therefore
no rain can wash off or disintegrate a cold water paint
made by means of pigment and glue. The Nile clay
and Nile mud largely used in building are slightly alka-
line and in many respects similar to the adobe mud
in New Mexico and Arizona. This mud contains a
small percentage of free lime, and any earthy sub-
stance which contains free lime will' in time act like
a weak cement and become firmly bound. It is there-
fore my opinion that many of the decorations made
by the Egyptians were made without any binder other
than the lime naturally found in the soil, and in a
few cases glue was used. I also judge, from the nature
of the implements used, that the pigments were
rubbed into the surface and they in time became part
of the surface.
I do not refer to the splendid decorative work in the
wooden sarcophagi when I say little or no binder was
used, for in these coffins and on the outside of the
linen wrappings there are some reaily wonderful decora-
tive paintings in which binders were used. The por-
traits outside of the mummy wrappings in the second
century were done with wax and resins and are excel-
lent works of art, although these paintings have nothing
to do with the pigments of the Tomb of Perneb.
320 Fifth Avenue
New York City
THE PREPARATION OF N/100 PERMANGANATE
SOLUTIONS
By J. O. Halverson and Olaf Bbrgsoi
Received August 1", 1917
The preparation, standardization and conditions
iii olumetric analysis of N and .V, 10 solutions.
oi potast permanganate have been studied with
LJnforl innately, how > tin of the
lUtions which have thus been shown to l"1 neces-
' See Gooch's "Mi-tliii'i I il Vnol Ed . New York.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. Xo. 2
sary for accurate work have been commonly neg-
lected in the literature, even in handbooks of general
and applied analytical chemistry. As a result of this
and of the widening application of permanganate
titration methods, especially in biochemistry, certain
methods based on this principle have been recently
suggested which possess unnecessary inaccuracies.
Common errors are the use of too much sulfuric acid
in titrations and a lack of appreciation of the great
sensitivity of permanganate solutions to traces of or-
ganic matter. In the determination of very small
amounts of substance, as, for example, in the estima-
tion of calcium as oxalate in small portions of biological
fluids1 where permanganate solutions approximately
N/100 must be used, the elimination of these sources
of error is a necessity.
Where a standard permanganate weaker than N/10
was desired it has been customary to make this shortly
before using by dilution of a stronger permanganate
solution,2 in spite of the fact that ordinary distilled
water contains appreciable amounts of organic matter
which can be removed only with great difficulty.
For instance, we have found that water redistilled
from both acid and alkaline permanganate may still
cause an appreciable deterioration (as much as 2 or
3 per cent) when used in diluting permanganate from
N/10 to N/100. This was true even where the weak
solution was used at once. If allowed to stand for
any length of time, or if less carefully distilled water
was used, the permanganate was almost entirely de-
composed, this process being hastened by the catalytic
action of theoxifies of manganese which were formed.
To avoid the inconvenience as well as inaccuracy
of dilution we have endeavored to prepare permanent
N/100 solutions. The principle used is not new,
but the technique as we have adapted it and some
data pertaining to the keeping qualities of dilute
permanganates and of oxalic acid solutions used as
standards may be of interest.
PREPARATION OF N/lOO POTASSIUM PERMANGANATE
Dissolve 0.40 g. pure potassium permanganate
crystals in one liter of redistilled water in a thoroughly
clean Florence flask which has been rinsed with the
same water. Digest at or near the boiling point for
36 hrs. A funnel covered with a watch-glass may be
used as a reflux condenser. Cool and allow to stand
over night. Without disturbing the sediment of man-
ganese oxides, filter with gentle suction through a 3-in.
Buchncr funnel lined with ignited asbestos. Both
funnel and filter flask should be rinsed with redistilled
water. Transfer the permanganate solution to a
glass-stoppered bottle free from traces of organic
matter. The solution should be kept in the dark
when not in use. If the asbestos becomes clogged
with oxides these may be dissolved out with hot con-
centrated hydrochloric acid, followed by washing
with redistilled water without disturbance of the pad.
After standing two or three days this permanganate
solution may be conveniently standardized
1 Halverson and Bcrgcim, J. Biol Chem., i* (1916), 22; 29 (1917),
J37; Halverson, Mohlcr and Bcrgcim. J. Am. Med. Assn., 68 (1917). 1309.
•Sec Michaelis, Bwihem. Z., 69 (1914). 166. and Ellinger, Z. physiol.
Chem., 38 (1903). 192. for example.
N/50 oxalic acid (0.1261 g. pure crystals to 100 cc.)
or sodium oxalate of similar strength. To 10 cc. of
the oxalic acid solution add 10 cc. of 10 per cent
sulfuric acid which has been treated with just sufficient
permanganate solution to give it a faint pink color.
Place in a water bath at 65 ° C. for a few minutes.
Then titrate at once to a definite pink color which per-
sists for at least a minute. Correct for the blank ob-
tained by titrating 10 cc. of the sulfuric acid and the
same volume of water to the same end-point.
If kept in a'dark place, the oxalic acid solution used
in standardization does not lose appreciably in strength
in from ten days to two weeks. Ordinarily the per-
manganate solutions after they have stood several
days will not vary over 0.1 per cent per week (see
Table I). On account of the sensitivity of the re-
agent it is, nevertheless, desirable to check it up
rather frequently. This also serves as a control on
technique.
Table I — Permanency of Permanganate Solutions, etc.
Cc. Perman-
ganate Re-
quired for
Definite
Volume
Age of Oxalic
No. Solution Solution Acid
1. A7100 Potassium Permanganate. . . 10 days 20.14
23 days 20.20
148 days 20.62
185 days 20.65
386 days 21.05
2. AT/75 Potassium Permanganate 2 days 11.88
5 days 12.04
15 days 12.15
2. Separate Bottle 2 days 11.81
223 days 11.99
3. AV50 Potassium Permanganate 1 day 8.14
6 days 8.17
19 days 8.25
47 davs 8.31
68 days 8.45
125 days 8.50
180 days 8.55
4. AY80 Potassium Permanganate (by
direct dilution of AY 10) Theoretical 13.70
15 minutes 14.20
5. N/100 Potassium Permanganate (by
direct dilution of A'/ 10) Theoretical 17.50
15 minutes 17.83
6. Same as Sol. 5 Theoretical 1 7 . 50
15 minutes 17.81
7. Same as Sol. 5 Theoretical 17.43
1 5 minutes 1 7 . 69
1 day 17.77
2 days 18.18
8. Oxalic acid 0.1101 g./lOOcc. (0.0175
normal) 1 hour 20.62
18 days 20.58
22 days 20.47
72 davs 18.06
9. Oxalic acid. 0. 1101 g./lOO cc 1 hour 20.54
11 days 20.62
14 days 20.62
10. Oxalic acid, 0. 1101 g/100 cc 1 hour 8.34
6 .lavs 8.32
10 days 8.30
14 days 8.23
19 days 8.27
The solutions on which the above data were
obtained were kept away from the light except while in
use. Solutions i and 3 were used almost every day.
They were kept at room temperature throughout one
summer and in the case of Solution 1 two summers.
In the dilution tests redistilled water was used.
CONCLVSI
The preparation of weak permanganate solutions
by direct dilution is inaccurate and inconvenient. By
means of the procedure outlined in this paper N/100
potassium permanganate solutions may be prepared
which will retain their strength and usefulness for an
indefinite period.
Department of Physiological Cum
jbkfbrson medical college
Philadelphia. Pa.
Feb., 1918
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
THE USE OF MICROORGANISMS TO DETERMINE THE
PRESERVATIVE VALUE OF DIFFERENT BRANDS
OF SPICES'
By Freda M. Bachmann
Received July 25, 1917
In a former paper2 the sensitiveness to spices of
several microorganisms was discussed. In my work
at that time I used only one brand of spice. Further
studies with spices from different sources gave results
widely divergent and indicate that the sensitiveness
of one or more microorganisms to a spice may be a
criterion of its preservative value.
ORGANISMS
The organisms used for this study were various
species of bacteria, yeasts and molds. The bacteria
were Bacillus subtilis, Bacillus coli, Bacillus prodigiosus,
and Sarcina lutea. Five yeasts were used, one of
which was isolated from the commercial yeast foam,
another from Fleischmann's compressed yeast. The
other three were old laboratory cultures of Saccharo-
myces cerevisiae, Saccharomyces ellipsoideus, and
Saccharomyces anomalus. Professor E. M. Gilbert has
very kindly examined cultures of the molds and finds
them to be Aspergillus niger van Tieghem, Penicillium
glaucum Link, Rhizopus nigricans Ehrenb., and an
Allernaria which is probably Allernaria tenuis Nees.
METHOD
The methods used for determining the preservative
value of various brands of spices were the same as
those used in my former studies.3 The medium was
sterile, nutrient agar containing a definite amount of
spice. The bacteria and yeasts were grown in test-
tubes, the bacteria on beef broth agar and the yeasts
on wort agar. For the molds a shallow watch-glass
of 1V2 in. diameter was placed inside a Petri dish and
then both were sterilized in the oven. Thaxter's
potato hard agar, consisting of potato broth with 3
per cent agar and 2 per cent glucose, when sterile was
poured into the Petri dish and the same kind of medium
containing a definite amount of spice was poured into
the watch-glass. When the agar in each was thoroughly
hardened it was inoculated with a suspension of mold
spores in water by means of a platinum loop. This
double plate shows the growth on the spiced agar and
also the effect of the volatilized substances on growth
of the organism on non-spiced agar. Unless the
amount of spice used is so great that the growth of the
organism on both the spiced and non-spiced agar is
completely inhibited, the agar without spice outside
the watch-glass serves as a control plate to prove the
viability of the spores used for inoculation. This
double plate method is not recommended as ideal
because there is some slight variation in results which
may be due to the way in which the cover of the Petri
dish fits the lower part. If the edge of the lower part
of the dish is uneven, more of the volatile substance
will escape and permit a better growth of the organism.
1 Published by permission of Director of the Wisconsin Agricultural
Experiment Station.
• Bachmann, "The Inhibiting Action of Certain Spices on the Growth
of Microorganisms," Tins Journal, 8 (1916), 619.
1 Loc. cit.
Unless the plates are kept in a damp chamber, this
unevenness may also allow considerable evaporation
and the resulting drying of the agar may inhibit
growth. It is desirable that the Petri dishes to be
used should be carefully examined to have the covers
fit well. With this precaution observed, the amount
of variation in the sensitiveness toward spice of the
organisms used for this study has been considered
negligible.
In the study of several brands of spice the molds
were grown in the double plates described above and
also on spiced agar in test-tubes. The following
tabulated results of mold growth are all from Petri
dish cultures. It is seldom that the minimum dilu-
tion of a spice which permits growth is the same in a
Petri dish and in a test-tube. The minimum dilution
is usually somewhat less in a Petri dish. This is
doubtless to be accounted for in the more shallow
layer and the greater surface area of spiced agar in the
Petri dish which results in a more rapid loss of volatile
substances.
For the results given in this paper only the ground
spices were used. Spices of different brands were
obtained from various sources.
In the following table are given the results obtained
after inoculating potato agar containing various
amounts of cloves with suspension of mold spores in
water. The different brands of cloves are given as
A, B, C, D, and E. The results are from cultures on
agar in Petri dishes as described above. In my
former paper attention was called to the difference in
sensitiveness to spice of the mycelial filaments and the
spores of molds. This phenomenon has been frequently
observed in the Petri dish cultures. There is often no
growth on the spiced agar until the mold has grown
abundantly on the agar without spice. When the
filaments reach the sides of the watch-glass they grow
upward and over the edge of the watch-glass and on
the spiced agar. In the following table such a growth
of the mycelium is indicated by the letter m. It may
be observed that such mycelial growth is frequently
given for Rhizopus, only once for Allernaria, and not
at all for Aspergillus and Penicillium. This is not
to be interpreted as an equal sensitiveness of the
mycelium and spores of Allernaria, Aspergillus, and
Penicillium. It is explained by the fact that in
Rhizopus the mycelium produces a more vertical
growth and thus is much above the surface. These
filaments readily grow over the sides of the watch-
glass embedded in the agar. In Allernaria , Aspergillus,
and Penicillium the growth is more horizontal and
close to the substratum. The same growth of the
mycelium of Allernaria, Penicillium, and Aspergillus
from non-spiced to spiced agar has been frequently
observed in such plates as were described in my former
paper1 where the non-spiced and spiced agar is in
contact.
It will be observed from Table I that cloves A and
B are much more effective in inhibiting growth than
C, D, and E. The species of Rhizopus which I have
used appears to be more sensitive to cloves than any
1 Loc. cil.
THE JOURNAL Of INDUSTRIAL AND ENGINEERING I II I. MIST RY Vol. 10. Xo. 2
Tabu; I — Effect OS I mfphrhnt Brand: d Growth
Dilutii d Brand Brand Brand
Mold pice A B C 1 > E
Rhizopus nigricans 1 : 25 0 0 0m m
.SO (I II m + +
inn 0 0 m + +
.'on m m + + +
400 .. + + + +
Alternaria tenuis I : 25 0 0 0 0 m
ill 0 0 0 + +
loo 0 0 + + +
+ + + +
300 + + + + +
PenicMium glaucum 1 : 25 0 0 0 0 +
50 0 0 + + +
loo
0
+
+
200
+
+
+
400
+
+
+
1 : 25
0
0
+
50
0
0
+
10(1
0
+
+
200
+
+
+
400
+
+
+
of the other organisms and the Alternaria is more
sensitive than the species of PenicMium ami Asper
villus. This is in agreement with my earlier studies
in which I found that Rhizopus ami Alternaria were
more sensitive to eugenol than PenicMium and Asper-
gillus.
Brands A and B inhibit growth in the Rhizopus in
dilutions up to 1:300 or greater in Petri dish cultures.
With Brand B a dilution of 1:3°° greatly retards
growth but after a mycelium is produced it grows
fairly well. When grown in test-tubes a dilution of
1 : 400 is probably near its maximum tolerance for
this brand of cloves. With this dilution I failed to
get growth several times bu1 a1 and her time succeeded.
With Brands D and E the organism always grows
well in a dilution of 1: 50 in Petri dish cultures.
In Table II are given the results of inoculating wort
agar containing cloves in dilutions from 1 : 25 to
1 : 400 with yeast. There is very little variation in
nsitiveness to cloves in the different strains of
yeast which I have used. Brand A is again the most
effective in inhibiting growth and Brand E least
effective.
Table II — Effect of Different Brands of Cloves on Yeast Growth
Dilution Brand Brand Brand Brand
Yeast of spice A B C E
Yeast Foam — culture from 1 : 25 0 0 0 0
50 0 0+ +
[i ii i 0 0 0 +
200 0 + + +
■1011 + + + +
Fleischmann's compressed — cultt
from
■ myces cerevisiae.
Soccharomyces ellipsoideus.
Saccharomyces anomalus. . . 1
1 : 25
50
loo
100
. 1 : 25
50
loo
00
1 : 25
...
loo
■ inn
0
0
0
0 +
+ +
+ +
-50
Kill
400
[n Table 111 a the results of inoculatii
broth agar containing cloves in dilutions from i : 50
to 1 : 400 with four species 0 The brands
of spice vary in their preservative value in the same way
as they were found to vary when molds am!
were used. Brand A has the greatest preservative
value, next Brands B and C, and Brand E least of all.
As with molds, there is likewise considerable variation
in sensitiveness among bacteria to any one brand of
spice. In my former studies I found B. sublilis to be
very sensitive to cloves. This fact has been fre-
quently observed in the presc: >'■■ prvdigiosus,
on the other hand, has considerable resistance to
cloves.
Table III — Effect op Different Brands of Cloves on Bacterial
Growth
Dilution Brand Brand Brand Brand
Organism of spice A B C E
B. sublilis
100
200
300
400
B.coli 1 : 50
100
200
3O0
400
B. prodigiosus 1
0
0
+
Sarcina lulea 1
+
+ +
0 +
+ +
+ +
+ +
+ +
0 +
0 +
+ +
100 0
200 0
300 +
400 +
50 0
100 0
200 0
300 0
400 + + + +
A similar study has been made with a few brands of
cinnamon and of allspice. In Tables IV and V are
given the results of this study.
Table IV — Effect of Different Brands of Cinnamon on the Growth
of Molds and Bacteria
Orcanism of spice
Alternaria lenuisU) ' : 25
Brand Brand Brand
Rhizopus nigricans 1
Aspergillus niger 1
B. sublilis 1
B.coli 1
B. prodigiosus 1 : 25
0
0
0
+
0
+
+
+
+
+
0
+
+
+
+
+
0
0
0
+
+
+
It may be seen from Tables IV and V that g
of the above species of m ml yeasts has
varied little on media containing different brands of
allspice and cinnamon. Although the brands of all-
spice and cinnamon which I have used are thus more
nearly equal in preservative value than the different
brands of cloves, yet it is quite evident that Brand A
of both cinnamon and allspice has considerably more
preservative value than Brand B or Brand C.
It is desirable that tile test organism used in de-
termining the comparative antiseptic values of differ-
i spice be [airly the spice so
that high dilutions of . uld be used.
Here again, as in my former studies. I have found
that Rhizopus nigricans is not very sensitive to cinna-
mon. Aspergillus nigcr is somewhat more sensitive
to this spice than the Rhizopus and shows nicely the
difference in the preservative value of the different
brands that I have used. Rhizopus grows so readily
Feb., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
123
Table V — Effect of Different Brands of Allspice on the
of Molds and Yeasts
Growth
Dilution Brand Brand
Organism of spice A B
Brand
C
Allernaria tenuis(?) 1 : 25 0 0
Rhizopus nigricans. 1
spergillus niger 1
Yeast Foam — culture from 1
Fleischmann's compressed — cultu
Saccharomyces cerevisiae. . . I
Saccharomyces ellipsoidcus 1 : 25
Saccharomyces anomolus
on media containing cinnamon that it shows no
difference at all between Brands B and C in the dilu-
tions used. Penicillium, on the other hand, is very-
sensitive and in dilutions up to i : ioo showed no
difference in the brands used for the results tabulated
above. It may be that some species of Aspergillus
would, by its growth on media containing cinnamon,
show the comparative preservative value of many
brands. It is highly probable that other organisms
may be found which will serve the purpose even
better than these which I have used.
Some observations have been made on the varia-
tion in sensitiveness of two other strains of Rhizopus.
For the results given in this paper I have used a
culture of Rhizopus nigricans which I have designated
No. 4 in my cultures. It produces a very vigorous
growth on culture media and grows much more readily
on media containing some kinds of spice than a plus
strain of Rhizopus nigricans. With a dilution of
i : 7500 of cinnamic aldehyde. I found when I used
Rhizopus nigricans No. 4 that there was scarcely any
retardation of growth. With a minus strain of
Rhizopus nigricans growth was somewhat delayed, but
later quite vigorous, while with the plus strain there
was no evidence of germination of the spores even
after incubating the culture for a week. Using a
1 : 600 dilution of three brands of cloves, I found the
plus strain of Rhizopus nigricans somewhat less
sensitive to this spice than the minus strain.
It is again evident from the data recorded above that
there is considerable difference in sensitiveness of any
one organism to the different spices and also that no
one spice has an equally inhibiting effect on the growth
of different organisms. This makes it difficult to
determine the minimum amount of spice necessary to
preserve any food product. It is necessary that
further data OB the effect of spices on other organisms
be obtained. That, of the different spices, cinnamon
is the most generally effective as a preservative, as I
stated earlier,1 does not seem to have 1
Results of further study with different brands of spice
1 Lot. cit.
indicate that cloves may be just as effective as cinna-
mon. The best grades of these spices certainly exert
a very considerable preservative effect, and although
the amount used in flavoring a food product may not
be sufficient to preserve it from spoilage, yet it
may be a large factor in its preservation.
CONCLUSIONS
Molds, yeasts and bacteria show a marked varia-
tion in sensitiveness to different brands of spices.
The amount of growth of such organisms in a given
time on media containing spice may be used as a
means of determining the relative preservative values
of the different brands of the spice.
SUMMARY
Microorganisms have been used to determine the
preservative value of different brands of spices.
Spices of molds, yeasts and bacteria were grown on
nutrient agar containing varying amounts of spice.
Tabulated results of such a study using five brands of
cloves, three of cinnamon, and three of allspice are
given. The results show that there is considerable
variation in the preservative value of the brands used
and that the growth of microorganisms on a spiced
medium may be used as a criterion of the preservative
value of the brand of the spice.
Bacteriological Laboratory
Agricultural College
Madison, Wisconsin
DISINFECTION WITH FORMALDEHYDE
A SUBSTITUTE FOR THE PERMANGANATE-FORMALIN
METHOD
By C. G. Storm
Received December 7, 1917
The method proposed by H. D. Evans and J. P.
Russell in 19041 for the rapid liberation of formalde-
hyde gas from its water solution, the "formalin" of
commerce, in a condition suitable for practical dis-
infection, has been found by numerous investigators
to be superior to most of the other known methods of
formaldehyde disinfection, as regards simplicity,
rapidity, cost and efficiency. This method consists
in pouring the formalin quickly upon crystals of
potassium permanganate contained in any suitable
metallic vessel (for example, a water bucket), the
oxidation of a part of the formaldehyde furnishing
sufficient heat to cause rapid evaporation of the re-
mainder of the formaldehyde together with the water.
The permanganate method has found very general
application and is widely used in this country in
tion work. Its use has, however,
received a serious set-back by reason of the present
scarcity of potassium permanganate and the resulting
e cost of this chemical. Prior to the war in
Europe, potassium permanganate was obtainable in
this country at prices ranging usually from 9 to 10
cents per lb. It is now obtainable only at many
1 II, I). Kvans and J. P. Russell, "Formaldehyde Disinfection," 13lh
Ann. Kepi tat B I "I Health of Maine, and /. Am. Chem. Soc, 87
(1905), 714. See also Daniel Base, "Formaldehyde Disinfection," J.
Am. Chem. Soc, 88 (1906), 964-96.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No.
times its former price, having held at approximately
$4.00 to $4.25 per lb. for the past six months.
This fact has impressed the writer with the de-
sirability of publishing a note regarding an analogous
method for generating formaldehyde, devised by him
in October, 191 1, which it is believed has never been
proposed for practical use, which preliminary tests
indicate to be safer, as rapid, and almost as s<mple of
operation, and which will be much less expensive,
owing to the relatively low price of the material used.
The new method depends upon the action between
the water solution of formaldehyde and a soluble
chlorate, and is apparently analogous to the per-
manganate method, in that the oxidation of a part
of the formaldehyde furnishes a sudden evolution of
heat which serves to vaporize the remainder of the
formaldehyde. It was suggested to the writer in the
course of analysis of a potassium chlorate explosive.
On adding formalin to the water solution of the ex-
plosive and heating the mixture, a violent evolution
of gas resulted , increasing in intensity even after the
tube containing the mixture was removed from the
flame of the burner. The gas evolved was largely
formaldehyde, apparently liberated from its solution
by the heat generated in the oxidation of a part of the
formaldehyde by the chlorate.
An examination of the solution remaining after the
reaction had subsided, showed the presence of large
amounts of chloride which had resulted from reduction
of the chlorate. Repeated trials showed that the
violent evolution of gas resulted only from concen-
trated solutions, but that the reduction of the chlorate
to chloride, with a corresponding oxidation of formal-
dehyde, took place even in the case of very dilute
solutions of chlorate. It has been demonstrated that
under proper conditions this reaction is quantitative,
and the results of the study of this quantitative method
for determining chlorates will shortly be published.
The object of this paper is merely to call attention
to what it is hoped will be a satisfactory substitute for
the permanganate method of disinfection, and to
offer an opportunity for a more complete study of the
method, the writer's investigation having necessarily
been quite incomplete because of lack of time and
facilities for conducting work of this nature.
Potassium permanganate reacts immediately on
coming in contact with formalin at ordinary tempera-
tures, and if the permanganate is finely powdered
instead of crystalline, the reaction may be violently
explosive in character.1 If formalin is poured on
crystals of sodium or potassium chlorate, no action
results until the mixture is warmed by application of
external heat to about 650 C. This may be considered
as a disadvantage, but as a matter of fait the 1
may be started with very little difficulty. The chlorate
and formalin are placed together in a suitable metal
container, such as a water bucket, of sufficient size to
prevent the reaction mixture from foaming over, and
the bucket, properly weighted so it will not float,
placed in a large shallow pan (an ordinary dish pan
' G. B. Frankfortcr nnd R. M. West. J. Am. Chrm. Soc. S8.0906).
1234.
will answer the purpose) containing water heated to
about the boiling point.
The mixture becomes heated to the reaction tem-
perature in a few minutes, when bubbles of gas begin
to be evolved, this evolution increasing rapidly until
it is so violent that the mixture may foam over the
top of the bucket. The action is completed in 2 or 3
min., and with the proper proportion of chlorate and
formalin the residue remaining in the bucket is prac-
tically dry and consists chiefly of chloride together
with some unreduced chlorate.
Sodium chlorate seems to give just as satisfactory
results as potassium chlorate, and has the distinct
advantage of costing less than one-half as much as the
latter. Potassium chlorate is now quoted at 50 to 55
cents per lb., while sodium chlorate is listed at 24 to
25 cents.
Several investigators have attempted to determine
what proportion of formaldehyde used in the perman-
ganate process is liberated as gas and what proportion
is oxidized by the reaction. Frankforter and West1
obtained an evolution of 62 per cent to 75 per cent of
the formaldehyde from formalin by this process in a
long series of experiments under laboratory conditions,
using glass apparatus and absorbing the evolved gas
in water, the strength of the resulting solution being
determined. D. Base,2 in experiments with the pro-
cess on a practical scale, used a specially prepared
room of 2,000 cu. ft. capacity, determining the amount
of formaldehyde gas in the room by drawing 5 to 10
liter samples through standard KCN solution, adding
excess of standard AgN03 solution and titrating the
excess of the latter with sulfocyanate. Base found
that not over 40 per cent of the total amount of formal-
dehyde used as formalin was evolved in the state of
gas in the room.
It has been suggested that the reaction between
formaldehyde and potassium permanganate is prob-
ably as follows:
4KMnO, + 3HCHO + H;0 = 4Mn(OH), +
2KcCO, + CO,
It is, however, likely that other reactions proceed at
the same time, in which part of the formaldehyde is
oxidized to formic acid. Assuming this reaction,
however, it is calculated that with the proportions
recommended by Evans and Russell (100 cc. of 40
per cent formalin to 37.5 g. KMnO<) 5.34 g. of for-
maldehyde, or about 13.35 per cent of the formalin,
would be oxidized by the KMnO,. With the pro-
portions recommended by Base i^ioo cc. of formalin
to 50 g. KMnO<) 7.12 g. HCHO or 17. S per cent of
the formalin would be destroyed. These figures are
considerably lower than tl found in the investiga-
tions mentioned above. In any event it is apparent
that in the permanganate process a considerable part
of the formaldehyde used as formalin is destroyed by
oxidation, the reaction supplying the heat which
causes the rapid volatilization of the remainder.
It may be assumed that the behavior of the chlorate
with the formalin is entirely analogous to that of the
' J. Am. Chtm. Soc. M (1906), 1234.
I Ibid., 28 (1906). 964.
Feb., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
125
permanganate, and that the reaction occurs according
to the equation
2KCIO3 + 3HCHO = 2KCI + 3H0O + 3CO2.
Experiments have shown that the proportion of 25
g. of chlorate to 100 cc. of formalin is approximately
the one giving best results, that is, with these pro-
portions there is practically no liquid left in the residue
after the reaction subsides, the formaldehyde being
either driven off as gas or oxidized and the water
evaporated at the same time.
A simple calculation shows that, according to the
above reaction, 25 g. KCIO3 will theoretically oxidize
9.18 g. HCHO or nearly 23 per cent of the formal-
dehyde in the 100 cc. of formalin, leaving the re-
maining 77 per cent to be volatilized. It is probable,
however, that other reactions occur, such as
KCIO3 + 3HCHO = KC1 + 3HCOOH.
In fact, appreciable amounts of formic acid, as well as
CO2, are evolved by the reaction of formalin with
either permanganate or chlorate.
In an attempt to determine in a simple manner the
best proportions of formalin and chlorate, a series of
roughly quantitative experiments were made, using
varying proportions of the two materials. A weighed
amount of powdered KC103 was treated in a beaker
with a weighed amount, of the 40 per cent formalin
and the beaker immersed in hot water in order to start
the reaction. The residue left in the beaker after the
reaction had ceased was dissolved in water and titrated
with standard solution of silver nitrate to determine
the amount of chloride present. From the amount of
KC1 found, the weight of formalin representing the
formaldehyde destroyed in the reduction of KCIO3
to KC1 was then calculated from the reaction
2KCIO3 + 3HCHO = 2KCI + 3C02 + 3H20.
The results of these tests are shown in the following
table. It is to be noted that if the reaction
KCIO3 + 3HCHO = KC1 + 3HCOOH
is assumed, the calculated amounts of formaldehyde
consumed will be just twice those given in the table.
Tkst3 op Residue Remaining after Reaction between Formalin
and Potassium Chlorate
HCHO oxi- Formalin (40%)
KClOt Formalin Calc. KClOi dized (equiv. equiv. to HCHO
Test Used Used Reduced to KC1 found) oxidized
No. Grams Grams Grams Grams Grams
1 7 12 3.917 1.439 3.59
2 6 12 3.817 1.402 3.50
3 6 12 3.620 1.329 3.33
4 5 12 3.750 1.375 3.44
5 4 12 3.726 1.369 3.42
6 3 12 2.990 1.098 2.75
2 12 2.010 0.738 1.85
In Tests 5 and 6 a very small amount of liquid
remained in the residue after the reaction; in Test 7 an
appreciable amount of liquid remained and a de-
termination of formaldehyde showed 1.104 g. HCHO,
equal to 2.76 g. of 40 per cent formalin. In Tests 1
to 5, inclusive, where the weight of KClOj was at least
one-third of the weight of the formalin, the amount of
HCHO oxidized was fairly constant, the KC1 found
indicating that only part of the KCIO3 had been
reduced. In Tests 6 and 7 the excess of formalin
was such that practically complete reduction of the
chlorate was effected and the amount of formalin
oxidized much less.
A number of qualitative tests were made using
formalin and sodium chlorate in proportions varying
from 6:1 to 2:1, the maximum temperatures
reached during the reaction being noted. With the
ratios 2 : 1, 2.5 : 1, and 3:1, this temperature was
108-109 ° C., while with lower proportions of chlorate
(4 : 1 and 6:1) the temperature was slightly less,
104° to 105° C. In each case the reaction started
at 60-65 ° C., was violent at about 75 ° C, and lasted
only about 30 seconds, the maximum temperature
being indicated near the end of the reaction.
The writer hopes that comparisons of the actual
disinfecting efficiencies of the permanganate and
chlorate methods will be made by those who may be
interested in the practical side of the question and that
the chlorate method may be found to be of some use.
Ordnance Department, U. S. R.
Washington, D. C.
EFFECT OF FERTILIZERS ON HYDROGEN-ION
CONCENTRATION IN SOILS1
By F. W. Morse
Received September 29, 1917
Most of the fertilizer plots at the Massachusetts
Agricultural Experiment Station have been con-
tinuously treated for more than 25 years, and there
are marked differences in their crop-producing powers,
which in some instances appear to be due to chemical
or physical changes in the soil and not to a deficit
of the usual constituents of a fertilizer.
Among methods of investigating these soils, the
measurement of the hydrogen-ion concentration in
water extracts of the soils has given some interesting
results.
The method of procedure has been as follows:
25 grams of air-dry soil were weighed into an Erlen-
meyer flask of 300 cc. capacity, and 250 cc. distilled
water were added. The flask was repeatedly shaken
during a period of an hour, and then the mixture was
filtered through a dry paper filter. The first portions
of the filtrate were usually cloudy and were returned
to the soil flask. When the paper became well coated
with soil, the filtrate would, as a rule, be clear, with
the exception of some limed samples which would
persistently retain a slight turbidity from clay. The
soil and water were in contact for about 3 hours before
filtration was completed.
The colorimetric method was used for determining
the hydrogen-ion concentration. The range for the
soils was found to be covered by the indicators methyl
red, paranitro phenol and rosolic acid. The standard
salt mixtures used were Walpole's2 acetic-acid-sodium-
acetate mixture, Sorensen's* mono- and dibasic phos-
phates, and Clark and Lubs'4 mixture of monopotassium
phosphate and sodium hydroxide. The last named
covers practically the same range as Sorensen's and
is much more convenient to prepare.
1 Presented before the Fertilizer Division, at the 55th Meeting of the
an Chemical Society. Boston. September 10 to 13. 1917.
' Biochem. J.. 1914; J. Chem. Soc. 1914.
' Ergebnisse Physiol . 1912.
' J. Biol. Chem., 26 (1916). 504.
126
THE JOURNAL OF INDUSTRIAL AND ENGINEERING ' HEMISTRY Vol 10, No. 2
Ten cubic centimeters of the soil solution were com-
pared with an equal volume of the standard mixture
appropriate for the concentration of hydrogen ions
in the former. Small porcelain dishes served the
purpose for comparisons in nearly all cases, bu
hen necessary to check doubtful results.
The 1 tilizers that had been used on the
investigation were acid phosphate, nitrate
of soda, muriate of potash, sulfate of potash, double
sulfate: of ammonia,
land pli ':.', ri cultural lime.
The range of II etween
I'm 1 5 and >'n 7-o-
Neutral salts of strong bases and strong
sodium nitrate, potassium chloride, potassium sul-
fate, calcium sulfate, produced little, if any, effect
on the ion, in comparison with unfertilized
soil. The acid phosphate, a strong base
moderately weak acid, behaved like the neutral salts
just mentioned. Sulfate of ammonia behaved like a
weakh d and carbonate of lime like a weakly
ionized base, and the extremes of the range were always
due to these two compounds.
When agricultural lime was used in conjunction
with the other chemicals, it was noted that plots
dressed with nitrate of soda or calcium sulfate re-
tained the neutralizing effect of the carbonate of lime
longer than the plots receiving potash salts, probably
through a protective effect on the solution of the lime
as bicarbonate. I have not yet demon
point, however.
The effei I oi an application of 2,000 lbs. of hydrated
lime per acre is perceptible on the crop and on the
soil reaction for several years, but ultimately dis-
appears, probably due to both leaching and trans-
formation, but apparently due more to the former.
The comparative results obtained during this se
investigation of our plots are as follows:
North South Field A
Acid phosphate. .. l'„ 5 2 I'„ 6.15 Nitrate of soda P„ 6.0
Nitrate of soda. .. . 5.22 6.5 Sulfate of ammonia. . . 4.9
Muriate of potash.. 5.25 6.15
Calcium sulfate ... 5.0 6.65 No nitrogen 5.4
Calcium carbonate. 6.4 7.1
Unfertilized 5.25 5.96 Lime 6.0
Mas qrici i.ti kai. Experiment Station
Amherst, massaoh -setts
THE SEEDS OF THE ECHINOCYSTIS OREGANA
H\ Mn.o RBASON 1 > a
Received I Ictobei 26, 1917
This investigation was made to determine thi
1 ill- indu ;( rial -. alue of tl if 1 lie planl
Echinocystis m more commonly known
Man-in-the- Ground <>r Wild Cucumber.
It is a ] 'ire of which
is its gigantic rool which pen
to 2 meters and may weigh ,}o or more kilograms.
1 Manz,s ami Young3 examined the ■
the Megarrkiza < alifornu <i . a planl belonging to the
ii Echinocystis, and reported on its
pharmaceutical value. Heaney found a bitter gluco-
i Am J. Pharm., 48 (1876), 451.
•Ibid.. S3 (1881
I Ibid , 66 1883), 195.
hich he called megarrhizin. The root of the
Echinocystis is decidedly bitter and is therefore unfit
for food. The Indians are said to use it as a drastic
purge in dropsy.
The fruit, which is borne on slender herbaceous
stems varying in length from 3 to 9 meters, is egg-
shaped. It varies from 25 to 50 mm. in the short'
er and is covered with soft green spines, a fact
which explains the origin of the name "echinos" or
hedgehog. It becomes lighter in color as the seeds
reach maturity, and breaks open at times at the free
end, leaving the seeds more or less exposed. Each
uitains from one to several seeds, which are]
orbicular in shape, averaging 19 mm. in breadth and
half as thick as broad. to fifteen hundred
of the seeds make a kilogram. The thin outer shell '
of the seed is readily broken and hence it is easily
ground in a food chop;-
The Echinocystis is distributed along the Pacific
rom British Columbia to California, growing
ami thriving along railroad tracks, fence rows, in fields,'
ines, and in the foothills. It is
drouth-resistant, maturing its seeds under unfavorable J
conditions. So far as known no attempt has beeni
0 grow this plant in quantity. Bearing in \
mind the character of the root it is readily seen why
sider it a pest,
collected for three successive years had the
following percentage composition:1
Table I
Sample No. I II III
Date of Collection 1915 1916 1917
Ether Extract (Fat) 30.10 34.92 35.45
Protein (N X 6.25) 23.71 20.64 21.54
Starch 9.21 12.05 10.31
Crude Fiber 22.07 21.55 20.01
Moisture 4.04 3.90 4.54
Ash 2.89 2.64 2.60
Samples of oil were prepared by extraction with
mi ether, boiling point 44 to 65 ° C, and by{
expression in the cold from the whole seed previously
ground in a food chopper. The expressed oil was-
thoroughly agitated with fuller's earth from which.
it was separated by means of a centrifugal machine.
The constants of the oils thus obtained were:
Table II
Extracted Oil Expressed On.
Color Golden yellow Olive-green
Specific Gravit) it25°C.).. 0.9267 0.9166
Refractive Index .it 25° C.) 1 4722 1.4701
Solidifying Temperature 4-5to — 8 +5 to — 8
Iodine Number 117.0
Saponification Number 189.1
Judged by these results, the oil from the seeds of
the cottonseed oil group.
The oil tastes like olive oil. Both the extracted and
expressed oils become turbid when cooled to a tem-
poral un the former
le latter is more
Nearly 40 per cent of the 0 is expressed
with the apparatus empl this purpose. The
pressure applied was approxii g per square
centimeter or nearly 1200 lbs. to the square inch.
Freshly ground se& :; color,
which faded in a few days in bright light to a golden.
1 All analyses were made in August. 1917.
Feb., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
127
yellow. Seeds which were ground for two weeks be-
fore pressing gave an oil of greenish red color in re-
flected light and dark olive-green in transmitted
light.
When subjected to hydrogenation at 220 to 240 °
C, with powdered nickel — prepared from nickel oxide
just previous to its addition to the expressed oil —
there was produced a bland yellowish white fat with
a melting point of 29 to 360 C, a solidifying tempera-
ture of 25° C, and an iodine number of 76.6.
Feeding experiments with mice attested the non-
poisonous character of both the original oil and the
hydrogenated fat.
Department of Chemistry
Oregon State Agricultural College
corvallis
VARIATION IN THE ETHER EXTRACT OF SILAGE1
By L. D. Haigh
Received May 26. 1917
Having occasion to repeat the analysis of some
samples of silage 10 months after the first analysis was
made, considerable variation in the samples was
cipally to the presence of acetic acid, and lactic acid.
The former is volatile in a vacuum, the latter is not.
Table III illustrates the determination of the acidity
of silage based on this fact.
Table III — Acidity
of Air-Dry Silage
Total Acidity
Acidity
.4s Lactic Acid
Volatile
Total Acidity
Original After
Vacuo
lage
Air-Dry Drying
Figured as
Acetic and
No.
Silage in Vacuo
Lactic
Acetic
Lactic Acids
1
4.43 4. 13
0.30
0.20
4.33
2
4.78 4.40
0.38
0.26
4.66
3
4.66 4.25
0.41
0.27
4. 5->
4
3.93 3.56
0.37
0.25
3.81
Comparison was made of the acidity of the samples
before and after the determination of moisture and
before and after the determination of the ether ex-
tract, in order to study the effect of the acidity upon
these two determinations. The results are shown
in Tables IV and V. The last column in Table V
shows that water will wash from silage not only the
acid but also other substances soluble in ether.
No attempt is made in this report to explain the
causes for the above variation. Further studies are
being made with a view of ascertaining what these
causes are. We only wish to indicate at this time
that variations do occur in value for ether extract
2/17
3/16
2/17
4/16
4 5 lh
6.02
5.52
6.51
Table I — Analysis of Air-Dry Silage — New
-A — Results in Percentages on Air-Dry Basis
10 Months Later
. B — Results
21.07
19.43
19.40
17.74
20.05
19,53
22.68
21.67
Protein Nitrogen-Free Ether
Ash Nitrogen NX6.25 Extract Extract
5.20 1.32 8.25
56.33
59.75
59.45
61.13
53 . 82
58.85
50.58
55. 15
3.82
2.71
3.98
2.87
5.50
2.93
Crude
Fiber
22.31
20.68
20.53
18.98
21.76
20. 7"
24.46
23.07
6.21
6.09
6.92
6.95
Nitrogen
1.40
1.19
1.19
1.16
1.35
on Dry Basis *
Nitrogen-
Protein Free
N X 6.25 Extract
8.73 59.63
7.45 63.58
7.45 62.92
7.22 65.39
8.41 58.40
7.95 62.39
8.56 54.56
noted. The ether extract in particular showed great
variation, much less being found in the old than in
the fresh silage. Table I shows the comparative
results of the analyses of silage when new and also
io months later. The results show that some factors
entered into the determination when the silage was
fresh which did not appear in the silage io months
later.
Inasmuch as the sample must be dried before the
ether extraction the effect of vacuum and oven drying
on the percentages of moisture obtained was first
studied. The results arc shown in Table IIA. The
effect of vacuum and oven drying on the results for
ether extract are shown in Table II B.
Methods
Moisture
Table II — Results on Air-Drv Basis by Differ!
op Drying
A — Pi Etc] ' 01
Dhvis.. Method USED Silage 1 2 4
Vacuum 6.02 6.51 5.67 6.09
Vacuum + Oven 'IS miii I (, m 6.90 6.18 6.64
Oven (100 to 105° C.) 8.73 9.31 8 71 9.13
B — Percentages op Ether Extract
DKYINO Method Used Silage 12 3 4
Vacuum, before and after Extraction. . . 2.55 2.99 2.71 2.75
• fore and after Extrac. 2.01 2.11 I 90 2.12
Vacuum before, vacuum + oven
Extra. Imn .'87 3.27 2.94 3.06"
I' wa , idity of silagi
some part in the v for moisture
and ether extract. The acidity of silage is due prin-
1 Presented at the 54th Meeting of tin- American I hernial Society,
Kansas City. April 10 to 14, 1917.
depending upon changes in the sample itself on standing
and upon the drying operations employed.
It is evident that the analyses should be made as
Table
IV — Effect of
Acidity of
Air-Dry Silage upon
M
DISTUR
Determi
nation
Acidity of
Silage
Acidity
% Loss on
% Mixture
Original
After
Volatilized
Drying at 100°
After
By
Air-Dry
Drying
.4 cetic
Moisture
Deducting
Vacuo
Silage
Acetic &
at 100°
and
and Some
Volatilized
Cor-
No.
Lactic
Lactic
Lactic
Acidity
Acidity
rected
, ,, f
1.80
2.53
8.78
6.25
1.89
2.44
8.68
6.24
5.82
, « <
1.89
2.77
9.39
1.97
2.69
9.24
6.55
6.25
. =,)
1.88
2.64
8.68
6.04
1.75
2.77
8.75
5.98
5.40
1.61
2.20
9.11
6.91
1.56
2.25
9.15
6.90
5.84
Effect of Acidity of Air-Dry Silage upon the Deter
tion of Ether Extract
Acid
Acidity as Lactic
Of Air-Dry Of Residue
Silage after after
Silage Drying Extraction
No. in Vacuo with Ether
4. 13
3 4.25 j
4 3.56
3.47
3.4S
3.69
3 t,\
3.04
3.06
traded
by
Ether
0.66
0.68
0.71
0.77
0.63
i) 63
0.52
0.50
Total
Ether-
Soluble
Material
Pound
2. S3
2.56
2 . 90
3.08
2.88
2.55
2.70
2.80
Ether
Less
Ether
Soluble
Acidity Water
1.87
Extract
After
Washing
1 .
2. 19 |
2.31 I
2.25
1.76
1.50
1.30
""■I as po isible after the feed is used and I ba1 a uni
form method of drying be employi i varia-
o ii i lided .
.Kicui.TiiKAL Experiment STATU
Columbia. Missouri
128
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 2
LABORATORY AND PLANT
SOME METHODS OF ANALYSIS FOR NEBRASKA
POTASH SALTS AND BRTNES
By A. H. McDowell
Received October 29, 1917
The so-called Nebraska potash salts consist of
alkali carbonates, sulfates, and chlorides in varying
proportions, with a small amount of Si02 (usually-
less than 0.3 per cent), a small amount of organic
matter, and moisture from o per cent up.
These salts are produced by evaporating to dryness
the brines (salines) obtained from wells driven into
the beds of certain alkaline lakes in the Sand Hills
section of western Nebraska. They are largely used
in the manufacture of fertilizers and are of value on
account of the potash occurring in them, the price
per unit K20 (per cent per ton of 2000 lbs.) being the
basis on which they are sold.
The determinations most frequently called for
are K20 and moisture at 1200 C. and the potash con-
tent of the commercial product is rarely less than 20
per cent or more than 30 per cent. Complete anal-
yses are not needed in connection with sales, but
furnish useful information for investigations and de-
velopment work.
The analysis of brines is essential principally in
connection with prospecting for new sources of sup-
ply. In this connection it is of interest to note that
the composition of mineral solids is not necessarily
constant in different parts of the same lake, or in fact
at different depths in the same well, and that the per-
centage of solids may vary widely in samples from
wells driven in different parts of the same lake. The
usual analysis includes specific gravity, mineral solids,
and the content of the solids in K20, CI, and alkalinity
as Na2C03. In general, the alkalinity will be found
between 45 per cent and 80 per cent and in most cases
a relatively high alkalinity is accompanied by rela-
tively low K20 and vice versa.
The details of the following methods of analysis
have been developed during several months' experience
with these materials. The platinum chloride method
for K20 is given preference because it is simple, ac-
curate, and official with the A. 0. A. C, and because
of the ease with which both platinum and 80 per cent
alcohol may be recovered.
METHODS FOR COMPLETE ANALYSIS OF SALTS
moisture — A 10 g. sample (30 mesh) is dried at
1200 C. to constant weight. Two hours are usually
sufficient. Weigh to the nearest milligram.
K20 (modification of the official lindo-gladding
method) — A 5 g. sample (30 mesh) is dissolved in
500 cc. of water and 20 cc. (0.20 g.) are taken for a
determination. The portion for analysis is measured
into a porcelain or platinum dish and 2 cc. of 1/1
sulfuric acid are added carefully to avoid spattering.
Evaporate the water on the steam bath and con-
tinue the evaporation over the flame very cautiously
to drive off H2SO«, finally heating every part of the
dish to redness to destroy all organic matter and de-
compose bisulfates.
Cool the dish and add a drop or so of concentrated
HC1 and about 10 cc. of water from a wash bottle,
washing down the sides of the dish. Warm to com-
plete solution of salts and filter through a small paper
(to remove Si02) into another dish. Wash the paper
thoroughly with hot water.
Add 2 cc. 10 per cent platinum solution for ma-
terial carrying up to 20 per cent K20, or 3 cc. for material
carrying up to 50 per cent. Evaporate on the steam
bath to a pasty mass (that will solidify on cooling).
Wash the precipitate six times with 80 per cent
alcohol, using 4 or 5 cc. each time and pouring the
washings through a tared Gooch crucible. During
each washing rub the precipitate hard with a police-
man to break up lumps. This also aids in separating
the sodium sulfate which is easily distinguished from
the yellow crystals of K2PtCL;. Wash the Gooch cruci-
ble twice with alcohol.
Continue washing the precipitate exactly as above
(six times by decantation and twice in the Gooch)
but using 20 per cent XH4C1 solution saturated with
K2PtCl6 to remove impurities not soluble in alcohol.
Pipettes are used for measuring the wash solutions,
insuring uniformity of procedure and doing away
with the ammonium chloride wash bottle, which is
generally messy.
Finally bring the precipitate on the Gooch cruci-
ble with alcohol and wash free from NHiCl. Taste
the bottom of the Gooch. A sour taste indicates in-
sufficient washing.
Dry at no" C. one-half hour and cool in a desic-
cator one-half hour. Calculate K2PtCLs X 0.1938 =
K20.
Keep alcohol washings separate so that platinum
and alcohol may be recovered.
CI — Use 100 cc. of the above solution. Acidify with
HN03; rendr: ikaline with XaHC03; add a
few drops of saturated potassium chromate solution
and titrate with .V 10 AgNOj solution.
C02 (ai salinity) — Titrate 40 cc. of the above solu-
tion with .V 5 H.-SO«, methyl orange indicator. Make
deduction for soluble silica determined later.
SOj — Determine asBa S0< in 100 cc. of the above
solution.
loss on ignition — Heat a 1 g. sample of salts in a
tared platinum dish to quiet fusion and weigh after
cooling in a desiccator. The weighing must be done
quickly as the fused salts absorb moisture very rapidly
from the air.
insoluble matter— 1 g. sample of salts
with hot water and filter. Ignite the paper and
weigh.
Feb., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
129
Na20 and Si02 — Evaporate the filtered solution with
an excess of H2SO4. Ignite and weigh the mixed
sulfates and Si02, using a tared platinum dish. After
weighing take up with hot water and filter to remove
Si02. Deduct Si02 and calculated K2S04 from the
weight found for mixed sulfates and calculate the re-
maining Na2SOj to Na20.
METHOD FOR THE ANALYSIS OF BRINES
specific gravity — Determine with the Westphal
balance. Temperature correction is 40° F. = 0.010
sp. gr. The specific gravity at 6o° F. is an approx-
imate indication of the per cent solids. Thus 1.100
sp. gr. indicates about 10 per cent mineral solids.
solids — Use a pipette to measure into a tared plat-
inum dish an amount of brine containing about 1
g. of solids. Evaporate to dryness and fuse. Cool
and weigh rapidly to the nearest milligram.
CI, alkalinity and K20 in solids — Using the
same pipette as in the determination of solids, measure
out the same amount of brine for the determination
of CI. A similar sample is taken for alkalinity, and
a third similar sample is made up to 100 cc. and 20
cc. taken for the determination of K20. The methods
given on the preceding page under "Analysis of Salts"
are used.
From the weight of solids found the size of sample
taken for the other determinations and the percentages
found can be calculated.
RECOVERY OF ALCOHOL AND PLATINUM
alcohol — Most of the platinum in the alcohol
washings will be found precipitated as (NH4)2PtCl6
by the NH4C1 in the final washings. The alcohol is
decanted through paper to separate it from this pre-
cipitate. The filtered alcohol is then distilled on the
steam bath. The residue not distilled over is treated
as below for Pt recovery and any platinum precipi-
tated in the distillation flask is dissolved in aqua regia
and reprecipitated with the other platinum solu-
tions for recovery.
platinum — The contents of the Gooch crucibles
containing K2PtCl6 are washed into a beaker and
treated with hot distilled water slightly acidified with
HC1. This will dissolve the K2PtCl6, leaving the
asbestos, which may be used again. This solution
is filtered (through the filter previously used for the
alcohol washings) into the alcohol suction flask con-
taining the bulk of the (NH,)2PtCl6. Washing the
asbestos is continued until all Pt salts are in solution.
This solution is then transferred to a wide-mouth bot-
tle, where the Pt is precipitated with aluminum. A
piece of aluminum rod 3/s inch diameter and about
'/< inch long is convenient for this purpose. Pre-
cipitation is not complete until the solution is clear
and colorless. It may be necessary to add more acid
to complete the precipitation within a reasonable
time.
The solution above the precipitated platinum is
decanted and filtered through paper with or without
suction. The remaining precipitated platinum is
washed into a beaker, where it is heated with fairly
strong HC1 until effervescence entirely ceases. This
is to remove any adhering Al or other metallic impuri-
ties. Stirring at this point will aid flocculation and
make filtering easier. The Pt is then washed onto
the filter previously used and washed with hot water
until free from acid. It is then dried, ignited to
destroy the paper, and weighed. It is then dissolved
in aqua regia and evaporated to small volume several
times to remove CI and HN03. This solution is
filtered through a tared Gooch crucible and the weight
of insoluble matter is deducted from the amount
weighed as Pt. The weight of insoluble matter is
usually a few centigrams and probably consists of
unburned carbon from the filter paper.
The platinum solution for use in analysis is of such
strength that 10 cc. contain 1 g. of platinum.
The Hord Alkali Products Company
Lakeside. Nebraska
SUGGESTIONS ON SOME COMMON PRECIPITATIONS
By George H. Brother
Received October 20. 1917
A number of my friends engaged in analytical
work have spoken to me about filtration difficulties
they have encountered in some of the most common
determinations. According to their statements, they
are unable to get filters which will "hold" unless they
resort to the very retentive, but comparatively slow
papers. After considerable investigation of the sub-
ject, I have come to the conclusion that their blame is
largely misplaced. The fault, in the great majority
of cases, lies not so much in the paper used as in the
method of precipitation. For this reason I am giving
a few "tricks of the trade" which, I am sure, will be
helpful to any analyst not already acquainted with
them, if used in standard methods given in any reputa-
ble reference, such as Treadwell-Hall.
BARIUM SULFATE
The sulfate solution should be about 200 cc. in vol-
ume and weakly acid with hydrochloric acid (1 cc.
1.2 sp. gr. to a neutral solution). It should be heated
to a temperature just below boiling,1 and about half
of the solution of barium chloride necessary for ex-
cess added drop by drop, stirring well meanwhile,
and allowed to digest for about 5 minutes. The re-
mainder of the precipitant is then added (not neces-
sarily so slowly, though the solution should be stirred
during the addition) and it is allowed to digest 10 or
15 minutes longer. It is then ready for filtration.
A precipitate formed in this way will be found quite
crystalline and will be readily retained by a paper
of moderately close texture. I have quite satisfac-
torily used Whatman 40, C. S. & S. 589 "White Rib-
mi Munktell's o instead of the slower Whatman
42, C. S. & S. 589 "Blue Ribbon," or Munktell's 00.
In this way time may be saved in the filtration as
well as in the much shorter period of digestion.
' "Just below boiling" gives all the advantages of precipitation and
digestion in hot solution nnd eliminates the risk of superheating and loss
through frothing or bumping.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 2
CALCIUM OXALATE
olution of the calcium salt to just below
boiling. Add excess ammonium oxalate solution,
then just enough hydrochloric acid (sp. gr. 1.2) to
tin precipitate. Add ammonium hydroxide
solution drop by drop until distinctly ammoniacal,
then run in a good excess. Digest at a temperature
just below boiling for about half an hour. Filter
while hot and wash precipitate with ho1 water.
The important point in this determination is the
acid oxalate solution from which calcium oxalate is
precipitated by the addition of ammonia. The forma-
tion of calcium hydroxide is in this way pr<
and a crystalline precipitate of the oxalate insured.
The method works otit the same if the original calcium
solution is made acid, the ammonium oxalate (or oxalic
acid) added, then the ammonium hydroxide solution,
as above. The objection to this procedure is, of course,
the absence of an indicator to prevent the addition of
an unnecessary excess of acid. For volumetric lime
determinations, where an ashless paper is an unneces-
sary extravagance, Whatman 3 and 30 or Munktell
100 will be found quite satisfactory if the precipitation
is done by this method.
AMMONIUM PHOSPHOMOLYBDATE
The principal difficulty with this precipitation is
the adherence of many analysts to the old ride, viz.,
heat the phosphate solution to about 700 C, pre-
cipitate and digest at no higher temperature. If this
procedure is followed, digestion for several days is
necessary to secure a filterable precipitate, and even
then success is uncertain. I have found the method
of YVoy with modifications, as given in Treadwell-
HalPs "Quantitative Analysis," (1915), p. 437, to be
very satisfactory. The essential point of this method
is precipitation and digestion at a temperature just
below boiling. The phosphate solution should be
made distinctly alkaline with ammonium hydroxide,
then nitric acid added to slight excess. This is a con-
venienl way to insure the presence of ammonium ni-
trate in the solution and 1 1 the addition of too
1 js of nitric acid. 1 1 should be he
then, while stirring, add thr ammonium molyb-
date solution drop by drop from a pipette. Digest
on a hot plate a1 ature just below boiling
until the supernatant liquid is clear and colorless
(usually about 15 minutes). Decant, wash and filter
as usual. ( Vcasionally R
no precipitate immediately forms, but ins:
1 1. hi 1 >ei urn . coloi escribed
above, will bring ion and
conversion of the yellow solution to colorless, but in
such cases more than [5 minutes' digestion is usually
required. The precipitate thrown down in this way
is coarse enough to be retained by quite O]
papers, such as Whatman 1 and ji, C. S. & S. 595, or
Munktcll's OB.
MAGNESI1 \i \M\io\n \i PHOSPHATE
Here, again. I think the difficulty lies in the use of
old methods, which called for the addition of mag-
nesia mixture to an ammoniacal solution of the phos-
in the cold. The method of B. Schmitz, as out-
lwell-Hall (LoccU.), p. 434, gives much
more satisfactory results. The phosphate solution
ed with excess magnesia mixture solution, hy-
ric acid added just to dissolve the precipitate
and it is heated to boiling. Ammonium hydroxide solu-
tion is added slowly until a crystalline precipitate
forms. If the precipitate is not crystalline, it should j
be redissolved by the addition of hydrochloric acid
with ammonia. When a distinctly
crystalline precipitate has formed, the solution is
made ammoniacal, it is removed from the hot plate
and allowed to cool. When cold, add a volume of
ammonia (sp. gr. 0.9) equivalent to about one-fifth
the volume of the solution, and at the end of about 10 |
minutes it is ready to filter.
reverse of these determinations, i. e.. the
determination of magnesium by precipitating
with a soluble phosphate, are carried out analo-
gously. A number of chemists in brass work are having
trouble with filtering tin dioxide. I have undertaken
to investigate this determination, and hope to have
some results on it before long.
Ottawa, Canada
A NEW PORTABLE HYDROGEN SULFIDE GENERATOR
By W. Faitoutb Munn
Received November 5, 1917
Because of the objections to hydrogen sulfide
>rs in general, namely, the renewal of the acid,
the leaking of gas following the completion of the
ation after the supply is not further desired,
and bulkincss, the following apparatus is recommended.
The generator is quite light, practically in one piece,
self-adjusting, made in a size adapted to most analytical
work, and is supported by a condenser clamp to an
iron support, thus enabling the chemist to carry it
easily to all corners of the laboratory. Although de-
signed for the preparation of H2S, it may be used for
preparing COj, H, or any of the other gases.
The fairly heavy glass tube B, which is the main
part of the apparatus, has a stopcock, C, fused to it
near the upper extremity. Two bulbs are blown on
ower half of the tube and below these bulbs a
stopcock, D. with a fairly wide bore, is fused. A lead
plate, with holes .;s shown in the drawing, is supported
between the bulbs by means of a piece of tubing hav-
ing about the same diameter as the plate and cut to a
length such as is required to bring the plate support
to a point between said bulbs. This glass support
rests on the lower part of bulb ;;. Both the plate and
support should be of such diameter as to just allow
them to easily clear the wall of tube B.
The tube .1 of the apparatus, and at least the capacity
as given, acts as the reservoir tor the acid. This con-
sists of a 2l/t to 3 in. diameter tube. 5 to 6 in. long,
with a * 8 in. diameter tube 101 -2 in. long sealed to its
lower extremity. This tube passes through a rubber
stopper placed near its upper end. while the lower
isses through the filter plate and nearly to the
Feb , 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
bottom of bulb 2. The stopcock C, which has al-
ready been mentioned, has its tube bent as shown in
the figure and supports a 1 in. diameter fairly heavy-
walled test-tube, which in turn has a side tube fused to
it near its upper end. This test-tube contains a small
quantity of water and acts as a purifying chamber
for the gas evolved. No support for this tube is re-
quired.
To fill the generator, the glass tube for supporting
the lead plate is first carefully placed in position. The
lead plate is then cautiously slid in. The tube sealed
Hydrogen Sulfide Generator
to the lower extremity of .1. after putting the cork in
position, is lowered into the bulb B, until the end lias
just passed through the center of the lead plate. (The
center hole in this plate must be of a size which will
allow the free passage of this tube.) The apparatus
is then inclined and small lumps of iron sulfide cau-
tiously rolled into tube B, until bulb 1 is filled. The
tubes are then placed in a vertical position and tube .1
lowered until the lower extremity of the glass tube
reaches the bottom of bulb 2. When the tube has
reached this point the rubber stopper should be at
the correct point for securely fastening in the neck of
B. The apparatus is now fastened to a condenser
clamp, at a point just above bulb 1, of tube B. Stop-
cocks C and D should be closed, and then dilute
H2SO4 (1 : 8) poured into the top of A, until about
full. The cock C is now opened until the acid has
filled half of bulb 2. The cock C is then again closed
and enough acid added to A to again fill it. The com-
parative volumes of tubes A and B should always be
kept in mind because if A is made smaller than herein
given, or bulbs 2 and 1 made larger, A will not be
large enough to hold sufficient acid to supply bulbs
2 and 1, and still have space enough for the returning
acid when the supply of gas is stopped. It is there-
fore advisable to make tube A about 6 in. in length
to keep on the safe side.
By opening the cock £>, the lower portion of acid,
which has been in contact with the iron sulfide and
which finally becomes inactive, may be removed with-
out disturbing the apparatus or causing the escape of
gas. This arrangement allows one to use all of the
acid added to the generator and permits complete
renewal of acid in a very short time. The removal
of spent acid through cock D also washes out the black
sediment which is always left after the decomposi-
tionof the sulfide.
The firm of Eimer and Amend have made up one
of these generators for exhibition purposes.
Research Department
I.ederle Laboratories
New York City
AN AUTOMATIC HYDROGEN SULFIDE STOPCOCK
By Carl H. Classen
Received November 15, 1917
In students' laboratories there has long been a need
for a simple, efficient, and fool-proof hydrogen sulfide
stopcock. Metal stopcocks, in general, are obviously
impossible. Hard rubber or glass stopcocks are very
useful so long as they do not stick or break, but in
themselves they do not furnish any safeguard against
being left open, or any easy control of the flow of gas.
Rubber tubing with pinchcocks is also useful, but the
prolonged squeeze of the pinchcocks rapidly weakens
the rubber. Although screw pinchcocks give an ex-
cellent control of the flow of the gas, they, too, do not
furnish any safeguard against being left open; also,
ively squeezed
with the consequent danger of
p1 I'm- the injurious squeeze and the loose
adjust in ordinary pinchcock come
ory solution is par-
ticular! .
Lon with numerous branch pipes from l>
sulfide mains.
ipproach t" a satisfactory
i is the device which is being used this year
132
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. a
at the Rice Institute, Houston, Texas. To each small
branch pipe of the hydrogen sulfide main, thin-walled,
gum-rubber tubing one foot long and of convenient
diameter is attached. Near the branch pipe, and in-
side the rubber tubing, is a glass "pearl" made from
glass tubing of a diameter slightly larger than that of
the rubber tubing — the rubber should not be stretched
too much. The device is merely another application
of a similar device that is used with ordinary Mohr
burettes.
A- Rutter Tubing
B- Gl,x* J Ptarl
Longitudi nol
Cross Section
bQ
Closed
In use
The advantages of the device are obvious: the stu-
dent must "be on his job;" open stopcocks are impossi-
ble; the flow of gas can be regulated with certainty
and extreme ease; the device is not easily put out of
order; it is easily and quickly replaced; there is no
prolonged, excessive squeeze; the pearl may be moved
to a new position when necessary; the cost is ridicu-
lously low; the gas is not wasted.
The device has been in use only one month and,
consequently, it is too early to say that it is an entire
success where the durability of the parts is concerned.
Where its use by the student is concerned, there can
be no question of its entire success; its simplicity, and
the ease and neatness of its manipulation make a
"hit" with the student. Undoubtedly improvements
in design and material are possible.
Rick Institute
Department op Chemistry
Houston. Texas
A SIMPLE AND EFFICIENT FILTERING TUBE1
By William M. Thornton, Jr.
Received October 8, 1917
The apparatus here depicted was designed particu-
larly for handling those precipitates whose solubili-
ties are sufficient to necessitate great economy with
the liquid used for transferring and washing. Although
it resembles somewhat the filtering devices of Zopfchen1
and of Bailey,3 it is not, however, identical with either.
Moreover, the appliance can easily be put together
from materials to be found in any well-equipped lab-
oratory.
A straight glass tube, having a stopcock at its mid-
dle point, is sealed to a carbon filter tube. The latter
' Published by permission of the Chemical Director, E. I. du Pont de
Nemours & Company.
» Chem.-Ztg., 26 (1901), 1008.
• J. Am. Chtm. Soc., SI (1909), 1 144.
is fitted with a two-hole rubber stopper. The stem of
a Walter crucible holder passes through one hole of
the stopper while the other contains a right-angled
exit tube. The rubber hose leading to the suction
pump is intercepted by an ordinary T-tube, the free
end of which is joined to a short piece of rubber tubing.
A Mohr clamp is kept in readiness. The whole is
held in position by a stand with two clamps appro-
priately placed — one to grasp the main tube and the
other to support the T-tube.
The manipulation is quite obvious. Having pre-
pared the asbestos felt in the regular way, the per-
forated crucible G is set in the collar II'. After the
suction has once been adjusted, it need not be inter-
rupted throughout the entire filtration. When the
cock 5 and the clamp M are closed, the carbon tube
C serves the purpose of a small filter flask. When
the clamp M is opened and pushed upward past the
shoulder on to the tube /, atmospheric pressure is re-
stored within the apparatus (or nearly so); and then,
on opening the cock 5, portions of the clear filtrate
can be delivered into the original beaker. The cocks
To the suction pump
are then closed, and, after the usual application of
the "policeman," the liquid is again poured over into
the perforated crucible G. These operations can, of
course, be repeated as often as may be desired.
With the aid of the above-described outfit, the author
succeeded in transferring and washing a certain pre-
cipitate (the washing being accomplished by four small
portions of iced water successively applied) so that the
sum total of the filtrate and washings did not exceed
27 cc. Furthermore, the apparatus is so convenient
that filtrations can be very quickly performed with its
help — thus reducing to small dimensions the losses
incurred in handling those precipitates which suffer
an increase in solubility on rise of temperature.
Johns Hopkins Chemical Laboratory
Baltimore, Maryland
Feb., 191S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
ADDRL55L5
THE AUTOMATIC CONTROL AND MEASUREMENT OF
HIGH TEMPERATURES1
By Richard P. Brown
Probably no employee causes the average works manager
so many sleepless nights as does the furnace man, on whose
shoulders rests the responsibility for the accurate heat treat-
ment of the steel and the uniformity of the product. This is
not only true of a steel plant, but is also equally true in the chem-
ical industry, where the temperature of numerous processes
must be accurately controlled; in the glass industry, where the
melting of the glass and its annealing must be carried on within
very narrow limits of temperature; in the brick industry, where
the kiln firing is of the utmost importance, and I might continue
the list throughout the whole industrial field.
The old furnace man, through years of practice, will endeavor
to gauge the temperature of the furnace with his eye. Pro-
viding he has not been up all the previous night and his eye is
clear, he will probably judge the temperature fairly accurately.
If he is of a reasonably kind disposition, he may permit the
manager to install pyrometers to guide him in controlling the
temperature, and he may even in time use the pyrometers and
rely on them.
But we can pardon the works manager or director for asking,
"Suppose John dies, gets sick or quits his job, how am I to handle
the output of these furnaces?" He would like to have an under-
study for the old furnace man, but the latter does not like the
idea. So he wonders why someone does not develop a device
to automatically control the temperature of the furnaces, so
that he can cease worrying about them.
This is one reason why a great amount of study has been
given, not only to perfection of pyrometers, but also to the
automatic control of temperature. It has, however, been only
recently that real results have been accomplished in automatic
temperature control.
First of all, it was necessary to perfect the temperature-
measuring instrument in order that it could be relied upon to
uniformly indicate the actual furnace temperature. It was
then necessary to apply to the pyrometers attachments to throw
the switches on the electric furnaces, or to open or close the
valves on gas or oil furnaces.
My experience in the United States has shown that, for in-
dustrial service, an instrument actuated by the expansion of
nitrogen gas is the most satisfactory for temperature measure-
ments up to 800° F. or 425 ° C. The gas-expansion instrument
consists of a bulb of copper which is inserted in the heat, and
this bulb is connected by capillary tubing to an indicating or
recording gauge containing a helical expansive spring.
The expansion of the gas in the bulb exerts a pressure in the
capillary tubing which is conveyed to the spring in the instru-
ment, and the pointer, attached directly to this spring, moves
across the scale or chart.
It is essential in this instrument that the capacity of the bulb
be some 50 times as great as the capacity of the capillary tub-
ing and spring. This is essential to reduce to a minimum
errors due to changes in atmospheric temperature along the
capillary tubing or at the instrument. In consequence this
instrument is not desirable for use where the gauge must be
placed more then 100 feet from the bulb.
For use at moderate temperatures, where the measuring in-
strument must be placed at a considerable distance and for tem-
peratures above the range of the gas-expansion instrument,
the thermo-electric pyrometer has been almost universally
adopted in the United States. A thermocouple of base metals,
1 Read before the Faraday Society, London, by the Secretary of the
Society, November 7. 1917.
usually formed of one wire of nickel 90 per cent and chromium
10 per cent, and the other wire 98 per cent nickel and 2 per cent
aluminum, is preferred for temperatures to 18000 F. or 1000 ° C.
For temperatures above this, and as high as 28000 F. or 1500°
C, thermo-electric pyrometers using a platinum-rhodium
thermocouple are the most satisfactory. For still higher tem-
peratures, a radiation type of pyrometer is available, consist-
ing of a thermocouple in the focus of a reflector at the rear
end of the tube, which is pointed at the door or opening of the
furnace.
For measuring the voltage produced by a thermocouple,
whether of base metal, platinum-rhodium, or the radiation
type, high resistance millivoltmeters are available. We are
producing in the United States such millivoltmeters of some
1000 ohms or more. This remarkably high resistance is natur-
ally desirable to practically eliminate the errors due to changes
in the resistance of the line or wiring connecting the thermo-
couples and the instrument, and also to nullify the effects of
any changes in the resistance of the thermocouples due to
heating.
Changes in resistance may be due to actual changes in length
or changes in atmospheric temperature, which in turn affects
the resistance of the line or wiring. We have been able to se-
cure this exceedingly high resistance by reducing the weight
of the moving element to a minimum, and I have a sample of
this moving element for exhibition.
The total weight of the moving element in our high-resistance
pyrometer, including pointer and springs, is 526 mg. This
extreme lightness is secured by the use of an aluminum alloy
wire, which we have succeeded in enameling. The enamel
coating is much thinner than the silk insulation formerly used
and more turns can be secured on a coil of a given width. Like-
wise, by the use of the aluminum wire, the weight has been
reduced 662/s per cent as compared with copper wire which was
formerly used for these moving elements. The aluminum
wire is 0.003 mcb in diameter and drawing this wire has been
quite a mechanical problem.
The pointer tubing in this moving element is of aluminum
with an inside diameter of 0.008 inch, an outside diameter
of 0.012 inch, or a total thickness for the wall of the tubing of
0.002 inch. Even this weight for the pointer tubing could
probably be reduced by the use of magnesium instead of alu-
minum, but to date we have been unable to satisfactorily draw
magnesium.
I only cite these points regarding the construction of our
present-day high-resistance pyrometer millivoltmeter to show
what development work can produce. Instruments of this
type made by Siemens and Halskc, of Germany, were never
developed to this extent, at least, prior to the outbreak of the
war, and their moving element was several times as heavy as
the sample I have here, and in consequence the resistance of
their pivoted meter was several times less. Incidentally, I
think we have about reached the limit of development along
this particular line.
It will be understood that the same electrical system, such
as I have described, «an be used either to indicate the tempera-
ture, or, combined with the proper apparatus, to record the
temperature constantly on a recording sheet. There are both
portable and wall-type indicating pyrometers, and recording
pyrometers are produced to make a record on a circular chart
8 inches in diameter, or to make a continuous record of the
temperature on a roll of paper lasting two months or more.
By the introduction of suitable switching mechanism a record
of the temperature of quite a number of thermocouples can
134
THE JOURNAL OF INDUSTRIAL AND ENGINEERING < 111. WISTRY Vol. 10, No. 2
be made on the same record sheet. These temperature records
arc distinguished by using different colors for each record lini .
by using numbers corresponding to each thermocouple, or
the form of line- produced on the chart for identifica-
tion.
I'm even greater precision in temperature measurements
than is secured with the high resistance millivoltmeter, we have
developed a new instrument, which we call the Brown Precision
Heal Meter. This instrument is suitable foi either tempera-
ture measurement or automatic control of temperature, and
brief description of this new instrument might be of interest.
Mv idea in the heat meter has been to eliminate all the bad
features or drawbacks met with in using a millivoltmeter for
ti tnpi 1 'lure measurement.
Possible sources of error in the use of a millivoltmeter in tem-
perature measurements, even one of high resistance, consist
in changes in resistance of the circuit comprising the thermo-
couple ami the leads or wiring, due to changes in length or changes
in atmospheric temperature; also errors can occur due to tem-
perature coefficient of the meter, that is, errors caused by changes
in atmospheric temperature in the meter itself. Another source
of error is a change in the actual indication of the instrument,
due to spring fatigue, abuse or sticking, and to overcome these
possible sources of error we have developed this rather inter-
esting instrument.
Briefly, its operation is as follows:
With our standard millivoltmeter of high resistance, we sup-
ply an ordinary dry cell about i1 1 inches in diameter by 2l/2
inches long, and furnish suitable rheostats to reduce the volt-
age of the dry cell from approximately i'A volts to a range
from o to 60 millivolts, the maximum voltage produced by the
thci mocouples.
In our first operation, we oppose the voltage developed by
the thermocouple to the reduced voltage of the dry cell, and
when the pointer stands on zero, it indicates that the voltage
from each source is the same. We now in operation No. 2 cut
out with a switch the voltage of the thermocouple and read
the voltage of the dry cell circuit b\ direct deflection. This
eliminates the line resistance entirely as in a potentiometer.
We now have a deflection indicating the actual temperature
developed by the thermocouple at the moment of reading the
instrument, but fluctuations in temperature of the thermo-
couple will not lie indicated, as we are reading the voltage
from the dry cell. We have, however, incorporated other opera-
tions in this metei
lii operation No. ,3 we connect the thermocouple with the
metei instead of the dry cell circuit and we note whether the
indications ate the same. By switching back and forth quickly,
Hi, voltage from the thermocouple circuit 01 bom the dry
cill circuit can be noted. If excessive line resistance has caused
the indications of the millivoltmeter to be lowered as compared
with the dry cell circuit, a rheostat i. operated to bring up
the indications of the thermocouple eneini in that shown
when v\e are reading the voltage of tin- dry cell circuit.
We now leave the instrument indicating on the thermo-
couple circuit and the errors, if any, which might in dm to
line resistance or changes in t< mperatun of the hue. hav< been
eliminated, and we have a direct reading millivoltmeter, indi-
cating i I ' mperatures.
\ rheostat of 15 ohms is supplied in the meter which permits
of adjusting the indications I'm a total change of line resistance
equivalent to 15 ohms, 01 a circuit of two copper wires almost
a mile long.
We have eliminated the temperature coefficient of the meter
by furnishing a copper- resistoi in the metei equivalent to the
eoppei or aluminum of the coil; hence, in balancing the voltage
from the dry cell against that of tin- thermocouple we also
automatically eliminate errors due to the temperature coefficient
of the meter itself.
is now left only one possible source of error, the change
II thi tctual indications of the meter due to sticking of the
pointer, abuse of the instrument, spring fatigue, etc. To obviate
this source of error we can supply with tin instrument a stand-
ard cell with suit. ibli n 1 tors, and by the potentiometer method
used in testing the meter we can check this meter. We supply
?!ii. ■ 11 istors, for example, where a meter is calibrated for. 00
millivolts we furnish resistors equivalent to a deflection of 20,
|O0l 60 millivolts on the scale), and after balancing the standard
1 ' II against a part of the voltage of the dry cell, through these
suitable resistors we can note whether the pointer swings to 20,
(.0 and 60 millivolts, respectively, on the scale. If it does not,
'In can lie noted and the actual error in calibration is de-
tected.
Win 11 the instrument is supplied with standard cell the tem-
perature of the instrument should always be between 50 C.
and 40° C, or 40° F. and 105 F.; in fact, standard cells of
cadmium sulfate or zinc sulfate will be injured if the tempera-
III )i ii falls beyond these limits. This is true of any stand-
ard cell employed in instruments
In this instrument we have all the good features of the poten-
tiometer method of measuring temperature with the advantage
that we have a direct reading instrument which can be adjusted
once every day or oftener if desired, for the actual line resistance
with which it is used and the surrounding atmospheric condi-
tions. The meter will then indicate correctly throughout the
whole scale range, and the furnace man has the instrument
to guide him without hand manipulation, and an inspector can
daily check the calibration of the instrument.
Naturally, this instrument is equally as suitable for automatic
temperature control as the instruments previously described,
when properlj designed for this service.
RATI RE CONTROL
Attempts have been made in the past to electrically operate
switches and valves by permitting the pointer of the pyrometer
in .nun in contact with adjustable contact arms on each sjile
of the pointer. Unfortunately, the millivoltmeter, used with
the thermo-electric pyrometer, has an exceedingly weak control
for the pointer. One is easily able to blow the pointer across
the scale with the breath.
In., resequence, simply permitting the pointer of such a pyrom-
etei to move into contact, is not sufficiently positive to be
i ory for automatic control work.
The automatic control pyrometer exhibited here 0]
in the following 111:1111111 A thermocouple formed of a uickel-
chroiuimn alloy is installed in the electric furnace, the tempera-
tun "I which is being controlled. The thermocouple actuates
a high resistance millivoltmeter. Below the pointer and ad-
justable throughout the whole scale range, is a tabic curving
two cout. id i'n thin puce of insulating ma-
inch thick The depressor arm driven by a small
electric motor, 01 bj ■> clock if preferred, depresses the pointer
1 niteiv.ds, usu.illv every ten seconds, and in doing so
the pointer forces togethei thl two contact pieces below.
Let us assume the pyrometer controller is required to control
the furnace at a temperature of exactly 140,1° F, The knob
on the left of the instrument is turned until the index in front
ol the scale stands at [400 F This index corresponds to the
position of the thin insulating material which separates the high
and low contact
The switch connecting the furnace in the line is closed and
the pointer slovvlv uses across the scale as the temperature
of the furnace rises i\s the switch is already closed, when the
pointer is depressed on the low contact, the switch continues
to remain closed, and no change occurs until the pointer passes
Feb., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
135
over the neutral insulating piece and is depressed on the high
contact. The switch indirectly operated by a solenoid and re-
lay is now instantly actuated and the circuit opened. The tem-
perature of the furnace begins to slowly fall, and when the
pointer is again depressed on the low contact, the circuit is again
closed. This operation continues as long as the furnace is to be
operated.
When the switch opens and closes the main circuit, the cur-
rent is either full on or off, and the fluctuations are continuous
within narrow limits of some io° to 200 F. These continuous
risings and fallings of temperature can be largely reduced and
closer control can be procured by the use of two rheostats in
the furnace line. The solenoid-operated automatic switch is
then used to simply cut in and out of circuit the second rheo-
stat.
Assuming it is desirable to continually maintain 14000 F.
in the electric furnace, irrespective of fluctuations of voltage,
the two rheostats are set. so that with only one rheostat in the
circuit the temperature will rise to approximately 15000 F.
With the second rheostat in the circuit the temperature drops
to 1300° F.
When we now use the solenoid-operated switch to cut in and
out the second rheostat, we naturally control the temperature
only between 15000 and 1300° F., and we do not have the rapid
surges or ups and downs in temperature, and thus maximum
control is secured.
It is realized that the same form of switch can be used to
operate a valve to control a gas or oil furnace. We have found
it desirable to use an automatic valve in a by-pass so as to
control simply a portion of the gas or oil supply, and in the same
manner as in the electric furnace control, eliminate the maximum
fluctuations caused by the complete opening and closing of the
switch or valve.
Assuming that we have a 2-inch supply pipe for the gas to
the furnace, it is customary for us to by-pass this and use a
Vi-inch automatic valve, which gives us approximately 25 per
cent control. This is sufficient to control the usual fluctuations
in gas supply and secure very satisfactory control. This method
also eliminates the difficulty which would occur where the gas
is completely shut off and then turned on in full, as would occur
without the by-pass control.
TEMPERATURE SIGNALING PYROMETER
In addition to an instrument to automatically control furnace
temperatures, there has been a demand for an instrument
to automatically signal by lights whether the temperature is
too high, correct, or too low in any particular furnace.
It has been common practice in plants in the United States,
where there are a number of heat-treating furnaces, to main-
tain an operator at a central pyrometer and by colored electric-
lights at the furnace to signal whether the temperatures are
right or not. It is common practice to locate three lights above
each furnace red. white and green; the red light burns when
the temperature is too low, the white light when the tempera-
ture is within certain limits, for example, within 20 I' o) tin-
correct temperature, and the green light burns when the ten
perature is too high. The fireman who operates tin- furnace
is guided entirely by the lights and a central pyrometer is used
to control thi temperatures.
We have been able to develop an instrument t" automati-
cally signal by lights whether the temperature is correct 01 not,
and in this way the services of tin- operatoi 't the instrument
are eliminated, The same form of instrument is used for this
lutomatically < ontrol thi fui
tures, and the point'
seconds onto contact corresponding to tin red, white and
gni 11 light
• of current than an ordinary
service line, is required to operate these lights. The supply
may be 1 10 or 220 volts, either a. c. or d. c. The current which
lights the lamps does not follow through the instrument, but is
made and broken by an auxiliary device containing the neces-
sary mechanism. A high resistor is in series with the circuit
connected with the pyrometer, which reduces the current flow-
ing through the contractors within the instrument, to less than
0.07 amp. This prevents sparking at the contractors and
errors due to the heating effect of a current of higher amperage.
The lamps may be any. reasonable distance from the pyrometer,
in fact, they are operative at a mile or more if desired.
The various thermocouples in each furnace are connected
successively to the instrument through switching mechanism,
and at the same time a switching mechanism connects the various
sets of lights at each furnace. We have constructed an instru-
ment of this character to automatically take care of signal
lights at 12 furnaces.
This form of equipment gives the fireman or operator of the
furnace an indication by lights which he can easily understand,
and he adjusts the valves or fires the furnaces accordingly.
It is simple to instruct a man to keep the white lights burning
and to explain what the red and green lights mean, and it re-
quires a less experienced workman to control the furnaces in
this manner than to read temperatures on a pyrometer scale.
This newly developed instrument also eliminates the man re-
quired to read the temperatures at a central pyrometer.
The extensive use of pyrometers to measure or record high
temperatures will serve to
(1) Eliminate guess work as to the temperature.
(2) Reduce fuel consumption through the maintenance of
the correct temperature and not excessively high tempera-
tures.
(3) Reduce time for heating of the product due to the main-
tenance of the correct temperature.
(4) Increase efficiency in operating a plant through the sav-
ings outlined above.
Instruments to automatically control the temperature, when
properly constructed and applied, will eliminate entirely the
personal element. The maintenance of the correct tempera-
ture in the furnace is automatic, and this is a step forward
and an improvement over temperature control through pyrom-
eters.
I do not doubt but that the next few years will see further
improvements in pyrometers and temperature control. There
will always be room for improvement, and the cooperation of
the industrial works and the pyrometer manufacturers will
largely hasten the development of practical instruments for the
measurement and control of high temperatures.
Tin: Brown INSTRUMENT Company
Philadelphia, Pennsylvania
AIRPLANE DOPES'
By GuS I ' LBN, JR.
"Dope" is tin lishes used on the wings
of airplanes to render the fabric taut and waterproof. All air-
plane wing is made bj rame work of the pro
ami shape with a linen 01 cotton fabric. There arc then applied
to the fabric si 1 suitable varnish, of which the base
is eithei cellulose nitrate The term "dope"
have arisen in tin slang of the factory workman, but
is now firmly fixed and is used to distinguish the cellul
1 varnishes made up of gums
and oils, which an ohm tun ' The
chief function of the dope is to tighten U] old give
a smooth
1 1.. the NTortheai taction of the Amcricnn
1917.
136
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 2
and preferably also to oil and gasoline. It also adds to the ten-
sile strength, the percentage increase depending somewhat
upon the strength and character of the fabric, and upon how
much the fabric was stretched before doping. The tentative
specification of the Bureau of Standards requires an increase
of at least 25 per cent in the tensile strength of linen fabrics,
and of 15 per cent with cotton fabrics. In practice considera-
bly greater increases are often obtained.
The fabric most in demand for airplane wings is linen, because
of its strength and toughness and the difficulty with which it
tears. Owing, however, to the present scarcity of linen, specially
woven cotton fabrics are being developed. While some of the
latest of these have a tensile strength as great as that of the
best linen, they still seem to tear more readily. The average
weight of an acceptable fabric is about 3V2 to 4 ozs. per sq. yd.,
and the tensile strength is in the neighborhood of 90 to 100
lbs., per inch width. In general, the dope, when dry, adds about
2 to 2V2 ozs. per sq. yd., but in certain types of war machines
it is considered necessary not to let the combined weight of
fabric and dope exceed 6 ozs. per sq. yd.
The dopes which are at present in use may be divided into
two classes: first those consisting essentially of a solution of
cellulose nitrate or pyroxylin; and second, those made by dis-
solving cellulose acetate. The usual concentration is about 8
ozs. per gal. Among the more common solvents for the acetate
are acetone and combinations consisting largely of tetrachlor-
ethane and alcohol. The acetone may be either pure or some
of the commercial grades containing methyl acetate and methyl
alcohol. To dissolve the nitrate, the usual solvents such as
amyl acetate and acetone are used, and the solution diluted to
the proper strength with suitable non-solvent liquids. In ad-
dition, some substances are usually added to preserve the flexi-
bility of the coating, or modify the shrinkage power, as, for ex-
ample, castor oil, which is often present in nitrate dopes. It is
possible in this way to get all gradations of shrinking power
from almost none to an amount sufficient to twist the frames out
of shape.
The great outstanding difference between the coatings given
by cellulose acetate and cellulose nitrate dopes is the inflamma-
bility of the latter, a difference which will probably be empha-
sized more and more as the use of airplanes for peaceful purposes
increases Cellulose acetate dopes leave a non-inflammable
finish. The relative behavior of the coatings left by the two
types of dope is well illustrated by the fact that some gasoline
can be poured on a piece of fabric coated with a good cellulose
acetate dope and allowed to burn, and the fabric does not ignite.
The same test applied to a pyroxylin-coated cloth results in
the immediate ignition of the coating, and in a very short space
of time there is nothing left of the fabric or coating but a puff
of smoke.
The initial cost of pyroxylin dopes is somewhat less than that
of cellulose acetate dopes, and on this account some manufac-
turers have tried to effect a compromise between expense and
inflammability by applying three coats of pyroxylin first, and
finishing with two or three coats of acetate. This gives a fire-
resisting surface, even though the coating is not non-inflammable
all the way through. In Europe only acetate dopes are used,
and it seems to me only a matter of time when the users of air-
planes in this country will demand that every possible factor
of safety be taken advantage of. which will mean the use of a
non-inflammable dope.
You perhaps remember that in one of the editorials of the
September number of This Journal, Mr. Leon Cammen,
Vice-President of the American Aeronautical Society, is quoted
as saying that the ideal dope "should make the fabric watci
proof, air-proof, fire-proof, or at least slow-burning should give
low visibility, prevent deterioration, and be non-poisonous."1
> This Jouruau, 9 (1917), 826.
In these specifications, one or two essential points have been
omitted, probably because they were taken for granted. One
of these is smoothness and another adhesion. Smoothness
is a quality which in this case can readily be measured by the
wind resistance, and much attention has been and is now being
given to such measurements.1,2 An interesting calculation has
been made by Gibbors2 showing that in a moderately large
machine the difference in wind resistance between a doped and
an undoped fabric would correspond to a difference in lifting
power of from 150 to 180 lbs., in other words, the weight of one
man. As regards adhesion, a good dope should adhere well
to the fabric, so that in case of an accident causing a break in
the cloth, the coating will not be started and peel off. The
dopes at present on the market vary' considerably in this respect,
but it sometimes happens that dopes are blamed when the real
fault lies in the sizing of the cloth One of the factors which
seems to affect adhesion is the penetration. As a general thing,
dopes do not penetrate well on sized fabrics. These are excep-
tions to this rule, and the explanation may be that in those
cases where dopes do penetrate well on sized fabrics, the par-
ticular sizing involved is soluble in the solvent used, and blends
with the dope. Another factor which probably enters in, is
the character of the solution which constitutes the dope. While
it has not been definitely established, the indications are that
the more nearly the dope approaches being a true solution, the
greater the penetration; whereas the more colloidal it is, the less
it will penetrate. For any given dope, it has been demon-
strated that it will penetrate better, adhere better, resist atmos-
pheric conditions better, and wear better in every way when
applied to an unsized fabric than it will on the same fabric sized.
A reasonable way of accounting for this would be to assume
that where there is no sizing the dope has a greater tendency
to penetrate the fibers of the fabric, rather than merely between
the fibers, and thus when dry becomes more nearly a part of the
fabric. Since most sizing can readily be removed by boiling,
either in soapy water or a weakly alkaline solution, it is a simple
matter to insure good adhesion.
It may be interesting to know how near to the ideal the
present-day dopes come. As to being waterproof and air-proof,
all dopes which are used at all fulfill these requirements, be-
cause those are the first properties to be tested, but the extent
to which they resist continued exposure to atmospheric condi-
tions varies with the dope. The usual method of testing dopes
is to try them out on linen stretched on frames about 12 to 15
in. square, and expose them on some convenient roof. This is
much more severe treatment than airplanes ordinarily receive.
The first desirable property to disappear is usually the flexi-
bility, and the length of time before this happens can ordinarily
be taken as a measure of the relative value of different dopes.
The great difficulty with this test is that it varies so according
to the season of the year, owing to the wide variation in atmos-
pheric conditions. Another objection to the test is that it is
not strictly parallel to service conditions, in that a wing in actual
service is subjected to a very severe vibration to which the
test panel is not. On the other hand, if a dope remains flexi-
ble the vibration alone should not cause it to crack. The Bureau
of Standards at present requires a dope to retain its flexibility
at least 60 days when constantly exposed to the weather. There
is a certain weakening of the fabric on exposure, and tests'
have shown that this is much less with acetate thai' with nitrate
dopes. Especially is this true of cotton and in a less marked
degree of linen. This is what might be expected when one re-
calls that cellulose acetate is a much more stable compound
than cellulose nitrate. In addition, any free nitric acid formed
• Zahm, Phil. Mat-, 8 (1904), 58.
1 Report of National Advisory Committee for Aeronautics for 1916,
pp. 1766.
> Gibbons and Smith. Ibid., p. 168.
Feb., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
137
by the decomposition of the pyroxylin would have a much
greater weakening effect on the fabric than would a similar amount
of acetic acid, ever if the rate of decomposition of the two cellu-
lose esters were the same. In one instance the tensile strength
of cotton fabric doped with a nitrate dope after 3 weeks' ex-
posure was reduced to 48 . 5 per cent of the original, while linen
coated with the same dope was reduced to 68 per cent. With
an acetate dope under similar conditions, the tensile strength
of the cotton was reduced to only 87 . 2 per cent and the linen
to 84.8 per cent. All of these were taken in the direction of
the warp.
In order to give a more waterproof surface, it is the general
practice with some companies to apply one or two coats of spar
varnish over the usual dope. The use of spar varnish has one
disadvantage, however, and that is in the matter of patching.
As a rule, a hole in a wing can be patched with a piece of fabric
by using dope as a glue. On spar varnish, however, most dopes
do not stick, so that in order to make a repair, the varnish
first has to be removed.
There is one bane of the dope room which might be mentioned
here, and that is the formation of white spots during the drying
of the dope. They are due to moisture condensation during the
drying and show up as a rule only on humid or rainy days. They
can be removed by going over them with a little solvent, or bet-
ter by applying a cellulose acetate dope designed for the purpose.
Of course, the white spots can be prevented, even on damp
days, by regulating the amount of moisture in the air of the dope
room, but this, as a rule, requires a rather elaborate ventilating
system.
Of Mr. Cammen's ideal properties, we have now considered
all but the last two, viz., that of being non-poisonous and that of
low visibility. The biggest bone of contention as regards poison-
ing has been tetrachlorethane. Tetrachlorethane is one of the
best solvents for cellulose acetate Unfortunately, however,
its vapors when inhaled affect the liver, and before its poisonous
character was recognized, a few deaths had resulted abroad.
These were the result of inadequate ventilation. As soon as
suitable ventilation was provided, the trouble almost entirely
ceased. Some argue for the total exclusion of tetrachlorethane
as a solvent in cellulose acetate airplane dopes, but it gives
the finished wing a certain resilience which nothing else does.
Some of the British experts are very strong in their assertions
that it is indispensable as a constituent of dopes for scout ma-
chines. However, the report is that for some months the use
of tetrachlorethane has been forbidden in England. The policy
for this country has not as yet been absolutely established,
but should it prove desirable to use tetrachlorethane, it would
seem possible to do this, if ample ventilation of the proper
type were provided.
As regards low visibility, the dopes, being transparent and
almost colorless, do not make the fabric appreciably more visi-
ble than if it were not doped, except possibly when the sun
might be temporarily reflected from a glossy wing. The use
of a dull surface would obviously remedy this. Should it be
found that some color other than that of natural linen would
blend better with the color of the sky background, either the
dope or the fabric could be dyed. The goal of low visibility,
however, is a transparent wing. Doubtless many of you saw
a newspaper account a little over a year ago of a foreign air-
plane that did not have transparent wings. That no further
reports of such machines have appeared would seem to indicate
that as yet, at least, they are not very common. The wings of
the machine in question were made of transparent cellulose
acetate sheets, and it was claimed that at a height of a few
thousand feet, the machine was almost invisible. It had the
further advantage that the field of vision of the opei
much increased. Cellulose acetate sheets in a thickness of
"/1000 of an inch, which thickness has the necessary strength,
weigh about nine ounces per sq. yd., which is a little heavier
than most doped fabric. The chief difficulty in using them is
the fact that a tear once started spreads very rapidly. A
patent has been taken out for remedying this difficulty by re-
inforcing the transparent sheet by means of a fabric such as silk
woven rather loosely. As is readily seen, a wing of this sort
would be waterproof, air-proof and non-inflammable, would
have low visibility, would not affect the workmen applying it,
and would give no trouble from stripping or peeling. In other
words, there seems no doubt that if it can be obtained of the
proper weight and strength, it will prove to be the ideal wing
covering.
Chemical Products C<
Boston, Mass.
THE COLLABORATION OF SCIENCE AND INDUSTRY1
By V. Grignard
I am much honored that you have asked me to speak before
you, but I must apologize for my ignorance of the English
language which prevents my speaking at length without abusing
your courteous attention.
I appreciate deeply the great honor done me in making me
honorary member of the Mellon Institute and I wish to express
my deep gratitude to the corps of professors and especially to
the Director, Mr. R. Bacon.
My collaborator, Monsieur Engel, who speaks English fluently,
will tell you better than I of the excellent impressions we have
received in the course of our visit in your beautiful country;
but I wish to emphasize myself all the gratitude which I feel
toward your great industrial establishments and scientific
institutions for the uniform kindness which we have received
from them, for the courtesy with which they have facilitated
our visits and have furnished us with literature.
I wish to express to you also all the admiration which I feel
for the remarkable scope of your industry. You have made
magnificent use of your immense natural resources, thanks to
your will, your initiative, your faith in the future. These
valuable traits the American race owes to the very conditions
under which it has evolved: the first colonists, a small group of
enterprising men constituting an elite because of their aptitude
and their scientific knowledge which two centuries ago (and even
less) was the lot only of the privileged few, found themselves
struggling in a nearly virgin land with the many difficulties
which social life has imposed upon humanity. They acquitted
themselves with honor and if they did not always find the
most scientific solutions, those which they did bring forward
were marked for their daring and practical character.
And it happened sometimes that some of these solutions,
obtained uniquely in the experimental way., proved superior
to those of the European engineers; this was the case, for ex-
ample, with the turbine.
But life becomes more and more difficult even for the most
prosperous nations such as yours and the problem becomes
singularly complicated when it is no longer simply a question
of supplying a national market, largely open, but of entering
into commercial competition, from within and from without,
with new industries strongly organized. It becomes necessary
then to reduce the net cost to the minimum searching out the
most rapid and most economical processes, allowing no loss of
anything which represents any value.
Furthermore, the terrible war which has been imposed upon
us and in which wc are fighting side by side for the triumph of
justice and of liberty, this terrible war has demonstrated that
there exists for each large nation a certain number of vital in-
dustries which it cannot neglect without exposing itself to the
danger of some day being at the mercy of its enemies. The
nature of the problem changes. Scientific and technical in-
■ Translation of address delivered In French at Mellon Institute on
December 8, 1917.
138
THE JOURXAl OF INDUSTRIAL AND ENGINEERING < HEMISTRY Vol. 10, Xo. 2
Struction become necessary and in this your universities succeed
wonderfully.
Bu1 this again does not suffice; it is necessary that the manu-
facturer should not allow himself to be elated by his earlier
success and should understand thi ol commencing,
i.of continuing the contest, without waiting for this
prosperity to be menaced by bettei informed competitors.
And thai still is not all; when the manufacturer has compre-
I led his real concern it is not always possible for him to erect
suitable laboratories, to endow them with the necessary equip-
ment, ami above all. with a specially trained personnel.
It is then that institutions like the Mellon Institute come
into play, a production of genius which has solved in a manner
truly American a problem already old but without satisfactory
solution in Europe — that of direct collaboration between science
and industry. In visiting it the day before yesterday I took
account of its strong organization and of the incalculable- service
which it can render.
Between the too naive disinterestedness of the majority of
the French investigators and the German form, fruitful without
doubt, but too materialistic, which has made of too many
German scientific schools veritable industrial laboratories, for
the glory and above all the profit of their directors, there was
room for a solution considering the rights of the manufacturer
but also considering the dignity of the university. This solu-
tion you have found and the success of Mellon Institute since
tdation proves that the way in which you have been
doing it is the proper one.
Without doubt it will be necessary to struggle for a long time
yet against acquired habits, as we say, against the routine, but
further it will be necessary that the manufacturer have well
impressed on his mind this truth: in the period of beginning the
improvements to be realized are numerous, researches give
results rapidly, but little by little the framework contracts,
t ions require more and more specialized work, more
time, and more money. And it will not be necessary that the
manufacturer's interest should clash with that of research,
the more difficult it becomes the more raison d'etre will it have
in the midst ol 1 nomic struggle which, after the war,
will array, on a new account, one part of the world against the other.
France, who has never considered herself behind in the march
of progress, cannot fail to organize all her forces for this collabora-
tion, too much neglected by her, of science and industrv. She
cannot be inspired by a better model than the Mellon Institute.
Again, it will be necessary that our manufacturers accept the
necessary sacrifices for the foundation of laboratories and of
scholarships for research. But we can. I trust, have all confidence;
the war has opened our eyes and demonstrated once again the
truth of the proverb, "He who does not advance, falls behind."
I, therefore, salute with all my heart your magnificent Insti- I
tute which I consider a wonderful instrument of scientific and I
industrial progress.
PERKIN MLDAL AWARD
The Perkin Medal for 191 S was conferred on Auguste J.
Rossi, in recognition of his distinguished contributions to the
metallurgy of titanium, at the meeting of the Xew York Section
of the Society of Chemical Industry, held at the Chemists'
Club, January' 18, 1918. Introductory remarks by Mr. Jerome
Alexander, Chairman of the Section, were followed by an ad-
dress on "A. J. Rossi and His Work," by F. A J. FitzGerald,
Past President American Electrochemical Society. The presen-
tation of the medal by Dr. William II. Nichols, Past President
of the Society of Chemical Industry, was followed by an address
of acknowledgment by Mr. Rossi. The addresses are printed
in full herewith.
The usual informal dinner was held before the meeting in the
dining hall of the Chemists' Club, giving the members the op-
portunity of meeting the recipient of the medal. — Editor.
We will, therefore, proceed with our program, and hear an
account of Mr. Rossi's life and work from a gentleman well
known to you all, Mr. Francis A. J. FitzGerald, Past President
of the American Electrochemical Society.
National Gem and Mica Company
New York City
INTRODUCTORY ADDRESS
By Jerome Alexander
Nothing could be more illustrative of the cordial solidarity
that unites us to our Allies. England and France, than this
evening's meeting; for here before the New York Section of a
British Society we air about to award the Perkin Medal to
Auguste J. Kossi, a native of France.
France I How the hi in, yes, of every
true democrat throughout the world, leaps at the mention of
that n.nii' I her fields and beautiful her cities, but
France is inn. h HI all these her artistic, literary,
scientific and spiritual gifts to humanity and civilization have
1 'i hei debtors toi all tune; and to d 1 ,1 world
is fighting undei hei slogan of "Liberty, equality, fraternity."
As a consequence of this dreadful war. and under the lash of
its stern necessities, we have Fortunatelj been brought in closet
relationship with our French fellow chemists. For some months
past we have been planning the Formation of a New York
Section of the French New.;, it Ckimie IndustrieUe, tin sistei
societ] of the British mical Industry; and to-night,
immediately following our meeting, it will be formally organized
MR. A. J. ROSSI AND HIS WORK
By F. A. J. FitzGerald
It was, I think, in the year 1899 that I first made Mr. Rossi's
acquaintance. There was much speculation in Niagara Falls
at that time as to what he was doing. In those days there was
always much gossip whenever some new work was started at
Niagara Falls for it was still in the early period of power develop-
ment before the MacFarlands and politicians got busy and we
were all watching eagerly the rapid electrochemical developments,
- aluminum, carborundum, caustic soda and chlorine, calcium
carbide, etc. Wonderful stories would float about as to what
newcomers were doing. When the 1 lldbury Chemical Company
started. the most astonishing storu s were afloat, caused I think
largelj by the high brick wall winch surrounded the factory.
: breath that this works was engaged in the
manufacture of cordite by a new and secret process and that you
could not gel inside the brick wall except over the body of an
armed guard.
I cannot recall now what various stories were told about
some remarkable work in the Porter house and the old stone barn
which stood where the Acheson Graphite Company's plant now
is. but these were sufficiently startling, and all agreed that it was
a French Chemist named Rossi who was working on some new
invention.
acquaintance, for in the electrochemical
work of those days there was a tine spirit of cooperation, which in-
deed has become to a great extent permanently characteristic
of Niagara Falls, and before lou, 1 gol to know him very well.
During visits to him I learned a treat deal about his researches on
the smelting of titaniferous ores, about the experiments he was
then making on the manufacture and use of ferrotitanium and
Feb., 1018 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
139
about many other chemical and engineering works with which he
had been associated in his varied professional career. Although
I may repeat some things which Mr. Rossi speaks of himself, I
believe you will be interested in a brief history of his work.
In the year 1855 at the early age of 16 Rossi graduated from
the University of France with the degree of Bachelier des Sciences
et Lettres and four years later, after he had also graduated from
the Ecole Central of Arts and Manufactures, where the studies
covered mechanical, civil and metallurgical engineering work,
he came to New York. Here he soon obtained a position as
assistant engineer with the Morris and Essex R. R., holding this
until 1864 when the railway was taken over by the D. L. and W.
After this he got a job which kept him busy for a year making the
survey of a property in Boonton, N. J., which was to be converted
into a park under the
direction of Mr. Calvert
Vaux, the architect of
Central Park, New York.
Next we find him engaged
in building a railway to
the Boonton Iron Works;
but when Fuller, Lord
Company of that concern
found out that Rossi had
studied chemistry and
metallurgy at the Ecole
Central they put him in
charge of a laboratory at
the Iron Works.
It was here that Rossi's
attention was first called
to titanium, for the ores
used in the blast furnaces
at the Iron Works were
magnetites from Morris
County, N. J., containing
in the best samples about
one per cent titanic oxide
and in others 2.5 per cent
or more. Beyond noting
the existence of titanium
in the ores Rossi was not
particularly interested in
it until he met the work
of Professor Cook, the
State Geologist of New
Jersev. This work called
attention to the existence
of titanium in nearly all
the New Jersey ores, from
fractions of one per cent
to as high as 15 per cent
titanic oxide. Professor
Cook also established a
relation between phosphorus and titanium in the ores, low phos-
phorus apparently going with high titanic oxide content. This
set Rossi to work hunting up all the scanty, and incidentally
very contradictory, literature he could find on the subject of
titanium. None of this work was of any practical importance
so far as the running of the Boonton Works was concerned, but
several years after he had left his metallurgical work to devote
his attention to tests on the pumping engines at Fall River, to
calculations of the stability of the Beaver Bridge Dam, to work
on refrigeration and the manufacture of ice-making machinery,
: BXi hea on titanium became of value because of a law suit
in relation to his old firm of the Boonton Iron Works.
This law suit was of great importance so far as Rossi's future
work was concerned as it no doubt established his reputation 1
AUGUSTE J. ROSSI. PERKIN MEDALIST, 1918
an expert in the smelting of titaniferous iron ores. Thus, after
Rossi had established an office in New York as a consulting
engineer and when in 1890 Mr. James MacNaughton was inter-
ested in the development of the immense titaniferous ore deposits
of the Adirondacks, it was to Rossi that he went for advice.
Since that date Rossi has devoted most of his time to titanium.
The problem presented in this case was a study of the feasibility
of smelting the titaniferous ores of the Adirondacks. Rossi,
as a result of his researches years before, was well acquainted
with what had been done in Europe in this field and of special
interest were the records he had of some blast furnaces near
Stockton-on-Tyne, England, where ores running as high as 35
per cent titanic oxide had been smelted successfully by forming
a slag that consisted of a silico-titanate of lime. This, of course,
involved adding consider-
able quantities of lime
and silica to the charge.
Here lay the great ob-
jection to the Stockton-
on-Tyne practice, for on
account of the low iron
content of the ore it was
necessary to make about
4 tons of slag for 1 ton of
iron.
Rossi told his client
that success with the
Adirondack ores could be
obtained provided that
the titanic oxide could be
slagged off without using
an enormous excess of
fluxes and that so far as
the pig iron produced was
concerned, it would prob-
ably be of a very superior
quality.
The upshot of the con-
sultation was that Rossi
went to examine the ore
deposits and two small
blast furnaces which had
been run there by Mr.
MacNaughton's grand-
father from 1840 to 1858.
In a curious old iron chest
Rossi found the blast
furnace records. Study-
ing these and knowing the
composition of the ore,
the fluxes added and the
amounts of these going
into the charges of the old
blast furnaces, Kossi
found thai the practice oi the Stockton-on-Tyne furnaces had
been anticipated. He also found that the iron produced was
of such superior quality that a Gold Medal had Ween awarded
to it in the great London Exhibition of 1851. Moreover, certain
steel made from this iron won liii;li commendation from the Navy
Springfield and Washington, the report stating thai
11 compared favorably with the best Swedish steel.
iii' 11 began a series of experiments on slags with the ob-
ject of replacing silica with titanic oxide in the normal blast fur-
nace slag and. following his success in this diret tion, built what
might be described as a laboratory blast furnao in which several
hundred pounds of excellent pig iron were made from thi titanii
erous iron ores. Next followed a small blast furnace built
at the New York Car Wheel Works in Buffalo, where the Mill
140
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 2
Pond ore running 16 to 17 per cent iron was successfully
smelted.
In this way Rossi did the pioneer work in demonstrating the
value of the great ore deposits of the Adirondacks in 1894.
Twenty years later we find this work confirmed by Mr. Frank E.
Bachman, General Manager of the Maclntyre Iron Company,
Port Henry, N. Y., in an interesting paper, "The Use of Titanif-
erous Ore in the Blast Furnace," presented to the American Iron
and Steel Institute in October, 1914.
Turning now to ferrotitanium — Rossi was convinced from
what he had observed in the work on smelting titaniferous ores
that titanium had a beneficial effect in the manufacture of iron.
A natural deduction from this was that an alloy of iron and titan-
ium would be of value for the treatment of iron and steel in the
process of manufacture.
This led to a series of experiments in small electric furnaces and
finally to the construction of larger furnaces in Niagara Falls in
1899 where considerable quantities of ferrotitanium were manu-
factured, thus permitting of a great number of tests being made
on a large scale in steel works and foundries.
This may be considered as closing the experimental period in
the development of the manufacture and use of ferrotitanium.
Rossi had now convinced himself of its value and the next prob-
lem was the education of others in its use.
I shall not go into the consideration of the commercial de-
velopment of titanium, but merely discuss the principal causes
of the great difficulty Rossi experienced in convincing the tech-
nical world of the value of his invention.
Perhaps this may be most vividly shown by means of an
analogy presented by the practice of medicine. There are a
number of drugs of known value, some of them absolute specifics,
in the treatment of human ills, but every year we have added to
our drug list a number of new medicines. Some of these are at
once recognized as of real \ alue by a few, but it often happens
that their general recognition is delayed by the exaggerated
enthusiasm with which they are greeted at their first appearance;
moreover, it frequently happens that the injudicious use of the
new drug gives it a bad name. Now, there cannot be any doubt
that the very same causes which often delay true appreciation of
a new medicine existed in the case of ferrotitaTiium. Among
some there was an unwarranted enthusiasm as to the field of its
usefulness and there were plenty of examples of complete failure
in its application due simply to ignorance of the proper methods
of using it. While, therefore, the value of ferrotitanium has
always been recognized by some, there existed for a long time a
prejudice against it in the minds of many and in some quarters
this exists even to-day. Thus, in spite of all Rossi showed as
regards the possibilities of titanium seventeen years ago, skepti-
cism was for long very general and is not yet completely elim-
inated. I hope, therefore, that you will pardon me if I call
attention to a brief note I made some three years ago on certain
statistics in regard to the use of titanium iu rail Steel, which I
think very clearly disposes of the assertion frequently made at
that time, that titanium has no effect on steel.
In this note are given the statistics of 155 heats representing
the production of 90OO tons of rail steel, in some of which titanium
was used while in others it was not Where no titanium was used
only 36 per cent of the steel came within the particular specifica-
tion limit. Where 0.053 l"'r cent of titanium was used 43 per
cent passed, with 0.077 per cent titanium 84 per cent, and with
0.10 per cent titanium too per cent passed.
In the earlier days of the exploitation of titanium the chief
drive was made on its use in rail steel and the data I have given
show something of what can be done in that way. But of recent
years much greatei efforts have been expended in applying titan-
ium to miscellaneous steels. Thus in the last ten years the ratio
between titanium going into other kinds than rail steel has enor-
mouslj increased, for while a decade ago the miscellaneous appli-
cations were only 1 2 per cent of the total, they are now 96 per cent
and have increased in volume about 150 times.
Thus Mr. Rossi, after more than a quarter of a century of work
followed with the greatest perseverence and undaunted by diffi-
culties of all sorts, has not only shown what can be done with the
titaniferous iron ores formerly regarded with distrust by the iron
smelter, but has demonstrated that the very element supposed
to make these valueless can actually be used for improving the
manufacture of the metal they yield.
The FitzGerald Laboratories. Inc.
Niagara Falls, N'. Y.
PRESENTATION ADDRESS
By William H. XicbolS
The world is beginning to get a gleam of what it owes to the
chemist, and the chemist himself is beginning to be better under-
stood. As a rule he works so much in the quiet of his labora-
tory and without the aid of that publicity which is such a promi-
nent part of our life to-day, that many of his most important
discoveries are made known only to his fellow chemists, who
in turn incorporate them in their own fund of knowledge and
thus make use of them. Once in a while, however, something
very striking comes out of a laboratory and attracts attention
by its novelty, or by its usefulness, or both Under this cate-
gory comes the wonderful discovery of young Perkin which has
given to the world, through those who have succeeded him, the
great synthetic dye industry, the long list of synthetic remedies,
and the various contributions to the "gentle art of war," which
have followed Perkin's original work What wonder, therefore,
that when fifty years had elapsed, the chemists of the world
should fittingly celebrate the work of the young Englishman,
and what wonder that the occasion should be seized upon for
the founding of a medal to be given to those who, following
Perkin, should give to the world something of themselves which
should forever be of great value to all mankind. Thus the
Perkin Medal was founded, and thus it has annually been be-
stowed upon some great man who has made the world a better
place to live iu because he has lived in it himself.
Since the founding of the Medal, we have been exceedingly
fortunate in having it presented annually by our own Professor
Chandler, who was the first American selected to fill the great
office of president of the Society of Chemical Industry. We have
been in the habit of looking forward to these annual occasions
and the part which Professor Chandler would take in them, and
I am sure we all greatly regret that he has not found it practica-
ble to be with us to-night to assume this duty which we are so
in the habit of associating with him. Unfortunately, his health
does not permit it, but let us hope that next year, and for many
more to follow, he will stand in this place and perform this act
in his usual graceful manner. It, therefore, falls to my lot as
the next succeeding American president to present the Medal,
and this task I undertake with great diffidence, feeling, as I do
the disappointment which you all sustain in not hearing from the
grand old man himself. It is not, however, the first time in
which I have undertaken this work, ;is I had the honor of pre-
senting the first Perkin Medal to Perkin himself during the
jubilee celebration in New York
It is particularly appropriate that this Medal should be pre-
sented at one of the stated meetings of the New York Section of
that great English Society of Chemical Industry which counted
among its presidents so many great Englishmen, including
Sir William himself. During the recent terrible years, the mem-
bers of this Society have almost remade Great Britain from a
chemical standpoint. Similar work of the highest grade has
been accomplished by our French brethren American chemists
have taken great interest in the Rritish society, and they are
now to have an opportunity of doiug similar work for the Soci£t£
de Chimie Industrielle, the New York Section of which is to
Feb., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
141
be formed to-night. We have always had a warm place in our
hearts for our French friends and I am glad that we are going
to have an opportunity of again proving this, if any proof be
necessary.
You have heard from Mr. FitzGerald a statement of some of
the work which Mr. Rossi has done and it is not my intention
to add to that list a single statement. If Mr. FitzGerald has
omitted anything, Mr. Rossi himself will please supply as much
of the deficiency as his modesty will permit.
CONFERRING THE MEDAL
Mr. Rossi, there have been several candidates for the honor
which is to be conferred upon you to-night. The claims of each
have been carefully weighed by a committee, whose only desire
has been to select the candidate best qualified to receive the
Medal this year, when everything has been considered. You
have been their choice, and are, after a long life full of hard work
and the usual disappointments that come to every successful
man, to receive the greatest reward which your fellow chemists
can bestow upon you You are joining a body of very brilliant
men. You may well feel gratified that those who know best
consider you worthy of the honor of that company, and in token
of that selection I beg to express to you, what I am sure is the
thought of every man in this room and of every other who knows
of your work, our hearty congratulations on a life well spent,
and our cordial "bon voyage" as you turn your face to the
setting sun. Coupled with this is the hope that you have be-
fore you yet many days of usefulness, and that you will be
able to return our confidence with something accomplished of
even greater value than what has gone before. With the heart-
felt respect of the entire chemical fraternity, and a hand-clasp
as its token, it is my privilege to present to you the Perkin
Medal of 1918.
New York City
ADDRESS OF ACCEPTANCE
By Augusts J. Rossi
I am not much used to making public speeches. True, once
upon a time, I was asked by the president of the Polytechnic
Department of the American Institute to deliver a lecture on
"Ice and Refrigeration" at Cooper Institute. It seemed to be
appreciated, at least so the president told me, but it was very
long ago, so long that I am afraid I have forgotten about it.
It was on a subject with which I was familiar, but to-night
I have not only to speak on a definite subject of applied science,
but to express my feelings for the distinction you have conferred
on me and of which I appreciate all the honor. I have had oc-
casion to notice that sometimes brilliancy of diction covers a
multitude of sins, but to such brilliancy I cannot lay claim.
However, there is another aspect to the question to-night — one
which tells — it is the part which comes from the heart, the part
which makes one say what he feels, not the way in which he
expresses it, and that is precisely my case to-night, so I will let
my feelings speak, not my oratory.
By your conferring on me this honor, I see an appreciation,
a recognition of a continuous and continued work in lines which
had not been much investigated before, so far, of course, I mean,
as their industrial possibilities. I thank you heartily for this
honor, personally, but also because it will prove an incentive
for me and for others to devote to any researches they may pur-
sue, this truthfulness, this interest that any professional chemist
or technical investigator worthy of the name must give to his work.
This I have tried to do and I see to-night with all my heartfelt
thanks and appreciation that it is to this devotion to science,
to this perseverance in working out a comparatively new prob-
lem, to the sincerity of the work done as much as to its value,
that you have conferred this honorable reward to stand as a
beacon to guide others, entering young in the career, to be as
thorough, as devoted to an idea, as conscientious in recording
results, as they can be. It is in part, I am sure, to this perse-
verance in trying to overcome such difficulties as have arisen,
such criticisms and doubts as have been expressed that you
have given your appreciative recognition by this honorable dis-
tinction you have conferred on me, and which can only en-
courage me, even at this stage of my life, to persevere to the end
and develop certain possibilities of titanium compounds for
other than metallurgical purposes, in other branches of industrial
chemistry; and now that I have let my feelings speak and ex-
press how proud I am of the appreciation of my peers, I may be
allowed, as an interesting history of the case, to explain to you,
as briefly as possible, what little encouragement I could find in
what had been written on the subject in a literature curiously
contradictory and so many times misleading.
My special attention was called to the subject of the possi-
bilities of titaniferous iron ores in 1890 by Mr. James Mac-
Naughton, a graduate of Yale, interested in these immense
Adirondack deposits, as an inheritance from his grandfather,
Mr. Maclntyre — deposits of such a magnitude that Mr. Berken-
bine, then president of the American Institute of Mining Engi-
neers, at the Montreal meeting of the Institute in 1893, said of
them, "these marvelous deposits seem to have been placed by
Providence where most inviting, as they can be made available
to tide water." I had been directed to Mr. J. MacNaughton
by Professors Chandler and Rickett, as one who could give
information on this subject as I had had occasion before to
write a paper entitled "Titanium in Blast Furnace" for the
Journal of the American Chemical Society.
Having been for some eleven years (1864-1876) technical
director of the Boonton blast furnaces (Boonton Iron Works,
Fuller, Lord Co., proprietors), I knew from actual practice that
the presence of titanic dioxide (Ti02), averaging 1.50 per
cent in Morris County, New Jersey, ores which we were
smelting and 2 to 2.50 per cent in our slags, had had ab-
solutely no effect on the working of our furnaces, or the
behavior of our slags as to fluidity and fusibility, so much
so that I even ignored its presence, considering it as so much
additional silica in the ores.
And still when the question of smelting these ores, alone or
in mixture, arises, one can read in the proceedings of a well-
known scientific technical society (A. I. M. E.) "that 1 per cent
of TiOj in a slag was enough to make it pasty to impossibility
of tapping " The advanced copy of the paper (in my hands)
says, "the slags had to be pulled out with tongs." How can
young men, new in the profession, be blamed for being skeptical
about the smelting of this class of ores after such statements
as I have quoted verbatim?
In 1876 the death of the two owners of the Boonton Iron
Works and the legal complications it involved between the
estates forced the closing of the works, involving rolling mills,
plate mills, puddling and re-heating furnace, nails machines,
etc. The furnaces were blown off, but not dismantled. Work-
men and all had to leave and the small town was deserted for
several years.
Later on in the 8o's, Mr. Eckert of Reading, Pa., who was
making there what is called stove iron, having decided to use
our puddled cinders of which we had the accumulation of years,
with some of our ores containing 2 per cent TiOj, leased the two
blast furnaces which were still standing with all the blowing
apparatus and appurtenances. They made a failure of this
run for technical reasons foreign to my subject and which could
easily have been foreseen by one familiar with blast furnace
work. Having stopped the furnaces after a very few months'
run, they tried to get out of their contract binding them to
use a stipulated number of tons of puddled cinders and ores by
claiming that the presence of Ti02 In OUJ cinders and ores had
been the cause of their non-success. I was retained as an ex-
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THE JOURNAL OF INDl STRIAL AND ENGINEER! \<, CHEMISTRY Vol. 10, No. 2
pert by the estate and had no difficulty in proving by my books
of analyses and statements of founder and keeper and others
that the presence of TiC>2 to the extent their own analyses had
shown in the materials of the charges was in no way greater
than the amounts that I had found during an eleven years'
practice to have had absolutely no effect on the working of the
same furnaces, so they had to compromise and pay a heavy
forfeit. I had to enter into these details to render intelligible
what follows.
The suit came before the chancellor of New Jersey and I have
on hand the brief submitted by the plaintiff, containing all the
sworn testimonies of their experts.
No. 1 — One of the experts, Mr X, manager of one of the
Durham furnaces (Cooper, Hewitt and Co.), testified, under
oath, that 0.75 per cent of TiO? in an iron ore rendered it unfit
for blast furnace purposes as it would be only a matter of a
short time before the furnace would be "clogged up" if the use
of the ore were not stopped.
No. 2 — Also a manager of another Durham furnace, Mr. Y,
testified, under oath, that not 0.75 per cent but 0.25 per cent
of Ti02 in an iron ore excluded its use in a blast furnace, it being
merely the matter of a little longer time before the furnace should
be clogged up.
No. 3- — Mr. Eckert, of Reading, Pa., under oath, testified that
from his 20 years' practice in iron making in blast furnace,
not 0.25 per cent, but traces of Ti02 were sufficient to produce
the same result as above mentioned, ores containing traces of
of TiOj being unfit for blast furnace uses.
This is only one of the many examples, if really a striking one,
of the criticisms, prejudices and objections f met with in my fight
for these much-abused ores. Such was the encouragement I
found in the profession. When in 1894, at the New York
Car Wheel Works, Buffalo, N. Y., in a small furnace of a capacity
of three to four tons a day, which I planned and erected,
at Buffalo, I melted, without mixture, titaniferous iron ores
from the Adirondacks, containing 15 to 18 per cent TiC>2 and
55 to 56 per cent metallic iron, the slags as run from the furnace
analyzed 25 to 30 per cent TiOs, with some 15 to 18 per cent
silica with lime, alumina, and magnesia as bases, magnesia
having been recognized by me as an essential constituent of
the slags to insure the best running. These ores, being inaccessi-
ble to a railroad had to be transported on corduroy roads at
that time to North Creek where they could be loaded on cars.
It brought their cost to $15 per ton delivered at Buffalo. This
excluded the idea of making a test on a larger scale, unless
we could find a furnace small enough, one of some ten tons'
capacity, which it proved impossible for us to do. Within
the last two years, Mr. Bachman has smelted similar titaniferous
iron ores in one of the large blast furnaces of Weatherbee-
Shcrnum & Co., at Port Henry, making with these ores some
15,000 tons of a pig iron which he found in the tests for tensile
or transverse strength of superior quality. In a very elaborate,
comprehensive, scientific and technical report, Mr Bachman
has given tin- fusibility and fluidity of the titaniferous slags
run in the furnace, analyses of all materials and results of tests
1 gth as compared with those of the average pig irons
run without titaniferous iron ores in the charges. His con-
clusion .^ a whole is a confirmation of my own as drawn from
this run in Buffalo in 1S94-95 in my small furnace. One of
them particularly is worth mentioning, as I had come to the
same Conclusion in Buffalo. He says. "This run with titanifer-
ous ores was made with an economy of fuel per ton of pig metal
smelted," ami one can read in technical publications in 1894
that tin- smelting of titaniferous ores even if admissible meant
such an excessive consumption of fuel per ton of iron, that on
this score alone they are unsuitable, leaving aside titanium de-
posits 111 the Furnace and pasty slags,' .111 obvious contradiction.
If the furnace is to be "clogged up," as claimed, by titanium de-
posits which remain in the furnace, they do not go into the
slag and the latter need not be pasty on this score, or, if it goes
into the slags making them pasty, it does not remain in the
furnace as titanium deposit. These titaniferous ores of the
Adirondacks are magnetic, associated with ilmenite (FeTiO»),
an iron titanate, just as iron silicate is found (FeSiOa) in cer-
tain ores (ferruginous periodotite) . They are like almost all
titaniferous ores, low in phosphorus and sulfur, some as low in
phosphorus as 0.017 per cent and sulfur 0.02 per cent, with 55 to
56 per cent metallic iron and little silica, 1.50 to 2 per cent.
The iron smelted from them is an ideal open hearth steel and
to-day open hearth steel has superseded Bessemer steel.
Tests made by me and in many foundries of such pig metal
added to ordinary pig iron in certain proportions have shown an
increase of strength over cast iron not treated, of 29.5 per cent
in tests made and reported by Wm. Cramp and Co. and an in-
crease of 4 per cent over cast iron treated with nickel.
These titaniferous iron ores, at least those found in the
Adirondacks, are of plutonic origin. Professor Kemp told me
they are not stratified or in veins but the metallic mass seems
to have been pushed through the rock formation in fusion.
He showed me photomicrographs in which you could see the
rock, perfectly distinct and clear from ore, with big black patches
of titaniferous ores free from rock. A corroboration of this
fact is found by soundings made at the foot of a solid wall of
ore, some 400 ft. wide and some 50 ft. high. The soundings
at the foot of this ore wall went down 450 ft. of ore with only
10 per cent of rock, so the word inexhaustible seems not to be ex-
aggerated as applied to these deposits as, on that property, the
same kind of ore has been prospected on some 9000 acres. I
have always claimed that these ores and similar ores would
prove the resources of the future. Abundant, rich in iron,
50 per cent or more metallic iron without concentration, free
from phosphorus and sulfur to such an extent as they are found
to be, they are what were called Bessemer ores par excellence;
and ores of this kind non-titaniferous, low in phosphorus, have
been taxed to the utmost, so much so that what was called the
Bessemer limit in phosphorus for steel making, had to be raised
from a few hundredths of 1 per cent (0.08 or less) to 0.10 per
cent.
If such work as I have done, confirmed by the very recent
blast furnace runs on a large scale made by Mr. Bachman,
has had arrd will have the result of calling the attention of the
metallurgists to these much-abused ores, I will not have worked
in vain.
But however much value these ores may have, alone or in
mixture with othei ores as blast furnace stock, their use for
making alloys of iron or copper with titanium for the treat-
ment of cast iron, steel, copper or copper alloys has opened
a new and more important field of applications in metallurgy.
Cheeked by the difficulties I met in securing such large quan-
tities of ore as are required for blast furnaces of the size and
capacity of our present furnaces, as explained above. I pro-
posed to Mr. MacXaughton in 1900 to make, so to speak, a
concentrate of titanium which, added to ordinary cast iron or
steel, would be likely to secure for the metal baths thus treated
the same beneficial influence which tests had shown to be se-
cured in pig metal smelted from these ores. TiOi not being
reduced to any great extent by carbon at the temperatures
prevailing in the blast furnace, I had to have recourse to electricity.
And I may say here that Mr MacXaughton was the one who
supported me in these times of trial by his implicit confidence
in me and in the possibilities of my work He died in 1905.
About 1900 I started making ferrotitanium at Niagara Falls
at the old Porter house by the electric current, the furnace it-
self, made of a masonry of graphitic materials, forming the
cathode, and a carbon electrode, movable vertically in the cavity
of the furnace by means of proper mechanical device or auto-
Feb., 1918
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
143
matically by the current itself, forming the anode. It was an
arc furnace. A mixture of the titaniferous material and of the
carbon required for the reduction of both the Ti02 and the oxide
of iron, properly comminuted, was then charged gradually into
the furnace as the current was turned on. Whenever the rela-
tive proportion of the Ti02 and the oxide of iron of the titanifer-
ous material were such as to produce an alloy higher in titanium
than desired some scrap iron was charged with the mixture to
dilute the alloy, so to speak. I made in this manner alloys con-
taining from 10 to 25 per cent or more, but practice in steel and
other works has shown that an alloy containing some 15 per cent
of titanium, or thereabout, was best suited for most purposes.
Whenever the presence of carbon in the ferrocarbontitanium
was considered objectionable for special applications, I reduced
the titaniferous materials by my aluminum bath process. In-
stead of using a mixture of finely powdered aluminum and ti-
taniferous materials as per Dr. Goldschmidt's Thermit process,
the aluminum I used for the reduction of the oxides was melted
in the electric furnace and the titaniferous materials (omitting
the carbon) charged directly into the bath of aluminum. In
such cases I used preferably Ti02 as rutile, in order to avoid
using the aluminum which would have been required for the
reduction of the oxide of iron of the ore, charging scrap iron with
the rutile to dilute the alloy to the content of titanium desired.
In this manner I made ferrotitanium practically free from carbon,
containing only from 0.18 to 0.50 per cent carbon more or less,
and by reducing the amount of scrap iron added, I was able to
make ferrotitanium containing as high as 80 to 85 per cent
titanium. Titanium as a metal is as white and as shining as
silver but very hard and brittle, so that, as such, it has no particular
use. The high alloys of titanium, such as 75 to 85 per cent of
titanium and even those with less titanium, are also white like
silver and scratch glass and even quartz deeply
This aluminum bath process is of a more general application.
If into the aluminum bath a tungstic ore containing oxide of
iron is charged, a ferrotungsten is obtained free from carbon.
I have made thus 85 per cent tungsten alloy.
By using manganiferous ores I was able to make in the elec-
tric furnace 85 to 88 per cent ferromanganese free from carbon;
by using chromic iron, a ferrochrome at about 80 per cent
chrome, free from carbon.
The advantages of the electric furnace and of the use of baths
of aluminum lie in the fact that if the reduction can be secured
in a blast furnace as for ferromanganese, for ferrochrome, ferro-
tungsten, and other ferroes when high in the constituent metal,
the ferroes obtained would be melted with difficulty, if at all,
in the blast furnace in certain cases.
By adding to a bath of steel, for instance, or to cast iron a
ferrocarbontitanium containing some 15 per cent of titanium,
the bath of metal was cleansed of dissolved or occluded gases
such as oxygen and nitrogen and also of such oxides of iron gen-
erally present in steel, especially in Bessemer steel made by the
pneumatic process. When air is blown through the molten
pig iron, the titanium of the alloy combines with the oxygen to
form TiOj, with the nitrogen to form titanium nitride, and the
oxide of iron is reduced to iron by the titanium and the carbon
of the alloy, the titanium combining with its oxygen to form
T1O2, and the slag, carrying with it the titanic dioxide and the
titanium nitride, rises to the top of the ingot or ladle, the TiOi
rendering the slag more fluid and fusible as experiments I have
carried on for Dr. P. H. Dudley, the expert of the N. Y. C. R. K.,
have proved. A slag collected by him at the top of an ingot and
containing 6.5 per cent of Ti02 had a melting point of 1290° C,
lower than or about the same as that of ordinary blast furnace
slag. By adding enough TiOj to such a slag as to have in the
slag some 13 per cent Ti02, its melting point was lowered to 11900
C, as determined by Mr. FitzGerald. This infusibility of titanic
slag was another objection I met to the use of these ores; it can
be read in the Geological Survey of New Jersey in an article on
the refractory properties of fireclay that 3.50 per cent of Ti02,
frequently met with in these clays, lowers their melting point
two or three cones of Ziegler. "So," it is added in this report,
"Ti02 must be considered in these clays as a flux." As traces,
or only a few hundredths of 1 per cent at most, of titanium are
found in the steel treated, the titanium seems to act as a scaven-
ger, as it has been called sometimes.
The presence of titanium in steal to the extent of 1 per cent or
more imparts to the steel certain very special properties to which,
later on, I may have occasion to call attention more particularly.
The head of a crucible steel ingot treated with titanium, cast
in 1900 at Atha & Illingworth's, East Newark, was drilled with
five holes to obtain specimens for analysis. These holes are
as bright now as they were when first drilled, though exposed to
the air in my office. It contains 1 to 1.10 per cent titanium and
the sheet was so hard that it was drilled with difficulty.
Copper, as is well known, absorbs, when melted and exposed to
air, a large amount of gas and the bath contains oxide of copper.
For the treatment of copper and its alloys such as bronzes,
brass manganese or aluminum bronzes I have made a copper-
titanium containing any amount of titanium, though 10 to
15 per cent appears best adapted. The titanium of such an
alloy acts, as in steel, as a scavenger of the copper bath. I have
also made aluminumtitanium containing 45 per cent titanium
for seasoning aluminum bronzes. They are made in the same
manner as ferrocarbontitanium or ferrotitanium in the electric
furnace. For coppertitanium, Ti02 and aluminum are charged
in the furnace in a bath of copper. For aluminumtitanium,
the Ti02 is charged directly in the bath of aluminum. The re-
action of aluminum on oxides being exothermic, much less current
is required for the reduction proper.
As is well known the affinity of titanium for O and N is such
that the metal burns at 8oo° C. or thereabout in an atmosphere
of these gases (Wohler and St. Claire Deville). It is such that
when large cakes of alloy free from carbon, such as we make,
are cast in the casting trough from the furnace at a dazzling
white heat and broken while hot, the section exposed to the air
colors itself with fine irisations presenting all the colors of the
rainbow; blue (probably TiO), gold (probably nitride), copper
color (probably cyanonitride formed by the small amount of
carbon still present in the alloy) and combinations of these
colors. I have been able to reproduce these irisations artificially
on small pieces of alloy. These pieces look like gems, scratch
glass deeply and even cut it. I had occasion to show samples
of these at a meeting of this Society last year. All the details
of these operations have been fully described in the patents
which I have secured for our company, as also in many articles
which I have written on this subject in technical publications
here and abroad. In short, this modest beginning at the Porter
house has developed into the manufacture of these alloys for iron
and copper on a scale which requires the labor of several hundred
men.
Some of my work has been in an entirely different line, I have
used for purposes of artificial production of cold instead of
liquefied gases such as sulfur dioxide, carbon dioxide, or ammonia,
a binary liquid composed of one moderately volatile liquid
holding in solution the vapors of a much more volatile liquid.
In ice-making and refrigeration the volatile liquids are charged
in a special vessel, the refrigerator being immersed in a bath of
uncongcalable liquid so called, such as a strong solution of sodium
or magnesium chloride, or glycerine; or indirectly, by causing
this liquid to circulate in a tank in which cans, containing the
water to be frozen, are immersed, or circulated through pipes in
the cellars of the brewery or storeroom. By relieving the pres-
sure of the volatile liquid on itself, at ordinary temperature, by
mean of a double acting pump run by any power (steam engine
or other), the liquid boils and by its latent heat of evaporation
144
THE JOURNAL OF INDUSTRIAL AND ENGINEERING I ///. UISTRY Vol. 10, No. 2
cools the refrigerator contents. The vapors entering the pump
are compressed in a condenser cooled by circulating water, are
liquefied again under this pressure and cooling, and combined
again, re-forming the original volatile liquid, which is returned
by proper devices to the refrigerator, rendering the operation
continuous.
One of the binary liquids I proposed and used for machines
erected in breweries and cold storage plants was ordinary ether
holding in solution sulfurous dioxide. Ether will absorb its own
weight of S02, showing but a very few pounds of pressure (5 to 6 lbs.)
per sq. in. at 90° F. By using such binary liquid instead of
SOs, for instance, when the mixed vapors enter the compressor
to be compressed and discharged into the condenser, ether lique-
fies first being cooled by the circulation of water around the con-
denser, absorbing anew the SO* and causing the pressure in the
compressor and condenser to reach the figures it would have
reached had SOj alone been used, thus saving on the mechanical
power required. I have a patent in collaboration with Mr
Tessie Du Motay for this system of refrigeration.
The other liquid I used was sulfurous dioxide which can ab-
sorb carbonic acid gas to the extent of some 5 to 10 per cent of
its weight. In this case, the same advantages as with the ether
binary are secured, but to a much greater extent. C02 gas
boils at about ioo° F., and the pressures required to liquefy
its vapors are considerable. On this subject of artificial re-
frigeration and the thermodynamic questions it involves, I have
contributed several articles to the technical paper Ice and Re-
frigeration, published in Chicago, and to other technical publi-
cations here and abroad.
In the domains of metallurgy I have written a paper which
1 read at the meeting of the Electrochemical Society at Lynn
and Cambridge, Mass., on the utilization of the blast furnace
waste gases for generating power in gas engines for electrical
purposes or other. In districts in which pig iron is manufac-
tured on a large scale, as in the Pittsburgh district for example,
and even in others, the amount of these waste gases is far above
what is necessary to heat the blast and I proposed to use this
surplus in gas engines to generate power which could be utilized
for the blast engine, leaving a large surplus for generating elec-
tricity for illumination, making alloys of metal, or any other
purpose. In the paper I have written on this subject, assuming
the most conservative figures for the volume of such waste gases
and their calorific potentialities, it could be shown that after
having utilized for the furnace itself a part of it, a surplus of
some i.ooo.coo H. P. could be obtained in the Pittsburgh dis-
trict and some have placed this figure at nearly 2,000,000 H. P.
But assuming even a possibility of only 500,000 H. P.. what a
waste of power easily saved with gas engines, at a time when
waste counts for so much! Even in districts much less favored
than the Pittsburgh and more or less isolated, the same possi-
bility would exist for local purposes, and were electricity to be
generated it could be transported and utilized through a very
extensive radius. At the Falls we send electric power to
Buffalo, some 23 miles distant, and even to Syracuse, over 200
miles away. A careful scientific study of this question appears
to us to justify a more complete investigation.
Before dismissing this subject of titaniferous iron ore, I
will say a few words on the results I have obtained in experi-
ments made in smelting titaniferous ores in mixture with phos-
phoric ores even to the extent of obtaining a pig iron high in
phosphorus. I used phosphoric ores containing as much as
1.50 to 2 per cent of phosphorus pentoxide (P5O5). even adding
apatite (lime phosphate) to the mixture so as to obtain a pig
iron as high in phosphorus as I could. Contrary to what might
have been expected, the pig metal containing 0.40 per cent ti-
tanium and from 2.50103.50 per cent phosphorus had the strength
and the rating of fair No. 1 or No. 2 pig iron. This suggested
treating phosphoric pig metal, generally weak and close grained.
with ferrotitanium so as to incorporate a divided amount of
titanium in it. The results were very encouraging and were
published by me in a paper read before the A. I. M. E at the
Pittsburgh meeting in 1896. They were commented on in the
Engineering and Mining Journal.
I have proposed using copper titanium to treat the copper
which is used with gold and silver for coin or jewelry. The use
of the alloy making the copper denser and harder, the gold and
silver alloyed with such copper could be expected to be hardened,
which for coins would prove quite a saving in circulation or in
transit. The Philadelphia Mint considered this scheme very
favorably and asked us to make such alloys for them to try.
Obviously if there is anything in the scheme, such tests to have
any value should be made officially by the Government, and I
did not give any more special attention to it.
But if titanium alloyed with other metals has found important
and increasing applications in metallurgy, if its ores have been
shown to supply a valuable stock for blast furnace smelting,
other of its compounds possess such special properties as to
justify industrial application in other lines.
If a ferrotitanium, practically free from carbon, made by
my aluminum bath method, preferably as high in titanium
and low in iron as possible, is dissolved in hydrochloric acid, in
which it readily dissolves at a gentle heat, a fine violet solution
is obtained, a ferrous titanium chloride, and with such violet
solution I have been able to bleach cotton, silk and wool. As
is well known, silk and wool cannot be bleached in agents capable
of generating free chlorine which injures and attacks these
fabrics. Still I was able to bleach completely some 2000 yards
of such fabrics by digesting them in this diluted violet solution
at boiling temperature, for a shorter or longer time according
to the intensity of the dye to be bleached or the yellowish tint
of the white fabrics. Silk and wool, colored or yellowish, were
thus bleached without injury to the fabrics. Such double
chloride contained about 40 to 50 per cent titanous chloride,
TiClj, the balance being ferrous chloride. During the operation,
especially as the temperature approached the boiling point,
TiOj precipitated, thus showing clearly that the chlorine must
have been set free, and, as I explained it or tried to, must have
combined with the ferrous chloride to form ferric chloride,
the chlorine generated acting in the nascent state without even
appearing as free chlorine in the solution. The experiment
repeated several times with the same success was conclusive and
suggests the possibilities of a very important application.
The fact that the TiOs was precipitated from one of its com-
pounds by these organic matters suggested to me the possi-
bilities of precipitating TiOj from other of its compounds by
vegetable or animal organic matters and the results were very
remarkable. If to a solution of titanic sulfate, Ti(SO<)«, is added
a water extract of vegetable or animal substances and the liquid
gently digested to boiling and boiled for a short time, TiO»
is precipitated, and when calcined is obtained as a soft, smooth,
fiour-like, pure white powder requiring no mechanical pulveriza-
tion. This is so characteristic of the action of these organic
substances that a number of them, such as water extracts obtained
from dry leaves, green leaves, sawdust, tannin, wood pulp, wood-
pulp liquor, horsechestnuts, beans, docks, cranberries, radishes,
etc., and urea itself, have given the same result, a TiOr, smooth,
soft, pure white. One of the interesting features of this process
of obtaining TiOi as a pure white, smooth, and impalpable powder
is that if this same titanic sulfate solution be precipitated by
NHj or Na-O and boiled, and the TiOj calcined, the product is
granular and buff-colored. Even if this solution is freed by proper
treatment of such metallic oxides as .ire found in the ores and
remain in the solution during the process of extraction of the
melt, the T1O5 precipitated by alkalies is white but granular,
requiring mechanical pulverization for special uses. As by
Feb., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
US
addition of these organic extracts to the solution of crude titanic
sulfate, the TiOa precipitates white and smooth by boiling, it
must be that these metallic oxides are likely to form with these
organic matters, compounds which are retained in the solution
while the Ti02 precipitates. This seems to be confirmed by
experiments I have made, adding to the crude solution iron
oxide, copper oxide, manganese oxide, dissolved in sulfuric acid.
By boiling such solution with the same organic compounds as
I had used with the crude titanic sulfate solution without these
additions of metallic oxides, the Ti02 precipitates as a white,
smooth, impalpable powder. The patent for this method of
obtaining Ti02 white and smooth by means of organic substances
has just been granted within the last two or three weeks.
This method finds a direct application in the production of
a white titanic pigment, a product which our company, working
under several other patented methods, is to manufacture on
a large industrial scale in a special department of our works.
Ti02, calcined, possesses the remarkable property of covering
when used as paint material alone or in mixture with such other
pigments as are used in the trade for paints. Its superiority
on this score when prepared with proper oils over white lead
or zinc white is remarkable, and in addition, Ti02 pigment
is not attacked by sulfurous gases and is stable under climatic
and atmospheric influences.
I have found that TiC>2, obtained as a gelatinous titanic acid,
Ti02.2H20, and dried at 2i2°F., has the property of fixing color-
ing matters like that of alumina. It can be prepared by known
methods, but the one I have studied is much more economical,
as I can obtain it from a waste product of some of our manufacture.
In that state it dissolves readily in oxalic acid yielding a titan-
ium oxalate which can be used in the same manner and for the
same purposes as potassium titanium oxalate which is much
more difficult and costly to make.
Thanking you once more for the honor conferred on me,
I will show you some photographs of historic interest in the case.
1 — A photograph of the small furnace which I planned and erected
at Buffalo in 1894-95 to smelt titaniferous ores without mixture.
2— The old Porter house where ferrotitanium was made on an
industrial scale for the first time as early as 1900.
3 — The transformer room.
4 — My primitive laboratory.
5 — The furnace room.
6 — The furnace in operation.
7 — Titanium jewels and other specimens.
And for the convenience of those who might be interested
and cannot see them to-night I will leave them at the Chemists'
Club temporarily.
Niagara Fai,i,s, N. Y.
BRITISH PROGRL55 IN DYL5TUFF MANUFACTURE,
BRITISH DYES LIMITED1
By James Fa[.coner, M. P.
Gentlemen, I rise to move the adoption of the report which has
been circulated to the shareholders, and before doing so I would
like to state that Sir Gilbert Claughton, one of the members
of our Board, is unavoidably prevented from being present by
public business of an urgent nature, which makes it impossible
for him to leave London to-day ; and Dr. Forster, another member
of our Board, is at present in America conducting some investi-
gations. The circumstances under which this report has been
issued have been explained. The fact that we have not been
able to submit a balance sheet is due to its having been found
impossible, for an indefinite time, to arrange the allowances
and other amounts which have to be adjusted with the Ministry
of Munitions and the Inland Revenue Department, with regard
to the munitions levy and excess profits tax. You can under-
stand it is as much a disappointment to us as it is to you that we
have not been able to submit these figures to you in the ordinary
course, but it seemed to us to be better to have our meeting,
as many other companies have, and do our business, rather
than wait indefinitely before meeting one another to discuss the
work of the year.
Our subscribed share and loan capital, as on April 30,
1917, amounted to £2,084,138, as compared with £1,851,914
at the commencement of the year, being an increase of £232,224.
The number of our shareholders is now 1,445.
As regards the financial results of the year, it is not possible to
make any satisfactory estimate, and I shall, therefore, refrain
from submitting any particulars, except to say that I am sure
when we are in a position to submit them they will be generally
regarded as satisfactory. Our policy has been to charge prices
for our products which would enable us to build up a fund suffi-
cient tf> meet the great extra cost of constructing our works during
the period of the war, and with that fund to write off our plant
so as to reduce it to a reasonably low figure. We are satisfied
that the results of the year will enable us to go a long way in this
dire tion, to the extent of a good many hundreds of tl 9flnd
1 Chairman's Address delivered at the Second Ordinary General
Meeting of the Shareholders of British Dyes Ltd . HuddersBeld, October 31,
1917.
of pounds, but I do not want you to get any exaggerated esti-
mate of the profit we have made. Apart from the amount which
is necessary to enable us to meet the depreciation to which I have
referred and to pay the interest and the limited dividend, it
will be no object of this Company to make large profits, because,
being a controlled establishment, we should simply hand them
over to the Exchequer. We are assured and have the authority
of the Auditors for being satisfied that we may safely pay the
shareholders 6 per cent. The amount of the interest on the
Government Loan has been paid, viz., £40,615. The dividend
at 6 per cent on the ordinary shares will amount to £30,945,
making together £71,560. Whatever we may make, 6 per cent,
of course, is the maximum we are allowed to distribute.
Now, in dealing with the work which we have carried out during
the year, I would like the shareholders to realize that we have
three departments of work, each of them of great importance.
The first is for carrying out certain work of national importance
for the Government; the second is for the supplying of dyes for
the immediate needs of our shareholders; and the third is for
the building up of a national industry for the permanent supply
of dyes for this country.
First, as regards the Government work to which I have re-
ferred ; the situation did not permit me to refer to this question
in the previous year for reasons that no doubt will be obvious.
The position is that when we acquired the business of Read
Holliday & Sons, Ltd., there were certain arrangements in force
with regard to the work and certain negotiations were taking
place. A few months after we took over the business the ar-
rangements were all settled and new contracts were entered into
for different products, all of them of real importance. I am
glad to be able to say that we have punctually fulfilled all our
obligations and at present our deliveries are all months ahead
of our contract dates. At that time our deliveries were of vital
national consequence and when you cast your thoughts back to
the winter of 1915-16 and realize the extent to which the fate
of our armies and our country was dependent on such supplies,
I am sure you will agree with me that it is a matter of great
satisfaction that we were able to do the part we undertook to do.
I have heard, from time to time, the criticism that other com-
panies were confining themselves to manufacture of dyes and
146
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 2
we ought to have done the same. That has not been our view-
either of our duty or of the true interests of the Company
With regard to the immediate supply, by which I mean the
supply of the needs of our shareholders during the period of the
war, our output during the year has been substantially increased.
Now the output of colors is more than three times the amount of
the pre-war output, and when you consider that we have, in
addition, made most of our intermediate products and many of
our raw materials to enable us to increase our output, I think
you will agree that this is a very substantial effort to have
accomplished. Not only is there the question of volume, but,
as you gentlemen know, there has been an increase in the variety
of dyes which we have supplied. In addition to our own pro-
duction we have continued, as far as the means of transport
would allow, the supply of materials and intermediates to Swiss
manufacturers to enable them to produce dyes and to send them
back to this country, either through us or directly. The result
has been that by our efforts and the efforts of other dye manu-
facturers, the users of dyes in this country have been kept sup-
plied, not with all they would like to have or would require in
ordinary times, but sufficient to keep their works running, and
I believe there has been no unemployment in any trade through
want of a supply of dyes. When you recall the situation at the
time when the Company was originally formed and consider the
apprehension which existed that workpeople would be unable
to find employment through the complete failure of the supply
of dyes, I think you will agree that the fact that we have so far
succeeded is a matter on which we may congratulate ourselves.
I come now to the third branch of our effort, the laying of the
foundation of a permanent supply of dyes for the country.
1 have said we have produced already a considerable number of
colors which we were not able to produce before. We are pro-
ducing a series of colors which, although far from what ultimately
has to be done, is nevertheless a substantial list. We have during
the year increased the plants for intermediates, some of them are
in operation, others are being pressed forward, and we must
always keep in view, in estimating the amount of work involved
in the manufacture of these intermediates, that they require for
their operation general services on a very large scale, steam,
power gas, electricity, water, compressed air and also supplies
of acids and other raw materials. To provide these services
requires plant on a scale which can only be properly realized by
inspection, and I am to express the hope, on behalf of the Board,
that as many shareholders as possible will take advantage of
the invitation to see the works. Every building that we have
is already allocated to plant, a good deal of which has been erected
or is in course of erection. To some extent the allocation is
in respect of plant for which arrangements for erection are being
carried through. I have heard the criticism that wc have
built too much. As a matter of fact, it is quite the reverse.
We made it our policy to press on the building as fast as we could,
knowing that difficulties of labor were going to increase, but we
find that we have not enough in the way of buildings, and in
order to accommodate the plant for necessary intermediate
products we must erect further buildings. When you look at
the number of buildings we have put up, then I think you will
appreciate the effort which must be made in order to fill these
buildings with plant, and to supply them with all the services
necessary to enable them to be successfully operated.
Our procedure with regard to the erection of plant is as follows:
We must first get the process worked out in the laboratory — I
am dealing now with some processes that we have not hitherto
worked. Then we have an experimental laboratory containing
plant on a small scale, but with everything working according to
the ordinary commercial conditions, and the process is put
through that experimental laboratory. Difficulties are thus
discovered and remedied and then the plant is erected on a com-
mercial scale. All this takes time, because these processes involve
great care and considerable delicacy in their operation and a very
small error will upset a chemical process. When you find,
therefore, that a plant has been put up you will know that a
great deal of study and experiment has been devoted to the task,
from first to last, until the plant is completely erected and
working successfully. In addition to these works to which I
have referred, we have purchased a site suitable for the erec-
tion of dwelling houses, because we see that a real problem is
coming in regard to the supply of dwelling houses for our work-
people. There is a greater scarcity of dwelling houses in Hudders-
field than probably in any other part of the country, and dwelling
houses are very' scarce everywhere. We are also providing
canteens in our old works and in our new works for the con-
venience of our workpeople, and we have established a club for
our chemists.
Now that is a very sketchy outline of the work that we have
done, but I think I have said sufficient to justify me in asking
the shareholders to acknowledge the efforts which have been
made by Mr. Turner, by the chemists, by the engineers, by our
workpeople and by all our staff, in doing this work during the
course of the year with which we are dealing. All of them are
overworked, all of them are full of zeal and, so far as the Board
are concerned, they have all our most sincere gratitude for their
loyal efforts on behalf of this Company during a time of so much
difficulty. And I think the country also owes to them an ac-
knowledgment of the very special work they have been doing,
and doing with such complete success, so far as the national re-
quirements are concerned.
Now at the same time, while I am bound to recognize the work
which has been done, I am bound also to say, in perfect frankness,
that it is only the beginning of the work that has to be done before
you can have a really adequate supply of dyes manufactured
in this country. In the report there is mentioned the magnitude
of the German concerns with a capital of £35,000,000; and I dare
say yTou all must know something of the dimensions of the Ger-
man works. While of course their output has been far in ex-
cess of what was required for Germany alone, still one can form
some opinion of what will be required here in the way of chemists,
in the way of scientific work, in the way of staff, if we are going
to reach our goal. I am not in the least disposed to take a de-
spondent view but, on the other hand, I am not at all disposed
to underestimate the task we must perform, and I think it
is well that the shareholders should realize its magnitude. The
Germans have been working on this problem for over 30 years,
with thousands of chemists and with almost tens of thousands
of experienced workmen; and we cannot hope in a year or two
to come up alongside of them. It will require earnest work for
many a long day before this country reaches the position to which
it ought to attain in providing a supply of dyes sufficient for the
needs of this country
I should like to refer to the necessity of research. There are
two ways in which research can be carried out. There are the
scientists who study the properties of substances or groups of
substances, seeking to learn the laws which govern their action
without any immediate practical purpose before them. They
go out merely seeking for truth In this field Britain has always
been supreme. If you think of the great discoveries made in
science you will almost invariably find they are the work of
great British scientists. The discovery of the principle of syn-
thetic aniline dyes is an illustration of it. That was not dis-
covered by a man who was looking for a method of making a
mauve dye by a synthetic process. He was looking for some-
thing else altogether, carrying out, no doubt, his research in the
most scientific ami careful manner possible. Many other dis-
coveries of the first magnitude have been made by British scien-
tists. My belief is. and my confidence in the industrial future
of this country' is largely based on this, that the people of this
country have a genius for original discovery and invention
Feb., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
147
which is not surpassed by any other nation, and indeed, so far
as the history of the past shows, no other nation has attained to
our position in the field of original research.
But there is another branch of research, and that is the study
of the application of scientific principles to particular problems
and to improvements in methods of operation. Take a great
example, the following out with extraordinary zeal and at great
expense of experiments with a view to discovering how to manu-
facture synthetic indigo commercially. In this and many other
instances where the original principles have been discovered in
this country by British scientists, the application of them to
industry had been left to other people. Others have reaped where
our scientific men had sown. Here, we must admit, in the past,
has been our failing. I am not going to discuss the vexed ques-
tion as to who is to blame most. You must have an enlightened
far-seeing spirit of commercial enterprise, with a body of scien-
tific men sufficient to do all the scientific work necessary to carry
forward discoveries to practical operation and to overcome all
difficulties that arise in practical operations. My belief is that
the reason for which the aniline industry left this country was
that, at that time, there was not available a sufficient number
of chemists qualified to carry through the operations and to over-
come the difficulties. There was much enterprise among the
commercial people and if there had been a body of chemists,
trained and qualified to carry out chemical processes, then, I
think the aniline color industry would probably have been de-
veloped in this country as it has been in Germany. I do not
enter upon the dispute as to whether it was the commercial
men who were to blame for not encouraging the chemists,
or whether the blame attached to the chemists in that they did
not adapt themselves to the requirements of the commercial
men. The really important point is that they must combine.
I have dwelt upon this question because I want to say, and to say
it with all the power of which I am capable, that it is essential
to the success of an enterprise such as ours that a sufficient body
of qualified chemists be provided for the carrying out of the work
of the future.
We have established in different universities, colonies of re-
search students who are in our employment, and who are acting
under the guidance of Professor W. H. Perkin at Oxford; Professor
A. G. Perkin at Leeds; Professor R. Robinson at Liverpool,
and we are greatly indebted to these gentlemen for placing them-
selves at our disposal for supervising the work of these research
laboratories. We have research work constantly going on in
our new works laboratories and elsewhere among the chemists
employed in our works since, when a man is carrying on practical
work, you cannot prevent him, when he has got brains, from con-
sidering what better method could be devised for carrying out
his operations. In order to encourage the supply of chemists,
we have made an offer to the universities that, if they will send
us a qualified chemist, we will find him a post at a satisfactory
salary with an engagement for three years. It seems to me this
is the best inducement we can offer to any young man thinking
of working at chemistry. We are offering special facilities to
the members of our staff of chemists to pursue their studies either
in Huddersfield or in Leeds. In that way we are trying to make
the most of all the material that exists But there is a further
difficulty, viz., that of men, and we have made up our minds
that we will take special steps to encourage promising young
men to devote themselves to chemistry and to send them to
technical schools and universities, and to do whatever is best
for them. That, of course, will take time and cost money, but
no figure that anyone can think of would be too much to pay for
securing a really efficient staff of chemists for our work in the
future, and we rely upon the support of tin- shareholdei I
expenditure we may have to make in order to cany oul that
scheme. We have a long way to go. We welcome the help of
all the experts that we can get. I do not say that we
where near our goal, but we are earnestly and diligently pressing
forward.
There are two questions to which I should like to refer. The
first is that of the manufacture of indigo. You will remember
last year I stated the steps which we had taken to place ourselves
in a position to manufacture indigo and to tender to the Govern-
ment for the purchase of Ellesmere Port Works, and that we
were refused permission to tender. I said we had made every
effort to ascertain the reason for which we were not allowed to
tender, but had been unable to do so. In one quarter or another
attempts were made to cast some doubt upon the statement I
then made, and as the question is a matter of great consequence
for the user of dyes I will tell the shareholders exactly how it
stands. When we were asked to submit evidence of our ability
to manufacture indigo by the process at Ellesmere Port, we ap-
pointed a committee consisting of Dr. Forster, chairman of our
Technical Committee, Mr. Turner, Mr. Dean, chief chemist
at the Turnbridge Works, and Mr. Robinson, an engineer of great
experience and ability, one of the first mechanical engineers in
the country, who was good enough to place himself at our dis-
posal practically as soon as the Company was formed, and who
has knowledge of our plant and premises. They went to Elles-
mere Port and saw the plant there. They then went to France,
to Creil, and saw a plant similar in every respect, in practically
every respect — there were, I believe, some little details of no
consequence — similar to that at Ellesmere Port. They made
a report which was submitted on behalf of the Board to the Board
of Trade. Here is a passage from their report which deals with
our ability to manufacture: "The indigo plant at Creil is an
exact duplicate of the Ellesmere Port plant. The plant was
working on the occasion of our visit and we carefully investigated
its operation at all the important stages. We also obtained
from the chemist information with regard to the quantities,
proportions, temperatures, times, etc., required in the operation.
We entertain no doubt as to our ability to manufacture indigo
with the plant at Ellesmere Port. Further, we have provisionally
arranged with the Ministry of Commerce that if the Company
should acquire the plant at Ellesmere Port, the services of the
chemist, who is a French subject, and a mobilized soldier, should
be made available to assist the Company in overcoming any
difficulty which might present itself."
We sent that to the Board of Trade with the intimation that
if there were any doubts we would be glad to supply further
particulars upon any point. The answer we got was that, after
considering the reports of the two independent referees, to whom
the reports from Messrs. Levenstein and ourselves had been
referred by the Board of Trade, they had decided that Messrs.
Levenstein. and Messrs. Levenstein alone, should be allowed
to tender. We asked them again and again to state the reason
for which we were not allowed to tender. We failed to get an
answer. We asked for an interview with the President of the
Board of Trade and the whole of our Board of Directors at-
tended We repeated the question, but still without obtaining
an answer
There are two things for which we have pressed. We have
asked whether tne referees recommended that we should not be
allowed to tender We have got no answer to that, except that
the decision of the Board of Trade was given after considering
the report of the referees, and on further pressure we were told
that it was not a matter which was referable. But I have got
no answer to the question: ''Did they or did they not in fact
recommend that we should not be allowed to tender?" It would
i- to answer.
I asked a further question: 'in what respect did tin
consider that we were not able to manufacture by the 1
Port process?" but I have got no answer to that. Now I have
had a good deal to do with references of one kind and another.
We were asked to submit our statement and Messrs. I.i
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. t
were asked to submit theirs We were asked to pay half the fee
and I think we should have been entitled to know what was the
award and why it has been kept back. My reason for pressing
this is that neither of the referees was a practical man. They
were both eminent scientific men — teachers of chemistry — but,
so far as I am aware, neither of them had anything to do with
the operation of any chemical process in connection with dye-
making. The process so far as the scientific theory is concerned
was well known and the only question was how to operate a
particular plant, and in the face of a signed declaration and the
statement of responsible practical men that they were perfectly
satisfied they could manufacture indigo by that process — in
the face 01 that particular declaration it was not for two pro-
fessors to say offhand that these men could not do so. That does
not seem to be the way in which business of the greatest im-
pcrtance to the textile industries and to the country should be
dealt with. Until I am shown their report and told in what re-
spect we are unable to manufacture indigo by the process, I
decline to accept the view either of the Board of Trade or of the
distinguished referees whom they appointed. I always make
this reservation, I gravely doubt whether these referees made
any recommendation which would justify the refusal to allow us
to tender.
Now there is another feature in connection with this matter
to which I think it right to refer. At the meeting of Messrs.
Levenstein, Ltd., shortly after I made the statement, Sir John
Lonsdale, who is the Chairman of Messrs. Levenstein, Ltd.,
referred to my statement and said he did not think we had any-
thing to'complain of. The reasons he gave were: that they had
long and intricate negotiations with the Board of Trade on the
subject of the Ellesmere Port Works so far back as February,
19 1 6; that they were the first firm in the country to approach
the Board of Trade intimating their desire to purchase; and that
as soon as the Receiver or Controller told them the minimum
price to be accepted they made an offer to purchase at that price.
Now, in the first place. Sir John is misinformed in thinking that
he made the first approach on the question of Ellesmere Port,
because long before February, 1916, 1 had made enquiry with
regard to it, and I was told that the Government proposed to
continue working under a Controller. At the end of January
I heard, incidentally, from the President of the Board of Trade,
that the Committee which was dealing with the shutting down
of German concerns in this country was going to consider the
question of closing down the Ellesmere Port Works and of selling
them. I then intimated that we should desire to purchase and
I was told that the purchase was going to be by tender, and that
the terms and conditions would be arranged by the Judge to
whom application would have to be made. And I was under the
impression that the sale was to be by tender, right down to
July, when we got intimation that we were not to be allowed to
tender. It, therefore, comes to me as a surprise that during
that period there should have been long and intricate negotia-
tions with one party, while the other was being held at arms
length. As a matter of fact it was with the utmost difficulty
that we could get the time extended to enable our deputation
who had visited France to come back. A sale by tender conveys
to my mind that everyone is to be treated in the same way and
to have the same opportunity. And if there were negotiations
with one party and if a price had been arranged I think it was
unfair that we should not have been informed. In fact there
should have been no such negotiations if there was to be a sale
by tender. Everyone should have had a fair chance, and I
suspect that these long and intricate negotiations which took
place had practically settled the question before the referees
were appointed, and before our memorandum went in. I raise
this question now, not for the purpose of swelling upon any
grievance, because everybody — every business man, at any
rate — knows that the least valuable possession any man can
have is a grievance. The best thing to do is to write it off and
to go on with one's work. But I raise it for two reasons. I
want to explain what has taken place in justice to our staff,
and to the men who signed the memorandum. I do not think
we could justly allow it to go out that we are not able to manu-
facture indigo by this process. In the second place, I want the
shareholders to know the serious position in which users of indigo
arc placed. This Company was formed, and the capital was
subscribed, on the invitation of the Government on the footing
that users of dyes would have an undertaking which would
control the supply of dyes as regards price and other terms,
and that everyone would be treated alike. Now we find that
this most important plant is given to a firm subject to no con-
trol as regards supply or price or conditions, such as making pur-
chase of other dyes a condition of giving a supply of indigo.
It would take a great deal to justify the action of the Government
in this respect. It is said that this process, along with other
processes, has been sold by Messrs. Levenstein, Ltd., to a large
American firm who had hitherto nothing to do with dyes, and
unless the conditions of sale submitted to us have been modified
there is nothing in them to prevent it. No doubt there could
be established in America, in that way, a very large undertaking
for the manufacture of indigo. They would have power to sup-
ply all the markets of the world, whereas our hands are tied.
But not only are Messrs. Levenstein, Ltd., allowed to do that,
but they are entitled to give to anyone else their power to manu-
facture by this process without any responsibility to the users
of dyes in this country. I venture to repeat that the trans-
action is one that has given us a shock. We have a process for
the manufacture of indigo, a different process, and we shall do
everything in our power to be placed in a position to manufacture
and to supply anyone. But the difficulties of putting up large
plants at the present time are undoubtedly very great. It will
require all the support of the shareholders and the support of
all the large users of indigo to enable us to carry out that pro-
gram, and in any event there must be delay before it could be
carried out even if we commenced it to-day.
Now there is only one other matter which I want to speak
about, and that is the question of cooperation which is men-
tioned in the report. The position is this — that in July of last
year arrangements were made for a meeting between all the dye
manufacturers in this country' for the purpose of endeavoring to
bring about some arrangement which would prevent overlapping,
and which would enable them to deal in the best way with the
supply of the country. But at that time the question was taken
out of our hands by the Board of Trade, who set on foot certain
negotiations by committees and otherwise. Our attitude is
this, and has been throughout, that we are in favor of any ar-
rangements which will enable us to work together for providing
a better supply. In the words of the report: "We would wel-
come any tangible proposals for cooperation with other manu-
facturers provided that the interests of the textile and other
industries dependent upon the supply of dyes are safeguarded,
and that the cooperation can be carried into effect in a manner
consistent with the object for which this Company was estab-
lished." Various suggestions have from time to time been made,
and we have maintained that attitude throughout. We have
been really anxious to bring about an arrangement but so far
nothing definite has been reached. The difficulties have not
been in the least of our making, but nothing has been arrived
at, and we are to-day practically just where we were 12 months
ago. Now let me say this. We still remain of the same opinion
and we shall welcome any practical tangible proposals that
comply with these conditions. But I want to say quite definitely
that, if you are going to have combination, it is essentia] in the
interest of the industries of this country that there should be
adequate control to protect the textile industries, and that a
monopoly of dye-making in the hands of one company without
Feb., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
140
control would be a danger to which the industries of this country
should not for a moment be exposed. I have had opportunities
of studying the operations of some of the conventions made by
the German dye-making combinations, and can assure you that
there are many ways in which industries may be punished through
the action of dye-making concerns which would probably never
come to the surface, or would be imagined by those who have
not had an opportunity of seeing the inner workings of those
concerns. I therefore want shareholders to understand our view,
viz., that it is essential in any such combination that there should
be adequate protection of the public interest and of the textile
industries. We are all in favor of cooperation and combina-
tion not only at home but with the Swiss and with the French.
Dr. Forster, at the present moment, is in America studying the
question of how we may be able to supplement the supply of
dyes to this country by cooperation with American manufacturers.
One thing I would say about this matter is, that it is no use
talking of cooperation unless there is a genuine desire for people
to work together, and I am bound to say that, as I study the
atmosphere at the present time, I find, instead of an atmos-
phere which would lead towards cooperation, what seems to me
to be an organized attempt to create hostility to this Company
which does not promise very well for cooperation. We have
taken no notice of general discussions on the merits of business
men and of scientists. It is absurd to waste time on that, but
there have been some definite statements made which do call
for notice.
The first of them was made by Professor Pope, one of the im-
partial referees on the Ellesmere Port transaction, in which he
says in the midst of a great deal of general discussion: "The
Government organization (that is our Company) has proved to
be not only a great failure, but has had the further effect of in-
hibiting the re-establishment of the coal-tar industry. That
is to say, the organization apparently was to do everything that
was necessary and consequently private effort was to a con-
siderable extent hampered." Another professor repeats the
statement. My object in referring to statements of this kind
in regard to this Company is to say, in the first place, that they
are not true. Further, the gentlemen who make them, so far
as I am aware, have never been inside our new works and know
nothing of the plant we have put down or of our program, nor
of the research we have been carrying out, nor of our general
policy. Why then these wild statements? As a rule you pay
no attention to them, but when talking of cooperation, if you
are going to cooperate, it can only be with people who are willing
to work honorably and loyally with you, and not with people
who write and publish statements like that in regard to you.
The situation with which we are faced is far too grave, too im-
portant, for men of science or others, who may be able to give
help, to indulge in recriminations or talk of this kind. And I
want to make an appeal to them and to all dye manufacturers
and to everybody engaged in the business each to carry on his
business in healthy rivalry, and do everything he can to make it
a success, but do not let us get into the old bad position of past
days when it was the business of every man to try to do as much
harm to his neighbor as he possibly could.
The task is one which is worthy of our best efforts. I can
assure you we are only too anxious to get the cooperation and
assistance of anybody and everybody able to help for the pur-
pose of producing the dyes which it is our object to supply to
the country.
LEVENSTEIN LIMITED
The following account appeared in the Journal of Commerce
and Commercial Bulletin for Thursday, January 10, 1918:
London, Dec. 21 —Instances of the progress made by the
British dye industry were given yesterday by Sir John Lonsdale,
presiding at the annual meeting of Levenstein's Ltd. That it
is possible for Great Britain to produce all the dyestuffs it needs
was one statement made by Sir John. On this point he said:
"If the Government is prepared to give the necessary financial
assistance and special priority for the erection of plant, we, for
our part, will guarantee to make this country independent of
Germany or any other foreign source for dyestuffs. Let there
be no misunderstanding on this point. In our organization the
State has an asset of the greatest value, for we have the knowledge
and experience to free the textile trade from German domina-
tion in dyes, and we shall undoubtedly produce the results re-
quired, given the necessary help from the State."
The original works of this company were erected by Germans
solely to comply with the Patents Act of 1907; they were only
designed to carry out the last stage of the manufacture of indigo,
no provision being made for the manufacture of the all-important
intermediate product without which it was impossible to obtain
the finished dye. The war shut off the import of this intermediate
material, and the present management, which purchased the
German property, proceeded to erect the large plant necessary
for the production of the essential intermediate.
PROGRESS OF DYE INDUSTRY
One of the many difficulties involved was the fact that the
Government had already commandeered all the supplies of the
raw material required. Accordingly, a new process from another
raw material was developed, and with the remarkable speed ex-
traordinary results were achieved. Ever since the outbreak
of war the company has been by far the largest supplier of aniline
dyestuffs to the War Office and Admiralty and to the Colonial
and Allied armies, also shipping large supplies to the United
States to cover the requirements of American textile manufac-
turers who had contracts with the Allied Governments. By
March, 1915, the company had sufficient plant installed to meet
the entire demands of the textile mills of the world for naval and
military purposes outside the Central Empires.
"This achievement, effected without any financial assistance
from the Government, entitles the chairman of the company to
speak with the highest authority," says the Financial News.
"The work done by Messrs. Levenstein at Blackley and Port
Ellesmere in relieving the dye famine of the world and helping
to break down the German monopoly of a key industry which
had become a source of great economic power is of the highest
national importance. But Sir John Lonsdale clearly demon-
strates that much remains yet to be done if the British dye in-
dustry is to be placed in a position rendering it capable of re-
sisting German competition after the war.
"Before the war the British textile industry and other dye
users were dependent upon Germany for 80 per cent of the dyes
employed — that is to say,. British industries, representing
£200,000,000 of capital, were practically at the mercy of German
dye makers. Now the peace requirements of these industries
are widely different from those of war time. The range of dyes
manufactured in this country to-day has to be very widely ex-
tended. The manufacture of the peace requirements of the dye-
using trades is limited (as far as Messrs. Levenstein, Limited,
are concerned) not by their scientific knowledge, but by the ex-
tent of their plant.
AID OF GOVERNMENT SOUGHT
"The intention underlying the formation of the British Dyes
Company and the investment of £2,000,000 of public money
therein was excellent, says Sir John Lonsdale, but it has not
solved the problem of securing adequate peace supplies of
British-made dyes. Messrs. Levenstein, he declares, manu-
facture to-day more dyes and a wider range of dyes than all the
other British makers of aniline dyes combined, but much more
remains to be done. The company possesses the knowledge;,
what it requires is more plant, and the provision of such addi-
tioaal plant is governed solely by financial considerations.
"Sir John Lonsdale, on behalf of his company, therefore.
iS°
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 2
throws out this challenge — or perhaps it should be termed in-
vitation— to the nation: 'If the Government is prepared to
give the necessary financial assistance and special priority for
the erection of plant, we, for our part, will guarantee to make
this country independent of Germany or any other foreign source
of dyestuffs '
"This is an undertaking which cannot be ignored by the
Government. In the Levenstein organization the country has
an asset of the highest economic value. After the war Ger-
many's dye industry will be one of her strongest economic
weapons. Tariffs will not exclude German dyes if the necessary
plant does not exist in this country' to meet trade requirements.
British Dyes Limited, in which the Government is interested,
has not yet displayed the capacity for production of the country's
requirements, and it is essential that further steps should be
taken. We hope that the fullest impartial consideration will
be devoted to Sir John Lonsdale's statement and that prompt
action will be taken, as the question admits of no delay."
CURRENT INDUSTRIAL NLW5
PLATINUM IN SPAIN
A memoir published by the Spanish Geological Survey gives
some details of the platiniferous deposits of the Serania de
Ronda. The region of Southern Spain, situated between
Malaga and Gibralter, is of very complex structure. It has
formed in recent years the object of investigations by mining
engineers commissioned by the Spanish Government. Samples
were taken of river sand and the gravel from a river the bed of
which is dunite, and others from rivers in which dunite was
absent. In the first case, the presence of platinum was revealed,
but not in the second. On washing considerable quantities of
sand and gTavel, small, lucent grains of platiniferous ore were
discovered, the platinum content of which varied from 78 to
82 per cent of pure ore. In some zones the ore contained from
2 to 3 grams of platinum per cubic meter of substance examined,
while in others the yield was as low as 0.25 to 2 grams per cubic
meter. From the economical point of view, the nature of the
platiniferous sand or gravel is considered excellent, as it does
not contain clay. The first river to be investigated system-
atically between February and June, 1916, was the Rio Verde
over a stretch of 3V2 kilometers. The platinum contained in
this area gradually increased from 8 to 20 centigrams per cubic
meter from the point at which prospecting was begun to the fin-
ishing point. — A. McMillan.
TUNGSTEN IN MALAYA
According to the Mining Journal, 119 (1917), 657, a rich de-
posit of mixed wolfram tin ore was discovered recently near the
village of Changloon in Sungei Sintok. The discovery was
made by Chinese who were working for tin on some small ad-
joining leases. The discovery caused a rush and as there were
over twenty applications for the area, the Kedah Government
decided to put the property up at auction. Subsequently,
however, the area of 3000 orlongs was given to a local firm.
The monthly output hitherto has been about 300 pikuls ( 1 pikul =
142.7 lbs.) but an increase to 800 pikuls is expected shortly.
The rich discovery seems to be confined to this localized area
and no further discoveries have been made outside. The ore
occurs in quartz veins but as no regular prospecting work has
been done upon it, no reliable idea can be formed as to its life. — M.
TUBULAR CYCLE COMPONENTS
A catalog issued by Messrs. Accles and Pollock of Birming-
ham, England, illustrates a wide range of tubular parts for the
construction of cycles, motor-cycles, and aeroplanes such as
handle bars, seat pillars, srat pillar laps, frame lugs, bridge
pieces and loop struts, stays and front forks, and steering tubes.
Full-size illusti 1 iven of 168 special sections in cold
ih awn, weldless steel tubing, as well as of a number of sections
from the Ail Board's standard lists, and there is a description
of an attachment called the "Apollo Mykarmo," which, when
cramped on the thimble of standard micrometer calipers, at
once converts them into a Hunt gauge having a toicT.iniL of
from 0.0001 in. to 0.022 in., with variations of 0.001 in. — M.
MAGNETO MACHINES FOR POCKET TORCHES
A recent issue of the Elektrotechnische Zeitung gives some par-
ticulars of a new type of pocket torch being developed in Ger-
many and Austria in which the lamp is supplied with current
from a small hand-driven magneto. The shortage of certain
material is putting a limit to the manufacture of dry cells and
small accumulators for public use and this is no doubt responsible
for the tendency to utilize hand-driven sources of current for
pocket lamps of various kinds. Lamps of this kind are more
expensive than the ordinary kind but do not require refills or
charging.
One of the types described depends on the release of energy
from a series of springs put into tension by the pressure of the
thumb on a lever. The whole arrangement weighs about 1 lb.
and is so contained that the release of the spring supplies enough
energy to keep the lamp alight for 3 min. In order to secure a
light for 10 min a heavier machine, weighing about 5 lbs. and
requiring to be wound up with both hands, has been designed.
In these lamps the armature is the rotating part but in another
variety, due to O. Pletscher, the field revolves in ball-bearings
round a T-shaped armature. This lamp is stated to weigh
only about l/j 'D- The application of this principle of portable
electric lamps seems quite simple and practicable.- — M.
THERMIT WELDING
The British Board of Trade have now given formal sanction,
says Engineering, to a new company with works in London and
Liverpool and known as the British Barimar Thermit Welding
Company to take up and exploit the Thermit-Welding process
which prior to the war was exclusively in German hands.
Thermit is especially applicable for tramway welding and for
repair of heavy castings and machine parts. The registered
offices of the new company are at 10 Poland St., London.
The Thermit Co., Ltd., of Commercial Rd., London, are not
connected with this new company which has only rights to work
certain of their patents. They continue their manufacture of
various Thermit compounds and are at present especially
engaged upon the manufacture of certain metals and alloys
in connection with the war M
REFRACTORY PROPERTIES OF MAGNESIA BRICKS
A contribution to the Proceedings of the Paris Academy of
Sciences was recently made bj MM LeChatelier andB.Bogitch
on the refractor] properties ol m irnesia bricks, either made
in the laboratory from pure magnesia or from commercial
specimens. The resistance to crushing was measured at 15,
1,000, 1,300, 1,500 and 1,600 ° C. for two bricks and at 15. 1,500
and 1,600 C foi the remainder All the magnesia bricks
show 1 sudden fall of resistance to crushing at a temperature
dependine, on the degree of purity, a fact which explains why,
in practice, it has been found that magnesia bricks stand less
well in furnaces than silica bucks, although their fusing points
observed in the ordinary way without reference to resistance to
crushing are higher than the silica bricks. — M.
Feb., 101S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY 151
PREVENTION OF SCALE IN BOILERS MINERAL PRODUCTION OF VICTORIA
The necessity of reducing to a minimum the formation of The annual report for 1916 recently published gives the
scale on the heating surface of steam boilers if efficiency is to be following yields of the various metals and minerals for the
maintained was referred to in an article in the Times Engineering year:
Supplement for September and in this connection Messrs. J. Gold 276 168 oz
Dampney and Co., of Cardiff, Wales, draw attention to their 5lack S?al; 4l7|l83 tons
„. . ,, , , , , Brown Coal 2,915 tons
Apexior compound as a remedy against both scale and the Antimony Ore 12,382 tons(a)
pitting of the plates. The compound consists of 98 per cent Manganese...! 'Is tons
pure amorphous carbon combined with a neutral organic vehicle. S,y??um ' '853 tons
r r Wolfram 314 tons
It is painted over the internal surfaces of the boiler and well Magnesite 100 tons
rubbed in, and, when dry, it presents a peculiar" surface which is ,.„..,_,. f°'°
. . . . (o) * lelding 3,259 tons concentrates,
antagonistic to the building up of a hard scale of crystallization. — M
Any deposit which may take place, the makers state, can generally
be removed easily without the use of a chipping hammer and MANUFACTURE OF ELECTRODES
falls off readilv over large areas by concussion. In cases where, , ,. ., T ..«.„.
,, . . , to. a. 1 * * 1 j u According to the Ironmonger, a companv called the Norske
through the use 01 solt water, the plates are attacked bv pitting, _, , . . , . .. r , „ . .. , ,»
, , . . , . ., Llektrodeverker is erecting a factory at Fredrikstad, Norway,
the compound not onlv acts as a preventive but also arrests the , ., . . . , , . . _.
, ,. .... ., .. , , . , „, . . for the manufacture of carbon and graphite electrodes. The
progress 01 the pitting 11 it has alreadv begun. 1 he substance .. . e . ,
, _ , , , . ... " . , capacity is 4,000 tons of carbon or 1,000 tons of graphite elec-
ls not affected by boiling water or by steam under pressure, and, . , , ., , . . . , .
,. ... . I", ., . mm., ^, ... . , trodes a year, and the works were expected to be in operation
owing to its nature and the thinness ol the rum, the translerence . .. . , ., _ , ,
c ., , ., ■ „. „ . . . , . ... „, by the end of the year 1917- Carbon electrodes are expected
of the heat to the water is practicallv not interfered with. — -M. ».../-. .• . . - . -™ , . . ,
to be the first article of manufacture. The machinery is almost
exclusively of American make. The orders already in hand are
ELECTRIC HEAT STORAGE IN BOILERS said to ensure the profitable working of the factory for some
In a recent issue of Engineering an account is given of a new time and it is stated that the factory is working in cooperation
type of electrical generator invented by Col. Revel, an engineer with the Norwegian Government. The company will use
in the Italian army. The essential idea in the apparatus is the power from the great waterfall of Sarpsfall, but in anticipation
direct conversion of electric energy into heat by making use of this being inadequate, it has purchased the rights to the
of the resistance of the water to be evaporated. Alternating entire power from the waterfall near Kristiansund. — M.
circuits of 200 to 3,600 volts can be applied and this apparatus
is stated to be automatic and to require no regulation. Lack
, , , . . ,. ■ • , ., , . ■ , . t , RECOVERY OF POTASH AND MAGNESIA FROM
of feed water merely diminishes the production of steam until p v n am t» t>
the supply of water is renewed. The efficiency is claimed to be
97 to 98 per cent. The Revel apparatus is constructed to work The Official Canada Gazette of September 8, 191 7, publishes
up to 14 atmospheres and can be connected up at any time to an announcement to the effect that the Committee of the Privy
the steam pipes of an ordinary boiler. In this way, temporary Council have concurred in the recommendation of the Minister
use can be made of hydroelectric supplies and their utility can of the Interior that he be authorized to lease certain lands
be judged by the fact that they were often used before the war abutting upon Lake Muskiki in connection with the recovery
when the price of coal in Italy did not exceed $8 per ton. An and utilization of minerals from the bed and waters of the lake,
illustration is given of an installation of 8 generators taking three- These minerals, chief among which are potash and sulfate of
phase current at 6,000 volts and each developing 900 to 1,000 magnesium, are intended for medicinal and other purposes and
kilograms of steam per hour. The production of steam varies preliminary plans submitted by the company show that the
according to the area of electrodes immersed. The sediment proposed utilization of the waters of the lake will require the
collecting at the base of the apparatus from water containing construction near the lake of a pumping plant, evaporating
calcareous material can be released without interrupting the machinery, bottling works, etc. The name and address of the
process M above-mentioned company may be obtained by manufacturers
desirous of supplying plant, etc., on application to the Board of
BRITISH BOARD OF TRADE Trade, 73 Basinghall St., London. Reference No. 374 should
During the month of November the British Board of Trade be quoted— M.
received inquiries from firms in the United Kingdom and abroad rnrp<?
regarding sources of supply of the following articles. Firms
which may be able to supply information regarding these things The fluxes commonly used in melting aluminum scrap, says
are requested to communicate with the Director of the Com- the Brass World, are fluorspar, cryolite and salt. An excellent
mercial Intelligence Branch, Board of Trade, 73 Basinghall way of utilizing such material when a part of the scrap is small
St Loudon V. C aid not c'ean is first to melt a bath of aluminum using solid
Artificial musk Flat handles for camel-hair brushes material and to allow it to reach a temperature of approximately
c1Selbtoi??rush1«UfaCtUrcr3Kanted) Machinery and Plant for: 85o° C, then to add the sweepings in such quantity that the
CnBmcAta: Making felt wads for use with sport bath will absorb them without losing its liquidity. The bath
C^U^^fb^eay1s(lSdtPiUted, PrSnfctiou of clocks and parts is then reheated and more sera,, charged, the process of charging
Sulfonated castor oil (50 per cent thereof an(] irritated until the Crucible is as full of
volume) Making clectnc light carbons " "
Strontium carbonate M:iple or hickory skewers, spoons and metal as desired. I In metal will most likrlv !h pasty and a
Bo^teTsodhinT13 NldS^wf-te ^ small , fused unc chloride is added .,,.,1 the bath well
Calcium silicidc Oiled cloth for electrical insulation stirred. The resulting action will fric the mixed oxides and the
London purple Pumice powder (20 to 50 tons) . . .,
Paris green Sclf-makint- stamp pads metal will assiuiH its natural lluidlty. 1 he crucible should
CoTm^dritd blood for phaxma- **&t "" '**" """* *** be emptied ,„i„„d,:,„ K i„„„,i„„, before any rea,
ccutical purposes Silver leaf for coating pills occur betwiin the metallic aluminum and the heated oxide
Iii':' i. tins: in« tunes Sugar-cane wax . - «
Disinfectant attachments for tele- Vegetable extract on the one hand and the OXygeD anil nit to:., n ..I tin- atmos-
KnStabSTl/JSXneter ':'cUpPo1iChmCOt """^ phere OH the Other, as SUCl .„'.:,l!„:,l„,ni,mm
— M. and greatly reduce the pero ' 'red. M.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol 10. No. 2
WATERPROOF VARNISH FROM OIL
A French patent for the above has recently been published,
in which oils vulcanized with sulfur chloride are dissolved in
amy] acetate. The following method of preparation is used:
One thousand parts of castor oil are mixed with 2,000 parts of
amyl acetate and stirred up well with 250 parts of sulfur chloride.
In a short time, the mixture sets to a fairly solid jelly and gives
off large quantities of hydrochloric acid from the acetyl chloride
formed. If, however, the product be left in a tightly closed
vessel for several days it will be found to have become com-
pletely liquefied and dissolved. The acid is then neutralized
with barium carbonate and, after the precipitate has been re-
moved by decantation and filtering, a clear almost colorless
liquid is left consisting of a perfect solution of the vulcanized
oil, hitherto regarded as insoluble. This solution may be used
for waterproofing fabrics, leather, paper, etc. On the other
hand, if it be mixed with other solvents, e. g., alcohol, benzene,
acetone, acetic ether, and employed to dissolve a certain amount
of nitrocellulose, there results an excellent varnish for glossy
leather — the gloss resisting action of soap, friction, etc. — a
leather polish, a varnish for oil cloth and when mixed with
pigments, a waterproof, quick-drying paint which will stand
washing and changes of temperature. — M.
SHELLAC DERIVATIVES
A paper on the "Investigation into the Inhibition Exhibited
by Some Shellac Derivatives" by Messrs. A. P. Laurie and C.
Ranken was read at the Royal Society, London. The paper
dealt with experiments made on the substances obtained by
boiling shellac with carbonate of soda or borax. The solid
substances, very similar in consistency to gutta-percha, are
found to expand rapidly when placed in water. The control of
the expansion by the addition of soluble salts is not the same as
in the case of gelatine, since, at any rate, in a large number of
cases, it does not seem to depend upon the nature of the salt
but simply upon the strength of the solution, and the amount
of expansion increasing with the diminution of the strength
of the solution. If the expansion is allowed to become complete
in cold water, the mass cannot be contracted again, but if ex-
pansion takes place in a salt solution, then contraction will take
place again if the mass is put into a stronger solution. Strong
salt solutions are also found to precipitate the soluble portions
of the shellac-borax compound.
As a result of the experiments described, the authors suggest
that the facts can be best explained by supporting the shellac-
borax mass to consist of a soluble organic nucleus surrounded
by elastic diaphragms through which the organic nucleus cannot
pass, but the salt molecules can pass, the organic nucleus being
soluble in water but insoluble in strong solutions of salt. — M.
CELLULOSE TURPENTINE
I luring the treatment of wood for cellulose by the sulfite
process there is obtained a considerable amount of a turpentine-
like oil mixed with various impurities containing sulfur and hav-
ing very objectionable odors. The amount of turpentine so
obtained reaches as much as 22 lbs. per ton of wood treated
where pines are used. The oil has recently been extensively
examined, says a contemporary, the sulfur compounds being
first removed by means of mercuric chloride dissolved in alcohol.
The principal portion of the oil consists of alpha-pinene which
is well known to be the main constituent of ordinary turpentine
oil. It is, therefore, clear that this terpene is very stable or it
could not stand the drastic treatment of the sulfite process
When the sulfite process is used, the pine is almost completely
broken down to para-cymene. lieta-pinene is also present in
the oil and probably di-pentene. M.
SUBSTITUTE FOR OIL IN PAINT
According to the Oil and Color Trade Journal, a mixture
of 100 parts of rosin, 20 of soda crystals and 50 of water melted
over a fire and mixed with 250 parts of water containing 24
parts of liquid ammonia gives a syrupy liquid which can be
used as a substitute for boiled oil or turps in the manufacture
of paint. Such paint dries quickly without requiring any driers
and has good covering power and withstands the influence of
temperature, wet and dry. The substitute is improved in
appearance and gloss by the addition of a mixture of 2 parts
alcohol, 31 '2 parts ordinary glycerine and 1 part of wax in pro-
portions up to 10 per cent. M.
DYE FROM SULFITE LYES
After chemical research succeeded in the useful application of
sulfite lyes for the production of alcohol and of coal dust for
heating purposes, an engineer in Finland, says the World's
Paper Trade Review, claims the economical production of valu-
able color stuffs from the remarkable sulfite off lye. He claims
especially the new production of methyl alcohol, cymol and
furfurol for the transformation into coloring material as they are
gained in Germany from coal tar. The inventor has claimed
patents in the Scandanavian countries, Russia and Switzerland,
and a color factory is being erected at Tammerfors, the centre
of the Finnish textile industry, with a capital of 200,000 marks.
The inventor, Dr. Wiljanen. delivered an interesting lecture
relating to his invention at the Technical Club, Tammerfors,
and exhibited about ten different colors produced from cymol
and numerous others containing cymol as a substantial part.
He explained that about 300,000 kg. of cymol are obtainable
in Scandanavia as a by-product wherefrom yellow and red
cotton and wool colors could be produced in a simple manner.
Finland's largest paper mill association has installed ap-
paratus in its factories for separating wood spirits, cymol and
furfurol and investigations are being continued at the new
Tammerfors factory with a view to obtaining new raw color
material from home products. Preparations are being made to
start, in the near future, the manufacture of cymol colors.
— M.
ELECTRIC ARC WELDING
The welded fastening, reports the Railway Mechanical Engi-
neer, has always been looked upon as a stronger fastening than
the riveted or bolted joint. As a general proposition the riveted
or bolted joint has the tensile strength of the original piece
while the welded joint is as strong as the original section. There
are two kinds of electric welding, known as the carbon electric
welding and the metal electrode welding. In the former, an
arc is drawn between a carbon electrode, the piece to be welded
and the metal to be added are fed into the arc in the form of a
"melt-box." The method is not used extensively in railway
work due to the fact that the welding may only be done in the
horizontal plane in this maimer and that the work is in general
inferior to that done with the metal electrode process. The
metal electrode process as the name implies- a metal electrode —
the arc being drawn between the electrode and the piece being
welded. The heat of the are melts the metal of the piece and
the metal of the electrode simultaneously. As the metal of the
electrode melts, it is drawn across the arc and a complete and
homogeneous union is formed with the molten metal of the piece.
With the exception of work with certain electrodes (manganese
steel and slag-covered electrodes'! the electrode is always made
the cathode or negative, ; »., the current flows from the piece
being welded to the metal electrode. The voltage required for
metal electrode welding is about 20 volts and direct current is
necessarv. — M.
Feb., 191S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
153
SCIENTIFIC SOCIETIES
REDUCTION OF WASTE
The importance of reducing and preventing waste has been
brought to the attention of the American Chemical Society
by the following communications:
December 22, 1917
To the Chairmen and Secretaries of the Sections of the
American Chemical Society:
The Alabama Section of the American Chemical Society early
this autumn passed resolutions looking to the prevention of all
wastes as far as possible and referred the question of a national
movement in the American Chemical Society to the President
of the Society. At a meeting of the Advisory Committee of
the Society held in New York on December 8, it was decided
to take up this movement as a most important one in which the
National Society could be and should be active. It was de-
cided that the emphasis should be placed not so much on a talk
propaganda against wastefulness but, since the Society con-
sists of experts in the field of recognizing and preventing waste,
to ask the Sections to emphasize the need of pointing out specifi-
cally in as many instances as possible where waste occurs and
how it is to be avoided. It is recognized that in many cases
large problems of research would be involved in reaching recom-
mendations as to how waste is to be avoided but chemists could
be active in pointing out these problems and urging that the
necessary investigations be undertaken by the concerns involved.
In accordance with this action, I would ask that you appoint
a committee of your ablest men to take this matter in hand and
to organize a campaign against waste in the most effective way
possible. It might be desirable in given localities to appoint
a very large committee to cover all the different kinds of waste
or to appoint a number of committees each to take care of a
definite field of effort. Such organization is left to the judgment
of the local sections. In conclusion let me say that Past Presi-
dent Little pointed out to the Boston meeting that the saving
of waste alone in this country would be sufficient to pay off the
tremendous war debt which we are incurring in the space of a
very few years.
In case any Local Section would like specific advice in regard
to any matter connected with this movement it is urged to bring
the matter up with the President of the Society.
Thanking you in advance for your cooperation in this most
important movement, I am
Yours sincerely,
(Signed) J. Stieglitz,
President, American Chemical Society
38 Albemarle Street
Rochester, N. Y.
Dr. Julius Stieglitz, December 2., 1917
University of Chicago,
Chicago, 111.
Dear Sir:
In reading an article in the July number of the National
Geographical Magazine on rats and mice, I was very much im-
pressed by the enormous economic loss to this country caused
by this pest. The thought struck me that it is most absurd
for the American people to strain at every point to conserve and
increase their food supply and yet to ignore wholly a cause of
loss which is estimated to cost the country from $100,000,000
to $200,000,000 per annum.
With this thought in mind I took up the matter with the
Rochester Section and obtained their approval for me to act in
this matter. Enclosed are copies of the correspondence to date.
My object in writing to you is to see if your views on the sub-
ject arc in accord with mine and, if so, whether it would not be
possible for you to help in this matter through your office and
the Local Sections.
I realize that it is impossible for any one community to make
a successful fight, for in the first place the rat, being migratory,
will appear again shortly after being exterminated locally.
In the second place, there is such an enormous indifference to
be overcome such as, "Rats never bothered me, why should I
worry?" that it is almost impossible to accomplish anything
unless there is governmental authority behind it. Therefore,
it appealed to me that there never could be a more fitting time
to start a campaign against this pest than the present when
nearly everybody is willing to do their bit. Besides the loss
of food enormous damage is done to property and, by no means
the least, there is the constant menace to health.
I would ask that you kindly give this matter your careful
attention and let me have your opinion relative to it.
I received your letter of December 17, and will carry out the
instructions given therein.
Sincerely yours,
(Signed) H. LB B. Gray,
Chairman, Rochester Section
Chicago, 111-
Mr. H. Le B. Gray, December 27, 1917
38 Albemarle St..
Rochester, N. Y.
Dear Mr. Gray:
I have your letter of December 2 1 with the interesting corre-
spondence in regard to the economic loss due to the rats and
mice in this country. A few days ago I sent out letters to all
the Sections of the American Chemical Society asking them to
cooperate in the elimination of waste in this country and es-
pecially to indicate in specific cases where waste occurs and how
it could be avoided. This letter no doubt has crossed your
present letter. I think a movement to reduce the destruction
by the rats and mice would be particularly desirable at this
time, as it would not only save food and other important products
but also be a safeguard in regard to the health of the community.
I have no doubt that we shall have the same experience as they
have had in Europe, notably in Germany, France and Italy,
where the food shortage has been the most severe, and shall
find that the necessity of saving of food will lead to reduced re-
sistance towards disease and the increase of disease in this coun-
try. In view of that situation it would be especially desirable
to offset this decreased resistance by such a positive element
toward health as the reduction in rats and mice that you pro-
pose. I would recommend, therefore, that you take up this
problem with each of the Sections of the American Chemical
Society as timely and important
Yours sincerely,
(Signed) JULIUS .Stieglitz
38 Albemarle Street
Rochester, N. Y.
January 4, 1918
Dr. Chas. H. IIerty,
Chairman, New York Section,
New York City.
Dear Sir :
Pursuant to the recommendation made by Dr. Stieglitz in
his letter of December 27, 1917, replying to mine of December
21, 1917 (copies of which are enclosed), 1 am writing you with
the hope that I may interest your Section in a matter which
appeals to me as vitally affecting the country, especially at the
present time. Local campaigns and those without official
154
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 2
authority would be futile and it seemed to me that by the com-
bined action of the Local Sections of the Society sufficient interest
could be aroused to start a national campaign backed by govern-
mental authority.
The matter has already been taken up with the U. S. Food
Administration and in reply they state, "You are advised that
the movement of your Society, as indicated hi your letter, has
our heartiest approval and support, and we trust your Society
will do its utmost to aid in the elimination of these pests and the
conservation of much needed food thereby" — and in a subse-
quent letter — "permit me to suggest that you take this matter
up with Dr. Hayward, Chief of the Bureau of Insecticides and
Fungicides, Department of Agriculture, who have their perma-
nent representatives in all sections of the country and would,
therefore, be in a better position to take charge of this matter,
the importance of which we realize, than the food administration."
A letter together with a copy of this one will be sent by me
to Dr. Hayward.
Any action which you or your Section may take to further this
movement will be greatly appreciated.
Very truly yours,
(Signed) Harry Le B. Gray
SEVENTY-FIFTH ANNUAL MEETING
AMERICAN ASSOCIATION FOR THE ADVANCEMENT
OF SCIENCE, PITTSBURGH, PA., DECEMBER
28, 1917— JANUARY 2, 1918
The seventy-fifth annual meeting of the American Associa-
tion for the Advancement of Science and the affiliated societies
was held in Pittsburgh, Pa., from December 28, 1917, to January
2, 1918.
The first general session of the Association was held in the
Music Hall of Carnegie Institute on Friday evening, December
28. President Charles R. Van Hise of the University of Wis-
consin, retiring President of the Association, delivered an address
on the subject "The Economic Effect of the World War in the
United States."
A meeting of Section C, Chemistry, was held on Friday morn-
ing, December 28, presided over by the chairman, Professor
Win. A. Noyes. The feature of the evening was the informal
but exceedingly enjoyable address of the retiring chairman,
Professor Julius Stieglitz of the University of Chicago, upon the
subject "The Electron Theory of Valence and Its Application
to Problems of Inorganic and Organic Chemistry." After an
extended discussion of the address. Doctor David Horn of
Bryn Mawr presented a paper on "A Chemical Study of For-
malin Fumigation." A paper by J. Davidson of the Bureau
of Chemistry, Washington, D. C, entitled "Do Seedlings Reduce
Nitrates?" was read by title,
On Friday afternoon the Section met with Section D, Engi-
neering, and the Society for the Promotion of Engineering
Education.
On December 29, a joint symposium was held with Section
E, Geology and Geography.
cers for 1918 were elected by Section C, as follows:
Vice-President and Chairman: Alexander Smith, Columbia
Unit ersity.
Secretary: A. II. Blanchard, Massachusetts Institute of
Technology.
Member of Section Committee: Benjamin F. Lovelace, Johns
Hopkins I niv< rsity
The sessions on the afternoon of the 28th and the morning
of the 29th were held in conjunction with the Section on Social
and Economic Science of the A. A. A. S. and at these sittings
papers on standardization were read by J. W. McEachren of
the Crane Company, Chicago, and by F. O Wells of the Green-
field Tap & Die Co., Greenfield, Mass. In his paper, Mr Wells
pointed out that he employed 1700 hands and that he calculated
that he would save Si 00,000 by the introduction of the metric
system. Other papers were read by W. C. Wells, of the Pan-
American Union, who discussed measures of volume in metric
and other measurements, and by H. T. Wade who pointed out
the importance of the metric system as a means of international
standardization.
The session held on the afternoon of the 29th was presided
over by Dr. John H. Brashear, of Pittsburgh, and was devoted
to reports from President George F. Kunz, Secretary Howard
Richards, Jr., and Treasurer A. P. Williams, showing the healthy
condition of the association. Fred R. Drake read the report
of the executive committee and outlined the activities of the
association in the way of publicity and of cooperation with other
national bodies. Dr. H. D. Hubbard, of the Bureau of Stand-
ards, gave an interesting address in which he pointed out some
of the fallacies of anti-metric arguments.
In the evening there was held a metric dinner with a menu based
on war-time cond Jons, the calorie value of each viand being
expressed in exact units. At the close of the meal impromptu
addresses were made, followed by an election of officers resulting
as follows:
President: G. F. Kunz, of New York.
Vice Presidents: William Jay Scheffelin, of New York;
E. P. Albrecht, of Philadelphia; and H. V. Amy, of New York.
Secretary: Howard Richards, Jr. of New York.
Treasurer: A. P. Williams, of New York.
ANNUAL MEETING TECHNICAL ASSOCIATION OF THE
PULP AND PAPER INDUSTRY, NEW YORK CITY
FEBRUARY 57, 1918
The annual meeting of the Technical Association of the Pulp
and Paper Industry will take place in New York City at the
same time as the annual convention of the American Paper and
Pulp Association, the Waldorf-Astoria Hotel being headquar-
ters for both associations. The program will consist of a sym-
posium on acid sulfite manufacture and a discussion of problems
relating to engine sizing.
AMERICAN METRIC ASSOCIATION
The second meeting of the American Metric Association was
held in Pittsburgh in conjunction with the meeting of the Amer-
ican Association for the Advancement of Science on December
28 and 29, 191 7.
NEW YORK SECTION OF THE SOCIETE DE CHIMIE
INDUSTRTELLE
Following the presentation of the Perkin Medal to Mr. A. J.
Rossi on the evening of January iSth at the Chemists' Club
in New York City, a New York Suction of the Societe de Chimie
Industrielle was organized. The Secretary of the parent or-
ganization. Lieutenant Rene Engel, addressed the meeting in
terms of grateful appreciation of the cooperation of the American
chemists with those of France. He traced interestingly the
origin of the new Society.
The following officers for the Section were then unanimously
elected :
President. L H. Baekeland; Vice-President, Jerome Alex-
ander; Secretary, C. A Doremus; Treasurer, G. F. Kunz;
Executive Committee. Charles Baskerville, H. Blum. M. T.
Bogert, C. F Chandler, EUwood Hendrick, W H. Nichols,
R. B. Orfila, G. B. Valabreque, K I'. V. Verge, Henri Enrique
Viteaux.
The constitution ami by-laws for the new Section were adopted
and after felicitous remarks by Ors Haekeland. Nichols and
Baskerville. the meeting closed with a strong address by Prof.
Y. Grignard of the French M
Feb., 1018 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
NOTL5 AND CORRL5PONDLNCL
TWO LETTERS ON THE CHEMICAL CONTROL OF
AMMONIA OXIDATION
Editor of the Journal of Industrial and Engineering Chemistry:
In a paper on the "Analytical Control of the Ammonia Oxida-
tion Process"1 Messrs. Guy B. Taylor and Joseph D. Davis
refer to the present writer's article2 and a brief statement seems
necessary by way of reply or further elucidation.
Taylor and Davis assert that the "statements of Schonbein,
Weith and Weber are not to be taken to mean that ammonia
is oxidized by hydrogen peroxide abundantly under all condi-
tions." But there is nothing in our paper that says they are so
to be taken. We said that hydrogen peroxide abundantly
oxidizes ammonia — which is true. We did not say that it
happened under all conditions. The course of this chemical
reaction, and for that matter, all chemical reactions, is de-
termined by the conditions of temperature, concentration, etc.
This is a sort of Theorem I of chemical dynamics, and is pre-
sumed in any discussion. It may well be true that under the
conditions of analysis as used by Taylor and Davis no such
oxidation occurs; we should be the last to dispute it as we have
no data to dispute it with. It does not appear to us, however,
that the evidence brought forward to show absence of oxidation
is sufficient to prove the case, under all conditions of analysis.
In the same paper the authors state (p. uoq) that "the reaction
2NO + 02 = 2NO2 occurs in measurable time." That is, it
requires a measurable time for the specified equilibrium to be
reached. To prove this, they cite five journal articles, most of
which are very long and full of data having no relevancy to the
issue. They give, however, no particular references; in fact
they might as well have cited the literature en masse. Let us
see what the literature says. In the first paper cited,3 od p.
2135, we find the statement: "these experiments show that two
volumes of NO and one volume of oxygen of different origins
(t. e., made by different manufacturing processes) at atmospheric
pressure are practically completely transformed into N02 and
N2O4." On p. 2134 is given a curve of time against pressure
decrease, which shows that the reaction practically runs its
course in half a minute or less. Thus with only the theoretical
amount of oxygen (which Holwech used) the reaction is prac-
tically complete in less time than would be required to go through
our apparatus, but our method of course requires a decided
excess of oxygen.
Perhaps the most important paper for the case on hand is
that of Foerster and Blich,4 and the issue amounts to this — ■
when the mixture of air or oxygen and NO is run into a dilute
caustic soda solution, does the reaction take place as follows?
2NO2 + 2NaOH = NaN02 + NaN03 + H20
The answer is, that it all depends on Theorem I above, and
there is nothing in the article bearing on our work because
Foerster and Blich did not duplicate our conditions. However
the results given in the table on p. 2019 "Versuchsreihe" Experi-
ment 16 (where the gases are dilute) and in Experiment 42 on
p. 2021 come as near as any in the paper to being comparable.
In both instances the reaction runs practically as specified in the
equation above. We do not base anything, however, on these
statements from the literature. What is said in our paper was
based on the fact that the amount of nitrite found in tin first
absorber was close enough to the reaction given to justify the
calculation. The fact is, that so far from being in the sense of
' This Joimii., 9 M9I7), 1106.
'Ibid., 9 (1917), 737.
' Holwech, "(jber die Reaktion zwischen Sticlcoxyd und SaucrstolT,"
Z. angtw. Chcm., 21 (1908), 2131.
* Z. antew. Chem., 23 (1910), 2017.
more nitrite as would be presumed from Taylor and Davis's
supposition, there was invariably less, i. e., more than half the
acid was nitric. The writer thought there might be a little
ozone in the oxygen but as the corrections involved were small, he
did not think the point worth pursuing. Doubtless the amount of
nitrite and nitrate are much influenced by the concentration of
the alkaline solution into which they are led. In the writer's
apparatus certainly all the NO yielded NO2 and a little N2O5.
However, Taylor and Davis admit that by our procedure
all the nitrous gases are absorbed, and all their contention
would amount to, even if valid, would be that the formula
would have to be modified. One does not adjust his testing to a
mathematical formula, but calculates what he wants to know
from the data he can get most conveniently and accurately.
Curiously enough, Taylor and Davis in their literature cita-
tions overlooked the only paper that could have been cited
with any effect. We refer to that by Mandl and Russ1 who
found that with some kinds of oxygen (e. g., that from elec-
trolysis and also that from barium superoxide, bichromate and
sulfuric acid, but not that from liquid air) the reaction between
NO and 0> did not go to completion.2 The objection would
apply of course to any methods requiring oxygen, including
those of Taylor and Davis. However, we were fortunate enough
not to get hold of any such oxygen. Mandl and Russ think
that the differences in oxygen of different origin may explain
the contradictory statements in the literature on the behavior
of NO and oxygen.
Method I of Taylor and Davis amounts substantially to our
method in that they have added oxygen to the gases before
absorption, the difference being that they omit the precautions
to prevent the oxidation of ammonia by the hydrogen peroxide.
The main fact is that nitric oxide (NO) is not nearly completely
absorbed by alkaline hydrogen peroxide. Sufficient oxygen
must be present to convert it into N02(N20.|). The writer
proved this repeatedly, when nitric oxide would go through three
absorbers, two of them filled with alkaline peroxide and beads, only
to burst into brown fumes on coming into contact with the air.
The essential features of our method are to insure by previous addi-
tion the presence of the necessary oxygen, and to avoid the oxida-
tion of ammonia which takes place under not well-understood
conditions. Now, Taylor and Davis have previously added the
oxygen but there is no certainty that it would be enough; this
difficulty is avoided by adding an additional dose in the large
(1200 cc.) displacement vessel after the absorption is com-
pleted. This plan, while not specially appealing to us on account
of the double titration and the necessity of getting the acid out
of the large container, will doubtless get all the nitrous gases
provided the mixture coming from the catalyzer contains enough
oxygen already to oxidize practically all the NO to N02. In
fact, with the saturators at 7 or 8 per cent ammonia (as men-
tioned in the article) we suspect that little or no oxygen would
be necessary. Supposing, however, that the gases from the
catalyzer contain all the combined nitrogen as NO, with little
or no oxygen, then only limited absorption1 trill taki
K", and. especially in a cool place, there would be ample oppor-
tunity in an hour for part of it to dissolve is the displ
md get lost. We see then that the method is
only for a highly special manner of operating the 1
and will be satisfactory only so long as there is
of oxygen present. The writer was never able to get complete
■ Z. angew. Chem., 21 (1908), 486.
"These results have not been confirmed by lata worker*, without,
however, disproving them. Holwech, Z. angno Chcm.. 21 (1908), -MM.
» Probably also irregular. See the reference to Schonbein in the
writer's original paper.
156
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol 10, No.
absorption with only one absorber, but possibly the absorber
K' is better than his. The use of a manometer is not very
convenient.
The same criticism applies to the evacuated bottle method as
described. A sufficiency of oxygen is not assured, except under
special conditions. Moreover, a pump capable of evacuating
to 2 mm. is necessary as well as connections and capillary stop-
cocks so well ground that they will retain the vacuum mentioned.
Fortunately a concession is made in the matter of ground glass
connections. What all these mean, it is unnecessary to state.
The statement that it is the only method permitting the de-
termination of ammonia escaping oxidation presumably applies
only to the procedures described in the paper, for it is perfectly
feasible by our method. We are convinced that anyone trying
the vacuum bottle method will find it exceedingly elaborate.
Presumably the plan could be modified by adding a measured
amount of oxygen first to the vacuum bottle, but it then becomes
even more complicated. A larger bottle will also be required to
cover all cases of gas mixture.
Messrs. Taylor and Davis present a method for eliminating
titrations because "the principle involved offers possibilities
for development of a rapid method of works control." The
essential novelty of the principle however — the running of a
gas into a definite volume of liquid stained by an indicator until
the indicator turns — had been stated already by the present
writer in the second and third paragraphs of his paper. They
have added an elaborated glass apparatus which would impress
us as being a great deal more troublesome than half a dozen
titrations.
Finally, and this a crucial point, catalyzers do not work uni-
formly and the taking of a sample should extend over con-
siderable time, in fact should be continuous. It seems to the
present writer that his is the only process which has this ad-
vantage; it is also free from limitations on the composition of
the gases. He hopes to publish shortly an account of an im-
proved and more compact form of his apparatus, together with
a new method of approximate factory control requiring less skill
than any of the proposed methods.
1605 E. Capitol Street Paul J. Fox
Washington, D. C.
December 11, 1917
Editor of the Journal of Industrial and Engineering Chemistry:
In reply to criticisms of Mr. Paul J. Fox, on our paper
"Analytical Control of the Ammonia Oxidation Process."
In regard to the oxidation of ammonia by hydrogen peroxide
in alkaline solutions, we are convinced that no such oxidation
occurs in any method used by us and would not occur in the
method proposed by Mr. Fox, even if hydrogen peroxide were
contained in his first absorption vessel. No experimental
evidence of such oxidation is presented by Mr. Fox, and certainly
none in the reference quoted by him.1 However, the question
is relatively unimportant since little or no ammonia is allowed to
pass the oxidizer in commercial operation.
In regard to the second point at issue, the completeness of
the oxidation of NO to NO., the literature cited by us and con-
firmed by our own experiments shows that this reaction is not an
instantaneous one and has a negative temperature coefficient.
The latter is important. If the gas is not cooled to room tem-
perature even with a large excess of oxygen, there is no assurance
that the reaction will complete itself unless a large reaction space is
provided before the gases enter the alkaline absorbing solution.
The apparatus sketched by Mr. Fox shows that the only re-
action space provided is the narrow tube conducting the gases
to the bottom of the absorption vessel. Since the gases must
be kept hot till they enter this tube to prevent moisture condensa-
tion, it appears likely to us that the reaction does not complete
' Ber., 7, p. 1745.
itself before the acid oxides are absorbed by the alkali. But
if Mr. Fox obtained practically equal quantities of nitrate and
nitrite in his absorbers from the hot oxidizer gases, we withdraw
the objection in our original paper.
We quite agree that NO is not absorbed by alkali or alkali
containing hydrogen peroxide. But a mixture of NO- and NO
in any proportions such that NO does not exceed that of NO»
is more readily absorbed by alkali than NOu alone.'
In our aspiration method a partial reaction of NO to N02
was all that was required. The use of oxygen was to clear
absorption vessel K" of air at the beginning of the test and of
the oxidizer gases at the end of the test and not to assist in the
absorption as assumed by Mr. Fox.
In our opinion no aspiration method is very satisfactory.
We do not agree that it is desirable to draw continuous samples
or samples over a period of time. In fact, to the authors'
knowledge, a commercial plant using an aspiration method
similar to that advocated by Mr. Fox, has recently discarded it in
favor of the vacuum method which they have recommended.
The vacuum bottle method has been in use over a year under all
kinds of experimental conditions and in actual plant operation,
where it has proved satisfactory. When high concentrations
of ammonia are being oxidized it is necessary to introduce a
little pure oxygen after taking the sample, but it is not necessary
to measure it and is no trouble whatever. One man with a
little experience can make a complete efficiency test including
calculation of results in half an hour if determination of the free
ammonia escaping oxidation be neglected.
Bureau of Mines GUY B. Taylor
Washington, D. C. J. D. Davis
January 3, 1918
AVOIDABLE WASTE IN THE PRODUCTION OF SUL-
FURIC ACID BY THE CHAMBER PROCESS
Editor of the Journal of Industrial and Engineering Cliemistry:
In connection with the subject of the increased production of
sulfuric acid called for on account of explosives requirements,
it is interesting to consider one phase which seems to have es-
caped general observation. In the United States we make some
four million tons of acid by the chamber process each year.
Very few chamber plant* are run on a scientific basis', in fact,
most of them operate by rule of thumb, this being particularly
true of the acid plants attached to fertilizer factories. While
there has never been a survey made of the average operating
conditions in the chamber plant acid industry, I am reasonably
sure from the data I have gathered during the past five years
that the average chamber plant space obtained by combining
all the plants in the country would be of the order of 13 cu. ft.
per pound of sulfur burned. With proper analytical control
of the gases, and with exact control of the volume and tempera-
ture of the acid circulated over the towers there is no reason why
the chamber space used should not be cut down to 11 ft. per
pound of sulfur burned per 24 hours Suppose, however, the
average improvement is no more than a reduction to 12 cu. ft,
we would have an increased output, -.cithout the construction of
additional plant, of some 300,000 tons of 500 Be. sulfuric acid
per year.
A questionnaire sent to the acid manufacturers covering
chamber acid output and chamber space per pound of sulfur,
would soon show the possibilities of increasing our acid produc-
tion in the way I have indicated, but, of course, such a query
to result in answers of real value would have to be sent out by
some department of the Government.
A. E. Marshall
Baltimore. Mo. Chemical Engineer
January 4, 1918
1 Foerstcr and Blich, Z. aniev. Chrm., it (19101, 2017-25.
Feb., igil
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
BROMINE PROCESS DECISION
According to the Oil, Paint and Drug Reporter for December 24,
1917, the case of the Dow Chemical Company vs. the American
Bromine Company and Arthur E. Schaefer, which has been
heard in both Midland and Wayne counties, Michigan, and which
was transferred to the Detroit district last June, has been de-
cided in favor of the plaintiff, the Dow Chemical Company,
by Circuit Judge Kelly S. Searl
This case was probably the most striking of recent suits in
the chemical industry based upon alleged disclosure of secret
processes by former employees, and also involving the ownership
of patents covering processes
The plaintiff, the Dow Chemical Company, asked a perma
nent injunction restraining the defendants from making use of
certain trade secrets, claimed to be the exclusive property
of the Dow Company and unfairly obtained from certain
of its employees and also asked that a certain patent be trans-
ferred to the Dow Company, since through contract with the
defendant Schaefer the property right in the patent was held to
belong to the Dow Company.
The taking of the testimony has consumed weeks, and in addi-
tion to models, marks and charts, the ordinary exhibits numbered
several hundred and several thousand pages of testimony were
taken.
justice searl's findings
The patent and the processes in dispute had to do with the
manufacture of bromine and bromides from brine by means of
an electrolytic cell and by other combined methods held in strict
secrecy by the Dow Company and, according to the ruling of
Justice Searl, used and copied by the American Bromine Com-
pany in its plant. Justice Searl, in his opinion filed on December
14, 1917, said in conclusion:
"The parties who subsequently incorporated under the name of the
American Bromine Company had apparently never heard of the Kossuth
cell. They did not undertake to build such a cell for their plant, but in-
stead they copied the Dow cell and are now using one so near like as to
require that they be restrained from using the same longer. The fact
that a patent had been taken out years ago in Germany for this Kossuth
cell is of very little importance in this case, and the same may be said of
the pther German and American patents. The existence of the majority
of these patents was unknown to the defendants until after the commence-
ment of this suit. They did not secure the right to use them nor to build
up their business in reliance upon disclosures from them which the public
by reason of the expiration of the patents were entitled to use
"On the contrary they set out, as admitted by them, to build a plant
aa near like the Dow plant as possible and not infringe the Dow patents.
Whether they have infringed any of the Dow patents is not a question to
be decided in this case. * * * but they did succeed in building and equip-
ping a plant in all essential respects like the Dow plant at a time when the
plaintiff was operating the only plant of that kind in this country — or
anywhere for that matter.
"Plaintiff, having by reason of the inventions of Dow and others
kept its processes secret and built up an extensive and thriving business,
is now entitled to the relief prayed for in the bill Sled in this cause.
"A decree may be entered accordingly, including a clause requiring
defendant Schaefer to assign his said patent to the plaintiff. And. inasmuch
as the American Bromine Company have under their contract with Schaefer
an interest in said patent, such defendant will also be required to relinquish
the same.
"The court will not at this time undertake to state the exact terms of
the decree, as counsel are better prepared than the court to frame and agree
upon the terms thereof. Each party may propose a decree, and if the same
cannot be agreed upon or settled by the court without doing so, a day will
be set apart for hearing counsel on both sides upon the settlement thereof.
Plaintiff will recover costs to be taxed as against the defendant."
COMPLAINT AS FILED
The bill of complaint set forth: That Herbert H. Dow,
of Midland, Mich., discovered the presence of bromine in cer-
tain brine from natural gas wells, and that after investigations
in 1888 and 1889 he discovered a new process by which the bro-
mine was extracted by blowing air through the brine and then re-
covered by bringing in contact with certain chemicals, resulting
in the formation of desired bromides; that during 1889 he manu-
factured bromide of iron by this process; that on October 28,
1889, he applied for a patent issued September 29, 1891 (No.
460,370), and reissued April 12, 1892 (No. 12,232), and that he
began the construction of a plant in Midland, Mich., in August,
1890. That subsequent investigations resulted in the develop-
ment of an electrolytic process, and that all processes were con-
veyed to the Midland Chemical Company and kept secret,
the works enclosed with a barrier, and specially guarded to pre-
vent the details from becoming public, the manufacture of
bromides being carried on in a separate building, also guarded.
That the two bromide plants of the plaintiff have a present ca-
pacity of 1,500,000 lbs. a year.
That on July 9, 1904, plaintiff employed Arthur E. Schaefer,
one of the defendants, as a chemist in its laboratory; that later
Schaefer had charge of the plaintiff's bromide plant and its
manufacture of bromides and the processes used, and that he
continued in that capacity until September 15, 1905; that about
February 1, 1908, he returned to the employ of the Dow Com-
pany and became the superintendent of the bromide plant and
continued in that capacity till July 1, 1910; that the Emerson
Drug Company, of Baltimore, and the Dr. Miles Medical
Company, of Elkhart, Ind., through their principal stock-
holders or stockholding interests undertook the organization
of the American Bromine Company on December 1, 1915,
and bought lands and erected a plant at Midland; that the
plaintiff was advised and believes a complete apparatus for the
manufacture of bromide identical with that used by the Dow
Company and including all the Dow secret devices and apparatus
was erected; that to acquire the knowledge of the processes
the defendant employed Julius Burow, A. M. Douglas, former
employees of the Dow Company, and sought to employ James
C. Graves, formerly general superintendent for Dow, but he
refused; that afterwards Arthur E. Schaefer was employed by
the American Bromine Company as consulting engineer and
expert adviser; that while Schaefer left the employ of the Dow
Company July 1, 1910, he was continued on the payroll for
three months under special agreement; that Schaefer obtained
a patent, No. 1,085,944, °n a method for the recovery of bromine
by the aid and for the use of a solution of ferrous bromide therein,
claiming he was the inventor and that the process was in use
in the Dow plant at the time Schaefer was employed there.
ANSWER TO COMPLAINT
The American Bromine Company in answer to the bill of
complaint filed affidavits to the effect that although it had em-
ployed a Dow employee, one Douglas, and he had collaborated
on the erection of a cell, the cell was not successful, and that
another cell was developed and also a process differing in es-
sentials from the Dow process. An improvement on the Dow
process of purifying the bromide brine as it passed through the
electrolytic cells was especially commented upon. The de-
fendant denied any intention to appropriate any secret of the
Dow process, and denied any effort or steps to do this.
The suit was to compel the disclosure of suras paid by the
American Bromine Company or any other person for right to
use patent 1,085,944, the assignment of the patent by Schaefer,
and perpetual injunction against the use of processes of Dow,
or the employment of any of the former or present Dow employees
or of disposing of the patent to anyone else, together with an
accounting, and that the existing devices and apparatus in the
American Bromine plant be ordered destroyed, together with
payment to the Dow Company of all sums found due them in
accounting as assessed by the court.
OPINION OF JUSTICE SBARL
The court traced the steps taken by Dow in perfecting an im-
proved process of recovering bromine, in place of the old boiling-
out process used previously, instancing the use of electricity and
158
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 2
the blowing-out process more fully developed later, and both
of which have been in use by the Midland Chemical Company
and Dow Chemical Company practically continuously since
1892. The Dow Company had practically no competition in
America, and although German manufacturers were shipping
some bromine to the United States, these shipments ceased
at the outbreak of the European war.
Justice Searl then proceeded: That the Emerson Drug
Company and the Dr. Miles Medical Company had purchased
bromides in considerable quantities, the former company as high
as 100,000 pounds a year on contract. With the increased
price demanded a controversy arose, the purchasing concerns
alleging that the Dow Company was charging an exorbitant
price because having a practical monopoly. In 1915 the Emer-
son Company considered the advisability of engaging in the
manufacture of bromide, and learned of Douglas and of the fact
that the Meyer Brothers plant at Midland was for sale. A co-
partnership was formed by the Emerson Drug Company and
the Dr. Miles Medical Company and the American Bromine Com-
pany was incorporated under the laws of Michigan in December,
1915 with the Emerson Company holding 60 per cent and the
Miles Company 40 per cent of the Bromine Company stock.
The court then reviewed the correspondence between Douglas
and the Emerson Drug Company, the discussion of the process
to be used and the fact that Dow was using an electrolytic pro-
cess. After all the correspondence and conferences "in which
the founders of the American Bromine Company were prac-
tically informed in so many words that the Dow Company
were operating under secret processes in addition to its patented
processes, Douglas was employed and set to work to build a
plant to make bromines and bromides, not by the use of bittern
waters as he recommended, but by the electrolytic process."
"The officials of the Emerson Drug Company." asserts the
court, "must have had full notice and knowledge that it was
proposed to duplicate the plant of the Dow Company in all
its essential details, except possibly where it might conflict
with the patents held by the Dow Company." Later, Schaefer
was employed to take the place of Douglas.
The court also says: "I find that except in some minor de-
tails the plant of the American Bromine Company is in its es-
sential characteristics a duplicate of portions of the plant of
the Dow Chemical Company and that in the manufacture of
bromine and bromides from raw brine the American Bromine
Company are now using the same processes as were used by the
Dow Company at the time Douglas and Schaefer were employed
by the latter company."
UNITED STATES TARIFF COMMISSION INQUIRY IN
REGARD TO CHEMICAL INDUSTRIES
The Tariff Commission is undertaking an inquiry into the
significant developments that have taken place in the chemical
industries since the passage of the tariff act of 1913. Changes
which seem likely to alter permanently the conditions of inter-
national competition or the course or volume of foreign trade
are to be special subjects of study.
All persons having direct knowledge of pertinent facts in re-
gard to any particular industry or product are invited to sub-
mit a statement of the Tariff Commission. Among the mat-
ters on which the Commission desires as full and complete in-
formation as possible are:
1. The manufacture within the United States of articles
formerly unavailable or obtained exclusively by importation,
for example, phosgene.
2. In the case of industries previously established in the
United States, the erection of new plants or increase in capacity
of existing plants; for example, the increase in capacity of ex-
isting plants for making caustic soda and chlorine and the in-
stallation of such plants at textile and paper mills.
3. The future of industries or establishments newly created,
or in which productive capacity has been greatly increased to
meet a direct war demand. How can these plants be utilized when
the war demand disappears? For example, the acetone industry.
4. Any general or significant differences in the prevailing
method of manufacture in the United States and abroad, such
as the relatively small use of the carbureted water-gas process
in England compared to the process in the United States.
5. Differences in the organization of the industry in the United
States and abroad.
6. The development or invention in the United States or abroad
of new or improved processes which are likely to influence the con-
ditions of international competition; for example, the hydrogena-
tion of fatty oils or the flotation process for concentrating ores.
7. Significant changes in the conditions of international
competition caused by the recent law-making patents owned
by citizens of enemy countries available to American manufac-
turers; for example, the patents on salvarsan.
S. Industries which have been seriously hampered in their
normal operations or in their development by difficulty in se-
curing materials or supplies formerly imported; for example,
the lack of potash for fertilizer or glass. If these difficulties
have been met by the introduction of substitutes, it is expected
that there will be a return to the old materials and methods
when foreign supplies again become available, or will the changes
be permanent2
9. Developments or changes in other industries which have
created a new or greatly increased demand for chemical prod-
ucts; for example, the manufacture of new varieties of glass in
the United States.
10. The discovery of new uses of materials, creating a new
demand or furnishing a market for materials formerly wasted;
for example, the use of aniline as an accelerator in the vulcan-
ization of rubber.
n. Any governmental hindrances in the United States or
abroad, either in manufacture or commerce; such as the export
duty on nitrate from Chile.
The Commission will publish only general statements or sum-
maries, which will not reveal the operation or plans of individual
companies.
SPECIAL CHEMICALS AND APPARATUS AVAILABLE
THROUGH THE CHEMISTRY COMMITTEE OF
THE NATIONAL RESEARCH COUNCIL
The Chemistry Committee of the National Research Council
will endeavor to locate for our chemical investigators chemicals
and apparatus where the need is definite and urgent, and where
the article required is not obtainable in the open market. In-
quiries for chemicals should be addressed to Prof. Roger Adams,
University of Illinois, Urbana, 111., who has already published
lists of certain of the products which are obtainable through his
office. Requests for aid in locating apparatus should go to
Mr. A. H. Thomas, W. Washington Square, Philadelphia, the
Chairman of our Sub-Committee on Chemical Apparatus.
As these gentlemen are carrying out this work as a patriotic
service for the welfare and security of our country and without
any remuneration for the labor involved, it is requested that
investigators in need of such supplies make sure that the material
required is not available through the ordinary commercial
channels before turning to these colleagues for aid, as the burden
of correspondence is already heavy. When the desired material
is located, the inquirer will be put in direct communication with
the owner, so that a loan or sale may be arranged. It will
assist these gentlemen in their labors if chemists and physicists-
having special or unusual chemicals or apparatus available for
loan or sale will forward full details concerning the same.
Washington, D. C. MarsTON Taylor BoGERT
January 14. 1918
Feb., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
iS9
AS TO PLATINUM
Editor of the Journal of Industrial and Engineering Chemistry:
Much has been written of late, and more said, regarding the
use of platinum in jewelry, and it has been broadly intimated
that the jewelers are not living up to their agreement of last
April with the Government. It is worth while to repeat the
terms of this pledge of the Jewelers' Vigilance Committee.
"We pledge ourselves to discontinue and strongly recommend to all
manufacturing and retail jewelers of the United States that they in a truly
patriotic spirit discourage the manufacture, sale and use of platinum in all
bulky and heavy pieces of jewelry.
"During the period of the war, or until the present supplies of platinum
shall be materially augmented, we pledge ourselves to discontinue and
recommend that the jewelry trade discourage the use of all non-essential
platinum findings or parts of jewelry, such as scarfpin stems, pin tongues,
joints, catches, swivels, spring rings, ear backs, etc., where gold would
satisfactorily serve.
"Be it further resolved that the jewelry trade encourage by all means
in its power, the use of gold in combination with platinum, wherever proper
artistic results may be obtained."
Having been in close touch with the platinum situation I
desire to state from personal knowledge my belief that the
jewelers have fully lived up to their pledges and in many cases
gone beyond them in efforts to conserve platinum.
It was the manufacturing jewelers who entered into this
agreement, and it is not surprising that some retailers have
been making great efforts to work off their stock on hand, and
have thereby opened themselves to criticism.
Whether a metal, so limited in supply and so invaluable in
scientific industry, ought to be used at all in jewelry is a fair
question, but it is not the question in point. A large and
legitimate platinum jewelry industry has sprung up in recent
years, and the question is whether the exigencies of the present
platinum situation demand the immediate wrecking of this
industry by having the Government commandeer all platinum;
personally, I do not believe that at present they do.
I hold no brief for the jewelers, but I think this statement
should be made in fairness to them ; and I may add that it is my
conviction, that, should the Government be placed in straights
from lack of platinum for the manufacture of war material, the
jewelry trade can be relied on to find a way of furnishing all that
is needed. Jas. Lewis Howe
Special Committee on Platinum,
Chemistry Committee of the National
Research Council
Washington and Lee University
Lexington. Virginia
PLATINUM RESOLUTIONS
At the recent Pittsburgh meeting of Section C (Chemistry)
of the American Association for the Advancement of Science,
the following resolution was unanimously passed:
Whereas (i) The Government of the United States has
purchased from Russia and safely brought to the United States
twenty-one thousand (21,000) ounces of platinum, the largest
amount that has ever been shipped to this country;
(2) The separation of so great an amount of platinum will
offer scientific investigators an opportunity to study the chemical
combinations and mineralogical associations of the platinum
group of minerals,
Therefore it is Resolved (1) That Section C, the Section on
Chemistry of the American Association for the Advancement of
Science, respectfully request that the War Industries Board,
the Bureau of Standards, the Bureau of Mines, the American
Chemical Society, and others who are interested in chemistry,
be offered the opportunity by the United States Government
to cooperate with it in the separation of the platinum
minerals of the above-mentioned material, and that the residue,
of which there may be thousands of ounces, be loaned to such
scientific investigators who can undoubtedly obtain interesting
scientific results, and
(2) If necessary, that one platinum works be commandeered,
with proper compensation, for a certain length of time so that
the work of separation can be carried on with the greatest care
and observation, and
(3) That as much as possible of this platinum be loaned to
those who have need of platinum for chemical investigation,
the platinum to belong to the Government of the United States
and subject to the call of the Government when needed for raw
or industrial purposes. As the expense of making crucibles or
other utensils is small in comparison to the value of the platinum,
this would offer a most unique opportunity to the chemists of
the country.
To present this matter to the proper authorities a committee
was appointed consisting of Dr. W. A. Noyes, Chairman, and
Dr. W. F. Hillebrand.
New York City
January 5, 1918
George F. Kunz
FUEL FOR MANUFACTURE OF CHEMICALS
Editor of the Journal of Industrial and Engineering Chemistry:
In view of the shortage in fuel supply and the great demand
for large supplies of cheap fuel for the manufacture of chemicals
and other products necessary for the war and agricultural pur-
poses, I am bringing to your attention our unusual supply of
natural gas at Shreveport, which is available to large industrial
consumers on a basis that makes it cheaper than water power
or that derived from the use of coal.
There is now available at Shreveport about one billion cubic
feet of gas daily, and on the basis of scientific estimate the con-
tent of the Shreveport field is two trillion cubic feet, and a
very small amount of this gas is now being utilized This esti-
mate includes only the field as already defined and does not
consider other fields which are being opened up near by in
drilling for oil. A prominent geologist has recently stated that
the Shreveport field has the largest supply of natural gas to be
found in the United States.
In addition to our gas supply, we have an abundance of raw
materials that are needed for war industries at this time. There
is close at hand an abundance of iron, petroleum, lignite, lime-
stone, sulfur, and salt, and generous supplies of asphalt, gypsum,
kaolin, sand, gravel, clay, etc. It ought to be especially noted
at this time that Louisiana has the largest deposits of sulfur
and salt to be found in the United States.
Shreveport, Louisiana
November 21, 1917
Rllis Smith
A STUDY OF THE ESTIMATION OF FAT IN CONDENSED
MILK, ETC.— CORRECTION
In our article printed under the above title [This Journal,
9 (1917), 1 111] the following changes should be made:
Page 1 1 13, 1st col., line 18— "0.4" should read "0.04;" Table
V, 3rd col.. No. 8 — "2.5005" should read "2.0505."
C. H. BlESTERKELD AND O. L. EvENSON
COMPOSITION OF LOGANBERRY JUICE AND PULP-
CORRECTION
In the article under the above title [This Journal, 9 (i9'7)>
1043] note the following rearrangement of 5th line, Table I:
1
11
in
(Alkalinity 0.4139 0.5785 0.4226
Per cent Ash { k,COi 0.4130 0.5075 0.288
should read:
Percent Ash 0.4139 0.5785 0.4226
Alknlimi (uKiCO 0.4130 0.5075 0.288
M R. Daughtbrs
i6o
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 2
CHEMISTS AND THE DRAFT
Editor of Ike Journal of Industrial and Engineering Chemistry:
The information contained in the editorial in the January
number of the Journal under the caption "The Chemical Service
Section of the National Army" must indeed be gratifying to
the members of the Society in that chemistry is now accorded,
for the first time, a definite and official place in the organization
of the War Department's activities.
Naturally, the organization of such a new branch of service
must be at present in its infancy, and subject to such alteration
and revision as experience may indicate. At the same time
there comes up in the mind of the writer the question — and the
same question must present itself to many others — of what will
be the status of drafted chemists who may be assigned to this
service; that is, whether a drafted chemist will be given the same
Tank as he might have been given had he sought a commission
instead of waiting to be drafted.
Any distinction between the rank assigned a volunteer chemist
and a drafted chemist of the same training, who does the same
type of work, must be an artificial one. Many chemists have
been deterred from seeking commissions by considerations such
as were expressed in Dr. Parsons' recent circular letter to the
members of the Society ; they have had to face the dilemma pre-
sented, on the one hand, by the impulse to volunteer their services
for work bearing immediately on the prosecution of the war,
and, on the other hand, by the obvious desirability of a con-
tinuation in their usual work, which, though it did not deal with
explosives or poison gases or gun-metal, was yet a necessary con-
tribution to the public welfare.
Is the drafted chemist to be given the rank of private, irrespec-
tive of what rank his training might reasonably be expected to
entitle him to, merely because he has waited for the draft, the
selective principle of which may be expected to utilize his ability
most efficiently? The question might appear premature, if not
foolish, were it not for the fact that some chemists called in the
first draft have been put on chemical research in the capacity of
privates. One inevitably draws a comparison to the conditions
obtaining with regard to physicians. To the writer's knowledge,
physicians drawn in the first draft have been commissioned when
they were assigned to medical work. There can be no essential
difference between the two cases. To be sure, the term "chemist"
(covering as it does everything from a routine analyst to a trained
researcher) is a much more flexible one than the term "physician,"
which in general represents a more uniform, though not always
more intensive, degree of training. Yet it seems almost too
obvious to say that the Ph. D. (or in many cases a lower degree)
in chemistry, with some years of experience in the practice of the
profession, represents as high a degree of training as does the
M.D., often without any experience to back it up. The raw
M.D. has been getting and does get a commission, if he is a cap-
able graduate of a reputable school. May not the chemist expect
equal consideration of the value of his services?
The writer believes that some statement on these matters,
derived either from information the Editor may have or from
additional information from the War Department, would be
welcome and illuminating to many readers of This Journal.
Edwin C. White
Jambs Buchanan Brady Urological Institutb
Baltimore, Md., January 16, 1918
WASHINGTON LLTTLR
By Paul Wooton. Metropolitan Bank Building, WashingtO
The outstanding feature of the month in Washington was the
"workless day" order of Dr. H. A. Garfield, the fuel administra-
tor. Many manufacturers of chemicals joined in the protests
against the order which descended almost in the volume of an
avalanche upon official Washington. Owing to the shortage in
most chemicals, reasons were presented why many manu-
facturers of chemicals should be included in the exemption list.
At the time this is written, however, J. T. Lewis Bros. Co.,
Lafayette Building, Philadelphia, manufacturers of chrome
green, C. W. H. Carter, 8 Ferry St., New York, manu-
facturers of linseed oil, and all manufacturers of optical glass,
are the only chemical industries which have been granted ex-
emption. Numerous others were under consideration, however,
and it is anticipated that various manufacturing chemists will
be added to the exemption list.
During the past two months, decided increases have been
attained in the manufacture of many much-needed chemicals.
In fact, the achievements in this direction have been so decided
that much of the uncertainty expressed as late as two months
ago has been dispelled.
Greatest concern just at this time is centered on sulfuric acid,
arsenic and ammonia, but the situation in each of these cases
has been relieved measurably. Many of the uncertainties,
which entered into estimates of the requirements of sulfuric acid
for nnH, have been removed, showing that many of the estimates
were too high. In addition, it has been possible to increase the
productive capacity of existing plants and it has been found
that considerable restriction in the use of acid can be practiced
without the serious unsettling of the industries affected. These
conditions combine to make the immediate situation less serious,
while the activities of the War Industries Board looking to the
construction of new plants give reassurance for the future. In
this latter work, M. F. Chase is prominent. His new duties
made it necessary for him to relinquish his work with the
chemical division of the Committee on Raw Materials. A. E.
Wells, the superintendent of the Salt Lake City experiment
station of the Bureau of Mines, has been assigned temporarily
to the War Industries Board to look after the work on acids
which heretofore has been handled by Mr. Chase. Mr. Wells
has been specializing on sulfuric acid for some time and has just
completed a personal visit to practically every acid-producing
plant in the country.
Special steps have been taken by the Fuel Administration to
insure a supply of coal for the sulfuric acid plants. In order
that this may be done intelligently, each manufacturer of sulfuric
acid has been asked to report the amount of coal on hand, his
monthly requirements and the name of the company supplying
the plant with coal.
Commendation for Charles W. Merrill has been forthcoming
from all concerned in the arsenic industry as a result of the
arrangements which he brought about with regard to the regula-
tion of profits and the restriction of use so as to insure ample
supplies for noxious gas manufacture and for insecticides.
The licensing system has been extended to all those engaged
in importing, manufacturing, storing or distributing ammonia,
ammoniacal liquor or ammonium sulfate. The enforcement
of the regulations which have been drawn up to cover this
trade will be in the hands of an interdepartmental committee
headed by Mr. Merrill. The other members of the committee,
each of whom is identified, directly or indirectly, with chemical
industry, are M. I,. Wilkinson and Carl I. Alsberg, Department
of Agriculture; Maj. Backus, Bureau of Ordnance; Lieut.-Col.
\Y. H. Walker. Chemical Service Section of the National Army;
Maj. M. J. Whitsm, Cantonment Division, Quartermaster
Corps; Admiral Ralph Earl, Navy Department; Maj. J. T.
Crabbs, Interior Department, and 1. 1. Summers, Council of
National Defense.
In the campaign for the conservation of ammonia, a propa-
ganda is being carried on looking to the harvesting of as much
natural ice as is possible.
A price of $75.50 per ton has been placed on the Govern-
ment's supply of nitrate of soda Approximately 100,000 tons
of nitrates were purchased by the Government in Chile and have
been transported to several American ports. It is to be sold
directly to farmers, who must agree not to re-sell and to use
it on their own [aims.
Exports of chemicals during the first eleven months of 191 7
reached the unusual value of $171,943,221. This is more than
Feb., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
161
$20,000,000 greater than the value of chemical exports during
the corresponding period of 1916. During November, 1917,
chemical exports totaled $15,428,809 in value. This was
slightly under exports in November of 1916, when they amounted
to $17,153,625. Sulfuric acid in November, 1917, amounted to
3,823,898 pounds, as compared with 2,975,602 pounds in Novem-
ber of 1916. For the first eleven months of 1917, exports of
sulfuric acid amounted to 57,311,684 pounds, or approximately
the same amount exported during the corresponding period of
1916 when exports were 60,361,638 pounds. The more striking
increases in exports were in acetate of lime, calcium carbide and
glycerine. Increased amounts of chemicals were sent to France,
Italy, Spain, United Kingdom, Brazil and Japan. Decreased
amounts were sent to Russia, Mexico and Canada.
In order to prevent undue inconvenience to the public and to
avoid the handling of large numbers of licenses, a very general
rule is being adopted by the Government agency issuing licenses
to exclude druggists, wholesalers and dealers handling only
secondary products. Persons using prime products solely as
ingredients in the manufacture of products not subject to license
also are being excluded.
The Bureau of Standards is taking up a study of methods of
analysis for molybdenum, tungsten and metallic products de-
rived from them. Samples are being prepared which will be
sent out to be analyzed by a number of experts. Thus con-
clusions will be reached as to the adequacy of the comparative
values of metals employed by various analysts. Out of these
returns, it is expected to show just where methods should be
improved.
The absence of opposition to the Garabed invention was
emphasized, when, in the midst of a busy day, no one in the
Senate objected when unanimous consent was asked by Senator
James for its consideration. The bill had been reported favor-
ably by the committee on patents and was passed without
opposition or discussion. The Senate Committee made a few
corrections in the phraseology but did not alter the salient
features of the measure, which had passed the House. It is
believed now that the President will sign the bill. This will put
the matter directly up to Franklin K. Lane, the Secretary of the
Interior.
While there was some decrease in the amount of iron pyrites
imported in 191 7, as compared with that brought in in 19 16, the
general policy with regard to imports remained unchanged.
Manganese imports in 191 7 were somewhat in excess of those of
the year preceding. The shipping question has grown more
acute, but still there is no organized effort to promote domestic
production of these two important war minerals. In order to
meet this situation, it has been found necessary to attempt to
secure legislation. As a result, the War Minerals Committee
drafted a bill which would place in the hands of the President,
for the handling of minerals, the same wide powers with which
he already has been vested for the control of food. The bill
has been considered by the House Committee on Mines and
Mining. Some amendments have been made, but the bill,
with its main features, which follow almost exactly those of the
Lever Act, is on the point of being introduced by Representative
Foster, the chairman of the House Committee on Mines and
Mining.
PERSONAL NOTL5
Assistant Professor Reston Stevenson, in charge of physical
chemistry in the department of chemistry in the College of the
City of New York, has been appointed Captain in the Sanitary
Corps of the Medical Department of the National Army, and is
at present in France.
Mr. Howard Adler, assistant tutor in physical chemistry in
the department of chemistry in the College of the City of New
York, was detailed to duty in Camp Upton, Yaphank. and subse-
quently placed in the chemical service of the army.
Mr. Arthur Davidson, assistant tutor in the department of
chemistry in the College of the City of New York, has been
appointed in the chemical branch of the United States Army.
Dr. Ernest E. Smith, of New York City, has been elected
president of the New York Academy of Sciences.
Professor Frederick G. Keyes, of the Massachusetts Institute
of Technology, who has been commissioned Captain in the
chemical section, has been granted leave of absence and expects
to go abroad soon. Dr. Duncan Maclnnes, now research
associate in physical chemistry, has been appointed to serve in
place of Dr. Keyes.
The main laboratory of the United States Fisheries Biological
Station at Fairport, Iowa, was destroyed by fire on December
20. The station is the center of most of the scientific work of
the Bureau of Fisheries in the Mississippi Basin.
Professor Wilder D. Bancroft, of the department of chemistry
of Cornell University, is serving as technical adviser in the
U. S. Bureau of Mines, Washington, D. C.
On January 12, 1918, Professor H. C. Sherman, of the de-
partment of chemistry of Columbia University, lectured before
the Harvey Society at the New York Academy of Medicine on
"Food Chemistry in the Service of Human Nutrition."
Dr. R. L. Kahn, pathological chemist of the Montefiore
Home and Hospital, New York City, has been commissioned
First Lieutenant in the Sanitary Corps, stationed at the De-
partment Laboratory, Southeastern Department, Atlanta, Ga.
Dr. Chas. E. Vanderkleed, formerly director of the chemical
laboratories of the H. K. Mulford Company, is now engaged
in the manufacture of synthetic chemicals. He is vice president
of the Markleed Chemical Corporation, New York and Camden.
Dr. Joseph Price Remington, Dean of the Philadelphia Col-
lege of Pharmacy since 1893, died on New Year's Day.
Dr. Charles T. P. Fennel, for fifteen years state chemist in
Ohio and later professor of chemistry in the Cincinnati College
of Pharmacy, has been appointed to the chair of materia medica
at the University of Cincinnati, to fill the vacancy created by
the death of Dr. Julius Eichberg.
Professor Arthur W. Browne, of the department of chemistry
of Cornell University, has been appointed chemical expert of
the Ordnance Department. He will continue his work at Cor-
nell University.
A General Science Hall, erected at a cost of $60,000, is under
construction at Defiance College, Defiance, Ohio. It is ex-
pected that it will be completed next July.
Mr. C. L. Brickman was recently appointed chief chemist
by the Rex-Hide Rubber Manufacturing Company, East Brady,
Pa. He was formerly in the research laboratories of the United
States Rubber Company. He is a graduate of Defiance Col-
lege and the department of chemical engineering of the Case
School of Applied Science.
The Lenz Apparatus Company, New York City, announces
that Dr. W. J. Lenz is no longer connected with or in any way
interested in that company.
Dr. F. E. Carruth, formerly of the Chemical Division of the
North Carolina Experiment Station, is now with the Schaefer
Alkaloid Works, Maywood, N. J.
The Hon. Sir Charles Parsons, K.C.B., F.R.S., member of the
Council of the Institute of Metals (London), is to give the 8th
Annual May Lecture before the Institute this spring. The
lecturer will speak on the subject of the formation of diamonds.
Dr. E. P. Wightman, research chemist of Parke, Davis & Co.,
of Detroit, Michigan, and Windsor, Ontario, has enlisted as a
chemist in the Gas and Flame Division of the Thirtieth Engi-
neers of the U. S. A.
Mr. Charles S. Purcell, formerly of the Bureau of Mines,
Pittsburgh, Pa., has been transferred to the Boston Station of
the Bureau of Chemistry.
Professor Charles H. La Wall delivered, on January 17. an
illustrated lecture on "Some New and Interesting Vegetable
Foods," at the Wagner Free Institute of Science, Philadelphia.
A society for the furtherance of chemical knowledge and cur-
rent scientific data has been organized by the technical chem-
ists and chemical engineers of Tacoma, Washington. The
president is Paul Van Horst and the secretary, B. H. Bennetts.
The work of the National Research Council has expanded so
tapidly that it has outgrown the space available in the Munsey
Building, and therefore the Council has rented the entire build-
ing at the corner of 16th and L Streets, N. W.. Washington,
I). C, occupied until recently by the Fuel Administration,
The office of the Chemistry Committee will be in Room 24,
second floor front.
l62
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 2
Dr. H. P. Corliss, former fellow in the Mellon Institute of
Industrial Research, Pittsburgh, Pa., is now with the Metals
Co. as research chemist and metallurgist, with
headquarters at the General Engineering Co., Salt Lake City,
Utah.
Mr. Samuel Ginsburg has resigned from the Drug Laboratory
of the New York Station of the United States Bureau of Chem-
istry to accept a position as chemist in charge of laboratory
with the National Gum & Mica Co. of New York City.
Mr. Roy Richard Denslow, assistant tutor in the depart-
ment of chemistry, College of the City of New York, has been
appointed instructor in Smith College.
Miss Grace MacLeod has accepted the position of Assistant
Editor of This Journal. Miss MacLeod holds the degree of
SB. from the Massachusetts Institute of Technology and of
M.A. from Columbia University, and for the past seven years has
been instructor in chemistry at Pratt Institute, Brooklyn, N. Y.
In spite of adverse industrial conditions brought about by the
war and severe weather conditions which interfered greatly with
traveling facilities, the Short Course in Ceramic Engineering is
entering upon the second week of its session with a registration
of twenty-one men coming from ten different states and repre-
senting eight different branches of the ceramic industries, in-
cluding the manufacture of brick, sewer pipe, drain tile, glass,
grinding wheels, terra cotta, and also including representatives
in geological surveys and the general engineering firms.
Mr. Robert J. Anderson has resigned as chief chemist and
metallurgist of the Cleveland Metal Products Company, Cleve-
land, Ohio, to take effect February 1, 1918.
Dr. Julius Stieglitz has been elected president of the Institute
of Medicine of Chicago.
Mr. W. J. Suer has accepted a position as chemist with the
Ault and Wiborg Company of Cincinnati.
The committee on the analysis of commercial fats and oils
of the Division of Industrial Chemists and Chemical Engineers
of the A. C. S. now consists of W. J. Gascoyne, H. J. Morrison,
J. R. Powell, R. J. Quinn, W. D. Richardson, Paul Rudnick,
L. M. Tolman and J. J. Vallertsen.
The Powdered Coal and Engineering Company, Chicago, 111.,
announce the addition to their engineering staff of Mr. Alex L.
Feild, formerly of the Pittsburgh Experiment Station of the
Bureau of Mines, and Mr. A. R. Detweiler, formerly with the
Tribullion Mining, Smelting and Development Company, at
Kelly, New Mexico, from which company he resigned with the
purpose of undertaking private investigations with a view to
inventing a process of recovering clay and slag from used re-
torts.
Mr. Benedict Crowell, of the firm of Crowell and Murray,
chemists, Cleveland, has been appointed Assistant Secretary
of War with the rank of Major in the Engineer Reserve Corps.
He has done a great deal of ore analysis work for firms manu-
facturing and selling Lake Superior ores, and with Mr. Murray
he is joint author of "The Iron Ores of Lake Superior." Major
Crowell was born in Cleveland in 1S69 and was graduated from
Yale in 1891. On the completion of his college course he be-
came chemist for the Otis Steel Company of Cleveland. He
left that company to engage in business for himself as a chemist
and later also took up mining engineering in connection with
his other work.
The fifth convention of the National Foreign Trade Council
will be held at the Gibson Hotel, Cincinnati, on February 7,
8 and 9, 1918.
Mr. Victor Yngve has been engaged as research chemist by
the Oldbury Electrochemical Company of Niagara Falls, N. Y.,
and will have charge of their research laboratory.
Professor Wilder D. Bancroft, of Cornell University, lectured
before the District of Columbia Chapter of the Sigma Xi,
December 20, on "Colloid Chemistry."
Mr. II. A. Baker, chief chemist of the American Can Com-
pany, has gone to Washington to act on the committee on con-
servation of tin plate.
Dr. K. L. Mark, head of the chemistry department and of the
School of General Science at Simmons College, Boston, has been
granted a leave of absence for the duration of the war to accept
a commission as Captain in the Sanitary Corps of the Army.
Assistant Professor Frederick E. Breithut, in charge of munic-
ipal chemistry in the department of chemistry. College
of the City of New York, has been appointed Director of Food
Conservation by the L'nited States Government Food Com-
mission to cover the territory of Greater New York City.
Mr. F. F. Beverly, of Sears, Roebuck and Company, has en-
listed in the Sanitary Corps, Gas Defense Service. He is now
employed at Akron, Ohio, inspecting gas masks.
Mr. Albert King, of the laboratory of Swift and Company, has
joined the Gas and Flame Regiment.
Dr. J. W. E. Glattfeld has been appointed a member of the
committee on the supply of organic chemicals for research during
the war.
The death is announced of Professor G. P. Girdwood, pro-
fessor of chemistry in McGill University.
Dr. Lawrence J. Henderson, professor of biological chemistry
in Harvard University, will give a series of lectures on food
conservation at Smith College.
INDUSTRIAL NOTES
Mr. Arthur W. Kinney, Industrial Commissioner, Los Angeles
Chamber of Commerce, in the following notes tells of the activity
in the development of the mineral and chemical industries of
Southern California:
The mineral output for the year 1916 was valued at
$22,809,461, petroleum being the largest single product ob-
tained. Second in importance of production was tungsten ore
and concentrates which reached the astonishing figure of 1931
tons, valued at $3,915,434. The value of the mineral output
for 1917 is not obtainable, but it will undoubtedly show a con-
siderable gain owing to the prevailing high price of petroleum
and the important increase in the output of potash products.
Potash is now obtained in large quantities in this region from
four sources: tin- Si arks Lake deposits, kelp, sugar waste and
from the various cement plants. One of the latter now employs
a leaching system installed for preparing high-grade potash salts.
In connection with its oil refinery at Fillmore the Ventura
Refining Company has expended several hundred thousand
dollars in the construction and equipment of a wax extraction
plant. Wax will be taken from lubricating stock and handled
in large quantities as a by-product.
fineries have shown a greatly increased output. Various
refineries, notably the Standard Oil Company and the General
Petroleum Company, have spent large sums of money in addi-
tions and equipment. The former company has expended
over one million dollars at the El Segundo refinery alone and
has shown a large increase in its output of lubricants. The lat-
ter company has installed furnaces for/ the/ cracking of low-
grade distillate into synthetic gasoline.
Southern California iron ore deposits have been found to be
extensive in quantity and of high quality. Experiments have
demonstrated that this ore can be reduced through the medium
of natural gas and electric furnaces Six companies have in-
troduced electric furnaces for various purposes during the
year. The Union Tool Company, at Torrance, has installed
an open-hearth steel furnace, making a total of three companies
thus equipped. There is a great demand for the utilization
of Southern Californian resources of iron ore and a great steel
industry is promised in the not far distant future.
At Los Angeles harbor the Union Oil Company has commenced
construction on the first unit of a two million dollar refinery
for the manufacture of lubricating oils, gasoline, kerosene and
other petroleum products. This company operates a fleet of
tank steamers and not only assists in supplying the industries
of the Pacific Coast, but is a large exporter of cargoes of refined
and lubricating oils to Australia, New Zealand, and the Hawaiian
Islands, and fuel oil to the west coast of Chili.
The Chemical Production Company, Los Angeles, is erecting
a fire-proof plant at Owens Lake, Inyo County, for the manu-
facture of soda ash. This will make the fourth establishment
of its kind now operating at this point and the second built
there during the present year, the other being the California
Alkali Co., at Cartego.
The Stauffer Chemical Co. is erecting a $100,000 plant on a
1 5 -acre tract in Los Angeles. The main buildings will be of re-
inforced concrete, and hydrochloric acid will be the principal
product manufactured.
Feb., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
163
In addition to the production of molybdic acid salts the Rose
Chemical Company, Los Angeles, has made commercially
during the year in its electric furnaces, ferrotungsten, ferro-
molybdenum and ferrochrome. This company will be soon
operating three furnaces using electricity in the reduction on a
large scale of California and Arizona ores. The American
Alloy and Chemical Company has also installed an electric
furnace for the making of ferrotungsten.
The Palau Metals Co. has erected a refinery in Los Angeles.
Machinery has been installed for the reduction, by a new process,
of platinum, palladium and other metals, the ore being brought
from Nevada. This plant is said to be the only palladium
refinery in America, and the only one in the world handling
this ore in the rock.
The Pacific Refractories Company, at Vernon, is now manu-
facturing magnesite brick from magnesite produced in this
region. For a long time California magnesite has been shipped
east for the making of brick.
Another new chemical plant in the Vernon district is the Cali-
fornia Chemical Company. This company, operating its own
oil refinery, is manufacturing a full line of orchard sprays.
At Long Beach the Western Chemical Co. is successfully
manufacturing strontium nitrate from celestite, a mineral found
in Imperial County. F. G. Mortimer, of Imperial County,
is also engaged in the making of this product, which is largely
used by manufacturers of fireworks and railroad fuses.
At Searles Lake two potash companies, the American Trona
Company and Solvay Process Company, have continued to
produce large quantities of chloride of potash. The former
company has made additions to its refinery at Los Angeles harbor,
costing several hundreds of thousands of dollars, and is now
shipping potash, soda and borax in large quantities.
The Western Calcium Chloride Syndicate has equipped
buildings at 2472 Hunter Street, Los Angeles, and is producing
calcium chloride.
The Southern Reduction Co. at Vernon is making chloride
of lime and caustic soda.
At Santa Barbara the U. S. Department of Agriculture,
under the direction of Dr. J. W. Turrentine, has erected at an
expenditure of one hundred thousand dollars an experimental
kelp potash plant. The principal product manufactured thus
far is kelp ash.
White oxide of antimony, said to be the best product ever
offered in this country and exceeding in solubility the highest
grade of the French product, is now being made by the Western
Metals Company at Harbor City.
The Crystal Hills Mine, Inc., has just completed a plant at
Huntington Park for the making of salts of aluminum and mag-
nesium sulfate, drawing on the extensive salt beds of Inyo
County for raw material.
The oxygen plant of the Linde Air Products Company, com-
pleted early this year, is now in full operation. The California-
Burdett Oxygen Company, making the same product at Vernon,
has erected new buildings and greatly enlarged its facilities.
The shipbuilding industry calls for a large supply of oxyacetylene
gas.
An important industry, the manufacture of oil from soya
beans, has been inaugurated at Vernon by the Globe Oil
Mills Company. This company has recently received, direct
from Russia, a cargo of 9,300 tons of these beans and is grinding
the same at the rate of 120 tons a day. The oil is refined, washed,
bleached and filtered and the material left after its extraction is
made into oil meal cake. This industry in connection witli the
manufacture of cottonseed oil and cocoanut oil will enable
the Globe Company to keep its plant busy every working day
in the year and thereby give employment to a large number of
people.
At San Diego the Lower California Chemical Co. is making
orcein dyes, using as raw material the orchilla, a moss found
growing in vast quantities along the western coast of lower
California.
The Western Aniline Products Co. is installing m "
and equipment in a fire-proof building at Tropico for the purpose
of manufacturing photographic developers and kindred coal-tar
products. The former are to be used as a substitute- for the
mctol which is no longer obtainable in the market. The new
product has already been Wed satisfactorily by the motion
picture film laboratories and others in Los Angeles.
At Pasadena the Rare Metals Refining Co. has erected a
modern plant and is engaged in the refining of various precious
metals.
The N. C. Ward Co., Los Angeles, has installed and is operat-
ing a complete plant for the manufacture of permanganate
of potash.
At Inglewood the Graphite Products Company is equip-
ping a factory for the making of crucibles and carbon elec-
trodes.
At Corona, the United Chemical Company, recently organ-
ized, is equipping a factory for the manufacture of citric acid
and other citrus by-products. This will be the second concern
engaged in this business at this place, the Citrus By-Products
Company, a cooperative organization composed of various
members of the California Fruit Growers' Exchange, having
opened a plant last year to handle cull lemons in that district.
We learn from the Journal of Commerce that the develop-
ment of the quicksilver deposits and the sulfur beds of the upper
border region of Texas has been greatly stimulated by the ex-
isting high prices of these minerals.
It is reported from Washington that the Federal plant at
Summerland, Cal., started as an experiment to demonstrate
the possibility of salvaging potash from giant kelp on a commer-
cial scale, has already proved a success. Dr. F. W. Brown, in
charge of the office of fertilizer investigations, who is father of
the project, has returned from an inspection trip much pleased
with the way the plant is working. As a result of the success
attained in California, an effort will be made to establish a sim-
ilar industry on the Atlantic coast. Mr. Brown expects to
start preliminary work soon on the Florida coast, where the con-
ditions are nearly the same as on the California coast.
A statement by the Bureau of Foreign and Domestic Com-
merce says the United States is now producing enough aniline
dyes to meet all domestic demand and leave a surplus for ex-
port.
Announcement has been made of the formation of the Dixie
Gas Company at Anniston, Alabama, under the laws of Dela-
ware, with a capital stock of $2,500,000. This company will
develop the oil and gas possibilities of Alabama on a huge scale.
The International Coal Products Corporation of Trenton
has been incorporated under the laws of New Jersey with a
capital of $11,000,000, by G. W. Bacon, C. L. Blair and J. B.
Dennis, of New York.
It is reported from Germany that Prof. Thorns, of Berlin, has
been making extensive experiments in poppy cultivation. It is
stated that he has succeeded in obtaining from poppies opium
containing no less than 22 per cent of morphine, and greatly
superior to the Turkish and Bulgarian opium in morphine
content.
Merck & Company have increased their capital from $250,-
000 to $1,000,000.
A company has been formed in Japan for the manufacture
of fish grease used in the manufacture of soap and glycerin.
The U. S. Potash Products Company, capital $5,500,000,
has filed a charter under the laws of Delaware. The company
is organized to produce and market potash and alum. The
incorporators are Dormann T. Connet, White Plains, N. Y.,
John F. Roach and Clarence K. Holm, of New York City.
Amalgamated Dycstuff and Chemical Works of Manhattan
has increased its capital from $50,000 to $500,000.
We learn from the Textile World Journal thai the paper in-
dustry has found a new use for sulfonated castor or Turkey-
red oil. This commodity is extensively used in cotton finishing
and dyeing. It has been found in a practical application that
a small quantity of an alcoholic solution oi this oil prevents
the formation of foam in the beat
A method of determining inauila fiber in rope and 1
covered in the research department of Axthui D Little,
[nc, Cambridge, Mass. The method has been adopted bj the
United States liureau of Standards. Briefly, it consists of free-
,n ■ 1 j 0 n.|H from oil, soaking it for twent) seconds in a solution
of bleaching powder acidulated with acetic acid, rinsing in
water, then to alcohol, and finally exposing it for a minute to
the funics of ammonia, Manila fibei turns russet-brown while
all other rope fibers turn cherry n d
164
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No.
The Mallinckrodt Chemical Works of St. Louis on December
19 celebrated the fiftieth anniversary of the founding of its
business by giving a banquet at the Mercantile Club, St. Louis.
About one hundred and fifty guests were present, including the
representatives of the various branches. An important feature
of the evening was the presentation to Edward Mallinckrodt,
Sr., president of the company, by the employees, of a beautiful
bronze tablet or medallion prepared from one of his recent
photographs.
An explosives manufacturing plant to require an investment
of $60,000,000 will be built by the Government at Hadley's
Bend, on the Cumberland River, near Nashville, Tennessee.
From 4000 to 5000 acres of land will be utilized for the site and
the buildings will cover about 2000 acres. It is planned to begin
explosives manufacturing within ten mouths. This factory is
one of the several big explosives manufacturing plants which
the Government has decided to build in connection with its
$90,000,000 expenditure for this purpose.
Secretary Lane has recommended to Congress an appropria-
tion of Si 00,000 to investigate the commercial and economic
practicability of utilizing lignite coal for producing fuel oil,
gasoline substitutes, ammonia, coal tar and gas for power.
There are immense quantities of lignite deposits in public land
but the coal is of such character that it does not stand trans-
portation in its natural state and is of small value for fuel ex-
cept in the immediate vicinity of the mines.
The Carbo-Hydrogen Company of America, with offices at
Pittsburgh, has increased its capital from §3,500,000 to $5,000,-
000.
Castor oil used in dyehouse preparations and for lubricating
airplane engines has become so scarce that the Government, in
view of the latter requirement, is arranging for the planting of
100,000 acres, 40,000 of which lie in Florida, with the India castor
bean. Contracts will be made with farmers in suitable sections
who will plant not less than 1000 acres, the Government under-
taking to purchase the beans at a fixed price.
The United Chemical Company, Wilmington, Del., has been
incorporated to manufacture chemicals and allied products. The
capital is $3,000,000. Incorporators: M. M. Clancy, C. L. Rim-
linger and C. M. Egner, Wilmington.
According to estimates of the U. S. Geological Survey, Depart-
ment of the Interior, the production of magnesite in California
in 1 91 7 exceeded that of all former years, being estimated at
2 15,000 tons. This quantity and the magnesite produced in the
recently discovered field in Stevens County, Washington, esti-
mated at close to 100,000 tons, makes an output of 315,000 tons
in 1917, or 15,000 tons more than the normal domestic
demand.
Regarding the explosion at the extensive Griesheim-Electron
chemical works in Germany recently, "Lloyd*s List," in an
article on the explosion, attributed to an authoritative source,
says:
"It will be remembered that on November 22 it was reported
that the large chemical factory of Griesheim-Electron, near
Frankfort, had been destroyed as the result of an explosion. No
details were obtainable at that time, and no great attention was
paid to the report in this country, no doubt from desire to avoid
exaggeration of what might after all prove to have been an affair
of no great importance.
"But the extreme care taken to prevent fuller accounts from
leaking out from Germany and the enforced silence of the Ger-
man press on the subject are the best proof of the German
Government's anxiety to conceal a very serious loss. The first
telegram which managed to escape from Frankfort made a
significant admission, which the subsequent silence only con-
firms. It announced that the excitement in Frankfort caused
by the explosion was tremendous. Information which has since
been obtained from perfectly trustworthy sources makes it
clear that there was good reason for excitement. For it is now
certain that the explosion caused the complete destruction of
one of tlu greatest munition factories in the world, by which
Germany has suffered a disaster comparable to a very serious
military defeat in its effect on the issue of the war.
"Under these circumstances it is a matter of supreme interest
to understand precisely to what extent German military equip-
ment was dependent on the source of supply which was wiped
out of existence a few weeks ago.
"The Griesheim factory was situated in the neighborhood of
Frankfort with an extensive frontage on the river Main. It
consisted of an enormous group of buildings covering an area of
over 54 acres. Twenty-eight large chimneys, one of them over
200 feet high, gave the impression more of an industrial town
than a single factory; and numerous piers abutting on the river,
combined with an extensive railway system, enabled this huge
concern to distribute its products among the world's markets
economically and quickly. Before the war it ranked as fourth
in importance of the great German chemical works, and was
always a flourishing company, paving a pre-war dividend of
14 per cent, and worth, as a going concern, well over 60,000,000
marks.
"Its commanding position in the chemical world rested not
only on its huge output, but on the extensive variety of its
manufactures. These comprised, among other things, aniline
dyes of every description, nitric, sulfuric and other acids, phos-
phorus, and alkali, with liquid chlorine, hydrogen and oxygen
as important by-products. What it meant to Germany as a
source of munitions of war can thus be readily understood.
Moreover, as one of the uncommon instances among German
chemical works possessing installations for electrochemical
production, it was of prime importance as a source of synthetic
nitrates ; and its splendidly organized research laboratory enabled
it to play a leading part in the production of poison gas, and the
other more refined forms of ftightfulness which Germany has
introduced in the course of the war. That the Imperial Govern-
ment has taken the fullest advantage of these facilities is shown
by the rapid increase of the works both in extent and output
since the beginning of the war, and by the fact that the company
has recently decided to increase its share capital by 50 per cent,
an increase in which the German Government is more than
suspected of having a financial interest.
"With regard to the productive capacity of Griesheim some
authoritative facts are available which cast an interesting light
on the war activities of this concern. It has been producing
saltpeter for the manufacture of black powders at the rate of
1,000 tons a day, and it is reputed to be the only factory' turning
out this article. To such an extent has its already impressive
output of soda nitrate and concentrated sulfuric acid been de-
veloped that it supplied the whole demand of five nitroglycerine
and dynamite factories, as well as two powder works, including
that of Rottweil, one of the most important in Germany.
Another explosive, which it manufactured in large quantities,
was tonite, through its facilities for making synthetic phenol
and consequently picric acid, from which acid this explosive is
derived.
"Another circumstance of special interest to us is the fact
that this factory supplied large quantities of electrolytic hy-
drogen for the inflation of Zeppelins, and possessed by way of a
reserve three gasometers with a total capacity of over 300,000
cubic feet. So important was it in this respect that a Zeppelin
shed, usually containing two or three airships, was erected in
close proximity to the works For the kite balloons at the
front the gas was supplied in steel tubes in the liquefied state.
Moreover, the extensive electrolytic plant was further utilized
to produce asphyxiating gas and lachrymatory and poisonous
shells. Indeed it was the greatest center of this manufacture in
Germany, and in 1916 the output of poison gases reached the
colossal figure of nearly 600,000 cu ft. a day.
"The extent of the material loss which Germany has suffered
by the destruction of the Griesheim factory can thus be easily
comprehended. But the disaster is of still wider significance.
The variety of the materials formerly produced means, in such a
closely interlocking industry .1- chemical manufacture, that
every concern in Germany is affected, both from the cutting off
of supplies which many of them formerly drew from Griesheim
and from the necessity of making the loss of these supplies good
from plants already working to their maximum. The deaths
of scores of trained workmen and specialists in the factory itself,
and in the dwellings within its confines, will make the task of
coping with this deficit all the more difficult.
"Even if the material lo>^ can be successfully replaced, the
problem of collecting miscellaneous quantities of explosives and
acids from various quarters and conveying them over the greater
distances thus made necessary is bound to complicate further the
transport difficulty, already regarded as exceedingly pressing in
Germany. It is impossible that the works can be reconstituted
during the war, and sooner or later Germany must show on her
fighting fronts the effects of this staggering blow which she has
suffered within her own territory."
Feb., 191S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
165
GOVERNMENT PUBLICATIONS
By R. S. McBride, Bureau of Standards, Washington
NOTICE — Publications for which price is indicated can be
purchased from the Superintendent of Documents, Government
Printing Office, Washington, D. C. Other publications can
usually be supplied from the Bureau or Department from which
they originate. Commerce Reports are received by all large
libraries and may be consulted there, or single numbers can be
secured by application to the Bureau of Foreign and Domestic
Commerce, Department of Commerce, Washington. The regu-
lar subscription rate for these Commerce Reports mailed daily is
$2.50 per year, payable in advance, to the Superintendent of
Documents.
GEOLOGICAL SURVEY
Gypsum in 1916. R. W. Stone. Separate from Mineral
Resources of the United States, 1916, Part II. 7 pp. Published
October 30. In 1916 for the first time the total value of the
gypsum products of the United States in a single year exceeded
$7,000,000. Since 191 2, inclusive, the annual output has been
approximately 2,500,000 tons of raw material, but in 1916 the
total production was over 2,750,000 short tons.
As might be expected from the general tendency of the times,
the average price per ton for gypsum and most gypsum products
shows a large increase over the price in 1915. The increase is
least for crude gypsum sold to Portland cement mills and greatest
for dental plaster. Dental plaster is reported as produced in
six states and at prices ranging from $6 to $23.50 per ton, with
an average price of $13.26 per ton. In former years it has ranged
from $3 to $15, with an average price of about $5. This greatly
increased average price in 1916 is due to the fact that the_ higher-
priced material largely predominated in the output.
The increased average price per ton of all calcined plaster
in 1916, due to higher wages and cost of all supplies, will doubtless
be greatly exceeded in 1917.
Gypsum imported into the United States comes almost wholly
from Nova Scotia and New Brunswick and enters the ports of
the New England and North Atlantic States. The proportionate
value of imports to domestic production is very small and de-
creasing. It was about one-seventeenth in 1915 and one-twenty-
second in 1916.
Peat in 1916. J. S. Turp. Separate from Mineral Resources
of the United States, 1916, Part II. 2 pp. Published November
19-
Peat was used in the United States in 1916 mainly for fer-
tilizer, soil builder and as stock food. Small quantities
were used for peat litter and fuel, and, as was predicted in the
report for 1915, very little peat fuel was produced in this country
in 1916.
During 1916, as in 1915, no new processes or machinery for
preparing peat were reported to have been commercially tried
in the United States, but several firms reported additions and
improvements to their plants. The total number of firms re-
porting production in 1916 was 13, all but one of which sold
peat for fertilizer. Two also sold peat for stock food. One
sold a small quantity for fuel. The 9 firms that furnished
data for 19 15 furnished data also for 1916, and 4 firms reported
that were not represented in 1915.
Peat Produced, Imported and Consumed in the Unite
Production Imports
1 ■•-.-:
Fertilizer and fcr
tilirer filler. . .
Miscellaneous.. .
Peat moss litter.
Quantity
Short
Tons
48,106
4,300
100
52,506
Value
$336,004
32,250
850
Quantity
Short
Tons
3.042
(369,104
3,042
States in 1916
Consumption
Quantity
Short
Value Tons Value
48,106 $336,004
4,300 32,250
100 850
$27,859 3,042 27,859
$27,859 55,548 $396,963
Hydraulic Conversion Tables and Convenient Equivalents.
Anonymous. Water Supply Paper 426- C, from Contributions
to the Hydrology of the United States, 1917. 24 pp. Published
October 31.
The Alaskan Mining Industry in 1916. A. H. Brooks.
Bulletin 662-^4, from Mineral Resources of Alaska, 1916-A.
62 pp. "This volume is the thirteenth of a series of annual
bulletins treating of the mining industry of Alaska and summar-
izing the results achieved during the year in the investigation
of the mineral resources of the Territory. In preparing these
reports the aim is prompt publication of the most important
economic results of the year.
"This volume, like those previously issued, contains both
preliminary statements on investigations made during the year
and summaries of the conditions of the mining industry, including
statistics of mineral production. It is intended that this series
of reports shall serve as convenient reference works on the mining
industry for the years which they cover."
Mining in the Lower Copper River Basin and the Prince
William Sound Region, Alaska. F. H. Moffit and B. L. John-
son. Bulletin 662- C, from Mineral Resources of Alaska,
1916-C. 66 pp.
Manganiferous Iron Ores. E. C. Harder. Bulletin 666-EE.
13 pp. The dependence of the United States on imported high-
grade manganese ore and ferromanganese is well known to steel
makers and other users of manganese. Normally the high-
grade manganese ore produced in this country constitutes less
than 2 per cent of the total amount of manganese ore consumed,
not including the ore represented by the manganese imported
in the form of the alloys — ferromanganese and spiegeleisen.
During 1916 the domestic production was about three times
that of 1915, largely on account of the high prices paid for ore.
The exploration for new deposits has also been stimulated, and
many discoveries of manganese ore are being reported. Even
with this outlook for increased production, however, it is not un-
duly pessimistic to say that the deposits of high-grade man-
ganese ore in the United States will probably never be able to
supply the manganese consumed in domestic industries. If,
therefore, the importation of high-grade manganese ore were
discontinued, numerous industries would be vitally affected.
Of these the steel industry consumes by far the largest quantity
of manganese.
There are in the United States large quantities of manganiferous
ores containing varying amounts of manganese. A very small
proportion of these can be used in the production of high-grade
iron-manganese alloys, but a large proportion can be used for
lower-grade alloys, and nearly all can be used in making high-
manganese pig iron. Compared with the manganiferous ores,
the reserves of high-grade manganese ores in this country arc-
insignificant. Hence, although a search for manganese ore is
desirable, a more promising solution of the manganese problem
would seem to lie in the direction of the utilization of low-grade
manganiferous ores. Up to the presenl time the use of these
ores has been very slight. Until a few years ago they were con-
sidered to have little value and were mined only Lncidentallj
In the West manganiferous ores would not be mined were it not
for their association with ores of other metals.
There are several ways in which the utilization of manganifer-
ous ores may be brought about: (1) It has been suggested thai
by nut hods of concentration resulting in the elimination of
iron, silica, or other constituents a product high in manganese
, 11,,. hi be derived from them, Such concentration has been at-
tempted locally but with very little success, owing mainlj to
i66
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol 10, No. a
the intimate mixture which manganese generally forms v.'ith
associated materials; (2) The steel-making practice mi^ht be
changed so that more spiegeleisen and less ferromanganese
would be used for deoxidizing. By the addition of small quan-
tities of high-grade manganese ore mucn of the manganiferous
iron ore could be used in the manufacture of spiegeleisen; (3)
The most effective solution, however, as has previously been
suggested, seems to be to so change the practice in the manu-
facture of basic open-hearth steel as to make possible the use of
high-manganese pig iron. Experimentation along this line is
extremely desirable. The successful application of such a change
would make large reserves of manganiferous iron ore commer-
cially available and would greatly decrease the quantity of high-
grade manganese ore consumed.
BUREAU OF FISHERIES
The Menhaden Industry of the Atlantic Coast. R. L. Greer.
Document 811, 30 pp. Issued October 18. Paper, 10 cents.
"Descriptions of methods of conducting the fishery, vessels,
factories, apparatus, and methods employed in converting the
fish into oil and scrap, and includes statistics of the fishery for
1912 and selected bibliography of papers relating to the subject."
BUREAU OF STANDARDS
The Latent Heat of Pressure Variation of Liquid Ammonia.
N. S. Osborne and M. S. Van Dusen. Scientific Paper 314,
6 pp. Issued November 16. Paper, 5 cents.
COMMERCE REPORTS—DECEMBER, 1917
Lubricating oil is being made from the liquid rosin obtained
in sulfite paper pulp factories in Sweden. (P. 849.)
Efforts are being made to develop salt beds in Holland, to
replace salt hitherto imported. Salt brine and solid salt have
been encountered in exploration work. (P. 853.)
Copper pyrites mines in Norway, formerly German owned,
have been purchased by Swedish firms. (P. 871.)
A new type of hard porcelain has been developed at Stoke-on-
Trent (England). It is made entirely of British materials, is
cheaper than ordinary earthenware, and the glaze (which is
leadless) is very satisfactory, and can be readily decorated.
The ware can be fired in either oxidizing or reducing atmospheres,
preferably the latter. (P. 872.)
American exports of aniline dyes are constantly increasing,
being now equivalent to about $4,700,000 annually, **. e., about
twice the domestic production in 1914. A similar increase has
occurred in the exports of vegetable colors. (P. 903.)
Efforts are being made to produce paper in Australia from
native grasses. Newsprint paper is now very scarce, and costs
four times the pre-war price. (P. 918.)
The tin plate situation in the United States is improving, as
shown by increased imports of pig tin and palm oil (used in
tinning), and by decreased exports of tin plate and terneplate.
(P- 947.)
It is proposed to subsidize for three years any organization
that will establish a paper factory in the Philippines. (P. 965.)
Exports of manganese ore from Brazil to the United States
are five times those of 1913, and could be still more increased if
the rich regions could be made more accessible. (Pp. 971 and
1155)
The Japanese steel industry shows an increase of over 50
per cent above last year's production. (P. 975.)
To provide steel for shipbuilding and oilier industries, a large
modern steel plant is to be erected in Holland at the entrance
to the North Sea Canal; and will use imported iron ores. (P.
978.)
The conditions and methods in use in the Scottish shale oil
industry arc described in some detail. The principal products
are naphtha, burning oil, gas oil (used as fuel and for enriching
gas), lubricating oils, paraffin, coke, gas (illuminating), and
sulfate of ammonia. (Pp. 990-1.)
The British Government has assumed control of all vegetable
oils and oil seeds, and hydrogenated oils (P. 993.)
Imports of chemicals into Great Britain in October showed a
slight increase, while exports showed a marked decrease. (P.
1031.)
The iron ore and steel industry' of the Biscayan Provinces of
Spain is described in some detail. (P. 1128.)
Proposed substitutes for gasoline as motor fuel in England
include denatured alcohol, coal gas and kerosene. The first is
not possible with the present demand for alcohol, though efforts
are being made to increase the cultivation of potatoes to be used
for industrial alcohol. The use of coal gas, especially in busses,
etc., is increasing. Containers are usually made of fabric made
gas-tight by various coatings. Kerosene is not extensively
used, as it requires special fittings, etc., and involves the use of
gasoline for starting. (Pp. 1132-5.)
Experiments were performed in India upon three new paper-
making materials- E. monoslachya leaves from Western
Australia, wood of the N. macrocalyx from East Africa, and bark
of brachyotegia from Rhodesia, all with encouraging results. (Pp.
1203-5.)
Efforts are being made to increase the output of asbestos
from Russia, in view of increased demands, especially from
Japan. (P. 1139.)
Most of the mineral products of India show an increased
output, the most important being coal, gold, manganese ore,
petroleum, salt, saltpeter, tungsten ore, lead ore, mica, silver,
tin ore, iron ore, and monazite. (P. 11 75.)
To meet increased demands for aluminum, especially in the
aircraft industry, large extensions of the plants in Scotland are
planned. (P. 1191.)
Further exploration of the manganese mines in Mysore,
India, has shown that the richness of the ore increases with the
depth. Manufacture of ferromanganese in India is being con-
sidered. (P. 1 192.'
Experiments are being conducted in the West Indies upon
the concentration of lime juice by freezing, to reduce the cost of
transportation. (P. 1219.)
Soya bean oil is obtained in Manchuria principally by the
"expression" process, only one plant using the benzene ex-
traction process. The oil by the latter process is inferior. (P.
1227.)
A firm in Scotland, experienced in the manufacture of gauge
glasses, has extended its plant and force to include chemical
glassware of high quality, including apparatus for HNOj con-
densation, miners' safety lamp globes, and special glass for air-
planes and marine mines. Prohibition of imports of chemical
and scientific glassware for seven years is urged as a necessary
step for the establishment of a permanent industry in Great
Britain.
Special Supplements Issued in December
Spaln —
1 5d
Straits Settlements
Ireland — 19*
56a
China
52J
and g Morocco —
75a
:
Statistics
Of
Exports to thb
Unitei
i States
Hongkong — 925
Sincapors — Sup.
56o
Jamaica —
1127
Antimony
Cassia
Annatto
Chemicals
Cubebs
Hides
lli.lLS
Cutch
Kola nuts
Leather
Peanut oil
Aniseed oil
s blood
Gambler
Gamboge
Gum
Logwood e
Sugar
Fustic
xtraet
Logwood
Paper
Sugar
Gum benjamin
Tin
Gum copal
London —
1137
Pakien, China — Sud.
Gum dain.tr
Rubber
Gutta joolatong
Tin
Albumen
Gutta pi l
Hides
Indigo
Bean ml
Gutta siak
Bean cake
Hides
Linseed
Mangrove i-.irk
Canary
Islands —
Tsinc.t.u-
-Sup. 52«
Cocoanut oil
Sup. 15c
1
Hides
Paraffin
Cochineal
Peanuts
Rubber
Copper matte
Peanut oil
Tin
Pumice
Feb., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
167
BOOK REVIEWS
Chemical Patents and Allied Patent Problems. By Edward
Thomas. John Byrne & Co., Washington, D. C. Price,
$2.50.
Patent law is a wilderness of decisions, a jungle of entangled
and interlacing precedents which, like most jungle vegetation,
can be found running almost any old way. However, still
pursuing the analogy, most of the main lianas pursue something
the same general direction with only occasional divagations.
Our usual legal custom, from which we have not departed in
patent matters, is to enact statutes in a few brief paragraphs;
and then leave it to the courts to find out what those para-
graphs mean as applied to any individual case. And in the
patent field, our judges have been reasoning from parallel case
to parallel case for something over a century now, with awe-
inspiring results considered volumetrically.
Every chemist is interested in patents at one time or another,
whether it be because he wants one or is afraid of one or for both
reasons together. Chiefly, he wants to know the law governing
compositions and processes; and for his purpose the ordinary text
books on patent law are more irritating than instructive. Nat-
urally, such books seek to cover the whole field and do not
specialize in these matters; the more so since in the United States
invention and litigation have been much more concerned with
matters of mechanics than with matters of chemistry.
Mr. Thomas' book is a specialization; it is, practically, con-
fined to the law of process and composition. It is hardly a
treatise on patent law; it is more what Mr. Thomas terms a
"finding list" of the decisions relating to chemical things. In a
way it is an attempt to do for chemical patent law what Beilstein
or Richter did for organic chemistry, viz., classify the literature
with just enough running text to give the classification. The
difference, and the difficulty, arise in that while Be.ilstein's
running text can give facts and avoid theory or controversial
matter, Mr. Thomas, in the nature of things, can only give
opinions. And opinions do not lend themselves to verbal
condensation as do boiling points and reactions. Any law suit
represents a difference in opinion which generally spreads itself
over many pages of testimony and argument with the court's
opinion coming as a lengthy equilibration of the difference.
This equilibration cannot well be compressed into a paragraph
or a sentence; in most instances, anyhow.
As a finding list, Mr. Thomas' book is extremely good. The
running text, considered purely as a classification, is also good.
It is so short and compressed that little difficulty is found in
glancing over it to catch a key word.
But because it is short and compressed, the running text is
open to more objection if it is to be considered a "statement of
the patent law." It says too positively that which is often-
times a matter of opinion. This is something Mr. Thomas could
not altogether avoid in a summary. To state the upshot of
any decision in a single sentence, a world of qualifications and
limitations must be omitted unless that sentence is to be, as
Mark Twain said of Germanic wording, "long enough to have
perspective." Nevertheless, Mr. Thomas might perhaps,
with advantage, have hedged a little in some of his statements,
The law is proverbially a thing of glorious uncertainty; and where
its conclusions are stated too categorically, the casual reader is
apt to receive fixed impressions which may afterwards have to
be unfixed. Or, Mr Thomas might have inserted a brief warn-
ing that in general the dicta given are merely his opinion of
what the courts' opinions were; and that wherever the matter
is of importance the original decision should be consulted.
Sometimes, Mr Thomas uses language which is a little con-
fusing It is not meant in the discussion in page 31, for example,
that the courts and Patent Office are coming to the view that a
thing demonstrably old can be re-patented merely because it
is made by a new process; but that there are some things, like a
fried egg, which can best be defined by a recital of the process
of making. See also the reference to "fusible tubes of water"
(page 6). And the collocation of sentences in the running text
is often just a little bewildering; like the dictionary, the text
changes the subject a bit too abruptly sometimes. For instance,
in pages 24 and 25, one sentence is talking about new matter in
re-issues while the next is devoted to infringement of an adrenalin
patent.
But of course it is easier to criticize than to do things; and the
fact is that Mr. Thomas has produced a very useful book; and
one which represents a vast amount of labor. It fills, and fills
well, a vacant place on the reference book shelf.
K. P McElroy
Explosives. By Arthur Marshall. Second Edition, Vol.
II, Properties and Tests. 8vo, 386 pp. and 80 illustrations.
P. Blakiston's Son & Co., Philadelphia, 1917. Price, $8.00 net.
The author's work, as evidenced in this second volume, is
of the same high character as set forth in the review of Vol. I.1
The extent of the revision is to a degree shown by the fact that
Part IX, devoted to "Properties of Explosives," has been en-
larged by twenty pages; PartX, "Special Explosives," by thirty-
eight pages; Part XI, "Stability, etc.," by eleven pages; and
Part XII, "Materials and Their Analysis," by twenty-two pages.
Besides the enlargement of each of the former chapters there
have been added one, of seventeen pages, on "Naval and Military
Explosives" and another of twelve pages, on "Commeicial
High Explosives," while to the "Thermo-Chemieal Tables" in
Appendix II have been added tables of heats of formation of
"Fulminates and Azides" and of "Aliphatic Nitrates and Nitro-
compounds." Novelties are found in the change of the legend
for Chapter 35 from "Safety Explosives" to "Coal-Mine Ex-
plosives" which latter is a much more accurate title, and in Part
XII, by placing in full-face type at the bottom of each page,
in addition to the marginal legends, the name of the substance
described and for which the methods of analysis are given on
that page. This section of the book will be much used and this
addition will undoubtedly prove very convenient and helpful.
The same degree of sensible frankness in treatment of devices
and materials now used for war purposes is noticeable in this
as in the first volume, and particularly in the chapter on "Naval
and Military Explosives" introduced into this edition. As
this information is without question already in the hands of the
enemy it would be foolish to withhold it from friends who might
be able to render useful service if supplied with the information.
In the first edition the author gave the composition of the chlorate
priming used by the U. S. in its small-arms ammunition. In
this edition he says of potassium chlorate: "If made by the
electrolytic method it always contains at least 0.05 per cent of
potassium bromate, and may contain as much as 0.6 per cent.
That manufactured by the old process does not contain this
impurity. As bromate may have a deleterious effect on the
stability of explosives made with it, especially if the explosive
also contains sulfur, an official order has been passed in Germany
that chlorate for the manufacture of blasting explosives must
not contain more than 0.15 per cent of bromate, for fireworks
not more than 0.10 per cent, and for cap composition none at
all," and he gives methods for the detection and determination
of the bromate.
As a rule, the author has covered each topic with full'
has cited the original authority with accuracy. A notable
1 This Journal. 9 (1917). 822.
168
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 2
exception, which therefore attracts attention, is that of the per-
foration of plates by hollow cartridges of detonating explosives
which is referred to Neumann under dates of 191 1 and 1914,
though these cartridges were devised in this country, the method
applied, and the results published so long ago as 1888 and
repeatedly later. Also it is noted that the Bureau of Mines'
Sand Test for detonators is attributed to Storm and Cope, though
these authors, in Technical Paper No. 125 cited by Marshall,
state that it had been devised by W. O. Snelling. These are,
however, but minor defects in a very valuable work.
Unfortunately, the printers' work is more open to criticism
and this is the more to be regretted as the author was so far dis-
tant from his publisher. Two flagrant errors are the numbering
of chapter thirty-six in full-faced Roman as Chapter XXX, and
the omission of a legend from the newly added table for the heats
of formation of the fulminates and azides. In addition dropped
letters, imperfect impressions, and uncouth formulas, due to
wrong case type or signs, are not uncommon.
Charles E. Munroe
Tube Milling. A treatise on the practical application of the
tube mill to metallurgical problems. By Algernon Del
Mar. x + 159 pp. Illustrated. McGraw-Hill Book Co.,
New York, 1917. Price, $2.00 net.
This book is of what may be called the standard dimensions
of page, the binding is good and the paper, type and illustrations
excellent. The latter are numerous and are in general clear and
well selected for their purposes.
The object of the work is shown in the statement in the
author's preface that "it is important that the principles in-
volved in their [tube mills] operation should be made common
property. It is for this purpose that the author has compiled
the present volume, hoping that it will meet the requirements
of the engineer and millman."
Chapter I is headed "General Description," and in addition
treats fully, more or less, what are called the essential factors
governing capacity, together with feeding devices, power re-
quirements, costs and foundations. Chapter II is entitled
"Amalgamating with the Tube Mill," Chapter III "Grinding
Ores with the Tube Mill for Flotation," Chapter IV "Crushing
Efficiencies," and Chapter V "The Use of Wrought Iron and
Alloy Steel."
There is also an appendix of six pages giving some useful
data, tables and notes on slime density relations, and some
information on assay methods, etc., for a cyanide mill laboratory.
There are a few evident typographical errors, among which
are the following:
Page 13. "0.5316 tons of dry feed" should be "0.5297 tons of dry
feed."
Page 32. "Guanajuanto" for "Guanajuato."
Page 51. In the formula m - ^"JTrff "*" should be "s"
Page 120. "Fig. 50" should be "Fig. 64."
Page 147. "Excising" should be "existing."
Criticism might be made as to some of the details of arrange-
ment. For example, on pages 104 and 105 the figures given as
"Cement Data" might have been more properly placed in the
appendix. Also in the chapter headed "Crushing Efficiencies"
there is a page and a half only on this subject, while the remainder of
the chapter, six pages, treats of screen gauges, screen openings, etc.
In the reviewer's opinion the notes on "Cyanide Chemistry"
in the appendix should either have been made very much fuller
or else omitted altogether and replaced by references to the
several complete treatises on the subject. These notes are con-
densed to such a degree that it would be very difficult for anyone
not a chemist familiar with cyanide laboratory practice to use
them to advantage.
These are all minor criticisms, of course. The main objection
to the author's treatment of the subject is his insufficiently
full and adequate handling of important divisions, with a result-
ing lack of balance. As referred to above, barely two pages are
given to the very important subject of crushing efficiencies,
although references are given to the literature. Over thirteen
pages are given to a discussion of the use of wrought iron and
alloy steels, with tables and diagrams. This chapter is not to
be objected to in itself, but, in comparison, the three pages of
text devoted to grinding ores with the tube mill for flotation are
certainly very meagre. A considerable volume of very valuable
data on this subject has either been published or could be secured
easily.
For a treatise the complete collection and arrangement of
important published information and data is always a very
valuable feature. The danger usually is that very often this
results in what is practically a compilation only. The author
is to be congratulated in that tne proportion of pure compila-
tion in the present volume is so decidedly less than the average
that the book is not open to this objection, nevertheless this
proportion could have been considerably increased to advantage
in some of the chapters.
G. D. VanArsdale
Everyman's Chemistry. By Ell wood Hendrick. Harper &
Bros., Philadelphia. Price, S2.00.
During the past few years the public has come to realize,
in a vague way, the tremendous importance of chemistry in its
application to daily life. Xo book, however, that the average
reader could comprehend has been written on this subject, and
it is gratifying indeed to welcome such a volume.
In his book Mr. Hendrick discusses the great problems of
the day in an interesting, instructive, and lucid manner, setting
forth the general principles underlying the subject of chemistry
in a language which is simple, direct and intelligible to all.
The delightful manner in which the subject is presented makes
the reader feel almost a personal contact with the author The
keen wit and sense of humor displayed throughout the text
relieves the monotony of dry scientific facts. Thus like a
sugar-coated pill one swallows the information without noticing
the bitter taste. Allen Rogers
Lubricating Engineer's Handbook. A reference book of data,
tables and general information for the use of lubricating en-
gineers, oil salesmen, operating engineers mill and power
plant superintendents and machinery designers, etc. By
John Rome Battle, B.S. in Mechanical Engineering.
8vo. Pp. 333. J. B. Lippincott Co., Philadelphia and Lon-
don, 1916. Second Impression. Price, $4,00.
After a careful perusal of the book, the reviewer has failed to
find any phase of the oil business that has not been discussed:
history, manufacture, tests, the varied uses, storage, oil house
methods, specifications, etc.. etc.
Two statements made are very interesting, one that the oil
supply of this country is about one-third used up (in about
fifty years), and, second, that the annual friction loss in the
United States is nearly 200 million dollars. If the book helps
to bring about a diminution of this, it will have served a useful
purpose. This statement is made on p. 69, "The so-called
gumming test for lubricating oils is of little practical value *
* * * * and the same may be said of evaporation tests."
On the other hand (p. 138), the statement is found, that "a
lubricating oil for forced feed in a steam turbine should have
a low gumming test." Speaking from an experience of more
than thirty years, the reviewer has found both tests of great
value: the first is an admirable sorting test, particularly for auto-
mobile oils, and the second is of cardinal importance to the in-
surance companies, having to do with textile mills.
The book was very much needed, and is eminently satisfac-
tory, in fact, about as nearly perfect as is humanly possible to
produce — but this might have been expected from the engineer
of the Atlantic Refining Company, "the largest manufacturers
of lubricants in the world." A. H. Gill
Feb., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
169
NLW PUBLICATIONS
By Irene DeMatty, Librarian. Mellon Institute of Industrial Re
eh, Pittsburgh
Antiseptics: A Handbook on Antiseptics. H. D. Dakin and E. K. Dun-
ham. 129 pp. Price, $1.25. The Macmillan Co., New York.
Biochemical Catalysts in Life and Industry. Jban Effront. 8vo. 752
pp. Price, $5.00. John Wiley & Sons, New York.
Chemistry: A Course of Instruction in the General Principles of Chemistry.
A. A. Noyes and M. S. Sherrill. 8vo. Price, $2.25. T. Todd Co.,
Boston.
ChemistTy: An Elementary Study of Chemistry. W. McPherson and
W. E. Henderson. 12mo. 576 pp. Price, $1.60. John Wiley &
Sons, New York.
Colloids: The Chemistry of Colloids. R. Zsigmondy and E. B. Spear.
8vo. 288 pp. Price, $3.00. John Wiley & Sons, New York
flotation: Testing for the Flotation Process. A. W. Fahrbnwald.
16mo. 173 pp. Price, $1.50. John Wiley & Sons, New York.
Foods and Their Adulteration. H. W. Wiley. 3rd Ed. 8vo. 646 pp.
Price, $4.00. P. Blakiston's Son & Co., Philadelohia.
Hydro-Electric Power Stations. E. A. Lof and D. B. Rushmore. 8vo.
822 pp. Price, $6.00. John Wiley & Sons, New York.
Metallurgy: A Practice Book in Elementary Metallurgy. E. E. Thum.
8vo. 313 pp. Price, $2.75. John Wiley & Sons, New York.
Minerals: Practical Instruction in the Search for and the Determination
of the Useful Minerals, Including the Rare Ones. Alex. McLeod.
16mo. 254 pp. Price, $1.75. John Wiley & Sons, New York.
Non-Metals: Elementary Experiments on the Non-Metals. J. S. Lono
and D. S. Chamberlin. 8vo. 78 pp. Price, $1.25. W. S. Rhode
Co., Kutztown, Pa.
Ore Mining Methods. W. R. Crane. Svo. 277 pp. Price, $3.50.
John Wiley & Sons, New York.
Refrigeration: Mechanical Refrigeration. H. Williams. 12mo. 406
pp. Price, $3.00. The Macmillan Co., New York.
Science: Experimental General Science. W. N. Clute. 12mo. 303
pp. Price, $1.00. P. Blakiston's Son & Co., Philadelphia.
Science: A Short History of Science. W. T. Sedgwick and H. W.
Tyler. 8vo. 474 pp. Price, $2.50. The Macmillan Co., New York.
Soil Conditions and Plant Growth. E. J. Russell. 3rd Ed. 8vo. 243
pp. Price, $2.00. Longmans, Green & Co., New York.
Steam Power Plant Engineering. G. F. Gebhardt. 8vo. 347 pp.
Price, $4.00. John Wiley ft Sons, New York.
Sugar: A Handbook for Cane-Sugar Manufacturers and Their Chemists.
G. L. Spencer. 6th Ed. 16mo. 561 pp. Price, $3.50. John Wiley
& Sons, New York.
Technical Periodicals. National Carbon Co. 12mo. 22 pp. Gratis.
National Carbon Co., Cleveland.
Wood: The Preservation of Wood. A. J. Wallis-Taylor. 8vo. 363
pp. Price, 10s. 6d. William Rider & Sons, London.
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The Iron Trade Review, Vol. 61 (1917), No. 25, pp. 1332-1334.
Boiler Plant Management. E Matiieson. Paper, Vol. 21 (1917), No.
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Chemist in the Textile Mill. Textile World Journal, Vol. 53 (1917), No.
26, pp. 21-23.
Coal: General Utilization of Pulverized Coal. H. G. Barnhurst.
Journal nf the Cleveland Engineering Society, Vol. 10 (1917), No. 3, pp.
145-163.
Compressed Air: Using Compressed Air in Forge Shops. C. A. Hirsch-
»"'■■ The American Drop Forger, Vol. 3 (1917), No. 12, pp. 391-397.
Cyaniding a Small Gold-Tailings Dump. A W. Allen. Engineering and
Mining Journal, Vol. 104 (1917), No. 24, pp. 1032-1039.
Displacement-Tanks. W. S. Weeks. Mining and Scientific Press, Vol.
115 (1917), No. 24, pp. 855-856.
Electrical Cleaning of Blast Furnace Gas. H. D. Eobert. The Blast
Furnace and Steel Plant, Vol. 6 (1918), No. 1, pp. 39-43.
Enzymes of Milk and Butter. R. W. Thatcher and A. C. Dahlberg.
Journal of Agricultural Research, Vol. 11 (1917), No. 9, pp. 437-450.
Evaporation: New Method of Increasing the Evaporation in Boilers.
Carl Hering. Power, Vol. 47 (1918), No. 1, pp. 10-13.
Flotation: The Effect of Addition Agents in Flotation. M. H. Thornberry
and H. T. Mann. Metallurgical and Chemical Engineering, Vol. 17
(1917), No. 12, pp. 709-713.
Flotation at Cobalt, Ontario. W. E. Simpson. Mining and Scientific
Press, Vol. 115 (1917), No. 23, pp. 819-824.
Forestry: A Financial Analysis of Forestry and Reforestation. Ell-
wood Wilson. Pulp and Paper Magazine, Vol. 16 (1918), No. 1, pp.
5-7.
Fuel Briquettes: Utilization of City Garbage for Fuel Briquettes and
Other Products. W. B. Phillips. Manufacturers Record, Vol. 73
(1918), No. 1, p. 85.
Furnaces: The Action of Flame in Furnaces. A. D. Williams. The
Iron Trade Review, Vol. 61 (1917), No. 25, pp. 1319-1323.
Fusion: Some Notes on Fusion Apparatus. Frederick Pops. Metal-
lurgical and,ChemicaI Engineering. Vol. 17 (1917), No. 12, pp. 704-709.
Gas Circulation in Regenerator Checkers. A. D. Williams. The Blast
Furnace and Steel Plant, Vol. 6 (1918), No. 1, pp. 29-33.
Gas Explosions at Blast Furnaces. F. H. Willcox. The Iron Trade
Review, Vol. 61 (1917), No. 26, pp. 1377-1380.
Gels: The Formation of Crystals in Gels. H. N. Holmes. Journal of
Physical Chemistry, Vol. 21 (1917), No. 9, pp. 709-733.
Heat Hazards — An Industrial Waste. J. A. Watkins. The Iron Trade
Review, Vol. 61 (1917), No. 26, pp. 1387-1388.
Hydrocyanic-Acid Gas as a Soil Fumigant. E. R. db Ong. Journal of
Agricultural Research, Vol. 11 (1917), No. 9, pp. 421-436.
Hydrosulfite of Soda: Preparing Hydrosulfite of Soda. Textile World
Journal, Vol. 53 (1917), No. 26, pp. 23-25.
Iron and Steel Technology, 1917. R J. Anderson. The Iron Trade
Review, Vol. 62 (1918), No. 2, pp. 156-161.
Microscopic Features in Silver-Deposition. F. N. Guild. Mining and
Scientific Press, Vol. 115 (1917), No. 24, pp. 857-864.
Platinum: Recovery of Platinum in Gold Dredging. J. W. Neill. Min-
ing and Scientific Press, Vol. 115 (1917), No. 23, pp. 825-827.
Potash: The Nebraska Potash Industry. E. E. Thum. Metallurgical
and Chemical Engineering, Vol. 17 (1917). No. 12, pp. 693-698.
Potash in 1916. H S. Gale. The American Fertilizer, Vol. 46 (1918),
No. 1, pp. 37-40.
Pulp Mills: The Chemical Development of Pulp Mills at Berlin, N. H.
Ellwood Hendrick. Pulp and Paper Magazine, Vol. 15 (1918), No.
52, pp. 1209-1213.
Pulpwood: Factors Influencing the Value of Pulpwood. S. D Wells.
f Paper, Vol. 21 (1918). No. 17, pp. 11-15.
Pulpwood Handling and Storage Systems. E. R. Low. Paper, Vol. 21
(1917), No. 15, pp. 11-13.
Redredging— Will It Pay? V H. Gardner. Engineering and Mining
Journal, Vol. 105 (1918), No. I. pp. 1-3.
Soils: Movement of Soluble Salts through Soils. M. M. McCool and
L. C Wheeting. Journal of Agricultural Research, Vol. 11 (1917),
No. 11, pp. 531-547.
Steel Production by the Duplex Process. J. K. Furst. The Blast Furnace
and Steel Plant. Vol. 6 (1918), No. 1, pp. 25-28.
Textile Mill Organization and Costs. Eugene Szbpesi. Textile World
Journal, Vol 53 (1917), No 25, pp. 23 and 48.
Tin Dredging in Portugal. !•* W. Footb and R. S. Ransom, Jr. Engi-
neering and Mining Journal, Vol. 104 (1917). No. 26, pp. 1109-1110.
Ultraviolet Light. Vin. Types of Apparatus Used for Sterilization and
Other Purposes. C. Ellis and A. A. Wblls. The Chemical Engineer,
Vol. 26 (1918), No. 1, pp. 28-34.
Wood: Economical Wood Splitting. H. G. SabckBR. Paper, Vol. 21
(1917), No. 14, pp. 16-17.
17°
MARKET REPORT— JANUARY, 19 IS
WHOLESALE PRICES PREVAILING IN THE NEW YORK MARKET ON JAN. 1 8
INORGANIC CHEMICALS
Acetate of Lime 100 Lbs
Alum, ammonia, lump 100 Lbs.
Aluminum Sulfate, high-grade Lb.
Ammonium Carbonate, domestic Lb.
Ammonium Chloride, white Lb.
Aqua Ammonia. 26°. drums Lb.
Arsenic, white Lb.
Barium Chloride Ton
Barium Nitrate Lb.
Bary tes, prime white, foreign Ton
Bleaching Powder, 35 per cent 100 Lbs.
Blue Vitriol Lb.
Borax, crystals, in bags Lb.
Boric Acid, powdered crystals Lb.
Brimstone, crude, domestic Long Ton
Bromine, technical, bulk Lb.
Calcium Chloride, lump. 70 to 75% fused Ton
Caustic Soda. 76 per cent 100 Lbs.
Chalk, light precipitated Lb.
China Clay, imported Ton
Feldspar Ton
Puller's Earth, foreign, powdered Ton
Puller's Earth, domestic Ton
Glauber's Salt, in bbls 100 Lbs.
Green Vitriol, bulk 100 Lbs.
Hydrochloric Acid, commercial, 20° Lb.
Iodine, resublimed Lb.
Lead Acetate, white crystals Lb .
Lead Nitrate Lb.
Litharge, American Lb
Lithium Carbonate Lb.
Magnesium Carbonate, U. 3. P Lb.
Magnesite. "Calcined" Too
Nitric Acid. 40° Lb.
Nitric Acid . 42 ° Lb.
Phosphoric Acid, 48/50% Lb.
Phosphorus, yellow Lb.
Plaster of Paris Bbl.
Potassium Bichromate, casks Lb.
Potassium Bromide, granular Lb.
Potassium Carbonate, calcined, 80 ffi 85% Lb.
Potassium Chlorate, crystals, spot Lb.
Potassium Cyanide, bulk. 98-99 per cent Lb.
Potassium Hydroxide. 88 @ 92% Lb.
Potassium Iodine, bulk Lb.
Potassium Nitrate Lb.
Potassium Permanganate, bulk Lb.
Quicksilver, flask 75 Lbs.
Red Lead. American, dry Lb.
Salt Cake, glass makers' Ton
Silver Nitrate Ol.
Soapstone, in bags Ton
Soda Ash. 58%, in bags 100 Lbs.
Sodium Acetate Lb.
Sodium Bicarbonate, domestic 100 Lbs.
Sodium Bichromate Lb.
Sodium Chlorate Lb.
Sodium Cyanide Lb.
Sodium Fluoride, commercial Lb.
Sodium Hyposulfite 100 Lbs.
Sodium Nitrate. 95 per cent, spot 100 Lbs.
Sodium Silicate, liquid. 40° Bi 100 Lbs.
Sodium Sulfide . 60%. fused, In bbls Lb.
Sodium Bisulfite, powdered Lb.
Strontium Nitrate Lb.
Sulfur, flowers, sublimed 100 Lbs.
Sulfur, roll 100 Lbs.
Sulfuric Acid, chamber. 66° Bi Ton
Sulfuric Acid, oleum (fuming) Ton
Talc. American white Ton
Terra Alba. American. No. 1 100 Lbs.
Tin Bichloride, 50° Lb.
Tin Oxide Lb.
White Lead, American, dry Lb.
Zinc Carbonate Lb.
Zinc Chloride, commercial Lb
Zinc Oxide. American process XX Lb.
ORGANIC CHEMICALS
Acetanllld. C. P.. in bbls Lb.
Acetic Acid. 56 per cent. In bbls Lb.
Acetic Acid, glacial, 99>/i%. io carboys Lb
Acetone, drums Lb.
Alcohol, denatured. 1 80 proof Gal.
4.00
2'A
9'/l
0
11
40.00
0
45.00
2.50
0
3.00
9
@
9>/»
7'/.
@
8
13 "A
0
15
nomiri
al
75
0
85
30.00
0
32.00
6.00
0
6.25
4>/«
0
5
18.00
@
30.00
8.00
0
15.00
nominal
nominal
9>A @ 10
1.50
18 @ 20
60.00 @ 65.00
7V»
1.70
1.50
1.90
1.70
nominal
83'.. @
35.00 @ 140.00
10 @ 10' i
30.00 @ 35.00
53 @ 56
10.00 @ 12.50
44
2.50
4.50
1.75
47.
6«A
75.00
15.00
3.00
4.60
2.00
80.00
18.00
9'/.
10'/. @ i:
nominal
e
Alcohol, sugar cane, 188 proof Gal.
Alcohol, wood. 95 per cent, refined Gal.
Amyl Acetate Gal.
Aniline Oil. drums extra Lb.
Benzoic Acid, ex toluol - Lb.
Benzol. Pure GaL
Camphor, refined in bulk, bbls Lb.
Carbolic Acid, U. S. P.. crystals, drums Lb.
Carbon Bisulfide Lb.
Carbon Tetrachloride, drums. 100 gals Lb.
Chloroform Lb.
Citric Acid, domestic, crystals Lb.
Creosote, beechwood Lb.
Cresol. U. S. P Lb.
Dextrine, corn (carloads, bags) Lb.
Dextrine, imported potato Lb.
Ether. U. S. P. 1900 Lb.
Formaldehyde. 40 per cent Lb.
Glycerine, dynamite, drums included Lb.
Oxalic Aud in casks Lb.
Pyrogallic Acid, resublimed. bulk Lb.
Salicylic Acid, U. S. P Lb.
Starch, cassava Lb.
Starch, corn (carloads, bags) pearl 100 Lbs.
Starch, potato, Japanese Lb.
Starch , rice Lb.
Starch : sago flour Lb.
Starch, wheat Lb.
Tannic Acid, commercial Lb.
Tartaric Acid, crystals Lb.
OILS, WAXES, ETC.
pure, white Lb.
Black Mineral Oil, 29 gravity Gal.
Castor Oil, No. 3 Lb.
Ceresin. yellow Lb.
Corn Oil. crude 100 Lbs.
Cottonseed Oil, crude, f o. b. mil Lb.
Cottonseed Oil. p. ». y 100 Lbs.
Menhaden Oil. crude (southern) Gal.
Neat's-foot OU. 20° Gal.
Paraffin, crude. 118 to 120 m. p Lb.
Paraffin Oil, high viscosity Gal.
Rosin. "F" Grade. 280 lbs Bb!.
Rosin Oil. first run Gal.
Shellac. T. N Lb.
Spermaceti, cake Lb.
Sperm Oil. bleached | winter. 38° GaL
Spindle Oil. No 200 Gal.
Stearic Acid, double-pressed Lb.
Tallow, acidless Gal.
Tar Oil distilled Gal.
Turpentine, spirits of Gal.
METALS
Aluminum. N«. 1. Ingots Lb.
Antimony, ordinary Lb.
Bismuth. N Y Lb.
Copper, electrolytic Lb.
Copper, lake Lb.
Lead, N. Y Lb.
Nickel, electrolytic Lb.
Platinum, refined, soft Ox.
Silver Ol.
Tin, Straits Lb
Tungsten (WO.) Per Unit
Zinc. N. Y Lb.
FERTILIZER MATERIALS
Ammonium Sulfate 100 Lbs.
Blood, dried, f.o.b. Chicmgo Unit
Bone. 3 and 50. ground, raw Ton
Calcium Cyanamid Unit of Ammonia
Calcium Nitrate. Norwegian 100 Lbs.
Castor Meal jjnit
Fish Scrap, domestic, dried, f. o. b works Unit
Phosphate, acid. 16 per cent Ton
Phosphate rock, f. o. b. mine:
Florida land pebble. 68 per cent Ton
Tennessee. 78-80 per cent Ton
Potassium "muriite." basis 80 per cent Ton
Pyrites, furnace size, imported Unit
Tankage, high-grade, f. o. b. Chicago Unit
O 5.23
nominal
% 5.23
3.15
&
3.23
1.10
&
1.15
6.30
m
6 45
10>/i
■
11
10
■
12
6'/.
■
"A
5>/<
•
6'/l
50
(4
60
78'/.
&
79
29
0
29>/l
nominal
18.65
0
IS
.75
17'/
s 0
20.25
—
@
—
2.70
@
2
80
11
®
ll'/i
36
0
37
2.8S
23 'A
23 '/l
1.62
35
30V
!4>/i
2.90
7.25
0 7.30
6.50
@ 6.53
31.00
@ 33.00
lominol
nominal
16.00
@ 16.50
5.50
@ 6.50
2.25
0 2.50
5.50
O 6.00
350.00
3 355.00
nominal
@ 25.00
Tne Journal of industrial
and Engineering Ghemistry
Published by THE AMERICAN CHEMICAL SOCIETY
AT EASTON. PA.
Volume X
MARCH 1, 1918
No. 3
Editor: CHARLES H. HERTY
Assistant Editor: Grace MacLeod
Advertising Manager: G. W. Nott
ADVISORY BOARD
H. E. Barnard, H. K. Benson, F. K. Cameron, B. C. Hesse, A. D. Little, A. V. H. Mory, M. C. Whitaker
Published monthly. Subscription price to non-members of the American Chemical Society, $6.00 yearly; single copy, 60 cents
Price per single copy to American Chemical Society members, 50 cents. Foreign postage, seventy-five cents, Canada, Cuba and Mexico excepted
Entered as Second-class Matter December 19, 1908, at the Post-Office at Easton, Pa., under the Act of March 3, 1879
All communications should be sent to The Journal ot Industrial and Engineering Chemistry.
Telephone: Vanderbilt 1930 35 East 41st Street, New York City
Subscriptions and claims for lost copies should be referred to Charles L. Parsons, Box 505, Washington, D. C.
ESCHENBACH PRINTING COMPANY, EaSTON, Pa.
TABLE OF
Editorials:
Where Are the Leaders? 172
A Long Step in the Right Direction 172
Facts for the Tariff Commission 173
A Patent Abuse 173
Wasting Waters 174
Spruce Turpentine to the Fore 1 74
Sugar and Soap 175
The Naval Consulting Board 175
Original Papers:
American Sources of Supply for the Various Sugars.
C. S. Hudson 176
The Deterioration of Raw Cane Sugar: A Problem
in Food Conservation. C. A. Browne 178
Theory and Practice in the Design of Multiple Evap-
orators for Sugar Factories. A. L. Webre 191
Notes on the Analysis of Molasses. Herbert S. Walker. 198
Relation between Efficiency of Refrigerating Plants
and the Purity of Their Ammonia Charge. F. W.
Frerichs 202
Testing Natural Gas for Gasoline. G. G. Oberfell. ... 211
The Valuation of Lime for Various Purposes. Richard
K. Meade 214
A Study of the DeRoode Method for the Determination
of Potash in Fertilizer Materials. T. E. Keitt and
H. E. Shiver 219
Laboratory and Plant:
Blue and Brown Print Paper: Characteristics, Tests
and Specifications. F. P. Veitch, C. Frank Sammet
and E. O. Reed 222
A Hydrogen Sulfide Generator. Louis Sattler 226
Distinguishing Manila from All Other "Hard" Rope
Fibers. Charles E. Swett 227
Current Industrial News:
Diesel Engine Blast Pressure Control; Hides and Skins
from Venezuela; Germany's Commercial Methods;
Coal-Mining Machinery for Argentina; Utilization
of Nitre Cake; Klectro-Technical Industry in Japan;
Tannin and Timber; Aluminum Goods for Brazil;
Wiring Supplies; Pure Bismuth; Chromium Steel
for Magnets; An Automatic Controller for Electrical
Heating Apparatus; Machinery for Korea; Auto-
and High Pressure Problems; South African
Industrial Developments; Utilization of Waste
Boots; Vegetable Wax from Colombia; Zinc Refining
in Japan; British Hoard of Trade 228
CONTENTS
Trade Associations:
The Chemical Alliance ; Dyestuff Convention ; American
Drug Manufacturers Association ^231
Chemists in War Service:
Government Recognizes the Importance of Chemistry
in the War 234
Notes and Correspondence:
Spring Meeting of the American Chemical Snciety;
War Risk Insurance for Chemists in Military Service;
Ramsay Memorial Fund; Chemical Research in the
Various Countries before the War and in 1917;
Licenses Required for Explosives and Their Ingredi-
ents; The Indexes to Chemical Abstracts; The
Utilization of Niter Cake; Readjustments at the
Massachusetts Institute of Technology to Meet
War Conditions; Directions for Assistant Editors
and Abstractors; Estimation of Phenol in the Pres-
ence of the Three Cresols — Correction; Electric
Furnace Smelting of Phosphate Rock, etc. — Cor-
rection 236
Washington Letter 239
Obituartes:
Charles Caspari, Jr.; Joseph Price Remington 240
Personal Notes 241
Industrial Notes 243
Government Publications 245
Book Reviews:
The Distillation of Resins; The Chemistry of Farm
Practice; An Introduction to Theoretical and Ap-
plied Colloid Chemistry; The Chemistry of Colloids;
Allen's Commercial Organic Analysis; Standard
Methods of Chemical Analysis. A Manual of
Analytical Methods and General Reference for the
Analytical Chemist and the Advanced Student;
Laboratory Guide of Industrial Chemistry 249
New Publications 25 1
Market Report 252
172
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 3
EDITORIALS
WHERE ARE THE LEADERS?
To back the man power of our military forces the
enormous industrial resources of the country are being
assembled. Chemistry permeates every fiber of our
national economic body. It is but logical, there-
fore, that intense chemical activity should prevail in
Washington at the present moment. Chemists from
every quarter have been called to this center of war
preparations. These men are giving all of their talent
and energy in loyal devotion to the interests of
America.
With characteristic foresightedness the Director of
the Bureau of Mines early began the development
of a great organization of research chemists to inves-
tigate the various problems connected with gas war-
fare— offensive and defensive. The War Department,
particularly the Ordnance Bureau, has added largely
to its staff of chemists for test, inspection and supply
of material vital to the successful prosecution of the
war. The Navy Department, always "on the job,"
is relying upon the applications of chemical princi-
ples. The War Industries Board is confronted con-
stantly with chemical questions of the first magni-
tude. The Chemical Service Section of the National
Army, attached directly to General Pershing's Staff,
functions as a field service, and is prepared to advise
him directly on pressing problems arising from day to
day in the manifold activities of a continually growing
army on French soil. The Sanitary Corps depends
upon its chemical experts for safe guidance in measures
to protect the physical well-being of the men in camp
and in field. The government chemical bureaus have
expanded their normal activities. Chemistry every-
where! So it should be, if the best results are to be
obtained.
The greater part of the work up to the present
time has been research. This has been well done,
and carried out with the utmost despatch. Now we
are entering upon — indeed, are already getting well
into — a new phase, namely, the production of materials
on an immense scale. Laboratory results must be
translated quickly into terms of plant operation. The
requisites now are rapid plant construction and a never
failing yield of abundant finished product.
As we view fairly and honestly the inauguration of
this phase of the work, candor compels the statement
that the feeling of pride in the accomplishments of
the initial stage has given way to grave apprehension
over the ultimate outcome of this all-important sec-
ond stage, for mistakes here will be measured in the
blood of young Americans now being trained for the
heart-rending days that are just before us.
A great chemical industry must be dc\
immediately. Through some strange concatenation
of circumstances men are now charged with the
responsibility of vast chemical developments who, in
times of peace and by those best qualified to judge,
would never have been thought of; others are daily
called upon to decide gravest questions of supplies
of chemicals who, it is commonly reported, know
not even the names of these substances save as they
have become familiar in the routine of the new duties;
much less is there full understanding of the interde-
pendence of these products and their relative values.
It is a serious situation and one which calls for wise
and courageous treatment. Where are the leaders,
the men who in peace times have made this country
what it is, so far as chemistry has affected its fashion-
ing? They are not in Washington. There they
should be, giving of their very best in talent, in expe-
rience, and in executive ability. Furthermore, now
is the time for the appointment of a man preeminent
among these leaders to act as a coordinating agent for
the multifarious chemical activities; to have at his
command the highest specialized talent in the land
for projecting into being the plants whose output
bears so directly on the future welfare of the
world; and to adjust the requirements of the
various Departments as supply steadily increases:
a man with chemical experience, with knowledge of
chemical personnel, with executive ability of the
highest order, and blessed with vision. Such a man
can be found. A sure road to his discovery would
lie in the request from President Wilson for a joint
recommendation from the Directors of the American
Chemical Society, the Chemical Alliance, the Amer-
ican Institute of Chemical Engineers and the Amer-
ical Electrochemical So
Give such a man the power to do things, and hold
him responsible to the nation for the use of that power.
The days for preparation are passingl
A LONG STEP IN THE RIGHT DIRECTION
The last number of This Journal contained an
editorial entitled "Somebody Please Cut the Tape."
It develops that on January 26, after we had gone
to press, the Adjutant General issued an order cor-
recting radical defects in the method of securing the
transfer of chemists to positions in which their train-
ing can best be utilized. On page 234 of this issue
statements from the Chemical Service Section of the
National Army are published, outlining the measures
initiated to pul 'his new order into effect. These'
communications are followed by important announce-
ments from Secretary Parsons. It is of particular inter-
est to note that the War Department is making no nar-
row and strictly technical definition of the term
"chemical engineer" in its attitude toward the return
for graduation of dratted chemical engineering stu-
dents. The red tape which bound those cards of in-
formation on tile in the office of Secretary Parsons
lias been cut, and it is gratifying to learn that common
sense is prevailing. Careful reading of these state-
ments is urged upon all.
There is one issue, however, which still deserves
most serious consideration by the authorities, namely,
the question of deferred classification of university
Mar., iqi8 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
instructors. Among others, Secretary Baker, General
Wood, and, more recently, Mr. Hoover have publicly
urged all students to remain in college unless actually
drafted. In orders promulgated by the War Depart-
ment, official recognition has been given of the neces-
sity for continued preparation of students in engineering
and in medicine. The successful training of both of
these groups of men involves fundamental instruction
in chemistry. Yet it seems that the Local Draft
Boards throughout the country are declining to give
any deferred classification to instructors in chemistry.
In practically every institution, members of the
teaching staffs have been assigned by the Local Boards
to Class i-A. In a few isolated cases, and only as the
result of strenuous effort on the part of university
administrators, District Boards have transferred these
men to Class 3-.K. Yet upon the instructors, for the
most part of draft age, must fall a large part of the
burden of instructional work, for already the staffs
of these same institutions have been seriously crippled
by the withdrawal of many professors for war investi-
gations in Washington, and for the Chemical Service
Section of the National Army, while many important
government researches are being prosecuted within
university laboratories. The candle is being burned
at both ends.
If it be considered necessary for the country's wel-
fare that students should continue their university
training, surely it is logical that these men should
have competent and adequate instruction. Other-
wise the entire program falls through.
The action of the Adjutant General in clarifying
the industrial situation warrants the hope that the
Provost Marshal General will likewise issue orders
to prevent the decimation of the instructional staffs
of the institutions where, at the direction of the
War Department, young men are to be trained in
order eventually to give to this country the greatest
service of which they are capable.
FACTS FOR THE TARIFF COMMISSION
From the Chairman of the Tariff Commission
we have received a copy of the letter and accompany-
ing questionnaire as to production and consumption
recently sent out to all manufacturers of intermediates,
dyes, medicinals, photographic chemicals, flavors,
synthetic phenol resins, and to those plants other
than coke plants and gas houses, manufacturing crudes.
In conducting this census the Commission is ac-
cumulating the evidence by which the President, under
the law as it now stands, will eventually be guided in
the matter of the possible repeal of the special duties.
We are confident that manufacturers, regardless of
the time and labor involved, will promptly and in
fullest detail furnish the Commission the information
desired. And it is directly to the manufacturer's
own interest to do so. The published summary of
this census will furnish facts which will prove the vin-
dication and glory of the American manufacturer and
constitute the certain basis upon which a repeal of the
sixty per cent clause can be recommended and urged.
Furthermore, this publication should serve as an ac-
curate and illuminating gude for the future coordina-
tion and intelligent diversification of the dyestuff
industry.
We have been especially interested in reading one
portion of the questionnaire and quote herewith from
the second footnote on page 7:
"The term 'indigoids' has not yet been defined by the courts.
It is. therefore, urged that special care be taken to explain the
chemical nature of all dyes which might be regarded as indigoids.
Such explanation will enable the Commission to make classi-
fications in accordance with future judicial interpretation of
this word."
Congress can relieve the courts of the necessity of
making any such "judicial interpretation" by striking
out the word.
It is altogether pleasant and assuring as we approach
the day of further legislation concerning tariffs and
especially tariffs on dyestuffs to sense a new standard
of action. The log-rolling spirit of previous years
has been put in the background and in its place
appears a desire for facts as a guide for action. For
this change we are largely indebted to the able
and comprehensive manner in which the Tariff Com-
mission has begun its labors. Then, too, the spirit
of the times precludes excessive partisanship; more
and more, selfish and purely local considerations
are yielding to whole-hearted devotion to national
interests. Such an atmosphere justifies the utmost
confidence as to the character of future legislation.
A PATENT ABUSE
The exigencies of the war period have led to feverish
activity in many laboratories in attempts to carry out
processes described in the literature and in patent
specifications, chiefly in the field of organic chemistry.
Within the past year we have frequently been apprised
by chemists of the lack of success in the preparation of
compounds by following directions, even by most care-
ful attention to the minutest details, in the official
records. Men who have experienced this difficulty
stand so high that no question of lack of skill and
technique can be involved, and we are forced to the
conclusion that deliberate misrepresentation has been
made, especially in the case of certain foreign patents.
If this is true it is extremely regrettable that the litera-
ture of chemistry is clogged with such deceit; in the
case of patent specifications, it is reprehensible, in that
a matter of perjury is involved. The demonstration
of such falsity would immediately invalidate the
patent, but this is a tedious process, necessitating a
great amount of laboratory work and expense and loss
of time in litigation.
Our patent system should be protected against im-
positions. This might be accomplished in one of at
least three ways: First, the Patent Office might test
the good faith of all applicants for chemical patents
by making greater use of existing government labora-
tories. It is doubtful, however, in view of the work
already engaging the attention of these federal labora-
tories, whether a further tax upon their courtesy would
174
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 3
be justifiable. Second, the Patent Office might be
provided with a control laboratory of its own. The
varied character of the applications for patents cov-
ering all fields of chemistry would necessitate a large,
efficiently manned laboratory. This would entail
considerable expense, nevertheless it would be an ex-
penditure operating for the benefit of the entire country.
Third, the Patent Office might require of the ap-
plicant a laboratory demonstration of the correctness
of the specifications. This would place the burden of
the proof upon the inventor, but would work no hard-
ship upon organizations having extensive laboratories,
though it might affect the man of small means.
Perhaps there are other practicable remedies. Cer-
tain it is that the abuse should be eliminated, and
the first step toward this end is the demonstration of
the correctness of the original premise, namely, that
the Patent Office files have been befouled with false
declarations. If evidence can be brought together,
we are fortunately in position to place it where it will
do most good, and we therefore urge all chemists who
have been led up a blind alley by following the direc-
tions outlined in patents, to communicate that fact to
this office, designating by number and subject the mis-
leading patent, and supplementing this by a brief
exposition of the difficulties encountered. This is
more than an invitation, it is an appeal, for nothing
can be more vital to the future of the chemical indus-
tries than the establishment upon a firm basis of the
patent system, whose raison d'itre is the stimulation
of the inventive genius of the Nation by affording full
protection of the law to those who record with it the
truth concerning their discoveries.
WASTING WATERS
An anomalous situation presents itself at Washing-
ton and at Niagara Falls. At Washington, under the
authority of the President, the power produced by the
several American companies at Niagara Falls, together
with that imported from the Canadian side, has been
requisitioned. The War Industries Board is now engaged
in the task of redistributing this power in a manner
"to assure the adequate supply of electric power for
the establishments engaged in war work at Niagara
Falls and Buffalo." There can be no difference of
opinion as to the wisdom of this step, regardless of
the fact that about one hundred and ten plants at
Buffalo, hitherto dependent solely upon this power,
may now use it only when it is not needed for war
work, or else must resort to steam plants requiring
that form of carbon which at present is, if anything,
more difficult to obtain than the crystalline variety.
Also at Washington legislation has been enacted for
the express purpose of relieving the power shortage
at Niagara Falls by authorizing the diversion of the
full amount of water permitted under treaty stipula-
tions. All this sounds hopeful and helpful. Such is
the state of affairs at the Washington end.
On the other hand, at Niagara Falls water sufficient
for generating 65,000 horse power, the diversion of
which has been duly authorized by Act of Congress, is
to-day flowing over the falls, serving no other purpose,
while the Nation's life is at stake, than the delecta-
tion of bridal couples having the temerity to journey
in such unseasonable weather to this classic resort
of newly-weds. Of the 80,000 horse power capable
of being produced under the legally increased take-off
of water only 15,000 has been developed.
The explanation is simple: the terms of the Act
are so restrictive that private capital will not risk
the necessary increased investment. To make this
clear, we quote from the joint resolution approved
January 19, 1917, which resolution on June 30, 1017,
was "continued and in full force and effect, and under
the same conditions, restrictions and limitations until
July 1st, nineteen hundred and eighteen."
"Resolved by the Senate and House of Representatives of
the United States of America in Congress assembled. That the
Secretary' of War be, and he is hereby, authorized to issue per-
mits, revocable at will, (or the diversion of water in the United
States from the Niagara River above the Falls for the creation
of power to individuals, companies, or corporations which
are now actually producing power from the waters of said river,
in additional quantities which, with present diversions, shall
in no case exceed the capacity of the generating machinery of
the permittee and tenant companies now installed and ready for
operation, nor an amount sufficient to enable the permittee to
supply the now existing hydroelectric demands of the individuals,
companies, or corporations which said permittee and tenant
companies are now supplying, but not in excess of the capacity oj
power-using appliances of said consumers now installed and ready
for operation* * *" (Italics are ours.)
We hold no brief for the power companies at Niagara
Falls, nor on the other hand can they be blamed for
failure to develop this power, under the restrictions
the law now imposes. We do, however, feel the same
impatient interest as would be aroused by the sight
of trainloads of coal controlled by the Government
burning on the railroad tracks, while the fire depart-
ment sat knitting sweaters for the boys at the front.
Sixteen and a half pages of the Congressional Record
devoted to the debate in the House of Representatives
on the reintroduced Garabed resolution which offers
to produce something from nothing, while water suffi-
cient for 65,000 horse power glides uninterruptedly over
the Falls! It may be that the bill of Representative
Waldow, recently introduced (H. R. 8491), "empower-
ing the President to take possession and assume con-
trol of projects for the generation of hydroelectric
power from the waters of Niagara River, etc.," will
prove the salvation of this situation, but it is too often
a long time between the introduction of a bill in Con-
gress and its ultimate signature by the President
Divert those wasting waters into channels where, to
the uttermost drop, their energy will turn the wheels
of the munitions plants of the Nation!
SPRUCE TURPENTINE TO THE FORE
The scene^ shifts rap'dly nowadays. Two months
ago we pointed out to sulfite pulp manufacturers the
necessity of recovering spruce turpentine for the pur-
pose of increasing the toluol supply of the Army On
Mar., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
i7S
February 6 we were shown a letter from the presi-
dent of one of the largest paper concerns, waving
aside the whole matter of spruce turpentine as being
not worth consideration. In spite of the judgment
of this high official we had the boldness on the same
evening to urge the members of the Technical Asso-
ciation of the Pulp and Paper Industry to devote
the full energies of their research laboratories and engi-
neering departments to this subject, on the ground
that in times like the present manufacturing
problems involving the supply of material needed
for our army in France pass beyond the realm of the
cold-blooded calculations of peace times — that busi-
ness must be conducted, where war material is con-
cerned, on a higher basis than one of mere profits.
An interesting confirmation of the soundness of that
contention was furnished on the following day, when,
at a conference of representatives of the War Depart-
ment and of the Association, a strong committee was
appointed to ascertain what supplies of spruce turpen-
tine may be available, and to cooperate with the War
Department in procuring the installation at mills of
suitable apparatus for its recovery. The committee
from the Association consists of Henry E. Fletcher,
Alpena, Mich., chairman; F. M. Williams, Watertown,
X. Y.; W. E. Byron Baker, York Haven, Pa.; P. A. Paul-
son, Kimberly, Wis.; Henry F. Obermanns, Erie, Pa.;
Morris W. Hedden, 736 Pittock Block, Portland,
Ore.; George K. Spence, Johnsonburg, Pa.; E. R.
Barker, 79 Milk St., Boston, Mass.; A. W. Nickerson,
501 Fifth Ave., New York.
It is not a hard tax upon the imagination to believe
that when peace has come again the availability
of so large a quantity of pure cymene will, through
the work of research laboratories, open a new chap-
ter in chemical industry.
SUGAR AND SOAP
We are fortunate in presenting in this issue four
distinct and important contributions bearing upon
various aspects of the sugar industry. It may be well
in this connection to call attention to the use of sugar
in the manufacture of soap, to produce transparency.
For this purpose fr.om five to ten per cent of sugar is
added. Its function is purely an aesthetic one; a
transparent soap delights the eye, but how pleasing
to the palate would have been that extra lump of sugar,
without which we have gone for months. This is a
day of demarcation of essentials and non-essentials,
and surely the transparent quality of soap is not es-
sential in attaining that cleanliness which, according
to the proverb, is next to godliness.
THE NAVAL CONSULTING BOARD
The first of the many war boards organized for
the purpose of civilian cooperation with the regularly
constituted authorities was the Naval Consulting
Board. It is unique in that its members were nomi-
nated by the chemical and engineering societies upon
invitation of the Secretary of the Navy. For this
reason chemists will be particularly interested in that
portion of the concise and impressive report of Secre-
tary Daniels referring to the work of this Board.
"During the year the work of the Naval Consulting Board,
organized and approved by Congress in 1915, has increased very
materially in importance and volume, its meetings have been
frequent and the work of the individual members has been such
in some cases as to occupy almost their entire time in the service
of the Government.
"Some time before the active entry of this country into war
the Board called a special meeting to which were invited some
50 of the leading scientists and industrial managers, whose
special study fitted them to advise on the methods of meeting
the submarine problem.
"Plans were immediately made to investigate every field to
develop a means of preventing destruction of vessels and of de-
feating the U-boat. The investigation was divided according to
the experience of the different members and associated scientists
and with the cooperation and valuable assistance of the various
manufacturing companies interested a highly developed system
of team work has been attained and results accomplished not
dreamed of at the beginning of the war.
"The services of the Board were offered to the Council of
National Defense and accepted by that body for the investiga-
tion of all inventions submitted. Its services were also accepted
by the War Department in an advisory capacity.
"Valuable assistance has been rendered merchant shipping
by the Board's activities. * * * In this field the Board's work
has resulted in materially reducing the shipping risk, with a
consequent lowering of marine insurance rates.
"Not the least result of its work has been the stimulation of
interest, in the problems brought up by the war, throughout the
country by the general invitation to submit ideas for investiga-
tion. Early in the calendar year 1917 this interest manifested
itself in the receipt of thousands of ideas weekly, and to care for
this the department's connecting office has been greatly enlarged,
the office of the Board in New York has been organized
on a working basis with a large force, and the whole movement
has received the approval and hearty assistance of the great
national engineering societies. The president of the Board,
Mr. Thomas A. Edison, has been giving his entire time to the
work of the Board in the service of his country, and has called
to his assistance a capable staff who are working diligently upon
naval problems.
"With war conditions increasing the need for labor and build-
ing materials, it was believed to be a wise policy to defer for a
time the building of the new experimental and research labora-
tory. Such experiments as have been warranted have been made
in private laboratories generously offered and at the Bureau of
Standards. The need for this establishment, however, is more
clearly shown than ever, and its support is urgently advised.
"The valuable results obtained by the work of this Board are
of too confidential a nature to make them the subject of a public
document. The members have given freely of their time and
scientific ability to the service of the Nation and have earned the
gratitude of all who know their unselfish and patriotic service.
I wish to express my sense of obligation for the cheerful coopera-
tion, wise counsel, loyal devotion, and personal sacrifice which
have characterized the membership of the Board of distinguished
civilians who responded, long before war was declared, to the
selectivi 'Iraft with all the enthusiasm and efficiency of youthful
volunteers "
Drs. L. H. Baekeland and W. R, Whitney, the repre
sentatives of the American Chemical Society, have
given generously of their time, energy and talents to
this service, and it will be gratifying to .ill to read these
words of appreciation of their ability and patriotic
spirit.
176
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 3
ORIGINAL PAPERS
AMERICAN SOURCES OF SUPPLY FOR THE VARIOUS
SUGARS
By C. S. Hudson1
Received January 16. 1918
The annual consumption of sugar in the United
States is approximately 4.300,000 short tons or nearly
86 lbs. per capita. The sources of this sugar are:
Cane Sugar from Cuba 49 per cent
Domestic Beet Sugar 21 per cent
Cane Sugar from Hawaii 13 per cent
Cane Sugar from Porto Rico 8 per cent
Cane Sugar from Louisiana 6 per cent
Cane Sugar from the Philippines 3 per cent
It will be noticed that 73 per cent of the sugar comes
from over the sea. The domestic beet sugar is pro-
duced principally in the states of Colorado, California,
Utah, Michigan, Idaho and Ohio, with smaller quanti-
ties from several others.2 The growth of beet sugar
production in the United States has been phenomenal,
the output having increased from 2.000 tons in 1888
to 430,000 tons in 1908 and 800,000 tons in 191 5. The
further extension of sugar production in the continental
United States will probably come from increased
plantings of sugar beets, and possibly also from the
growth of sugar cane in the drained lands of southern
Florida, though it must be added that the commercial
production of cane sugar in that locality is not yet
demonstrated and may not prove possible. It will
be borne in mind by those investigators who may be
seeking new sources for sugar that many plants yield
sweet sirups which might be used for sweetening pur-
poses if the natural accompanying colors and flavors
could be removed. In recent years this removal has
become a possibility through the use of active decolor-
izing carbons that may be prepared from wood in a
variety of ways.3
Crystalline dextrose (corn sugar) is produced in the
United States in very large quantities by the acid
hydrolysis of corn starch, and is used in commercial
baking, in tanning, in the production of wines in the
Middle West, and to some extent in the manufacture
of a type of vinegar. Commercial corn sugar is some-
what yellow in color, a fact which will be readily un-
derstood by chemists when it is recalled that dextrose
forms small crystals that are in consequence difficult
to free from adhering mother liquors.4
The third sugar of commercial importance is milk-
sugar, which was produced in the United States from
milk to the extent of about 3,500.000 pounds in 1014,
at 16 factories, the supply being increased by the im-
portation of nearly 600,000 pounds.
Crystalline levulose was imported from Germany
1 Presidential Address delivered before the Washington Section of the
American Chemical Society. January 10, 1918.
'Sugar statistics arc available from the annual Yearbooks of the I'. S.
Department of Agriculture and from Willctl & Grays Weekly Statistical
Sugar Trade Reports.
■ For a summary of work on decolorizing carbon, sec Schncllcr. Louisiana
Planter, 69 (1917), 154
4 Directions for the laboratory preparation of C. P. dextrose have been
published by Hudson and Dale, ./. .In i hem. Soc., 39 (1917),
before the present war for use by diabetics as a sweeten-
ing agent, but it does not appear to have been manu-
factured at any time in the United States. It is not
difficult to prepare levulose. either as a sirup or in crys-
tals, by forming from inverted cane sugar and lime
the crystalline calcium levulosate that Dubrunfaut dis-
covered early in the last century and breaking up this
compound into levulose and calcium carbonate by the
use of carbon dioxide. Indeed this very old process
is quite worthy of consideration as a possible method
of preparing a sweet sirup from plants that yield inulin,
since the latter is readily hydrolyzed by dilute acids
to levulose. Levulose is the sweetest of all the sugars.
Chicory, the Jerusalem artichoke ( Helianlhus luberosus),
and the sotol plant,1 a species of Agave {Dasylirion)
that grows abundantly in the wild state in Texas,
contain much inulin or inulin-like substance.
The lactone of a-glucoheptonic acid, which may be
prepared from dextrose by the cyanhydrin synthesis,
is rather sweet and apparently has been manufactured
to some extent in Germany for use by diabetics.*
Many sugars that are of much interest to scientists,
particularly chemists and bacteriologists, are almost
wholly unknown to the general public, even though
some of them are consumed in large quantities as natural
components of foods for man and domestic animals.
Thus raffinose is contained in cottonseed meal to the
extent of nearly 8 per cent; this portion of the weight
of the cottonseed cake that is produced annually in
the United States amounts to about 100,000 tons.
Cottonseed meal offers the best source for the prepara-
tion of crystalline raffinose,3 which is used in bacteriology
to some extent. From raffinose the disaccharide
melibiose may be prepared in good yield;4 the latter has
never been upon the chemical market and the raffinose
that has been used by scientists was imported from
Germany, where it was made from cottonseed meal
that came from the United States.
Many industrial chemists have sought to prepare
from starch by the action of malt the very palatable
sugar maltose, and the field of possible uses of this sugar,
either in crystalline form or as a sirup, is a large one.6"
Most maltose sirups carry a flavor of the malt and do
not quite represent the pleasing sweetness of a solution
of pure maltose; possibly this objection could be over-
come by the use of decolorizing carbon since it readily
removes many flavors as well as coloring matters.
Maltose forms small crystals that are difficult to wash
by commercial processes, but there has always been a
small market for C. P. maltose among chemists and
bacteriologists. The whole supply for such scientific
uses has always been importi
Hudson This Joi knvl. % 1910), 145.
: See Abderhalden's Bioekemisches Handiexikor,. First Supplementary
Volume to Vol 8 il"14>. 253.
' Hudson and Harding, J. Am. Chen 36 4 2110.
« Ibid., 37 (I91J
1 For a description of the principal ;.teps in making a maltose sirup,
sec an early article by Cuisinier, Suer, >•:<: , 20. Xi» 14; German translation
in Z Ver. Zuckerind . 19 ( 18821. 908.
Mar., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Mannose, a sugar of much interest to scientists on
account of its close kinship to dextrose and levulose,
has usually been prepared from the hydrolysis of vege-
table ivory, the seed of a palm (Phylelcplias macro-
carpa) that is native to South America. A large in-
dustry in the United States has been built upon the
manufacture of buttons from vegetable ivory; the
waste from these button factories, amounting to twenty-
five or more tons a day. offers a very cheap source for
the production of mannose. Since the sugar crystal-
lizes only with difficulty it has been customary to pre-
pare that small quantity of it which was used in re-
search by chemists and bacteriologists by separating
from the solution of the hydrolyzed vegetable ivory
waste a crystalline phenylhydrazone of mannose, re-
generating the sugar from this compound, and crystal-
lizing it. Germany has been the source of the marketed
product, and little has been imported by the United
States, partly because the cost of nearly $200 per lb.
has restricted its use even in research. But we now
know a process for crystallizing mannose directly
from the hydrolyzed vegetable ivory with a large yield,1
and this interesting sugar should come into more ex-
tended use in research chemistry and bacteriology
at a relatively low cost. Indeed the possible com-
mercial production of derivatives from mannose, such
as mannite (by its reduction) or the crystalline dilac-
tone of mannosaccharic acid (by its oxidation) should
not be lost sight of by chemists. It is very surprising
that perfectly pure mannose has a slightly sweet taste
that is followed by a distinctly bitter one. Its very
close relatives by structure, dextrose and levulose,
are both of a pure sweetness, the latter being the sweetest
sugar known.
The disaccharide trehalose, which is composed of two
molecules of dextrose, has always been a very rare
sugar. It is of very crystalline habit, resembling cane
sugar superficially. It might be useful to have a sup-
ply of trehalose available for bacteriological and chem-
ical research. The older sources of it, such as ergot,
mushrooms, or trehala manna, have been supplanted
by Anselmino and Gilg's2 discovery that the resurrec-
tion plant (Selaginella lepidophylla), a native of our
own arid Southwest, obtainable in large quantities,
contains 2 per cent of trehalose which may readily be
crystallized.
Galactose may of course be prepared from the hydrol-
ysis of milk sugar and this is a good source for the pro-
duction of such supplies of it as are needed by scientists.
It has recently been shown by Schorger and Smith3
that a native species of larch {Larix occidentalis) , a
lumber tree of our Northwest, contains a considerable
quantity of a gum that is easily hydrolyzed by acids
to yield galactose. This source seems to offer a way
for the economical production on a commercial scale
of useful derivatives of galactose such as its oxidation
product, crystalline much acid, and possibly dulcite
from its reduction. The last substance is very use-
ful in bacteriological work, and its price has heretofore
Hudson and Sawyer. J Am. Chem. Sac., 39 (1917), 470.
' Bet. pharm. („ II (1913), 326.
1 Tlllh JOOTMAL, S (1916), 49J.
been about $400 per lb. The supply of dulcite for
scientific research has come from Germany.
Arabinose may be prepared readily by the hydrolysis
of beet pulp, the insoluble residue from the technical
extraction of sugar beets with water. It has been used
by bacteriologists only to a slight extent on account
of its cost, but the expense of its production from beet
pulp is small. Its reduction product, arabile, is also
needed in the same field of science. Beet pulp is a much
better source for arabinose than the cherry gum that is
usually recommended by the textbooks.
An excellent source for the methyl pentose sugar,
rhamnose, is the bark of the American black oak tree
(Quercus tinctoria) which is extensively used in dyeing.
Its aqueous infusion is known as quercitron extract.
Since the early part of the last century, when Chevreul
isolated from it the glucoside quercitrin (a compound
of rhamnose with quercetin), it has been the natural
source of the commercial glucoside. There is needed
at the present time, however, a description of a depend-
able process for preparing rhamnose from black oak
bark.
The octacetate of cellose is readily obtainable from
the action of acetic anhydride and sulfuric acid upon
cotton, and the sugar cellose. a disaccharide composed
of two molecules of dextrose, may be prepared without
difficulty by the saponification of the octacetate.
During the last year two new sugars have been added
to the group by the work of LaForge.1 Both of these
are members of the seven carbon series of sugars, and
their occurrence in natural products indicates that the
heptoses are by no means restricted to the fields of syn-
thetic sugars from the chemist's laboratory, but are im-
portant natural substances. Manno-keto-heptose was
found to occur free in the avocado (Per sea gratissima),
a native American fruit that is used extensively as
human food. The name avocado is the Spaniard's
equivalent for the Aztec ahuacatl. Scdoheptose was
found in the free state in the stonecrop {Sedum specta-
bile), an ornamental European plant that is now domes-
ticated throughout the world.
The pentose sugar xylose, isomeric with arabinose,
was first found by Koch in the gummy portion of various
woods, but its isolation from such sources is rather
difficult and the yield low. Two much better sources
of American origin have recently come into notice,
namely, cottonseed hulls2 and corn cobs. In unpub-
lished experiments by Mr. T. S. Harding and myself,
yields of about 10 per cent of crystalline xylose were
obtained from the acid hydrolysis of corn cobs. While
it has long been known that xylose occurs in corn cobs,
the yields of crystalline xylose that have been reported
have never been as high as one per cent. The yield
from corn cobs is much larger than from cottonseed
hulls. If industrial uses could be found for xylose,
either in the pure state, through derivatives, or in the
form of the sirup that results from the hydrolysis of
'J. Bid. Chem., 28 (1917). 511; LaForge and Hudson, Ibid., 30
> Baler, Crundlagen unit Er/tebnine der Pflanzenchemie, 1 (1908), 44;
Hudson and Harding, .'. Am. Chem. See., 89 (1917). 10.18.
i78
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, Xo. 3
corn cobs, a way would be open for the use of a very
cheap and abundant waste product.
When one realizes that the best sources for nearly
all the sugars are to be found among raw products
and plants that occur abundantly in America, most of
them being of distinctly American origin, the poet's
lines,
"My Country 'tis of Thee
Sweet land of liberty,"
seem peculiarly appropriate in a novel sense.
Department of Agriculture
Bureau of Chemistry
Washington. D. C.
THE DETERIORATION OF RAW CANE SUGAR:
A PROBLEM IN FOOD CONSERVATION
By C. A. Browne
Received January 4, 1918
INTRODUCTION
The changes in composition of food products be-
tween manufacture and consumption involve some of
the most interesting problems of agricultural-chemical
research. The problems are also of great economic
importance, the financial losses, which result from de-
terioration of food materials during transportation or
storage, amounting each year to many millions of dol-
lars. In the case of cane sugar, of which there is at
present so serious a shortage, calculations based upon
careful analytical and statistical data show that the
losses from the deterioration of Cuban sugars alone
probably exceed one million dollars per year.
The chief ingredient responsible for the deterioration
of sugars is moisture. As far back as three centuries
age, when sugars began to be shipped from the West
Indies to Europe, it was observed that moist sugars
reached their destination in a much damaged condition.
The need of excluding moisture was quickly recognized.
Ligon,1 one of the earliest writers upon the subject,
in 1673 pointed out the necessity of keeping sugar
"drie in good casks, that no wet or moist aire come to
it."
But while early observers were agreed that moisture
played an important part in deterioration, the actual
cause of the phenomenon was for centuries unknown.
It was believed by some that the trouble was due to a
deliquescence produced by the action of chlorides and
other saline impurities upon the sugar; as late as 1848
Wray1 stated that in his belief it was possible for "this
deliquescence to continue, until the whole mass of
sugar is decomposed" and suggested as a possible
remedy for deterioration the precipitation of chlorides
from cane juices by means of silver nitrate. A more
common belief was that deterioration resulted from the
action of a glutinous fecula or ferment which occurred
naturally in the cane and, if clarification was imperfect,
passed into the sugar. The true explanation was not
forthcoming until after the work of Pasteur, when
1 "History of the Island of Barbadoes," London, 1673, 111.
'"The Practical Sugar Planter," London, 1848, 342-343. It is inter-
esting to note that Pekalharing (International Sugar Journal. 3, 434) as late
as 1900 found it necessary to combat the idea that deterioration was due to
the salts contained in sugars.
Dubrunfaut1 about 1869 discovered in a deteriorating
sugar microorganisms similar to the alcohol and lactic
educing organisms of Pasteur. After this the
deterioration of sugars began to be studied with in-
creasing interest from the standpoint of infection by
germs, until the subject has now become one of the
most important fields of research in industrial mycology.
After the invention of the polariscope, some three-
quarters of a century ago, it became possible to de-
termine the keeping power of sugars with an exactness
undreamed of by earlier observers. The refiners of
sugar, who were the first to put the polariscope to
practical use, employed this instrument not only for
determining the value of purchases and for controlling
factory operations, but they also used it for following
the keeping power of stored sugars. With the accumu-
lation of analytical data, which all such establishments
acquire, it was soon observed that other factors beside
moisture played an important r61e in the keeping of
sugars. It was noticed that impure molasses sugars of
high moisture content might keep perfectly when high-
grade white sugars of much lower moisture content
would rapidly deteriorate. In other words, it became
evident that the impurities or non-sucrose constituents
of raw sugars must be considered in connection with
the moisture content before a reliable forecast could
be formed as to keeping power. Various tables and
rules were devised, in fact, towards this end, although
but little of the valuable information thus gathered
was published. The best known of these rules is the
so-called "factor-of-safety" of the Colonial Sugar Re-
fining Company of Australia, according to which the
moisture of a sugar must not be more than half the non-
sugar if the product is to keep. In other words, if
W is the percentage of water and S the percentage of
W
sucrose, the quantity , m must not exceed
100— S — W
0.5; or simplified, the quantity —
exceed 0.333.
W
must not
EXPERIMENTAL PART
A — CHEMICAL OBSERVATIONS
In a report published two years ago the author1
called attention to the value of the "factor-of-safety"
of the Colonial Sugar Refining Company, and his more
recent investigations show that the rule is one which
can be relied upon in the great majority of cases. The
1 Comft. rend., 68 (1869), 663. The classic observation of Dubrunfaut
upon the deterioration of sugars is worth translating. In commenting upon
the fact noted so many times since, that raw beet sugars, which were not
made by an alkaline clarification, failed to keep. Dubrunfaut wrote as fol-
lows:
"By means of the microscope we were able to detect in impure beet
sugars the presence of those lower organisms, so accurately described by
M. Pasteur, and which arc the living causes of the alcoholic and lactic fer-
mentations. Nothing can be more simple, therefore, than to arrive at an
immediate understanding of the formation of the glucoses and of the acid
reaction in sugars which were not made by the old traditional sugar-house
process known under the name of the alkaline process."
Dubrunfaut attributed the deterioration of refined sugars to the im-
purities, ferments, etc., introduced into the factory by the raw sugar.
It is remarkable how here, as in so many other instances, the opinions
of this great French investigator (to whom the sugar industry is indebted
for more discoveries than to any other chemist) have been confirmed by sub-
sequent workers
1 "The Deterioration of Raw Su,;ar Samples." Louisiana Planter,
51 (1915). 281-2.
Mar., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
author's experiments indicate, however, that, for Cuban
and Porto Rican sugars at least, the constant 0.333
W
is a little too high, the value 0.3 for - — being
IOO b
more nearly correct.
This is shown by the following series of experiments
begun in 191 5: Eight sugars were selected of the
average Cuban and Porto Rican type with factors of
safety ranging between 0.25 and 0.35. Forty glass-
stoppered bottles of 8 oz. capacity were then filled with
the well mixed samples (making eight sets of five bottles
each) and the stoppers sealed hermetically with wax.
Periodic analyses were then made, one set of eight
bottles being analyzed at the beginning and the other
sets put aside for future comparison. The four sugars
whose factors ranged from 0.313 to 0.346 deteriorated,
while the four samples whose factors ranged from
0.253 to 0.289 suffered no appreciable loss in sucrose.
The results obtained upon the four deteriorating samples
are given in Table I.
Table I — Periodic Analyses of Bad-Keeping Sugars
Date
of
Anal-
ysis
May
1915
Polari-
zation
96.15
94.85
95.85
95.55
Water Sucrose
(W) (S)
Per by Clerget
cent Per cent
1.25 96.39
1.65 95.18
1.18 96.34
1.31 95.82
Invert
Sugar
Per
cent
0.91
1.22
1.13
0.86
Undeter
Ash mined
Per Per
cent cent
0.47 0.98
0.62 1.33
0.56 0.79
0.70 1.31
W
ido-s
0.346
0.343
0.322
0.313
Average
95.60
1.35
95.93
1.03
0.59
1.10
0.331
October A
1915 B
C
D
95.55
94.35
95.15
94.65
1.27
1.65
1.09
1.41
95.75
94.70
95.54
95.09
1.61
2.01
2.04
1.83
0.45
0.61
0.54
0.65
0.92
1.03
0.79
1.02
0.298
0.311
0.244
0.287
Average
94.93
1.35
95.27
l.§7
0.56
0.95
0.285
January A
1916 B
C
D
95.55
94.10
94.95
94.55
1.34
1.55
1.12
1.39
95.92
94.65
95.59
95.10
1.64
2.12
2.02
1.90
0.46
0.61
0.55
0.67
0.64
1.07
0.72
0.94
0.328
0.289
0.254
0.284
Average
94.79
1.35
95.31
1.92
0.57
0.85
0.288
August A
1917 B
C
D
94.30
93.10
93.85
93.05
1.40
1.58
1.23
1.59
94.61
93.72
94.80
94.06
2.30
2.61
2.65
2.69
0.43
0.67
0.57
0.68
1.26
1.42
0.75
0.98
0.260
0.252
0.237
0.268
Average 93.58 1.45 94.30 2.56 0.59 1.10 0.254
The results obtained upon the four samples which
did not deteriorate are given in Table II. As there
was but little change in composition only two of the
periods are given.
The results indicate that the limiting factor for good-
W
keeping is about - = 0.3.
100 — o
Anyone who has studied the keeping quality of
sugars can no doubt report numerous exceptions to
such a rule as the above. Examples can be cited of
sugars with a factor far beyond the limit for safe-keeping
which keep perfectly well and of sugars with a factor
well within the safety limit which deteriorate rapidly.
The exceptions of the first class need not detain us long
Table II — Periodic Analyses of Good-Keeping Sugars
Sucrose
(S)
Date Water by Invert Undeter-
of (W) Clerget Sugar Ash mined _,
Anal- Polari- Per Per Per Per Per w
ysis Sample zation cent cent cent cent cent 100 — S
May E 96.70 0.88 96.96 0.66 0.55 0.95 0 289
1915 F 96.15 1.02 96.42 1.40 0.50 0.66 0.285
G 96.35 0.94 96.53 0.92 0.78 0.83 0.271
H 96.45 0.81 96.80 1.05 0.51 0.83 0.253
AVBRAGB 96.41 0.91 96.68
January E 96.75 0.85 97.12
1916 P 96.15 0.99 96.71
G 96.05 0.92 96.37
11 96.45 0.75 96.98
1.01 0.59 0.82 0.274
0.65 0.53 0.85 0.295
1.12 0.50 0.68 0.300
0.94 0.79 0.98 0.253
1.05 0.50 0.72 0.248
for the probabilities in the case of moist sugars which
keep are that the organisms which produce deteriora-
tion are either absent or that the conditions of tem-
perature, alkalinity, etc., are unfavorable for their
development.
INFLUENCE OF TEMPERATURE UPON DETERIORATION
The author has noted moist sugars which kept perfectly
well in the climate of New York from October to May.
The organisms producing deterioration, however, were
present and with the approach of warm weather in
May, the conditions became favorable for their develop-
ment and the sugars suddenly began to undergo a rapid
decrease in polarization. As an example of such an
influence of temperature upon deterioration the follow-
ing analyses are given of a soft refined sugar with high
factor.
Polari-
zation
94.35
94.35
92.70
Moisture
Per cent
3.90
i!67
Sucrose
by Clerget
Per cent
94.42
94.42
93.10
w
March 18
June 10
100 — s
0.699
0.590
Average 96.35 0.88 96.80 0.94 0.58 0.81 0.275
In the cool season between January and March there
was no deterioration, but sometime between March
and June a very rapid destruction of sucrose began.
Cool weather may not only retard the commence-
ment of deterioration, but it may also check the pro-
cess after it has once begun. This can be seen from
Table I, which shows an average loss of 0.66 per cent
sucrose between May and October of 191 5. In January
1 916 the sucrose had undergone no further diminution
and the process of deterioration had apparently come
to a standstill. But the organisms producing the de-
struction of sucrose resumed their activity in the fol-
lowing summers so that we find in August 1917a further
loss of 1. 00 per cent sucrose. A correlation of analytical
and meteorological data shows that the destruction of
cane sugars by microorganisms does not usually take
place until the daily maximum temperature exceeds
20° C, which for the climate of New York is from about
the middle of May to the first of October. Raw cane
sugars of any class can be stored without serious risk
when the maximum temperature in the warehouse is
below 20° C. But if sugars are to be kept for the season
when the temperature maximum exceeds 200 C, then
only such sugars should be selected as have a factor of
safety below 0.3.
DETERIORATION WITHOUT LOSS IN POLARIZATION
Attention should be called at this point to a condition
of not infrequent occurrence, where a sugar during
storage in a warehouse undergoes no loss in polariza-
tion and yet is steadily deteriorating. This circum-
stance arises from the fact that the sugar during storage
is losing moisture and that the loss in polarization from
destruction of sucrose is counterbalanced by the drying
out of the product. The custom of making spot tests
from time to time in order to see if stored sugar is hold-
ing up is therefore of little value unless such polariza-
tions are controlled by moisture or invert sugar deter-
minations. The author has found the periodic analysis
of sealed samples to be a most useful criterion of what
is taking place in the warehouse. He has had excellent
opportunity of making such comparisons in connection
with the analysis of sugars for the New York Coffee
Exchange where the same lots of sugar in the warehouse
180 THE JOURNAL OF INDUSTRIAL
are resampled and retested with every change of owner-
ship. In every case where sugars in the sealed bottle
lost in polarization, deterioration was observed in the
stored sugar. Although the polarization of the latter
frequently showed no falling off, yet deterioration was
advancing as was indicated by the steady increase in
invert sugar.
The case of Sugar B in Table I is an illustration of this.
This sugar was part of a large lot that was stored in a
New York warehouse in May 1915. A sample taken
from the bags in the warehouse the following October
polarized 94.80 as compared with 94.85 when the sugar
was stored. This was taken by the owner as an evi-
dence that the sugar was undergoing no deterioration,
although a sealed sample of this sugar, kept from the
previous May, polarized only 94.35. A complete
analysis of the October warehouse sample showed,
however, that inversion was taking place.
Sucrose
(S)
Water by Invert Undeter-
(W) Clerget Sugar Ash mined „.
Polari- Per Per Per Per Per w
zation cent cent cent cent cent 100 — S
Sealed Sample. May 94.85 1.65 95.18 1.22 0.62 1.33 0.343
Sealed Sample. Oct 94.35 1.65 94.70 2.01 0.61 1.03 0.311
Warehouse Sample. Oct.. 94.80 1.21 95.19 1.76 0.66 1.18 0.251
The October warehouse sample shows an increase
of 0.54 per cent invert sugar: deterioration is thus plainly
indicated, but is concealed, when only a polarization or
sucrose determination is made, owing to the loss of
0.44 per cent water through drying out of the sugar.
Shrinkage in weight, without the attendant increase
in test, caused the owner of the sugar a considerable
financial loss.
uneven distribution of moisture — The exceptions
of the second class, where sugars of low factor deterio-
rate, are usually found upon examination to confirm
rather than to nullify the factor-of-safety rule. The
deterioration of a raw sugar is confined entirely to
the thin films of molasses which adhere to the crystals
of sucrose. The cases of low-moisture sugars which
deteriorate result nearly always from uneven distribu-
tion of moisture; the average percentage of moisture
is low but there are zones of sugar in the bag whose
percentage of moisture is relatively high. Uneven
distribution of moisture in the bag may result from
mixing together sugars of varying moisture content
at the factory, but it seems to be produced more com-
monly by the migration of moisture after the sugar is
bagged, with the result that the liquid films become
more concentrated on some grains of sucrose and more
dilute upon others. Fermentation will then set in
where the films are more dilute, the result being that
the average mixed sample of the lot shows deteriora-
tion, although the average moisture content may ap-
pear to be well within the limit for good keeping.
su 1 \iing — The sweating of raw sugar due to warm
packing or to unfavorable storage conditions is one of
the chief causes of moisture migration. The danger
of bagging sugar as soon as it is emptied from the centrif-
ugals has long been recognized. It is very evident
that when warm sugar is packed in a bag, there will be
an expulsion of water from the center towards the cooler
surface. Zones of high moisture content are formed
AND ENGINEERING CHEMISTRY Vol. 10. Xo. j
which, with the favoring warmth from the interior of
the bag, become exceedingly favorable for the develop-
ment of microorganisms. An examination of such
sugars when the bags are opened shows that deteriora-
tion is not evenly distributed but is confined to zones,
the polarization of sugar from different parts of the
bag showing variations sometimes of several per cent.
If such sugar be imperfectly mixed, extremely wide
variations may be noted in the composition of duplicate
samples. The following is an actual case of three
samples of a deteriorated sugar taken from the same
mix, drawn from 2420 bags of one mark in a Xew York
warehouse in December 1910.
Polarization Moisture
Sample No. 1 92 . 75 1 . 80
Sample No. 2 93.65 1.46
Sample No. 3 94.50 1.18
Migration of moisture may take place not only within
the bag but may proceed from one bag to another.
In the case of sweat-damaged sugars in the hold of a
ship or in a warehouse, the moisture from the lower
tiers may condense upon the ceiling overhead and fall
back in a shower upon the upper layer of sacks. A care-
ful manufacturer, who makes sugars that conform to
the rules of safe keeping, may thus have his product
deteriorate through the negligence of other people.
deductions from the "factor-of-safety"' rule —
If a fixed ratio between moisture and non-sucrose is
the governing factor in the keeping quality of raw
cane sugars, there are a number of deductions or corol-
laries which must follow from such a proposition.
The first corollary which we will consider is that
slight fluctuations in moisture content have a much
greater influence upon the keeping quality of high-grade
than of low-grade sugars. Thus o.i per cent increase
in moisture will raise the factor of a 900 sugar with
0.28 per cent moisture from 0.2S to 0.35, but will
raise the factor of a 900 sugar of 2.80 per cent moisture
from 0.28 to only 0.29. In other words, a high-grade
sugar of good-keeping quality can be made unfit for
storage by the absorption of only 0.1 per cent moisture,
while the keeping quality of a low-grade sugar
having the same factor will not be sensibly affected.
This conclusion is abundantly confirmed not only by
laboratory tests but by practical experience. The
storage of high-grade raw sugars or of moist refined
sugars has always been regarded as hazardous. Even
white granulated sugar has been found to deteriorate
in a humid atmosphere, owing to the absorption of
moisture. Low purity sugars, on the other hand, can
be subjected to considerable variations in moisture
content without loss of keeping quality.
A second deduction, which results from the factor-of-
safety rule. is that displacement or saturation of moisture
by non-sucrose constituents should render a question-
able sugar fit for storage. This conclusion has also
been confirmed by practical experience. It is cus-
tomary with some factories to wash the sugars in the
centrifugals with low-grade molasses instead of with
water. A superintendent, who had long followed
molasses washing, upon being asked why he did this
replied that sugars thus treated never went back in
Mar., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
181
storage. This superintendent, who knew and cared
nothing about "factors-of-safety," was yet unconsciously
making a practical application of the rule.
limit of deterioration — A third corollary, to which
the author called attention a few years ago, is that
sugars which are prevented from absorbing moisture,
as in a sealed container, can deteriorate only to a cer-
tain limit. In other words deterioration will continue
W
until the quantity becomes less than 0.3
100 — b
when the process must come automatically to a stand-
still. This deduction has been repeatedly confirmed
by making periodic analyses of deteriorating samples
that were contained in sealed bottles. The deteriora-
tion, after a few months or years, depending upon the
moisture content of the sample, came gradually to a
stop and subsequent analyses, even after several years,
showed no change in composition. The value of
W
— — at which a deteriorating sugar ceased to lose
100 — S
in polarization was found usually to be nearer 0.25
than 0.30. This would seem to indicate that although
the destructive organisms might not multiply under
conditions when the safety factor was 0.3, yet if a suf-
ficient mimber of organisms were already present in a
state of great activity they might continue for a time
to exert an inverting action upon the sucrose dissolved
in the liquid films.
It will be noted, for example, in Table I that the
average factor of 0.331 in May 1915, after remaining
the following winter at 0.288, underwent a further de-
crease to 0.254. The average factor of 16 sugars at
the end of deterioration, determined by the writer1
in 1914, was 0.251.
The fact that a sugar in an active state of deteriora-
tion may continue to undergo inversion, even though
its factor of safety be under 0.3, helps to explain why
many sugars of apparently good keeping quality fail
to hold up. A sugar may have been made with a
factor of 0.33 and, beginning at once to deteriorate,
have had a factor of 0.29 at the time of its arrival in
New York. The purchaser of this sugar, unaware
of previous conditions, might therefore be misled as
to its keeping quality, for the sugar being in an active
state of fermentation had not yet reached the limit of
deterioration.
That there is a certain limit of deterioration has been
intimated by previous investigators. L. Lewton-
Brain and Noel Deerr2 make the following statement:
"Another point of interest that requires further in-
vestigation is whether there is a definite maximum of
deterioration for each bacillus, for each percentage of
water or whether the deterioration will go on indefinitely
merely varying in rapidity according to temperature
and moisture conditions. The probability is that it
will go on indefinitely, but there is also a possibility
that an accumulation of by-products might inhibit
further activity when a certain point has been reached."
Samples," Louisiana Planter,
1 "The Deterioration of Raw Suga
»«, 282.
1 Hawaiian Sugar Planters' Associatio
» (1909), 32-3.
Division of Pathology, Bulletin
In answer to a letter requesting his present opinion
upon the subject, Mr. Deerr makes the following ad-
ditional statement:
"I now think there is a final maximum of deteriora-
tion for a percentage of water, but if the sugar is free
to absorb water, deterioration will continue to far
limits. If the sugar is in a stoppered bottle, I think
the deterioration is limited."
This opinion of Mr. Deerr coincides with the results of
the author's experience.
In 1 91 5 the writer1 suggested the explanation that
the limit of deterioration in a sealed sample was reached
when the liquid films were saturated with non-sucrose
ingredients, at which limit "the dissolved sucrose is
practically all inverted and no more sucrose can pass
into solution from the underlying crystal." Subse-
quent studies of the liquid films at the end-point of
deterioration show them, however, to contain a con-
siderable amount of uninverted sucrose. Experiments
made to reproduce the conditions in a deteriorating
sugar by coating fine glass beads with films of a molasses
undergoing deterioration likewise showed that all the
sucrose could not be destroyed under such conditions.
Unless, therefore, a sugar can absorb moisture from
the outside or produce moisture during fermentation,
deterioration never destroys the whole of the sucrose
originally present in the liquid films.
The possibility, suggested by Lewton- Brain and
Deerr, that an accumulation of by-products may in-
hibit the activity of the organisms which produce de-
terioration, derives considerable support from the fact
that after a few years fermented samples of sugar in
many cases fail to produce colonies upon agar or gela-
tine plates. It was only in cases where deterioration
was produced by organisms which formed resistant
spores or where water seemed to be formed as a fermen-
tation by-product that the author was able to obtain
colonies from old fermented sugars. The death of the
organisms in old sugars may be due to the formation
of substances actually toxic or to a concentration of
invert sugar which by its plasmolytic action2 causes
the destruction of life.
abnormal fermentations — Over 90 per cent of
the cases of deterioration of sugars studied by the author
correspond to the examples given in Table I, in which
the polarization and sucrose regularly diminish and
the invert sugar increases until the limit of deteriora-
tion is reached, the percentage of moisture remaining
practically constant throughout. A number of cases
have been noted, however, in which the fermentation
followed a different course. In some instances an
increase in polarization was observed which might
afterwards be followed by a progressive decrease in
test. Examples of this type of fermentation have been
1 "The Deterioration of Raw Sugar Samples," Louisiana Planter,
64 (1915), 281-2.
1 Prof. W I., nwen, Hactcriologist of the Louisiana Sugar experiment
Station, iu ■ recent conversation with the author, suggest! thai the degree
of osmotic pressure necessary to produce plasmolysis In the cells of the or-
ganisms which inhabit the sirupy films, may represent the limit to which
deteriorate. Osmotic pressure may. perhaps, ha the DftSi ol
i82 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, Xo. 3
previously reported by Watts and Tempany1 in the partly to some experimental error and partly to the
West Indies, by Deerr and Norris2 in Hawaii, and by formation of alcohols, esters, or other volatile products.
other observers. The increase in water, or volatile matter, seems to be
increase of polarization in abnormal fermenta- associated in some way with this type of fermentation.
tions — An initial increase in the polarization of stored As another example the following case of a Cuban
sugars is usually due to a partial drying out of the prod- sugar is given. Four jars of the well-mixed sample
uct. This increase, however, may take place without were filled and hermetically sealed in April 1015.
the sugar losing moisture, in which case there must be Periodic analyses of the samples showed the following:
either a production of some new dextrorotatory sub-
stance such as dextran or a destruction of some levo- "(sT*
rotatory constituent of the sugar such as fructose. The ™$? cl^get £„££' Ash v^"~
author3 has studied the production of dextran in fer- Date of Poiari- Per Per Per Per Per _w_
^ Analysis zation cent cent cent cent cent 100 — S
menting sugar-cane juice but has not been able to ob- Apr. 6. 1915 96. 00 1.14 96.43 1.17 o.si 0.75 0.316
serve its formation in raw sugars in any instance among ^^i.' i9i\6. '.'.'.'. li'.sl \'.l\ ls.47 o!87 o.si list oJ-JS
the several hundred cases of deterioration which he
has investigated. It seems more probable that the But little change is noted between the April and
increase in polarization of stored sugars, where loss of January tests. The August 19 17 analysis, however,
moisture does not occur, is due to the fermentation of shows an increase of 0.37 per cent in water, or volatile
fructose as suggested by Watts and Tempany.4 The matter, a decrease of 0.30 per cent in invert sugar, a
destruction of reducing sugars in stored samples of decrease of 0.15 in polarization, and a decrease of 0.96
sugar is in fact not unusual. per cent in sucrose. In the case of the first two tests
Watts and Tempany4 report an instance where a the Clerget value is higher than the polarization, while
muscovado sugar between May 6 and June 21 under- ;n the August analysis it is lower, as is usually the case
went a decrease in reducing sugars from 3.58 per cent wjth this type of fermentation. The undetermined
to 0.65 per cent and an increase in polarization from matter shows a marked increase, as does also the factor*
. 88.8 to 91.0. Deerr and Norris4 also report the case of 0f safety.
a sugar which, after four months storage, underwent a The fact that a raw sugar can underg0 a serious loss
decrease in reducing sugars from 1.65 to 0.22 per cent jQ Us sucrose content with but little change in polariza-
and an increase in polarization from 93.7 to 95.2. ti()n is only an additional miration of the inadequacy
In a case observed by the author a sugar on June of afl uncontrolled polariscope test,
m, iois, polarized 94.0s and contained 1.90 per cent
. v J ' r a t VOLATILE DECOMPOSITION PRODUCTS OF STORED
invert sugar and 1.54 per cent water; on January 10,
, ,. . , - .. i- , u j sugars. Alcohols and Esters — As shown by lable
1916, a duplicate sample of the same sugar, which had ... , .,, , , . . .. c
, ', • ,, , j 1 • ■. j 4. • j I the chief chemical change in the deterioration of
been hermetically sealed, polarized 95.55 and contained . . . °
, „ sugars is the inversion of a part of the sucrose. \\ ltn
0.89 per cent invert sugar and 1.73 per cent water. One , , , ,
, . , ., . .. c C an average loss of 1.63 per cent sucrose there was an
part of fructose conceals the rotation ot 1.4 parts of b . . . . ;
„ ... ., . ., , c average gain ot 1.53 per cent invert sugar wmen is
sucrose, and if we assume that the loss of 1.01 per cent , „ , V , .,_,.. ,
, , . . .. , , ., only 0.18 per cent below the theoretical. 1 his unknown
invert sugar was due to fermentation ot fructose there , c
, , , . . , ■ .. r t.- u loss may be taken as the average amount 01 sucrose
should be an increase in polarization of 1.41, which J . ., , , , j ...
,.,„..,.. u a converted into gums, acids, alcohols, esters, and other
agrees fairly well with the 1.5 increase observed. " ' '.
fermentation products. The inversion of 1.03 per
abnormal clerget values— If the fructose be fer- cent sucrose involves the loss of 0 o8 per cent water;
mented away from a mixture of sucrose and invert thg resu]ts of Table T however show an average in.
sugar, the residue of sucrose and glucose should give cfease q{ qiq pef cent water> Qr yolatile mattefj SQ that
a Clerget value lower than the direct polarization in- the unknown loss of 0 l8 per cent must consist alrn0st
stead of higher as is usually the case. The above whoUy q{ vo,atile constituents. The quantity of sam-
sample which polarized 95-55 gave a Clerget value of pks wag nQt suffident to determine whether the latter
95.26. An independent analysis, performed at the werg of an a,coholj aldehyde or add nature Xearly
author's request by Mr. A. H. Bryan, gave a polar.za- ^ the sampleSj upon opening, off a perceptible
tion of 95-60 and a Clerget value of 9536. The re- rum.Uke odor) so that u seems safe to assume that
suits indicate a destruction of fructose in this sample alcohols and esters make up a certain part o{ the vola.
by fermentation. tile decomposition products of stored sugars. The
formation of water (volatile matter) in ab- strong odor of esters, which is noticed upon entering a
normal fermentations — In the case of abnormal fer- warehouse or the hold of a ship, where raw sugar is
mentation previously cited, the water, or volatile stored, is sometimes regarded as an evidence of deteriora-
matter, increased from 1.54 per cent to 1.73 per cent. tion, but this is not necessarily the case. Sealed samples
This difference of 0.19 per cent may have been due 0f raw sugar may develop an intense rum-like odor with-
1 "Fermentation Changes Occurring iu Muscovado Sugars," West out showing the slightest loss in SUCrOSe.
Indian Bulletin No. II, 7 (1906). 226-36. n , n ■ ■• ™. , .-, , „j..^
• "The Deterioration of Sugars on Storage." Experiment Station of Carbotl DtOXtJc 1 he Volatile decomposition product
the Hawaiian Sugar Planters' Association, Bulletin 24. which is given off ill greatest quantity by Stored sugars
i "The Fermentation of Sugar Cane Products." J. Am. Chem. Soc., jg car^on dioxide. This gas seems always to be prO-
28, 45.^-469. , , . ., . .. * , . j . .
t Loc cil duced, whether or not the sugar is undergoing deteno-
Mar., 191!
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
183
ration. While the quantity of carbon dioxide in sealed
bottles of raw sugars is usually highest where the loss
of sucrose is greatest, this is not always true. In the
case of six samples of raw sugar which had undergone
deterioration the carbon dioxide content of the air in
the bottle after two years was found to be 625, 274,
31O1 33i I02 and 494 times the amount present in the
laboratory air. In the case of five samples of raw sugar
which had undergone no loss in sucrose similar figures
for carbon dioxide after one year were 226, 51, 26,
171 and 309.
In several instances where the air was drawn off from
bottles of deteriorating sugar the oxygen was found to
be almost completely displaced by carbon dioxide. It
was thought at first that the exhaustion of the oxygen
supply might be the cause of the death of the organisms
in the old samples of sugar but this condition of oxygen
exhaustion was observed in only a few cases and there
seemed to be no connection between the phenomenon
and the limit of deterioration. In the case of a soft
refined sugar undergoing deterioration the oxygen of
the air in the bottle was 91 per cent consumed after 8
months and 95 per cent consumed after 19 months.
The number of microorganisms per gram after 19
months was 550,000 and the sugar was still undergoing
inversion. The evolution of carbon dioxide from sugar
in the hold of a ship is sometimes so great that work-
men have been overcome upon removing the hatches.
spontaneous combustion of sugars — The absorp-
tion of oxygen and the evolution of carbon dioxide by
a stored sugar resemble the process of respiration which
fruits, vegetables, grains, tobacco and other products
undergo in storage. Under certain unusual conditions,
which are not perfectly understood, this absorption
of oxygen may proceed with sufficient intensity to
cause spontaneous combustion of the product. There
are, in fact, well authenticated cases where this has
happened to sugar in bulk. Schone1 mentions an
instance where 1000 tons of raw beet sugar in a German
factory underwent spontaneous combustion with almost
explosive violence. Wasilieff2 also mentions a similar
occurrence with raw beet sugar in a Russian factory.
Many of the cases where cargoes of raw cane sugar have
mysteriously caught fire no doubt resulted from spon-
taneous combustion. Certain sugar-containing prod-
ucts, such as molasses feeds, are particularly susceptible
to this phenomenon.3 That the heating of a mass of
moist sugar is produced by yeasts or other organisms
is well known, but how these organisms can elevate
the temperature far above the point at which they can
exist has seemed a contradiction. It has been held by
some physiologists that in the fermentation of sugar to
alcohol or lactic acid, certain unsaturated intermediate
products are produced. In the interior of a fermenting
mass of sugar, when the supply of oxygen is used up,
these unstable unsaturated products may possibly be
formed in considerable amount. If outside air sud-
1 Deut. Zuckcrind.. 36 (1911). 608.
' Z. Ver. Zuckcrind., 1902, 864.
■ Report of the Chief Inspector. Hureau for the Safe Transportation of
Explosives, etc., IJ. IC. Report No. 7, p. 47, discusses the spontaneous com-
bustion of alfalfa-molasses mixtures. Spontaneous combustion of bagasse-
molasses feeds has occurred in ships.
denly gained access to the interior of such a mass, the
intense absorption of atmospheric oxygen might easily
elevate the temperature to the point of combustion.
The conditions of moisture, air supply, etc., which
favor the spontaneous combustion of sugars are, how-
ever, of very unusual occurrence, and the financial
losses from this cause are slight in comparison with
the slower and less spectacular process of inversion
which, after all has been said, is responsible for the
greater part of the losses from deterioration of the
Cuban crop.
B MYCOLOGICAL OBSERVATIONS
previous investigations — Since the time of the
first observation by Dubrunfaut, fifty years ago, various
writers have referred to the action of microorganisms
in producing the deterioration of sugars. It is only,
however, within the last twenty years that the specific
behavior of these organisms and the method of prevent-
ing their action upon sugars have been subjected to
serious study.
In 1898 Shorey1 detected the mould Penicillium
glaucum in samples of deteriorated Hawaiian sugars and
suggested that the inverting action of this fungus was
a common cause of deterioration. Shorey bel'.eved
infection to take place through spores drawn into the
sugar by the current of air in the centrifugals, and made
the observation that the sugars which showed most
deterioration were usually made in dusty localities
where such spores would be most easily scattered. As
a protection against infection Shorey recommended
that the sugar in the centrifugal, during the process of
curing, be sterilized by a current of dry steam.
In 1902 Greig-Smith and Steel2 in Australia discov-
ered a sugar-destroying organism, related to the heat-
resisting so-called "potato" bacilli, which was found to
occur in raw sugar from Australia, Java, Mauritius,
Egypt, Peru, Fiji, France, Germany and Russia. From
its conversion of sucrose into the levorotatory gum
levan, Greig-Smith and Steel named their organism
Bacillus levaniformans and from its wide distribution
expressed the belief that it, and not the mould of
Shorey. was "responsible for the bulk of the deteriora-
tion of sugar during transit and in store, which has been
noted from various parts of the world." As a remedy
against the infection of sugars by this organism, Greig-
Smith and Steel recommended thorough cleanliness
of apparatus at all stages of manufacture and steam
sterilization in the centrifugals.
In 1909 Lewton-Brain and Deerr3 made a study of
the "Bacterial Flora of Hawaiian Sugars" and came to
the same conclusion as Greig-Smith and Steel that
moulds are not to be considered as a cause of deteriora-
tion. Lewton-Brain and Deerr isolated five different
kinds of sugar-destroying bacteria, two of which pro-
duced a gum similar to levan: these authorities came,
therefore, to the conclusion that the production of
levan cannot be held as characteristic of one particular
> "The Deterioration of Raw Cane Sugar in Transit or Storage," J.
Soc. Chem. Ind., 17 (1898), 555.
» "I.evan: A New Bacterial Gum from Sugar," J. Soc. Chem. Ind.,
21 (1902), 1381.
• Experiment Station of the Hawaiian Sugar Planters' Assoc.. Division
of Pathology and Physiology, Bulletin 9.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, Xo. 3
bacterium. According to Lewton-Brain and Deerr
"the best safeguard against deterioration is the main-
tenance of the factory itself in as aseptic condition as
possible, the avoidance of the introduction of bacteria,
as for instance in the use of unclean water at or about
the centrifugals, and the disinfection of the factory
during the off season."
In 1911 Owen,1 in Louisiana, came to the conclusion
that the deterioration of sugars is not due to inversion
but to a gum fermentation which is formed by a slightly
alkaline reaction. This gum fermentation, according
to Owen, is produced by a group of bacteria, comprising
the so-called potato bacilli, that cause the destruction
of sucrose by an enzyme levanase,- which is extracellular
in its action and breaks down sucrose according to the
equation:
C12H22OH = CeHnOe + CsHioOs
Sucrose Glucose Levan
The potato bacilli, which occur widely distributed
in the soil, can easily be introduced into the sugar
factory by dirt adhering to the cane, and the great re-
sistance of the spores of these organisms to heat offers
a means of their passing through all the stages of manu-
facture into the sugar. Owen in fact showed by experi-
ments in Louisiana that while 98 per cent of the organ-
isms occurring in cane juice are destroyed in the process
of clarification, in no stage of the manufacture is the
product entirely free from microorganisms and that
there is a remaining 2 per cent of heat-resisting spores,
which escape destruction and find their way into the
final sugar. As a remedy against deterioration Owen
recommends the use of antiseptic washes for the mills
and tanks of the sugar house and the exercise of greater
care in drying the sugars.
While the observations of the authorities just men-
tioned may in large measure be true for the respective
countries where their work was performed, it has seemed
to the author entirely too sweeping to assert that the
deterioration of sugar is never due to moulds or that it
is nearly always produced by one specific bacillus or
specific class of bacilli. Table I, which is typical,
shows that the deterioration of Cuban sugars, at least,
is mainly a process of inversion and that the formation
of levan and other gums is not of usual occurrence. Ac-
cording to cultural experiments carried out by the author,
the organisms most prevalent in Cuban raw sugars are
not bacteria but certain organisms belonging to the
budding fungi. The occurrence of such fungi in de-
teriorating sugars has in fact been previously indicated
by Schone.
In a sample of "farine" (powdered sugar) which
had undergone a loss of nearly 8 per cent sucrose,
Schone' observed a large number of yeast-like cells
mixed together with the spores and mycelia of moulds.
The deterioration, in Schone's opinion, was started by
a budding fungus of the Monilia class and then con-
1 "The Bacterial Deterioration of Sugar." Louisiana Bulletin 125;
"A Recently Discovered Bacterial Decomposition of Sucrose,"1 This Joiknal .
3 (1911), 481.
1 It should he noted in passing that levan is a polysaccharide (C(HioO»)n
and, therefore, could not be formed from sucrose by the hydrolytic action
of any such enzyme,
1 "Garungserscheinungen in K.irinzuckern," Dcut. Zuckerind.. 33
(1908), 638.
tinued by the moulds. In a second sample of deterio-
rated "farine" Schone isolated another budding fungus
of the Torula class.
PRESENT INVESTIGATIONS
preparation of CULTURE media — In the experiments
performed by the author a medium was prepared by
boiling a 30 per cent solution of raw cane sugar of the
ordinary 96 ° type with a little salt-free alumina cream,
filtering, and diluting the cold filtrate to a concentra-
tion of 20 ° Brix. This stock raw sugar solution was
sterilized and kept, with the usual precautions against
infection, in a large flask.
The agar medium for plating was prepared by dis-
solving 15 g. of agar-agar in 1000 cc. of the stock raw
sugar solution in a sterilizer and filtering through a hot
water funnel. The sterilized agar medium was kept
in test tubes and flasks, with the usual precautions
against infection.
method of plating — i g. of raw sugar was dis-
solved in 10 cc. of sterile dist'lled water and 0.5 cc.
of the solution was mixed with 10 cc. of the agar me-
*-A*
Colonies of microorganisms from a Cuban raw sugar. The dark colonies
belong to Torula communis, which, although white, appear black by trans-
mitted light- The large light-colored globular masses belong to Bacterium
inverlens. In the lower left-hand corner is a gTowth of Monilia nigra.
dium, previously liquefied at about 35° C, and poured
into a warm petri dish. After the agar had set. the
petri dish was placed in an incubator at about 300 C.
At the end of three or four days the colonies were
counted and examined under the microscope. If the col-
onies were too numerous, a new plate was prepared from
a raw sugar solution of lower concentration. Typical
growths wore selected from the agar plates and inocu-
lated into measured amounts of the stock raw-sugar
solution in order to study the specific action of each
organism. The behavior of the latter was also tested
upon concentrated raw sugar syrups and upon sterile
sugars. It is not possible in a chemical paper to give
in detail the results of all experiments and only a few
of the more typical observations are described.
number OF organisms — The average number of
colonies produced upon raw sugar-agar plates by the
method just described was 144.000 per gram for Cuban
sugars as delivered in Now York, the number varying
Mar., 1018
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
185
(from 3,500 to 571,000. During storage this number of
organisms might increase for a time if the sugar was
in a state of deterioration, and samples have been
noted which produced over 1,000,000 colonies per gram
of sugar. On very long storage, however, the number
of microorganisms undergoes a decrease; samples of
raw sugar after two years are frequently found to be
almost sterile.
An example of the colonies obtained from 0.05 g.
of a Cuban raw sugar upon an agar plate is shown in
Fig. 1.
kinds of microorganisms. Torula communis —
The most abundant organism observed in Cuban raw
sugars was a non-inverting Torula. A similar organism
was also found in raw sugars from the British West
Indies and in soft refined sugars. It appears to be one
of the most widely distributed of the microscopic flora
which thrive in cane sugar factories, and for this reason
has been named by the author Torula communis.1
Fig. 2X2
Colonies of Torula communis in different stages of growth. On the left
■is a small star-shaped cyst, the nucleus of the future colony; above it are
two colonies forming around their nuclear cysts. The large circles are fully
.developed colonies. The colonies are white but appear black by trans-
mitted light.
form of colonies — The colonies upon raw sugar-
.agar at the beginning have the appearance of minute
white cysts which under the microscope show an
angular contour of boat-shape or arrow-head form.
'The cysts increase in size to a diameter of 0.2—0.5 mm.
until the surface of the agar is reached, when the or-
ganisms spread out in all directions from the point of
emergence. The colony gradually assumes a circular
or heart-shaped form of grayish white color, varying in
diameter from 3 to 10 mm. and retaining the
original cyst as a dense white nucleus (Fig. 2). With
very old colonies a brownish color appears.
microscopic appearance — Under a high power of
the microscope Torula communis is seen to consist of
single cells, yeast-like in appearance and without
mycelium (Fig. 3).
1 Owen (.Louisiana Planter, 56, 173) mentions imone the microftrganisms
of unrefined sugars a non-inverting Torula, which is no doubt the same or-
ganism as the one described by the author as Torula communis. The specific
names, communis, nigra, fusca, etc.. employed by the author in this and
the following cases are used provisionally until the exact relationship of
the organisms to their genera can be determined.
growth in raw sugar solutions — Torula communis
grows readily in raw cane-sugar solutions from the most
dilute to the most concentrated. It forms a granular
sediment of cells and, at later stages of growth, a thin
Fig. 3 X 1000
Magnified cells of Torula c
marginal film. A slight evolution of gas takes place,
but never with froth or foam as with yeast. A strong,
fruity, ester-like odor is also characteristic.
action upon raw sugar solutions — The action of
Torula communis upon raw cane-sugar solutions con-
sists principally in a destruction of invert sugar, fruc-
tose being the ingredient mostly affected. Sucrose
is not inverted. The following fermentation experi-
ment upon 50 cc. of a solution of 64 ° Brix was con-
ducted for 21 days at 28 ° C.
Solution
Diluted to 200 Cc.
Polarization Clerget Value
Blank +76.60 76.78
Torula communis.. +76.85 76.56
Original 50 Cc.
Solution Contains
Sucrose Invert Sugar
Grams Gram
39.9256 0.8085
39.8112 0.2338
In the above experiment the blank solution lost
0.3458 g. in weight and the rorw/a-inoculated solution
0.7535 g-> the difference of 0.4077 g. representing the
loss due to evolution of carbon dioxide and other
volatile products.
A second fermentation experiment was conducted
upon 50 cc. of a clarified supersaturated raw sugar solu-
tion of 780 Brix for 27 days at 30° C. The excess of
sucrose crystallized out during the experiment, leaving
a solution of about 69 ° Brix.
Solution
Diluted to 200 Cc.
Polarization Clerget Value
Blank +98.70 98.86
Torula communis.. +98.95 98.27
Original 50 Cc.
Solution Contains
Sucrose Invert Sugar
Grams Grams
51.4072 1.1576
51.1104 0.1462
In the s-econd experiment the loss due to evolution
of carbon dioxide, alcohols, esters, etc., after correcting
for the loss in weight of the blank solution, was
0.6118 g. The distribution of this loss over the 27-day
period is shown in the following diagram. It will be
10
I
t
Bays
seen that the greatest intensity of fermentation was
between the gth and 15th days.
The two experiments show a marked destruction of
invert sugar. The selective action of Torula communis
upon fructose is seen by the increase in polarization and
— — - -
*» — — — -^^
/ ^*Si *.
/L =-.
? 10 20 30
i86
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 3
by the lowering of the Clerget value below the polari-
zation. The changes of this character, previously
noted in the case of certain stored sugars, are no doubt
due to this organism.
The inability to invert sucrose is characteristic of
many Torulac,1 although such inability does not pre-
vent these varieties from subsisting at the expense of
sucrose. A destructive action of this kind is shown in
the previous results, where there was a loss of o. 1144
g. sucrose in the first experiment and a loss of 0.2968 g.
sucrose in the second. The experiments show how a
raw sugar may gain in polarization and yet undergo
an actual loss in sucrose.
Although relatively harmless, in comparison with
the organisms which invert sucrose, the non-inverting
Torulae may become deleterious in the case of sugar
stored for a considerable period.
Among the most destructive organisms found by the
author in Cuban raw sugars were two varieties of
Moniliae, which from the difference in color of their
colonies upon agar have been named Monilia nigra and
Monilia fusca.
Fig. 4X2
Large colonies of Monilia nigra. The radiating growths consist of
hyphae covered with bud-cells. The tufted terminal growths are conidia.
Monilia nigra — Some of the raw sugars examined
by the author, when plated out, gave practically pure
cultures of this organism. In the case of one fermented
sample (A, Table I) which had been sealed over two
years, 1500 colonies of this Monilia were produced
from 1 g. of sugar (Fig. 4).
form of colonies — The colonies upon raw sugar-
agar have at first the appearance of small star-shaped
white dots, which under the microscope are seen to
consist of radial hyphae. The latter throw off a con-
glomerate of bud-cells, the mass of which increasing in
thickness soon gives the colony a starfish appearance.
This primary growth of the colony is usually succeeded
by a secondary growth, due to the propagation of the
bud-cells, which, without the formation of hyphae,
germinate like yeast and cover the center of the colony
with a white amoeba-like film. When the colony at-
1 For further particulars as to the action of the Torulaceae upon sucrose
and other sugars see Lafar's Ttchnische Mykologie. i (1907), 717. or Salter's
Translation, 3 (1911), 296.
tains a diameter varying from i mm. to 15 mm. the
ends of the hyphae projecting beyond the bud-cell
conglomerate and yeast films usually break up into
clusters of dark conidia (frequently of branched tree-
like form) which give the colony a jet-black color.
r -
# # *
Fig. 5X2
Small colonies of Monilia nigra
stages of growth.
From the latter circumstance the organism has been
named Monilia nigra. Sometimes the colony stops
growing before the conidia stage is reached, in which
case the white color remains unchanged. The latter
is particularly apt to occur when the colonies are so
numerous as to coalesce; the surface of the agar may
then be covered with a dense white growth of bud-cells
which at first glance might be mistaken for yeast
colonies. Variations in composition of the agar and
in temperature of incubation cause such difference in
the shape and appearance of the colonies that the latter
s
Fig. 6 X 50
Magnified colony 'of Monilia nigra. The radiating growths consist of
hyphae, covered with bud-cells. The black terminal growths are conidia.
The secondary growth of bud-cells forms the circular film.
might appear due to different organisms. The ap-
pearance of the colonies is shown in Figs. 4, 5 and 6.
microscopic appearance — The polymorphic charac-
teristics of Monilia nigra are also shown under the
microscope. The hyphae are sometimes smooth, of
Mar., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
187
the ordinary branched type, but are more often studded
with clusters of bud-cells. The latter are irregularly
elliptical in shape and when detached, depending upon
conditions, produce new hyphae or propagate like yeast.
When the mycelium approaches its maximum growth
the hyphae begin to break up at the ends into dark
thick-walled conidia. The latter often occur as twin
spores in which case they are produced by a process of
cell division. The disintegration of the hyphae into
thick-walled cells may also occur at other points than
the ends in which case they often have the appearance
of oidia. The various cell forms of Monilia nigra con-
tain large numbers of oil globules. The microscopic
appearance of the various cells is shown in Fig. 7.
growth in raw sugar solutions — M onilia nigra
grows readily in raw cane sugar solutions excepting the
most concentrated. The solution becomes turbid with
a growth of fibrous mycelia while the walls of the flask
about 2 mm. above the liquid often become coated,
after several days, with a margin of dark conidia 1 cm.
or more in width. There is a very slight formation of
gas; a mild, ester-like odor is also perceptible.
Fig. 7 X 500
Magnified cells of Monilia nigra. Below is the end of one of the hyphae,
covered with bud-cells and terminating in a cluster of dark conidia. Above
are a number of bud-cells germinating into a film.
action upon raw sugar solutions — The action of
Monilia nigra upon raw cane-sugar solutions consists
principally in an inversion of sucrose. The following
fermentation experiment upon 50 cc. of a solution of
210 Brix was conducted for three weeks at 28° C.
Solution
Diluted to 100 Cc.
Polarization Clerget Valu
Blank +40.55 40.94
Momlia nigra 4- 7.15 15.54
Original 50 Cc.
Solution Contains
Sucrose Invert Sugar
Grams Grams
10.6444 0.2952
4.0304 5.8965
Original 50 Co
Solution Contains
Sucrose Invert Su^a
A second fermentation experiment, conducted upon
50 cc. of a solution of 64 ° Brix for three weeks at 28° C.
showed the following results:
Solution
DlLUTBD TO 200 CC.
Polarization Clerget Value
Blank +76.60 76.78 39.9256 0.8085
Monilianigra +72.65 73.83 38.3916 2.1932
In the second fermentation experiment the solution
inoculated with Monilia nigra lost 0.0454 g. more in
weight than the blank, which shows only a very slight
evolution of carbon dioxide.
The experiments show that the inverting action of
Monilia nigra is considerably restrained by increasing
the concentration of sugar.
A third fermentation experiment was attempted with
a saturated raw sugar solution of 69 ° Brix, but the
organism was unable to thrive in 3 solution of this
concentration and no change in composition could be
detected after four weeks incubation at 30° C.
Fig. 8X2
: of Monilia fusca
stages of growth.
Monilia fusca — Besides the preceding form a second
more strongly inverting variety of Monilia has been
observed by the author in Cuban sugars. The colonies
upon raw sugar-agar (Figs. 8 and 9) resemble those of
Monilia nigra in some characteristics, but are distin-
guished from the latter by a much greater length of
hyphae, by a less pronounced tendency to form second-
ary yeast films, and by a greenish brown color in the
conidia stage instead of black. Owing to this differ-
ence in color the organism has been named Monilia
fusca. The principal microscopic features are shown
in Fig. 10.
growth in raw sugar solutions — Monilia fusca
grows in raw cane sugar solutions excepting the most
concentrated. The solutions become turbid and there
is a deposit of mycelia and cells. The walls of the
,»»,-*•"» v^Afci
,-v
Fig. 9 X 50
Magnified colony of Monilia fusca. The radiating hyphae arc covered
wiili bud iclls and dark conidia.
flask, to a distance of 3 cm. or more above the liquid,
become coated with a growth of dark conidia. There
is a very slight evolution of gas; a pronounced fruity
odor is also developed.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 3
action upon raw sugar solutions — The following
fermentation experiment upon 50 cc. of a solution of
210 Brix was conducted for three weeks at 280 C.
Solution
Diluted to 100 Cc.
Polarization Clerget Value
Blank +41.30 41.81
Monilia fusca +3.15 12.60
Original 50 Cc.
Solution Contains
Sucrose Invert Sugar
Grams Grams
10.8706 0.6368
3.2760 7.1869
A second fermentation experiment conducted upon
50 cc. of a solution of 64 ° Brix for three weeks at
280 C. showed the following results:
Solution
Dtluted to 200 Cc.
Polarization Clerget Value
Blank +76.60 76.78
Moniliafusca +43.75 52.01
Original 50 Cc.
Solution Contains
Sucrose Invert Sugar
Grams Grams
39.9256 0.8085
27.0452 10.9880
In the second fermentation experiment the solution
inoculated with Monilia fusca lost 0.0346 g. more in
weight than the blank, which shows only a very slight
evolution of carbon dioxide.
The experiments show that Monilia fusca has a much
stronger inverting action than Monilia nigra and that
the activity of the organism is less restrained by in-
creasing the concentration of sugar.
A third fermentation experiment was attempted with
a saturated raw sugar solution of 69 ° Brix, but the
organism was_unable to thrive in a solution of this con-
centration and no change in composition could be de-
tected after four weeks incubation at 300 C.
Fig. 10 X 500
Magnified cells of Monilia fusca. In the middle is a branched part of
the mycelium bearing 4 bud -cells; two of the latter (one germinating) are
shown at the left. At the right is the end of one of the hyphae, breaking
up at the end into 3 conidia and in the middle into 2 oidia.
The great variability of the Moniliae in habits of
growth renders them exceedingly adaptable to condi-
tions of environment, and for this reason they are to
be counted among the most destructive organisms
which thrive in raw sugars.
Bacterium invertens — In addition to the Torula
and Monilia forms just described, plate cultures of
Cuban raw sugars frequently exhibit a different type
of colony. The surface of the agar becomes covered
with an exudation of clear colorless drops (Fig. n)
which sometimes run together and cover a considerable
part of the plate. The organism producing this ap-
pearance is a bacterium which under the high power of
the microscope appears as rod-like cells, detached or in
chains, surrounded by a capsule (Fig. 12).
GROWTH IN RAW SUGAR SOLUTION — Bacterium in-
vertens grows best in raw cane sugar solutions of low
concentration. The solution acquires a milky turbid-
ity, a little sediment is formed and there is a slight
evolution of gas. A disagreeable putrid odor is also
perceptible.
action upon raw sugar solutioxs — The action of
the bacterium upon raw cane-sugar solutions consists for
the most part in an inversion of sucrose, from which
circumstance the organism has been named Bacterium
invertens. The following fermentation experiment upon
Colonies of Bacterium invertens
50 cc. of a solution of 2 1 ° Brix was conducted for three
weeks at 28° C.
Original 50 Cc.
Solution Solution Contains
Diluted to 100 Cc. Sucrose Invert Sugar
Polarization clerget Value Grams Grams
Blank +41.30 41.81 10.8706 0.6368
Bacterium invertens +22.30 27.53 7.1578 4.0862
A raw sugar solution of 64° Brix was inoculated with
Bacterium invertens and kept in an incubator for three
weeks at 280 C. The organism appeared unable to
thrive in a solution of this concentration. Xo percep-
tible change took place in the appearance of the medium
and an analysis at the end of the three weeks showed
no difference in composition from the blank.
The four microorganisms just described were the
most common forms observed by the author in Cuban
raw sugars. Other organisms, including moulds (such
as Penicillin in and Oideum) and various bacilli and
micrococci, were also detected in different sugars but a
description of these must be passed over. The con-
clusions which the author desires to emphasize are (1)
that the microorganisms of raw cane sugars, as re-
gards their action upon sucrose, are in part harmless
and in part destructive; (2) that
the destruction of sucrose in de-
teriorated sugar is not due to any
single organism or class of organisms;
moulds and budding fungi, as well
as bacteria, must be looked for, j.-IG 12 x 2000
when searching for the agents of Magnified cells of Bacu-
, . . . , . rium invertens.
destruction; and (3) that the tungi
and, bacteria, which cause the inversion of sucrose
in raw sugars, arc unable to thrive in saturated solutions.
The washing of raw sugars in the centrifugals, by dilut-
ing the saturated films of sirup to a point where the
inverting organisms can thrive, must therefore be re-
garded as a leading cause of deterioration.
Mar., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
ORIGIN OF THE INFECTION OF RAW SUGARS BY MICRO-
ORGANISMS— The opinions of various authorities upon
the infection of raw sugars from the air. from dirt
adhering to the cane, from contaminated wash water at
the centrifugals, from unclean tanks and unsanitary
factory conditions have already been mentioned. A
few other sources of infection remain to be considered.
infection from bagasse — Another possible source
of infection, to which attention has been lately directed,
is the contamination by fine bagasse particles (generally
called bagacillo from the Spanish diminutive) which
find their way, in greater or smaller amounts, from the
cane mills into the raw sugar. The contamination
may take place through the juice by reason of imperfect
filtration,1 or through the air by means of the wind.
According to Owen2 the only possible ways by which
bagacillo can affect the keeping quality of sugar are
Fig. 1J
Bottom of pile of sugar bags in a Cuban warehouse.
(1) by retaining microorganisms which would other-
wise be eliminated, (2) by providing nutritive material
for microorganisms, (3) by retaining moisturi
creating zones favorable for the growth of micro-
organisms. In Owen's opinion, whatever merit may
reside in the bagacillo theory is based solely upon the
retention of moisture.
The percentage of water-insoluble organic matter,
which consists mostly of bagasse particles, in Cuban
raw sugars was found from analyses made in the New
York Sugar Trade Laboratory to vary from 0.01 per
cent to 0.46 per rent, the average being 0.17 per cent.
The average per cent of water-insoluble organic matter
1 The possibility of deterioration of sugars resulting from infection by
bagacillo from high pressure mills through imperfect filtration is discussed
I". < . 111 1.. r . • . „,i Planter, 64, 348, and 66, 61.
« Louisiana Planter, 66, 174.
in sugars which deteriorated was found to be 0.22 per
cent, and in sugars which did not deteriorate 0.10 per
cent. In other words, the deteriorated sugars contained
twice as much water-insoluble organic matter as the
sound samples and this apparently would lend support
to the bagacillo theory of contamination. It seems
more probable, however, that bagacillo is not so much
the cause of deterioration as an indication of general
carelessness and sloppiness in manufacture. In other
words, if a superintendent is careless in his clarification
or filter-press work, he is probably equally careless about
protecting his sugars against infection or deterioration.
The washing of raw sugar in the centrifugals with water
from the cooling tower or other infected sources is
probably responsible for more losses than the introduc-
tion of bagasse particles. Without, denying the possi-
bility of bagacillo acting as a moisture carrier, it is
only necessary to point out the case of soft refined
sugars, the higher grades of which are exceedingly
subject to deterioration and yet are absolutely free
from bagacillo.
infection from the cooling tower — One of the
most dangerous sources of infection for raw cane sugars
is the cooling tower. In this contrivance the warm
condensation water from the factory is cooled by falling
in a shower over an outdoor framework into an ex-
posed basin, from which it is afterwards returned to
the factory. The cooling-tower water, which contains
any sugar lost by entrainment, is quickly invaded by
microorganisms, the conditions for infection and
growth being exceedingly favorable. The spray from
the cooling tower is not only carried into the factory,
where it can come into contact with bags and sugars,
but the cooling-tower water itself is sometimes used for
washing the sugars in the centrifugals.1 All things
considered, a more ideal source of infection than the
cooling tower can hardly be imagined.
infection from bags — Kamerling2 has suggested
that deterioration of sugars is produced by organisms
introduced from the bags. Although this idea has not
found general acceptance, much may be said in its
favor. While a mass of solid sugars offers more resist-
ance to the invasion of germs than does a liquid, the
sirupy films which surround the sucrose crystals are in
contact and form a continuous medium for the spread
of microorganisms. The ramifying mycelium of the
Moniliae also offers an easy means for this class of
organisms to penetrate to the interior of a sack of sugar.
Infection of bags may take place not only by welting
with spray from the cooling tower, but it may also occur
in the warehouse, or in the hold of a ship. Fig. 13
is a photograph of the bottom of a pile of sugar in a
Cuban warehouse. The dark discoloration upon the
floor consists of a slimy mass of fermenting molasses
and sugar dissolved from the bags by rain from a leaky
roof. The sugar in the bottom bags was in direct con-
tact with this filth and was in a bad stale of deteriora-
tion. Under such conditions infection might spread
' An instance in Hawaii where deterioration of the manufactured sugar
,i 10 the use of cooling-tower water for washing atthecen
, mentioned to the author by Mr. Noel I >■
1 International Sugar Journal, 3, 484. From Report of the West Java
periment Station "Kagok" for 1900.
190
/'///•. JOURNAL OF IS Dl STRIAL AND ENGINEERING CHE UISTRY Vol. io, No. 3
through a large pile of sugar. Fig. 14 shows the pile
of fermenting slime which had been raked up after
removing the bags of sugar.
PREVENTION OF THE DETERIORATION OF RAW CANE
sugars — In concluding the mycological part of this
paper a few words might be said about the means for
counteracting the destruction of sugar by micro-
organisms. In the matter of manufacture it is neces-
sary (1) to exercise the utmost possible cleanliness and
care in order to diminish infection, (2) to control the
moisture content of the sugar so that the ratio of non-
sucrose to water is within the limits of safety, (3) to
cool the sugar thoroughly before bagging to prevent
the migration of water and the formation of zones of
high moisture content. In the matter of storage it is
necessary (1) to keep the sugar perfectly dry in ware-
houses which are rain-proof, (2) to keep the warehouse
tightly closed in wet weather to prevent the sugar absorb-
ing moisture from the air, (3) to construct the warehouse
and store the sugar so as to secure in dry weather the
maximum ventilation underneath and between the bags.
Fro. 14
Pile of fermenting slime on floor of a sugar warehouse.
These precautions can be carried into effect with
comparatively little expense and would result in elim-
inating much of the needless loss which occurs at pres-
ent between the manufacture and refining of cane sugar.
ECONOMIC CONSIDERATIONS
Before concluding this paper upon the deterioration
of raw cane sugar there are several economic questions
which require discussion.
Inasmuch as there is always danger of raw sugars
becoming infected, no matter how extreme the condi-
tions of cleanliness in the factory may be, it is important
for the manufacturer always to make tin' moistu
tent of his sugars conform to the rules of safe-ko
If we accept t he formula W itei = 0.3 (100 — S) as
a requirement for safe-keeping, the moisture content of
different grades of raw sugars should not exceed the
following percentages:
Sucrose
Moisture
Sm-to.i'
Moisture
Sucrose
Moisture
er cent
Pel cent
Per cent
Per cent
Per cent
Per cent
99.9
0.03
96.0
1 20
90.0
.1.00
99.5
0.15
95 5
1 . is
89.0
1 ill
99.0
0.30
95.0
1.50
88.0
98.5
0.45
94.5
1.65
87.0
.1 90
98.0
0.60
94.0
1.80
86.0
4.20
97.5
0.75
9.1.0
2.10
B4.0
4.80
97.0
0.90
92 ,1
2.40
82.0
5.40
96.5
1.05
91.0
2.70
80.0
6.00
In order to see how near the manufacturing condi-
tions of Cuba conform to these requirements the fol-
lowing figures are given for the year 19 16.
Average polarization of sugar as sampled at New York 95.80
Average per cent moisture of sugar as sampled at New York 1 .35
The above per cent moisture, however, owing to dry-
ing out of sugar during transportation and during the
operations of sampling and mixing is about 0.3 lower
than when the sugar was made. As a conservative
estimate we may accept 1.5 per cent moisture and 95.65
polarization as the average condition of the sugar be-
tween manufacture and delivery. For raw cane sugar
of this polarization there is an average difference of
0.35 between polarization and sucrose content, which
would make the average condition of Cuba sugars be-
tween factory and refinery to be 96.00 per cent sucrose
and 1.50 per cent moisture. Sugar of this grade has
a safety-factor of 0.375 which is considerably above the
limit for safe-keeping. Such sugar, if stored for one
season, would deteriorate in New York to a factor of at
least 0.30 and in Cuba, where the climate is much
warmer, to a factor of 0.25. This would mean that the
average Cuban sugar of 96.00 per cent sucrose would
deteriorate if stored in New York for one year to 95.00,
and if stored in Cuba for one year to 94.00 per cent
sucrose.
The average amount of Cuban sugar stored in ware-
houses at any one time in 19 16 was 163,000 long tons
in the United States and 440,000 long tons in Cuba.
The average price of Cuban sugar per pound for 19 16 was
5.786 cents in the United States and 4.767 cents in Cuba.
1 per cent loss on 163,000 long tons at 5.786 cents per lb.
2 per cent loss on 440,000 long tons at 4.767 cents per lb.
$1,150,929
(a) This calculation can be checked in a different way. Sixty per cent
of the samples tested in 1916 deteriorated and the average loss in polariza-
tion per deteriorated sample was 1.8, which would correspond to an average
loss of 1.08 on the total 163.000 tons, or, at 5.786 cents per lb., of $228,161.
The above calculation does not take into account the
loss due to the deterioration of the 3,000,000 tons of
Cuban sugars during transportation. Allowing an
average loss of only o.i1 per cent sucrose during transit,
there would be a deficiency of $320,342 at Cuban prices
which would make the total calculated loss from de-
terioration for the 1916 Cuban sugars nearly $1,500,000.
Reducing the moisture content of raw sugars would
not only prevent the losses from deterioration but would
accomplish a considerable saving in the costs of trans-
ton. In the shipment of Cuban sugars for the
year 191 7 approximately 100.000,000 lbs. of water were
carried which, at the rate of So. 004 per lb., would make
an expenditure of $400,000 for transportation of a
useless ingredient. While the manufacture of moisture-
tree sugar is practicable only with the very highest
the moisture content of the ordinary qualities
of raw sugar can be reduced nearly one-half without
much extra cost of manufacture.
In conclusion the author desires to thank his assistants
H. Hardin and Mr. C. A. Gamble for help in the
analytical work of this paper, and Mr. J. A. Hall. Jr.. of the
A. M Byers Co., for photographs of Cuban warehouses,
Nkw York StrOAB Tkaok Laboratory. Inc.
80 South Strsbt, New York City
l'lii- is .i conservative estimate. Cuban sugars frequently show a loss
.irlv 1.0 in polarization between the times of shipment and delivery.
Mar., 1 91 8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
191
THEORY AND PRACTICE IN THE DESIGN OF MULTIPLE
EVAPORATORS FOR SUGAR FACTORIES
By A. L. Wbbre
Received February 7, 1918
The purpose of this article is to give a brief outline
of the data used in the proper design of a multiple
effect evaporator for sugar factories, and its applica-
tion in practice.
We shall assume a general knowledge of multiple
evaporation and, therefore, will not touch upon ele-
mentary considerations. In order to study in detail
we will subdivide our discussion as follows:
A — Heat transmission considered from the steam side
of the surface.
B — Heat transmission considered from the juice
or liquor side.
C — A typical problem.
D — Distribution of temperature drops in the various
bodies.
E — Heat balance showing flow of heat and liquor for
the problem under consideration.
F — Distribution of heating surface arrived at from the
heat balance.
G — Considerations necessary in the proper design
of a juice heater.
H — Proportioning of the bodies and vapor pipes.
I — The entrainment problem, its cause, provisions
required against it.
A HEAT TRANSMISSION CONSIDERED FROM THE STEAM
SIDE OF THE SURFACE
The transmission of heat from steam through the
surface of an evaporator is very similar to the opera-
tion of a surface condenser, with the exception of the
fact that the temperatures of the steam being condensed
are higher and, therefore, the specific volume per unit
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of weight much smaller. Professor E. W. Kerr in
his excellent papers on the subject has shown that the
coefficient of heat transmission varies quite consider-
ably with the temperature, being much higher as the
temperature increases, and we reproduce a curve
herewith showing this variation (Fig. i).
We also find that the presence of air or non-condens-
able gas mixed with steam or vapor has a marked re-
tarding effect. This is particularly true if a condition
of approximate quiescence obtains within the steam
space. It is, therefore, very evident that in order to
obtain good results proper provisions should be made
to overcome this difficulty. There are designs on the
market to-day in which this feature has been carefully
studied out, giving a rapid, uniform agitation on the
steam side. It is to be noted that particularly under
vacuum this difficulty will be more noticeable, for not
only does a given amount of these non-condensable
gases occupy a larger volume by virtue of the reduced
pressure, but from the very fact that the equipment
is under a pressure lower than the atmosphere, what-
ever leakage in joints, sight glasses and fittings may
take place, this leakage occurs from the outside inward,
and becomes mixed with the vapor which eventually
reaches the heating surface of the succeeding body,
resulting in an accentuated difficulty at this point,
so that the provisions relating to this trouble cannot
be too thorough.
Fig. 2 shows the writer's arrangement for this pur-
pose.
In this connection it can readily be understood that
it is against good logic to vent the steam space of each
effect into its vapor space, for in that way the non-
condensable gases removed from the steam space of
the first effect are in turn put into the steam space
of the second, and so on, thus accumulating the un-
desirable results. This, of course, is doubly true if
these gases have a tendency to attack the surfaces.
The best plan, and the one in general practice, is to
vent each steam belt into a large header connecting to
the vapor space of the last body. There are two de-
tails in connection with this header that are well worth
mentioning. The first is that the header should be in
a horizontal position with preferably a slight fall to-
wards the last effect, and that it should enter tto
belt without rising, for there is always a certain
of vapor condensing in this pipe, and if the discharge
192
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. Xo. 3
end is higher than the other, condensed water will
accumulate in the lowest point, partially choking the
pipe, or at least offering a considerable amount of fric-
tion. Under these conditions the steam belt of the
first effect which needs least venting will vent most
freely, and that of the latter effects which need the
most venting will be prevented from doing so, due to
the increased pressure at the point of attachment to
the header. The other point is that the size of the
pipe should be amply large so that the discharge from
the vent of the first effect will not prevent the last
ones from discharging freely. In fact, the writer has
obtained best results on multiple effects having a
large number of bodies by having an independent vent
for the steam belt of the last body, and having the
others connected to the manifold referred to above.
It is useless to state that the steam compartments
of the various bodies should be thoroughly drained
and water gauge glasses should be installed thereon
to make sure that such drainage is complete and
thorough, otherwise, of course, water accumulates,
blanking off the heating surface and decreasing the
work to that extent.
In brief, the above gives a fair idea of the problems
to be taken care of on the steam side of the heating
surface. We now come to a consideration of the liquor
side.
It- — III AT TRANSMISSION CONSIDERED FROM THE JUICE
OR LIQUOR SIDE
Liquid in ebullition in an evaporator corresponds to
the cooling water in a surface condenser, but the
problems involved and the general behavior of the
apparatus in operation are quite different. Perhaps
the best way to give a good idea of these is to describe
an experiment which was made for the purpose.
A small evaporator of the vertical tube type having
a central downtake was used. The tubes were of
copper 2 in. in diameter by 4.8 in. in length. This
equipment is shown in Fig. 3. The steam side was
baffled according to a design originated by the writer
and referred to above, and all necessary provisions
were made in order to obtain as nearly ideal conditions
as possible. For simplicity's sake the evaporator was
Operated atmospherically, i. e., with the top off, so
that a good and uninterrupted observation could be
made. The test was run with water, so as to eliminate
nsity and boiling temperature loss (discussed
later). The evaporator was filled until the level of
er was flush with 1 sheet. The water
was cold, about 6o° F. The steam valve from a con-
stant high pressure main was opened to a fixed point
and allowed to remain thus, so that the amount of
steam flowing through was fixed. The air vent was
opened t<> such a point as to make sui re were
practically no . in any pari of the
At iirst with tin.- water still cold, the pressure in the
steam space was 5 lbs., and as the temperature in-
this gradually rose until finally just before
ebullition started it was 11 lbs. By looking down
from the top a large quantity of small hubbies could
be seen under the surface of the water clinging to the
inside surface of the tubes. Finally the evaporator
began to boil and increased very quickly to rapid
agitation and circulation.
When this took place three things happened which
give a very good insight into the real operation of an
equipment of this sort:
I — The pressure dropped very quickly from 1 1 lbs.
to about s lbs.
II — The level as indicated by the water gauge glass
dropped to a point about two-thirds the height of the
tubes.
Ill — The level of the liquid inside showed intense
agitation, and the mixture of steam bubbles and water
rose to a point about 12 in. above the top tube sheet.
Let us consider carefully each of the above develop-
ments in detail with a view to logical interpretation.
I — Inasmuch as the pressure dropped very materially,
it follows that the coefficient of heat transmission must
have increased in proportion. This increase was due
l' 1 two causes:
First, the bubbles of steam which clung to the heat-
ing surface before ebullition started were liberated
and the surface blanked off by I hese bubbles was now
exposed to contact with water. This is merely a
duplicate of the oft-mentioned experiment of making
a teakettle heat faster by stirring the water with a
spoon and liberating the bubbles on the bottom.
Second, before ebullition started there was a quiescent
Mar., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
i93
condition on the inside of the tubes. Now instead
we had a rapid circulation. This undoubtedly had
a marked beneficial effect on the coefficient of heat
transmission. It will be remembered that Mr. Orrok
in his experiments on surface condensers found that
within certain limits the coefficient of heat transmission
varied with the square root of the velocity. Estimat-
ing as near as possible, the velocity in this case was
about 1 2 ft. per second.
II — The fact that the water went up on the inside of
the evaporator and that the water in the gauge glass went
down is explained in this way: The gauge glass shows
the static pressure at the bottom; the water on the top
is in a dynamic condition, for we must assume that the
velocity of the water coming out of each tube must
be nearly equal to the velocity of the vapor, and as
stated above, this was 12 ft. per second. If this is
so, the water left to itself would jump about two and
one-quarter feet above the tube sheet. Each tube
then is spouting up at this rate and a blanket of water
is practically kept in suspension by impingement from
below, and this impingement from the tubes near the
downtake prevents the free flow of water from the
outer diameter of the evaporator towards the center;
in other words, interferes with circulation, the result
being that a large amount of water is kept constantly
above the tube sheet. Now the net area of the diam-
eter of the evaporator being much larger than the net
area of the tubes, the original water which was con-
tained in the tubes, now being held in the evaporator
above the tubes, does not correspond to as much height
in the water gauge glass. In addition, a good part
of this water above the tube sheet, is in the form of a
spray in mid-air, we might say, and this does not show
on the water gauge glass. This lowering of the static
pressure as shown by the gauge glass lowers the pres-
sure on the bottom of the heating surface, and conse-
quently tends to cause an increase in the coefficient
by giving a larger net temperature drop at this point.
To make it plainer, before ebullition begins, the
hydrostatic pressure at the lower part of the tube is
4 ft. of water (the tubes being 4 ft. long), which
corresponds roughly to two points. The boiling tem-
perature at that pressure is about 2180 F. as against
2120 at the top of the tube. If we had 5 lbs. pres-
sure on the steam side at this point we would have
had 227 ° steam, with a net drop of 90, as compared
with 1 50 at the top. Now with the lower static head,
the boiling temperature at the lowest part of the heat-
ing surface is reduced to about 2160, and, therefore,
we can evaporate more inasmuch as the net tempera-
ture difference has been increased, which is the same
thing as saying that the coefficient of heat transmission
as a whole has been increased.
As a supplement to our experiment, the evaporator
was again filled to the top tube sheet, brought to ebulli-
tion as above, and the steam suddenly shut off, when
the level in the water gauge glass went back to ex-
actly the starting point.
Another experiment conducted with the same ap-
paratus was to carry a uniform pressure of 5 lbs. and
maintaining the levels at different points to determine
what would be the best working level, as shown by the
water gauge glass. In this case also there were several
surprises. The method of operation was to make time
runs in which either the feed or the condensate were
measured carefully and the coefficient of heat trans-
mission determined from this. Fig. 4 represents the
results obtained. Two things are apparent from this
curve. The first is that under our conditions of opera-
tion the best level was from one-fourth to one-third
the height of the tube; the second was that the slo wing-
up effect of carrying the level too high was much more
than expected. It is easy to estimate theoretically
what this should be. It is represented by the dotted
line above the graph.
The other things that were brought out by this
test were that contrary to the common impression,
circulation understood as the rapid traveling of the
liquor from the bottom of the evaporator to the top
and back again has a negligible effect on heat trans-
mission. Test runs were made at the following levels
above the bottom tube sheet: 6 in., 12 in., 18 in., 24
in., 30 in., 36 in., 42 in., and 48 in. At 6 in. and 12
in. the tops of the tubes were perfectly dry, and a
thermometer placed immediately above the tube sheet,
showed a superheat of a few degrees. The highest
coefficient was obtained when tops of the tubes were
just wet. In this case there was no liquor above the
tube sheet, at all, only a little spray out of each tube,
and this spray did not reach the down tube. There-
fore, we can say that there was no circulation in the
proper sense of the word, inasmuch as none of the water
returned to the bottom of the evaporator via the central
pipe. Of course, there was agitation and velocity of
travel caused by the rapid vapor currents coming out
of the tube, but there was no circulation. As soon as
the level was carried beyond this point to such a height
that water was going down the center pipe, the coeffi-
cient of heat transmission began to decrease, the result
being more and more marked, until when water showed
level with the tube sheet in the gauge glass, the rate of
evaporation was two-thirds of the maximum recorded.
We can then safely make the statement that we found
the critical point of maximum work to be the level
required to keep all parts of the surface we1
The function of circulation in the proper sense of
'04
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 5
the term is evidently a thorough mixing of the solu-
tion in order to prevent the material from concentrating
locally, resulting in excessive densities in certain parts
of the apparatus and low densities in other parts.
Under those conditions there should be selected for
the running point a sufficiently high level so that this
mixing will take place. This is only slightly above
the critical maximum point referred to in the dis-
cussion above. Any additional liquor beyond this is
a material detriment to the successful and efficient
operation of the equipment and should be carefully
avoided.
In order to accomplish this result, provision should
be made to insure positively against improper opera-
tion by using automatic level regulators, the selec-
tion of the design depending upon the character of
the work. For instance, in non-crystallizing solutions
in which the concentration is carried on continuously,
an overflow control is advisable, whereas in crystal-
lizing solutions, or solutions concentrated in batches,
a properly designed float control is necessary.
It will be understood the above-mentioned working
part of one-third the length of the tube only refers to
the particular equipment in question under the con-
ditions of the experiment. Changing the proportions
of the tubes, the temperature of ebullition, the sur-
face tension of the material being concentrated,
the percentage of solids contained, the viscosity, or
the rate of evaporation, all affect the behavior of
the equipment, and the best point should be deter-
mined in each case, and the control set so that the level
will be high enough to secure proper circulation under
all possible conditions of operation for the particular
apparatus in question.
Another factor which greatly affects the performance
of any equipment is the accumulation of scale, dirt or
incrustations on the liquor side of the tubes. It is,
therefore, most essential for uninterrupted opera-
tion to remove as far as possible all suspended
matter and scale-forming elements before the material
enters the evaporator. It is beyond the scope of
this paper to discuss in detail the character of each,
or the most advisable means for their removal, except
to state that in the sugar business the usual method is
to clean out at regular intervals, possibly once a week,
by boiling out first with a weak caustic soda solution
and then with muriatic acid. If the character of the
scale is very obdurate it may be necessary to supple-
ment this treatment by mechanically scraping the tubes.
It is far better in extreme cases to clean at shorter
intervals if the deposit is found to accumulate very
rapidly, as it is much easier to remove two thin layers
of scale than one thick layer. In this connection it
might be well to state that whereas rapid circulation
has a tendency to reduce the incrustations anil change
their character, it is far from being an infallible remedy.
Especially is this true in the case of calcium sulfate,
and calcium and magnesium carbonates. When the
incrustations consist of mechanically suspended matter,
on the other hand, rapid circulation greatly minimizes
troubles from this source.
C A TYPICAL PROBLEM
Having briefly discussed general considerations,
we shall now proceed more into detail by designing
a quadruple effect in accordance with standard
practice. We shall assume the following conditions:
Capacity of factory per 24 hours 1 ,250 short tons
Weight of juice. 1 20 per cent of wt. of cane 1 ,500 short tons
Weight of juice per hour 62.5 short tons
Weight of juice per hour 125.000 lbs.
Kvaporation per hour required, 75 per cent 93,750 lbs.
Initial temperature at juice heater 75° F.
Hot juice leaving heater -^5° ^'
Hot juice entering evaporator from defecator 180 F.
Initial density of juice entering evaporator 13.7 Brix
Final density of juice leaving evaporator 55 Brix
Exhaust pressure available first body 5 lbs.
Vacuum obtainable 26 in.
D DISTRIBUTION OF TEMPERATURE DROPS IN' THE
VARIOUS BODIES
We will select in this case a quadruple effect with
juice heating by vapors from first body.
The first item to consider in our design is the drop
of temperatures and vacua from one body to the
next, and the logical distribution of these drops.
The temperature of steam at 5 lbs. is 227 ° F.. and
that at 26 in. vacuum is 1250. Our total range of
temperature, therefore, is 102 °, to be divided up among
the four bodies of the evaporator. This is not equally
divided, being much more on the last body than on
the first, for a number of reasons:
1 The coefficient of heat transmission is not the
same in all the bodies, but is much more in the first
than in the last body. As stated before, therefore, it
follows that we should divide up the temperature fall
in each according to the coefficient for the particular
temperature of steam in the heating compartment.
This is true even if we had purely surface condenser
conditions, but we have no such conditions, and, be-
sides, there are other factors to consider. (Refer to
Fig. 1.)
2 — The coefficient referred to in the above paragraph
relates to the actual temperature difference between
liquor on one side and steam on the other. We find,
Mar., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
195
however, that as concentration goes on, and the per-
centage of solids increases, the boiling point rises
materially above that of water, which would be the
same as that of the vapor leaving the liquid. A
curve is shown in Fig. 5 which gives this increase for
normal cane sugar juice. We must then deduct from
our total temperature fall the summation of these
differences for each body.
3 — It is true that the pressure at which ebullition
takes place is in general represented by the vacuum
gauge on each body, which also represents the pres-
sure of the vapor going from there to the succeeding
effect, and, therefore, its temperature, but we must
recall that this is the pressure at the surface of the
liquid. Now, inasmuch as ebullition is going on from
.the top to the bottom of the tube it is fair and logical
to say that we should consider the average pressure
throughout the length of the tube as representing fairly
correct conditions, and not the pressure on the surface
represented by the vacuum gauge. There will, of
course, be a difference between the two which repre-
sents a net loss in the temperature fall, and should
be taken into account in our calculations. In this
instance we will assume, in conformity with accepted
practice, that the tubes are 2 in. in diameter and 5 ft.
long and that the level is maintained at one-third the
length. Our static pressure at the bottom of the tube
wilt then be 20 in. of liquid, and the arithmetical mean
will be 10 in. In converting this back to mercury
pressure, we must take into account the density of
the liquid which is always higher than that of water.
4 — The increased viscosity of the juices as the con-
centration increases also seems to use up temperature
'drop. The proper determination of this loss is not
yet thoroughly defined, but careful experiments by Pro-
fessor Kerr seem to indicate that for practical purposes
we can assume that in cane sugar juices under average
conditions it is substantially equal to the boiling tem-
perature loss.
Without going into the detailed calculations, below
is a table showing the temperature losses in each body
and the distribution of the "working drop" taking
into account the available coefficient of heat trans-
mission as affected by steam temperature, and finally
the steam and vapor temperatures with their corre-
sponding pressures and vacua (Fig. 6).
Bodies 12 3 4
Boiling temperature loss... 1.5 2.0 3.0 9.0
Static head loss 1.0 2.0 3.0 8.0
Viscosity loss 1.5 2.0 3.0 9.0
Total temperature losses. . 4.0 6.0 9.0 26.0
Working.drops 11.0 12.0 14.0 20.0
Total drops 15.0 18.0 23.0 46.0
Steam and vapor temp.... 227-212 194.0 171.0 125.0
Pressure and vacua 5 lbs. 0 lbs. 9 in. 17 in. 26 in.
E HEAT BALANCE SHOWING FLOW OF HEAT AND
LIQUOR FOR THE PROBLEM UNDER CONSIDERATION
Having studied the proper and logical distribution
of temperature differences, we are now in a position
to make up a heat balance, showing the flow and dis-
tribution of steam, vapor, condensate and juices. In
making up this heat balance, in order to avoid com-
plications, we have assumed that the specific heat of
sugar solutions will be unity in all cases. Of course,
this is not so, but the error introduced is so small that
it can be neglected. Also we have assumed that the
condensate coming out of each steam compartment
will leave at steam temperature. As a matter of fact
this condensate is always slightly cooler but the error
introduced is very small.
The cycle used is as follows:
i — Juice at 180° F. is fed to the first effect, then
to the second, to the third, and to the fourth,
whence it is removed in a concentrated condition by
the syrup pump.
2 — Steam is admitted into the first effect at 5 lbs.
pressure. The vapor from here goes partly to the
heater, where it warms the juice from 75° to 205°,
and the remainder goes to the second effect; the
vapors from the second to the third, and from the
third to the fourth, and from the fourth to the con-
denser.
3 — The condensate from the first effect goes back
to the boilers, that from the heater is wasted, that
from the second steam chest is passed to the third,
and from the third to the fourth, whence it is removed
by a pump.
The heat balance and diagram (Fig. 7) represent
theoretically what happens in the evaporator. The
steam consumption, however, will be slightly greater,
due to radiation losses. These are comparatively
small amounting to about 2V2 per cent in a well-in-
sulated equipment. It is advisable in basing calcu-
lations to allow s per cent, so that our consumption
undi • these conditions should be 40, 500 lbs. per hour.
196
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 3
Heat Flow Heat Balance1
First Body
Steam 38,250 lbs. at 5 lbs. = 38250 X 961 = 36,700,000
Deduct for heating 125,000 X (213.5 — 180 -
33.5) = 4,190.000
Liquor Flow
125,000
Available for evaporation 32,5 1 0,000
Lat2.2°=970,K = -™00° = 33.500
Transferred to' No. 2 91 ,500
Sbcond Body
Vapor from No. 1 32,510,000
Liquor Hash 91,500 X (213.5 — 196 = 17.5)= 1,600,000
Heat available 34,110,000
Deduct for juice heater 125,000 X (205 — 75
= 130) = 16.250,000
Available for evaporation 17,860,000
_ 17,860,000 _
E ~ 981 ~
L at 194°
Transferred to No. 3
Third Body
Vapor from No. 2 1 7.860.000
Liquor flash 73.300 X (196 — 174 = 22) =.. 1.610,000
Condensate flash 16,750 X (212— 194 = 18)= 302,000
L at 171°= 995, E
995
Transferred to No. 4 53,450
Fourth Body
Vapor from No. 3 19,772,000
Liquor flash 53,450 X (174—134 = 40) =.... 2,135,000
Condensate flash 34,950 X (194—171 = 23)= 805,000
L at 125° = 1021, E =
Concentrated liquor out 31,250
Note — The above figures are correct to slide rule accuracy.
1 Representing hourly work. All quantities in pounds.
F DISTRIBUTION OF HEATING SURFACE ARRIYID AX
FROM THE HEAT BALANCE
The next step is to determine the heating surface
required and its proper distribution. The total amount
of surface will depend upon the design of the evaporator
and a unit basis must be taken which has been proved
out in practice. In our case, we shall assume that we
are contemplating a standard effect and we shall take
an evaporation of 5V2 lbs. per sq. ft. per hour as a
fair basis for a quadruple under the assumed condi-
tions. Our total evaporation being 93,750 lbs. per
hour, the surface required will, therefore, be 17.000
sq. ft.
actual heat flowing through the surface of each
body per hour is as follows:
First effect 36,700,000 B. T. V.
Second effect 16,260.000 B. T. 1 .
Third effect 18,162.000 B. T. 1
Fourth effect 20,577,000 B
It is to be noted that all the heal given up by the steam
in the first body must be transmitted through the
It is likewise to be noted that the heat
represented by the liquor flash in the other
does not have to be transmitted. These facts have
veil due consideration in the above. If we
proportioned the surface in each effect in accordance
to the above, we should have four different-sized units.
We. therefore, make a comparison by making the
feet of one size, and the other three of .
size which will be an ap] mean of their in-
dividual requirements. By referring to the figures,
it is evident that practically we can do this, giving the
first body t\\ h surface as the others. Our
distribution then will be as follows:
First effect 6800 sq. ft.
Second effect 3400 sq. ft.
Third effect . . 3400 sq. ft.
Fourth effect 3400 sq. ft.
In this connection it might be well to correct a common
mistake which consists of giving to the first effect only
as much more surface as is contained in the juice heater.
This is entirely in error, for the evaporator is working
with a temperature drop of only 15°, whereas the heater
has a mean temperature difference of practically 720.
Furthermore, the two units being of entirely different
design and performing an entirely different class of
work, we can say that their coefficients of heat trans-
mission have no relation one to the other except that
both transmit heat into juice through copper tubes.
G CONSIDERATIONS NECESSARY IN" THE PROPER DE-
SIGN OF A JUICE HEATER
And while we are on the subject of the heater let
us say that it is a very material advantage to bring
the juice while passing through to as near steam tem-
perature as possible, for if supplemental heating is
to be done it must be accomplished by the use
of expensive single-stage heat. This being true,
the surface should be ample for the work. The steam
side should be designed so as to give good circulation
with thorough removal of condensed vapor and non-
condensable gas. The liquor side must be so pro-
portioned as to give rapid flow of juice through the
tubes, thereby minimizing fouling. This, of course,
is done by means of cells or divisions in the heads giving
many passes from the front to the back. The writer
has found that with a high juice velocity excellent re-
sults are obtainable; indeed the juice can be heated to
steam temperature if the unit is properly cleaned at
regular intervals. With a good design, as outlined
above, a coefficient of 250 can be obtained; therefore,
the surface required would be 1000 sq. ft. There
should be two such heaters, as they have to be cleaned
Qtly, the juice going through them not having
been defecated.
II — PROPORTIONING OF Till: BODIES AND VAPOR PIPES
Now going back to the design of the evaporator, it
is merely a question of laying out the tube sheet to get
the proper diameter. Downtakes or circulating tubes
should be provided, so as to get a complete mixing of
the liquor being concentrated. The height above the
tube sheet should be ample, not less than S to 10 ft.
The steam pipes must be large enough to take care of
the vapors without undue friction. We find that a
velocity of 100 ft. per sec. is good practice for exhaust
pipes and vapor pipes except in the case of the last
effect, when, due to the low density of the steam, it is
permissible to increase this to 200 ft. per sec. On this
basis the following sizes are advisable:
Exhaust pipe 20 i
20 i
15 i
l No, 2 15 i
Vapoi «'i No 18 i
Vapor ex. No. 3 24 i
Vapor ci. No ;
By maintaining th< and sizes as above, the
friction losses will be practically negligible. There
are, of course, other small details ■. hich it
is not in the scope of this paper to discuss as we are
Mar., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
To Heoi+er l(a75o
197
13 Ev. 3825o
*1
0 = 2/2*
b.Xz 2/35'
5lbs = 227'
*?.
9 = 194°
BTrl96*
o/fcs=2/2
17 = 17'°
6.7-174°
V. 9=/94e
TbCbod. 2?2oo.
2& = /25
67= 1 54"
Dia6ram roa-f io o£ <£>uci d ruple Ev fact
Showing flow o£ 5feam( C»nde"ta<t & Licjuo.- <;
confining ourselves to the important items. Such, for
instance, are the size and arrangement of liquor pipes,
drain pipes, air pipes, etc.
I THE ENTRAINMENT PROBLEM, ITS CAUSE, PROVISIONS
REQUIRED AGAINST IT
We now pass to another phase of our consideration.
This is entrainment. The loss of liquor from this
source can be divided up generally into two classes.
The first is foaming or frothing and occurs in the sugar
industry only very rarely, in cases where the juices
have been frozen or derived from burnt cane and fer-
mentation has taken place. It is very difficult to
overcome, perhaps the best method being to boil at
a high vacuum. There are a number of other expe-
dients, such as floating a small quantity of grease or
tallow on the surface of the liquid, carrying the level
very low, etc. This occurs so rarely, however, that
a brief mention of it is sufficient.
The other phase of the problem is loss by spraying
or spouting of the tubes, the liquor entering the vapor
pipes. The explanation of this is that while evapora-
tion is going on, theoretically at least, some of the
liquor leaving the top of the tubes must travel as fast
as the vapor driving it out. It is easy to estimate
what this is, for obviously all of the vapor generated
in each tube must pass through its upper end. Know-
ing the surface of the tubes, the rate of evaporation
per tube and the pressure or vacuum in each, we can
readily determine, not only the velocity, but the maxi-
mum height to which drops will be projected in this
way. Below is a table giving this information for
each effect.
Evaporation
per Tube (a)
Bodies Lbs. per Hr.
First effect 12.9
Second effect... 14.0
Third effect.... 15.3
Fourth effect. . 17.1
(a) Tubes are 2 in.
Cu. Ft.
per Lb.
26.8
37.4
58.6
Vol. per
Tube per Hr.
Cu. Ft.
346
524
896
3020
No. 1 6, 5 ft. 0 in. long
Speed
per Sec.
Ft.
5.01
7.60
13.00
43.80
0.390
0.896
2.625
29.800
stated previously.
It is therefore apparent that under normal condi-
tions, spray in the first and second effects is negligible.
This is not true of the third effect and very far from
being so in the last. It must be remembered that not
only is this spray projected very high in the last body,
but in the very act is broken up into a fine mist, which
is floated along by the upward vapor currents. There-
fore, one cannot be too careful in providing against
loss of liquor from this source. In addition to the
regular separators or catchalls commonly used, the
writer places baffles in the vapor space where by
shifting the direction of vapor currents at a low ve-
locity, it is possible to secure an excellent preliminary
separation before reaching the catchall, for it must
be remembered that once this spray enters the separator
the velocities obtained are so high that the particles
of liquor break into fine ones by impingement against
the baffles, resulting in a very fine mist which floats
along with the vapor to the condenser, with resultant loss.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 3
Along this same topic, it is a very wise precaution
to use great care in admitting the liquor from each body
to the succeeding one. If it is simply allowed to enter
into the bottom below the tube sheet, the "flash"
will be local, causing the tubes in the immediate vicinity
to spout violently, projecting liquor to the dome.
The proper remedy is to distribute this feed in the
bottom by means of a perforated coil or manifold,
or if this is not used, to provide a flush pot or recipient
on the outside of the evaporator, with the upper part
connecting with the vapor belt and the lower part
with the bottom. Still another way is to use a spray
pipe above the tube sheet, and still another is to feed
from above with the pipe extending to the center,
the opening facing downward.
Many have the tendency to make small of this
problem, but when it is recalled that enormous quanti-
ties are treated in a given time, it will be found that the
game is well worth the candle. For instance, a loss of
1/i per cent in the evaporator contemplated above
would amount to about 800 lbs. of sugar per day,
worth, on a six cent basis, $48, and in a campaign
of one hundred and twenty working days, this would
be $5760, which justifies almost any kind of provision
to recover it. And yet there are many evaporators
which lose more than 1/l per cent, but the man who
owns it does not know, for evidently the loss is greatest
in the last body when the vapor goes into the con-
denser, and in so doing is diluted about 30 to 1.
E. B. Badger & Sons Company
Boston, Mass.
NOTES ON THE ANALYSIS OF MOLASSES
By Herbert S. Walker
Received January 11, 1918
In comparing the results of a large number of de-
terminations of sucrose in final molasses analyzed by
students at the College of Hawaii and by myself, I have
noticed that the same sample of molasses appears to
contain from 0.5 per cent to i.o per cent less sucrose
if clarified with dry lead subacetate than if the lead
subacetate solution is used. These discrepancies were
at first attributed to personal errors, but as the dif-
ferences invariably persisted in the same direction, an
attempt was made to trace out their causes and ascer-
tain which, if either, of the two methods of clarification
could be relied upon.
The method of clarification by lead subacetate solu-
tion used in this laboratory is that prescribed by the
Hawaiian Chemists' Association. 35.75 g- molasses
are dissolved in water, clarified with 40 cc. of a solution
of basic lead acetate of 54° Brix, made up to 250 cc.
with water and filtered. 50 cc. of the filtrate are
treated with 1 cc. of a saturated solution of aluminum
sulfate, made up to 55 cc. with water and filtered.
Reading (in a 200 mm. tube) multiplied by 2 gives the
direct polarization. 75 cc. of the original filtra
inverted by the Herzfeld method and made up to no
cc. Reading multiplied by 8/3 is the invert polariza-
tion. The factor used is 142 — 0.5/.
For clarification with dry lead subacetate a method
derived from that proposed by Cross and Taggart1
> Louisiana Bullrlin 135.
has been tried. 35.75 g. molasses were dissolved in
water and made up to 250 cc. then clarified with 12 to
15 g. dry basic lead acetate and filtered. About 50
cc. of the filtrate were de-leaded and made slightly arid
by the addition of 0.3 g. dry powdered sodium bisulfite
and filtered for direct polarization. 75 cc. of the original
filtrate were inverted and made up as in the previous
method for invert polarization.
Since the same concentrations of molasses and of
lead subacetate were used in both methods, the direct
polarizations were both made in a slightly acid solution
and the inversion procedure was identical, it follows
that the difference in results must have been due
either to the volume occupied by the lead precipitate
causing too high results in the "wet" method, or to the
dilution in the "dry" method produced by an excess
of lead going into solution over that required to precipi-
tate impurities, which would tend to yield too low
figures.
VOLUME OCCUPIED BY THE LEAD PRECIPITATE
35-75 g- of a waste molasses were dissolved in water,
clarified with 40 cc. lead subacetate solution and the
precipitate washed by decantation during a period of
several days until the clear decantate from four con-
secutive washings showed no polarization in a 400 mm.
tube. This sugar-free lead precipitate was transferred
to a 250 cc. flask together with 22 g. granulated sugar,
made up to the mark with water and polarized in a
400 mm. tube, giving R = 68.36. 22 g. of the same
sugar made up with water alone in the same flask read
67.46. The difference of 0.90 or 1.33 per cent of the
total polarization could have been caused only by the
volume occupied by the lead precipitate. The volume
left in the flask for the solution in this case must have
been not 250 cc, but 250 X , , = 246.72 cc. The
68.36
precipitate itself then occupied 3.28 cc. The sugar-
free lead precipitate from another 35.75 g. sample of
this same molasses was placed in a 250 cc. flask with
32.50 g. granulated sugar, made up to the mark with
water, filtered and polarized in a 400 mm. tube, giving
R = 101.20. The same weight of sugar dissolved in
250 cc. water alone read 99.80. The presence of the
lead precipitate caused an increase of 1.40 per cent of
the total polarization. If the molasses from which
this precipitate was made contained say 35 per cent
sucrose, its apparent value would be increased by 35 X
0.014 = 0.49 per cent sucrose.
The washed lead precipitate from 35.75 g. of molasses,
from another plantation was still more voluminous.
Duplicate tests on it were as follows:
Reading
12.50 n siiKar made up to 250 cc. with water alone 99.74 99.83
32.50 g. sugar made up to 250 cc. with lead precipitate and
water 101.63 101.87
Increase due to lead precipitate 1 . 89 2 . 04
Average 1.96
If this molasses contained 35 per cent sucrose it would
appear to contain 35.69 per cent if analyzed by the
H. C. A. method, providing there were no other errors.
in the method.
Mar.. 191S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY i99
dilution by dry lead subacetate solution, and still not cause any inversion of sucrose
A solution of refined sugar containing 13 g. per 100 during the 15 min. or more required to filter and polarize
cc. polarized in a 400 mm. tube 99.51. To a portion a molasses solution. Fortunately the error introduced
of this solution was added dry basic lead acetate in in cane molasses analysis is not as large as might be
the proportion of 3 g. per 100 cc. The filtered solution supposed from the amount of time and labor spent in
then polarized 98.99, a drop of 0.52 per cent. To ob- attempting its correction. The invert sugar resulting
tain the maximum clarification of a half-normal molas- from the inversion of a normal weight of sucrose in
ses solution, up to 6 g. lead per 100 cc. may.be re- 100 cc. has a minus polarization of about 31.7 at 20° C,
quired. Assuming that half the lead goes into solution in neutral solution, while the same weight of invert
without being precipitated, a molasses containing 35 sugar in a solution containing 5 cc. concentrated HC1
per cent sucrose might suffer an apparent loss of 35 X per 100 cc. reads 32.7 to the left, the increased reading
0.0052 = 0.18 per cent sucrose on account of this due to acid being 1.0 in 31.7, or 3.2 per cent of the total
dilution. minus polarization. The amount of invert sugar
experiments with artificial molasses present in cane molasses, calculated from average
The great difficulty in testing a method for the de- d'fferences between direct polarizations and sucrose
termination of sucrose in molasses is of course due to values- has a total minus polarization of from about
the fact that we cannot know exactly how much sucrose 3 to s' so that we should exPect an increase in acid
there really is in the molasses. If it were possible to over neutral reading of from — 0.1 to —0.16, indicating
remove all the sucrose from a molasses without disturb- a fictltl0us increase in sucrose in the final calculation
ing its other constituents, it would be a simple matter of about °-x Per cent when direct polarizations are
to make up standard samples for testing out new made m neutral or weakly acid solution and invert
methods. An attempt in part to accomplish this was readmgs are taken in a solution containing 5 g. HC1
made by dissolving 1 kg. of molasses in 10 liters water, Per IO° cc- 0f course' if direct readings are made in
clarifying with 1 liter basic lead acetate solution and alkallne solution this error may be largely increased,
washing the precipitate by decantation until free from To test the above theory, a neutral solution of invert
polarization. The lead precipitate was then decomposed suSar was Prepared, containing about 24 g. per 100 cc.
by hydrogen sulfide, the lead sulfide filtered off and the 25 cc- of tms> containing somewhere near the amount
clear solution evaporated to about 1 liter, yielding a con- of mvert sugar ordinarily present in 35.75 g. waste
centrated solution containing most of the lead-precipi- molasses, were analyzed in duplicate by the H. C. A.
table impurities of the original molasses. 50 cc. of method for sucrose (omitting clarification and subse-
this "impurities" solution were found to require about <luent de-leading) with the following results:
40 cc. basic lead acetate for complete precipitation and Direct polarization in neutral solution — 4.44 —4.47
.i_ r 11 .1 ■ ■ ■ i_i '*.' Polarization after inversion (25.6° C.) — 4.62 — 4.61
therefore represent roughly the precipitable impurities -sucrose" o 14<7 o 12<7
in a 35.75 g. sample of molasses.
50 cc. of "impurities" alone analyzed by the H. C. A. 0n two more samPles the dlrect as wel1. as the mvert
method gave a direct polarization of -0.55, an invert reading was made m a solut,°n containing 5 cc. con-
■ ■ *.• x j 11 >> centrated HC1 per 100 cc. and gave the following re-
polarization of — 0.57 and sucrose — 0.02, or prac- ^""»<**"» ">-" f>-' & &
tically nothing. sults:
12 g. pure sucrose alone, analyzed by the H. C. A. Direct polarization —4.63 —4.65
. , r n . . . .... 1 . Polarization after inversion — 4.62 — 4.61
method for sucrose in final molasses but omitting clan- "Sucrose" o.oi — 0.04
fication and de-leading, indicated 33.59 per cent sucrose
T 2 0 This proves the absence of sucrose in the invert sugar
(based on a 35.75 g- sample) as against _ '— or 33.56 solution and gives an idea of the magnitude of the error
per cent actually present. introduced by making direct readings in neutral instead
12 g. pure sucrose mixed with 50 cc. "impurities" of acld solution.
and analyzed by the H. C. A. method indicated 34.1 5 12 g' pUre SUCr0Se together ™th approximately 6 g.
per cent sucrose, or 0.59 per cent too much. invert sugar were next a"alyzed by the HC- A; method-
12 g. pure sucrose mixed with 50 cc. "impurities" The readings (based on a 3 5-75 g- sample) were:
and analyzed by the dry lead method, using 15 g. dry Direct 28.94, Invert (at 24.6 ) -14.76, Sucrose
lead subacetate instead of 40 cc. of the solution, indi- 33-68 per cent against 33-S6 per cent actually present
. , „ o * * «*+i- The error involved appears to be in the neighborhood
cated 33.28 per cent sucrose, or 0.28 per cent too little. luc c"ul " , . , , „.,■-,• -^
of o 1 per cent sucrose, which is well within the limit
THE EFFECT OF INVERT SUGAR , r , , . „„.,„.
of personal error of most analysts.
Much has been written concerning the influence of
., , ,, n, . A„ ANALYSES OF RECONSTRUCTED MOLASSES
the invert sugar in cane molasses on the Clerget de-
termination and the necessity for making direct and A mixture of 1 2 g. sucrose, 6 g. invert sugar and 50
invert polarizations in solutions of the same acidity. cc. "impurities" was analyzed by the H. C. A. method.
I have made numerous experiments with many dif- The readings on two separate samples were
ferent acids and acid salts in a vain endeavor to find Direct 29.79 29.70
some concentration or combination of a weak acid invert — 14.8 — .
, . , . , . , ■ iturc 24.7° 24.7
which would cause invert sugar to polarize as strongly "Sucrose" .14.41% 34.26%
to the left as does 5 cc. of concentrated HC1 per 100 cc. Avbraoh 34.34 per cent sucrose
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 3
A mixture of 1 2 g. sucrose, 6 g. invert sugar and 50
cc. "impurities" analyzed by the dry lead method (15
g. dry lead subacetate) read
Direct 29.17 29.24
Invert —14.15 —14.15
Temperature 25.0° 25.0°
"Sucrose" 33.44% 33.50%
Avbrage 33 . 47 per cent sucrose
The method of clarification with basic lead acetate
solution, when worked on a reconstructed molasses of
a known sucrose content, is thus found to yield results
in this particular case 0.68 per cent too high, while
clarification with the dry subacetate gave a figure 0.09
per cent too low.
While the dry lead method previously described has
been shown to give fairly accurate results on known
mixtures, due in part to compensating errors, it still
suffers from the disadvantage that a large excess of
lead which is sometimes necessary for clarifying dark
colored products causes low results on account of the
dilution which it produces. Extreme care must also
be taken to add just the proper amount of de-leading
agent. Too little of this may cause too high a direct
polarization, while any excess over that required for
precipitation of the lead introduces a still further dilu-
tion of the solution. Especial care is needed when,
sodium bisulfite is used for de-leading; subsequent ex-
periments have caused me to abandon this reagent
altogether in sugar analysis, owing to the marked
specific effect it has on the rotation of glucose.
To obviate some of these difficulties the following
modification of the dry lead method for final molasses
has been evolved, and is submitted for trial and criticism.
NEW PROCEDURE FOR DRY LEAD CLARIFICATION
Dissolve a double normal weight of molasses (52 g.)
in water and make up to 300 cc. Clarify in a larger
flask with 15 to 20 g. dry lead subacetate and a few
grams of dry sand and filter. To 75 cc. of the filtrate
in a 100 cc. flask add 20 cc. of a solution containing
100 g. phosphoric acid per liter, make up to 100 cc. with
water and filter. (The addition of half a gram or so
of zinc dust just before filtration, while not usually
necessary, lightens up the color of the solution percep-
tibly and has no effect on the polarization.) Reading
in 400 mm. tube = direct polarization (D). Take
another 75 cc. portion of the original filtrate in a 100
cc. flask, add 2 cc. dilute HC1 (1 volume concentrated
acid to 1 volume water) to neutralize the alkalinity
due to excess of lead subacetate, heat to 65°-7o° C,
add 10 cc. HC1 (1 to 1), let stand in air 1 5 min. or more,
cool to room temperature, make up to 100 cc, add zinc
dust in slight excess and filter. Reading in 400 mm.
tube = invert polarization (I). Then
Sucrose = - — .
1.(2.1 0.5/
This method has several apparent advantages over
ordinary dry lead clarification of molasses. The ad-
dition of a moderate excess of phosphoric acid to a
1 of the first filtrate before making up again to
a definite volume throws down all the lead as a volumi-
nous, easily filtered precipitate whose volume compen-
sates for the dilution caused by any excess lead origi-
nally dissolved. A pale yellow filtrate results which
can be read with ease in a 400 mm. tube, so there need
be no multiplication of the reading error. The con-
centration of phosphoric acid selected (2 g. per 100 cc.
solution) is based on a number of tests made to deter-
mine the maximum acidity possible without danger
of inversion. While this amount of phosphoric acid
does not, in pure solution, produce quite as high a left
rotation of invert sugar as does 5 cc. of concentrated
HC1, yet, under working conditions of analysis, the
difference is so slight as to introduce practically no
error. A number of different acids were tried out in
this connection, but none was found to be as generally
satisfactory as phosphoric. Sulfurous acid in a con-
centration of 50 cc. of the saturated solution per 100
cc. total solution causes approximately as high a rota-
tion of invert sugar as does 5 cc. of concentrated HC1;
in fact, if sodium salts are also present, the left rotation
of invert sugar may become appreciably greater in
sulfurous than in hydrochloric acid solution, due not
to an increase in the polarization of fructose but to a
depressing effect on the rotation of glucose. More-
over, a molasses solution containing sulfurous acid of
this concentration is not absolutely free from danger
of inversion at tropical laboratory temperatures. I
have found a ioss in direct polarization of approximately
0.5 per cent sucrose in one hour at 260 C. Owing to the
finely divided condition of the lead sulfite precipi-
tate a very considerable time often elapses between
the addition of sulfurous acid and the direct reading,
so this chance of error, while not very great, is worthy
of note.
TESTS OF THE NEW DRY LEAD METHOD
CORRECTION OF DILUTION ERROR
To 500 cc. of a half-normal solution of refined sugar
15 g. dry lead subacetate were added. 75 cc. of the
resulting solution were made up to 100 cc. with water,
filtered and polarized in a 400 mm. tube, giving R =
74.24. To another 75 cc. portion 1 cc. of a 50 per
cent solution of phosphoric acid was added to com-
pletely precipitate the lea.!, the solution then made
up to 100 cc. with water, filtered and polarized in a
400 mm. tube, giving R = 74.53. The original solution,
before adding lead, polarized 09.51, corresponding to
74.63 if diluted from 75 to 100 cc. The loss in
polarization caused by a very considerable dilution
by dissolved lead is thus very nearly if not quite
restored by precipitating the lead from a definite
volume of solution and then making up with water to
another definite volume, the theory being that the
volume occupied by the lead phosphate precipitate is
practically the same as the increased volume caused
by solution of lead acetate.
TESTS WITH ARTIFICIAL MOLASSES
A solution of lead-precipitable impurities was made
by dissolving 1 kg. of waste molasses in 40 liters water,
precipitating with 2 liters lead subacetate solution, wash-
ing free from polarization, decomposing the lead precip-
itate with H.-S. filtering and evaporating the filtrate
ul 2 kg. too cc. of this solution required about
Mar., 191S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
40 cc. basic lead acetate solution for complete precipi-
tation. A Clerget determination on this solution of
impurities showed: Direct polarization = ■ — 0.02,
Invert polarization = 0.00.
12 g. "Domino" sugar and 100 cc. "impurities" were
analyzed by the H. C. A. method and gave D = 34.05,
I (27.2° C.) = — 9.64, "Sucrose" = 34.05 (based on a
35.75 g- sample).
J7-455 g- "Domino" sugar and 150 cc. "impurities"
were made up with water to 300 cc. and analyzed by
the new dry lead method, using 15 g. dry lead. The
results were D = 33.58, 1 (27.3 ° C.) = — 9.51, "Sucrose"
= 33-54 (based on a 52 g. sample). The sucrose
actually present in each case was 33.55 per cent.
INVERT SUGAR AND "IMPURITIES" WITHOUT SUCROSE
Samples were prepared containing approximately
the amounts of "impurities" and invert sugar found
in cane molasses (about 17 per cent invert sugar) and
analyzed for sucrose by three different methods with
the following results:
Method D I "Sucrose"
Sulfurous Acid.
Dry Lead
3.67
—3.74
0.05
-3.66
—3.52
— 0.11
3.42
—3.42
0.00
SUCROSE, INVERT SUGAR AND "IMPURITIES"
12 g. "Domino" sugar, 100 cc. "impurities" and about
6 g. invert sugar were analyzed by the H. C. A. method
and gave D = 30.20, I (27.0° C.) = — 13.58, "Su-
crose" = 34.07 per cent.
17-455 g- "Domino" sugar, 150 cc. impurities and
about 9 g. invert sugar were analyzed by the new dry
lead method, using 18 g. lead subacetate and gave
D = 30.01, I (26. 8° C.) = — 13.27, "Sucrose" = 33.63
per cent.
Sucrose actually present in each case = 33.55 per
cent.
The H. C. A. result was therefore 0.52 per cent too
high, while that of the dry lead method was 0.08 too
high, or practically correct within the limit of experi-
mental error, though a rather large excess of dry
lead was used for clarification.
For comparison, 20.142 g. "Domino" sugar (repre-
senting 33.55 per cent sucrose on a 60 g. sample),
170 cc. "impurities," but no invert sugar, were clarified
with 60 cc. lead acetate solution in a 300 cc. flask and
analyzed by Pellet's sulfurous acid method.1 The re-
sults were: D = 34.11, I (26.9°C.) = ■ — 9.58,
"Sucrose" = 33.99 per cent.
EFFECT OF VARYING AMOUNTS OF DRY LEAD
52 X 10/3 = 173.33 g- °f a waste molasses were
dissolved in water and made up to 1 liter. Three por-
tions of this were clarified separately with dry lead sub-
acetate corresponding to 10, 20 and 30 g., respectively,
per 300 cc. and analyzed as usual, except that in de-
leading, the amount of phosphoric acid used was varied
according to the amount of lead, 3, 4 and 5 cc, respect-
ively, of a 50 per cent solul ion being used.
I.i ad subacetate "Sucrose"
to 300 <
cc. solution D
I
1
10 g. 34.45
— 15.18
27.3°
38.64
20 g. 35.02
14.47
27.3°
38. S3
30 g. 35.71
— 13.90
27.1°
38.59
Increasing the amount of lead up to double that required
for efficient clarification has no effect on the sucrose
value.
For comparison, this same molasses was analyzed by
the H. C. A. method, using varying amounts of lead sub-
acetate solution and correspondingly varying amounts
of aluminum sulfate for de-leading.
Lead subacetate
for 35.75 g. molasses
"Sucrose"
in 250 cc. solution
D
I
t
Per cent
20 cc.
35.05
— 15.48
26.4°
39.23
30 cc.
35.27
— 15.25
26.2°
39.19
40 cc.
35.56
— 14.88
26.5°
39.18
50 cc.
36.08
— 14.57
26.2°
39.30
50 cc.(o)
36.01
— 14.64
25.9°
39.25
70 cc.
37.10
— 14.02
26.1°
39.64
(a) Sulfurous s
cid method.
Pellet. Intern. Susar J.. 1913 11
Within reasonable limits the sucrose indicated by this
method is independent of the amount of lead used for
clarification, but taking the new dry lead method to be
correct, the H. C. A. method yields results averaging
about 0.7 per cent too high. It will be noted that
practically no improvement in this respect results from
making the direct polarization in a solution strongly
acid with sulfurous acid. This is to be expected, since
the principal error, that due to the volume of the lead
precipitate, remains the same.
DETERMINATION OF BRIX, SUCROSE AND PURITY IN THE
SAME SOLUTION
The dry lead method lends itself readily to the de-
termination of gravity solids and sucrose in the same
weighed sample of molasses. As these determinations
are both required, some time may be saved by not
having to weigh out separate samples for each. The
only extra operation involved is to weigh the molasses
solution after making it up to 300 cc. preparatory to
clarifying. Knowing the water capacity of the flask
at standard temperature, the specific gravity and thence
the Brix of the molasses can readily be calculated. For
this method it is sometimes more convenient to take
86.67 g- molasses in 500 cc. instead of 52 g. in 300 cc.
An alternate method for making the two determina-
tions on the same sample is to prepare a large sample of
molasses diluted with 5 times its weight of water, de-
termine Brix on a portion of it and clarify another por-
tion with dry lead subacetate for the sucrose determina-
tion. The sucrose is gotten from special tables1 or
from the formula
26.121
Sucrose = R X — arr
100 X sp. gr. at 27.5 C.
An example of each of the above determinations
follows:
I — 86.67 g. molasses were dissolved in water and made up to 500 cc.
Weight of solution at 26.3° = 528.75 g.
Water capacity of the flask at 27.5" ■= 497.88 g.
528.75
Sp. gr. of solution = — gg = 1.0620 = 15.28 Brix = 15 19 Hrix cor-
rected for temperature.
528.75
15.19 X = 92.68 Brix of original mola
n cc. molasses solution after weighing were clarified with 30 g.
dij lead "■■- 'he following i
D = 34.96, I (26.3°) = — 14.94. Sucrose = 38.70, Gravity purity -
41.65.
Hawaiian Chemists' Association, "Methods of Chemical Control,"
Table I.
THE JOURNAL OF IX DUST RIAL AND ENGINEERING CHEMISTRY Vol. io, Xo. 3
II — A second sample was diluted with 5 times its weight of water.
Brix of diluted molasses by pyenometer at 26.2° C. = 15.51.
Brix corrected = 15.42.
Brix original = 6 X 15.42 = 92.52.
500 cc. of this diluted molasses were clarified with 30 g. dry lead and
Rave, when analyzed, the following results:
Direct reading (400 mm. tube) = 35.53.
Invert reading (26.3° C.) = —15.17.
Clerget reading = 39.32.
Sucrose (from tables) = 9.66.
Sucrose in original molasses = 9.66 X 6 X '/i X "V«oo = 38.64 per cent.
Gravity purity = 41.73.
SUMMARY
In an attempt to explain the discrepancies in results
obtained in Clerget sucrose determinations in waste
molasses, a large amount of experimental evidence
indicates that the method of clarification with lead sub-
acetate solution as recommended by the Hawaiian
Chemists' Association yields results from 0.5 to 0.7
per cent too high, this being mostly due to the large
volume occupied by the lead precipitate. Clarification
with dry lead subacetate gives figures more nearly ap-
proaching the true sucrose content of. the molasses,
but is apt to run a little low, especially if an excess of
lead is used in clarifying. A modification of the dry
lead method to overcome the dilution error is suggested,
and experimental proof of its correctness is offered.
College of Hawaii
Department op Sugar Technology
Honolulu, Hawaii
RELATION BETWEEN EFFICIENCY OF REFRIGERATING
PLANTS AND THE PURITY OF THEIR
AMMONIA CHARGE'
By F. W. Frericbs
Received January 5, 1918
Since writing this paper several months ago a sin-
gular case of unpreparedness has developed in the
ammonia trade.
As you all know, most ammonia is obtained as a by-
product from gas works and from coke oven plants.
In gas works and in the older coke oven plants the
ammonia is obtained by scrubbing the gas with water
and recovering the ammonia from the diluted gas
liquor by distillation, whereby free ammonia is ob-
tained, which may be used in the manufacture of
aqua and anhydrous ammonia and ammonium salts.
In the more modern coke oven plants the so-called
direct process is employed in which only so much
ammonia is obtained in the form of ammoniacal
liquor as condenses with the water distilling from the
carbonized coal. This amounts to only about 20
per cent of the total ammonia. The remaining 80
per cent is obtained by washing the gas with a slightly
acid solution of sulfate of ammonium in small appara-
tus. These plants produce therefore a large amount
of sulfate of ammonium, and they are not provided
with scrubbers by the use of which all ammonia
might bo obtained as ammoniacal liquor. This was
desirable in peace times because the larger part of
ammonium salts was used in the fertilizer trade in
the form of sulfate of ammonium.
But when the war demanded ever-increasing quan-
tities of nitrate of ammonium for explosives, the am-
1 Paper read at the 10th Annual Meeting of the American Institute of
Chemical Ungincers. St. Louis. Mo., December 5-8, 1917.
moniacal liquors were insufficient in quantity; and
although much sulfate of ammonium was available,
there was only one plant in the United States in which
aqua ammonia could be made from sulfate, and this
plant was entirely engaged in the manufacture of
ammonia for the refrigerating industry. And it had
become necessary to reconstruct this one plant to
adapt it to the use of crude ammoniacal liquor on ac-
count of the high price demanded by sulfate of am-
monium during the war. Upon request of the Food
Administration of the United States, remodeling of
the plant was temporarily abandoned and even a 50
per cent increase in capacity of the sulfate plant was
agreed to for the purpose of securing ample supply
for cold storage warehouses and ice plants, the Gov-
ernment aiding in obtaining a supply of sulfate of
ammonium at reasonable cost.
After this was arranged there arose a sudden and
large demand for ammonia for the manufacture of
nitrate of ammonium, and sulfate of ammonium be-
ing the only available material, it had to be manufac-
tured from this ammonium salt.
There exists the singular condition that we have
coking plants which are prepared to make much sul-
fate, but which can make only a limited amount of
ammoniacal liquor; and we have nitrate of ammonium
plants which can work ammoniacal liquor, but which
cannot make nitrate of ammonium from sulfate.
We have ample ammonia material, but we are utterly
unprepared to make nitrate of ammonium from it.
It is known that in England nitrate of ammonium
is made by double decomposition of sulfate of ammo-
nium and nitrate of sodium, but it is understood that
in this process about 20 per cent of the ammonia is
wasted. To investigate this process a Commission
went to England several weeks ago, and their report
by cable is expected now. But even in the case of a
favorable report, it is estimated that it will require
six months before works of sufficient size can be put
into operation.
Being familiar with the manufacture of ammonia
from sulfate, I was called to Washington to consult
with officials of the War Department. Complete
plans, patterns, assistance, and patent rights were
promptly offered and accepted for the purpose of
erecting new plants, each the size of our St. Louis
plant, a number of which are contemplated for the
various explosive works. We have the singular op-
portunity of witnessing unprecedented growth of an
industry which ^economically speaking) has outlived
its usefulness, and which after the war must die out,
being unprofitable under peace conditions.
Reconstruction of our St. Louis plant is being
carried on under great difficulties and I must ask
your indulgence if I show you this afternoon a sadly
disarranged plant, which must be operated while it is
being reconstructed. I had hoped to have the plant
finished for this convention, but Government demands
changed the plans, and if I wish to keep my promise
to you I must show the works as they are now.
The scarcity of ammonia is unprecedented and the
importance of saving ammonia has become para-
Mar., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
mount. Waste of ammonia must be prevented at
almost any cost, so much so that officials of the Gov-
ernment contemplate closing ice plants where waste
is permitted to continue.
For these reasons a report of the relation between
the efficiency of refrigerating plants and the purity
of their ammonia charge is of greatest interest at this
time, since it tends to prove that pure ammonia and
smallest waste of it are inseparable factors in the
operation of refrigerating plants.
When I visited the Loan collection of scientific
apparatus exhibited in Kensington Museum, London,
England, in 1876, I saw for the first time ice machines
on exhibit. They were small affairs, operated with
ether, carbon dioxide, sulfur dioxide, or with ammonia
by the absorption process.
In the years immediately following, Linde published
his classical investigations on the Ammonia Compres-
sion Ice Machine, laying thereby the foundation for
that type of refrigerating plants, which at present is
predominant here and abroad.
In 1880, when I arrived in the United States, arti-
ficial refrigeration was still in its infancy. But even
at that time the superiority of ammonia as a refrigera-
ting agent for larger plants, in preference to other
agents, was well established.
Liquefied ammonia gas, however, had not yet be-
come an article of commerce, and the compression ice
machines at that time had an attachment by which
liquefied ammonia gas could be made from aqua am-
monia. Aqua ammonia of great purity was not avail-
able and the quality of liquefied ammonia gas made
by non-chemists with simple apparatus in the ice
plant left much to be desired.
In a paper read before this Institute on the occasion
of its first annual meeting, I gave a full account of
the methods of analysis and the standards of purity
of liquefied ammonia gas up to 1908; and from this
account it would seem that in early times 2 per cent
impurity, or even more, was quite the rule. But in
those times the efficiency of refrigerating plants was
low. They were largely confined to wort cooling and
to cooling of storage rooms in breweries where con-
siderations other than economy were paramount.
Only when refrigerating machinery was utilized for
making ice in competition with natural ice, was greater
efficiency demanded, and this called for purer ammonia.
Refrigeration is not a chemical industry, and for
that reason chemists, as a rule, are not familiar with
the details of ice plants. But the importance of
chemical purity of the refrigerating agent cannot be
fully understood without reference to some details
of the plant in which it is used, and for this reason a
few words would seem justified to explain the function
of those parts of the apparatus which have a bearing
on the action of ammonia in ice machines. If these
are well understood, the importance of the purity of
the ammonia charge will become apparent and will
be easily appreci
In utilizing ammonia, the latent heat required for
evaporation of liquid ammonia is employed for the
production of "cold."
Liquid ammonia has a boiling point of — 28 ° F.
at atmospheric pressure. Its latent heat of evapora-
tion at o° F. is about 355 B. T. U., and this heat is
readily extracted from surrounding bodies having a
higher temperature than — 28 ° F., thus producing
"cold," which by suitable apparatus may be utilized
for the production of ice or for refrigeration.
The general arrangement of a refrigerating plant
is such that liquid anhydrous ammonia is evaporated
at a low pressure and a corresponding low tempera-
ture in a closed vessel which is submerged in a medium
like brine or air. In evaporating at low tempera-
ture, the ammonia extracts heat from this medium,
thereby lowering its temperature. The resulting am-
monia vapors are again reduced to the liquid state
by applying pressure and subsequent cooling in a
condenser, and the liquid anhydrous ammonia is re-
turned to the cycle of operations.
Refrigeration by ammonia is therefore a physical
process and in theory the chemical composition of
ammonia in the cycle of operation remains unchanged.
The transformation of ammonia from the liquid to
the gaseous state and vice versa can go on indefinitely
and, theoretically, a given amount of ammonia can
produce an infinite amount of "cold."
Any set of apparatus constituting a refrigerating
plant using ammonia for an agent includes, therefore,
a device in which liquid ammonia is evaporated and a
device to reduce ammonia from the gaseous to the
liquid state. The first operation, as a rule, takes place
in a pipe-coil which is submerged in the medium
which is to be cooled. The second operation can be
carried out in different ways, and from the method
employed, refrigeration plants are classified as absorp-
tion or compression plants.
In absorption machines the ammonia gas is absorbed
in cold, weak aqua ammonia to make strong aqua am-
monia of about 30 to 35 per cent. This operation is
carried out in the absorber. The resulting strong
aqua ammonia is forced by a pump into the retort or
boiler to be heated to about 1500 C, whereby it
splits into weak aqua ammonia, 15 to 18 per cent,
and hot ammonia gas standing under a pressure of
150 to 250 lbs.
The hot gas under this high pressure is led into the
condenser to be cooled and thereby liquefied, producing
in good plants liquid ammonia of 95 to 98 per cent
purity, the balance being water, which had evaporated
with the ammonia. The weak aqua ammonia is re-
turned to the absorber.
In compression machines, the ammonia gas com-
ing from the evaporating or freezing coil is taken by
suction into the ammonia pump, whereupon it is com-
pressed to 150 to 250 lbs. pressure per sq. in.; the
gas, hot from compression, is delivered to the cooler
or condenser to be liquefied to ammonia of approxi-
mately 100 per cent purity, which is to be delivered
again to the freezing coil, thus completing the cycle
of operation.
Comparing the principles involved in absorption
and compression machines, it is apparent that appara-
tus in which evaporation of liquid ammonia takes
204
THE JOURNAL 01 INDUSTRIAL AND ENGINEERING < EEMISTRY Vol. 10, Xo. 3
place at low temperature and low pressure, and the
condenser or cooler in which hot ammonia gas of
high pressure is reduced to the liquid state, are alike
for both types of refrigerating machines. The expan-
sion valve between the two apparatus and the valves
in the pump separate the high-pressure side from the
low-pressure side of the machine.
In compression machines the ammonia pump han-
dles ammonia in the gaseous state. The pump is
large on account of the great volume of ammonia gas
"tyA ftnssurr 3itt*
dbsorpfwn ffanf.
Fig. I
and its suction side has the same function as the ab-
sorber in absorption machines. The compression
side has the same function as the aqua ammonia
pump and the retort or boiler in absorption machines
combined, and it delivers ammonia gas under high
pressure to the condenser or cooler. In absorption
machines the ammonia pump is comparatively small,
since it handles ammonia in the liquid state, viz., in
the form of aqua ammonia which has a smaller volume
than the equivalent amount of ammonia gas. The
pump operates on cold aqua ammonia and does not
require lubrication of the pistons.
In compression plants, the ammonia pump is large,
operates on hot ammonia gas, and requires generous
lubrication of cylinder pistons. Therefore, in com-
pression machines, the lubricants require serious at-
tention.
The arrangement of the fundamental apparatus in
both types of machine is illustrated by the diagrams
Figs. I and II.
The object of both types of plant is to abstract
heat from the low pressure or evaporating side and to
deposit the same heat at the high pressure or con-
denser side. This transfer is accomplished by evap-
orating liquid ammonia at low temperatures, subse-
quently compressing the resulting ammonia vapors
either by application of heat in the retort of absorption
machines, or by application of power in compression
plants, and to deposit the heat which was extracted
at the low-pressure side in the condenser on the high-
pressure side, whence it is carried off by cooling water
which runs through the condenser.
The amount of heat used in the retort of an absorp-
tion machine or the amount of power consumed in a
compression plant multiplied by a constant is a measure
of the amount of refrigeration actually produced. The
value of this constant is the product of many factors,
one of which is the free and ready evaporation and
condensation of ammonia in the machine. All other
conditions being equal, the evaporation and condensa-
tion of liquid ammonia goes on most freely if the am-
monia is pure. If it contains substances either in
suspension or in solution, which retard evaporation
or which cause ammonia to boil only in a superheated
condition, or which retard the transmission of heat
to the ammonia, then the efficiency of the machine is
impaired. For this reason ammonia of high purity
will produce better results than impure ammonia.
Many impurities which retard evaporation are solu-
ble in ammonia and are less volatile than liquefied
ammonia gas. For this reason they may be detected
by the evaporation test. An account of this test
was given in an earlier ins actions I, page
133). But there are many substances less volatile than
ammonia, which are harmless and do not impair the
speed of how up in the evapora-
tion test. To distinguish between harmful and harm-
less impurities in this regard, the apparatus shown in
Fig. Ill was used to measure the time of evapora-
tion of a definite quantity of liquid ammonia under
constant conditions. The apparatus is made of glass
and consists of a cylindrical evaporatin
graduated on its side and having at its lower end a
Mar., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
2°5
narrow tube, B, in which liquid residues from evapora-
tion may accumulate. The upper part of A is drawn
out to a small cylindrical part, C, with tube D inserted
which serves to connect the apparatus with the nozzle
of the test valve on the ammonia shipping cylinder.
E is an outlet tube for discharging ammonia vapors
coming from the apparatus. A is surrounded by
jacket F, which is joined to tube B, and a piece of sheet
rubber having a round opening in the center is slipped
over tube C and is tied over the upper rim of jacket F
to make an air-tight connection. The air between
A and F must be dry. The lower part of the tube
B is surrounded by an evacuated bulb, H, and the en-
tire apparatus is set in a bath of a 20 per cent solu-
tion of calcium chloride, /, provided with agitator,
K, and thermometer, L, which serve to maintain a
uniform temperature in the apparatus. The calcium
chloride solution is contained in a glass jar, M, which
stands in a bath of ice water and crushed ice.
In evaporating, the ammonia takes heat from the
solution of calcium chloride, which in turn takes heat
from the melting ice. The object of the apparatus is
to make the transfer of heat to the ammonia uniform,
in order to make time the measure of evaporation.
Dry air in jacket F and the vacuum in bulb H being
bad conductors, all heat must travel through the glass
walls of tube B between a and b, which represents
the heating surface of the apparatus. Tube B ex-
tends into bulb H to serve as the receptacle for resi-
dues of evaporation, which may accumulate in this
place, without reducing the area of the heating sur-
face of the apparatus.
The operation of the apparatus is self-evident. By
operating the valves on the ammonia cylinder, the
apparatus is filled to the 100 cc. mark, whereupon
evaporation of the ammonia takes place regulated by
the amount of heat which travels from the calcium
chloride solution through the walls of tube B to the
ammonia.
When the ammonia in A is evaporated to point c,
the time of evaporation is noted, together with the
temperature of the calcium chloride bath, whereupon
a new charge of ammonia is admitted by filling the
apparatus up to the 100 cc. mark, and any number
of additional charges of liquid ammonia may be evap-
orated. In repeating the operation, the impurities
in the ammonia are concentrated and the time neces-
sary for the evaporation of successive portions is a
measure of the increasing amounts of impurities in
the ammonia.
Tables I and II give the results of two series of ex-
periments, one of which is made with pure ammonia,
similar to quality B in Table III, on page 209; the other
with less pure ammonia, resembling in composition
quality // in the same table.
Comparing the values in the two tables, it would
seem that the velocity of evaporation of liquid am-
monia is not affected by the presence of such small
amounts of impurities as are contained in sample H.
However, the velocity of evaporation decreases rapidly
as soon as the oily material, which separates in increas-
ing quantities from the ammonia in successive tests,
increases in volume, covering part of the heating sur-
face of the apparatus, and the table shows also that
by the time the entire heating surface is covered with
oily material the velocity of evaporation is reduced
by 50 per cent.
Among the substances not soluble in liquid ammonia
but always present in compression plants, is lubri-
cating oil from the compressor. Its retarding action
rests in its low coefficient of conductivity for heat.
If it enters the condenser it coats the inside of the am-
monia pipe, but owing to the high temperature the
oil is very liquid and the coating is thin. Neverthe-
less, the thin coating of oil in the condenser retards
the transfer of heat, but the amount of retarda-
tion is small and can be overcome by increasing the
pressure on the discharge side of the ammonia
pump. If the plant is operated at 200 lbs. pressure,
S lbs. of which is used for overcoming the retardation
caused by the coating of oil, then the loss of efficiency
for the sake of argument may be assumed to be 2V2
per cent.
Conditions in the evaporating coil are widely differ-
ent. The evaporating coil is cold, the oil is thick, the
coating of the walls inside the pipes is heavy, and con-
sequently the retardation is large. If in this place
the pressure is 15 lbs. per sq. in., and if it must be
reduced by 5 lbs. to overcome the retardation in the
travel of heat, then the loss of efficiency must be counted
as 33V3 per cent instead of 2V2 per cent, as was the
case in the condenser. For this reason the evapora-
ting coil must be kept free of lubricating oil.
Table I— Evaporating Test of Liquid Anhydrous Ammonia
Purity Similar to Sample B in Table III
Calculated
Time of
100 cc. Evaporation
Tempera- Evaporated Tempera- at 15 Lbs.
turE, Deo. Duration ture DEO. Pressure,
F. at Start of Test F. at End 15° F.
1914 Air(a) Water Brine Minutes Brine Water Air(o) Minutes
July 21 90 38 42 130 28 38 90
90 38 28 140 28 40 90 570
90 40 28 135 26 38 90 540
90 38 26 140 26 38 90 549
Average ;'■•■;"■•, $M
July 22 95 42 46 125 30 42 95 ...
' y 95 42 30 135 28 38 95 559
95 38 28 140 28 38 95 570
95 38 28 135 28 38 95 549
JulyR2A3GE 95" '46' ' ' 46 125 30 ' ' W ' 95 ...
95 40 30 130 28 40 95 538
95 40 28 140 28 36 95 570
95 36 28 140 28 36 95 570
Average ■ „■ • • w ' • "«-. 559
Tulv 24 97 42 48 125 28 36 97
1 Y 97 36 28 135 26 34 97 S40
97 34 26 140 26 34 97 549
97 34 26 140 26 34 97 549
Average *tl
Grand Average *f *
Probable Error ±2.5 ± '»
(a) Average temperature of air.
Note — No residue accumulated in the lower part of tube B, therefore
any number of evaporations of new quantities of ammonia could be earned
out with the same results. Evaporation of the first sample on every day
was not considered, because the high temperature of brine made results
irregular.
The evaporated ammonia is withdrawn from the
freezing coil by the absorber in absorption machines,
or by the ammonia pump in compression plants.
Here again the efficiency is greatest if the ammonia
is pure. If the ammonia is contaminated with gases,
which cannot be absorbed by water, then these gases
will accumulate in the absorber in the case of absorp-
2o6
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 3
Table II — Evaporating Tbst of Liquid Anhydrous Ammonia
Purity Similar to Sample // in Table III
Calculated
Time of
100 cc. Evaporation
Tempera- Evaporated Tempera- at 15 Lb.
jture, Dec. Duration Turk, Dec. Pressure
F!
at Start
of Test
F„
at End
15° F.
1914
Air (a)
Water Brin
Minutes
Brine
Water Air(a)
Minute.
Aug. 15
88
42
52
130
28
38
88
88
38
28
150
26
36
88
540
88
36
26
150
26
36
88
520
Aug. 17
94
42
50
135
28
38
94
94
38
28
150
28
38
94
560
94
38
28
150
26
34
94
540
94
34
26
150
26
34
94
520
Aug 18
95
40
50
140
28
36
95
95
36
28
150
28
36
95
560
95
36
28
150
28
34
95
560
95
34
28
150
28
34
95
560
Aug. 19
93
40
50
140
28
36
93
93
36
28
150
28
36
93
560
93
36
28
150
28
36
93
560
93
36
28
155
28
36
93
579
Average
550
Oily liquid at
a, Fig.
III
Aug. 20
88
48
54
140
28
38
88
88
38
28
155
28
36
88
579
88
36
28
155
28
36
88
579
88
36
28
155
28
34
88
579
Aug. 21
90
50
58
140
28
36
90
90
36
28
155
28
36
90
579
90
36
28
160
28
36
90
597
90
36
28
160
28
36
90
597
Aug. 24*
75
48
58
155
28
38
75
75
38
28
195
28
36
75
75
36
28
200
28
36
75
747
Aug. 25
70
50
58
205
28
36
70
70
36
28
205
28
36
70
765
Aug. 26
81
40
52
205
28
36
81
81
36
28
220
28
36
81
82 i
Aug. 27
75
50
58
225
28
36
75
75
36
28
235
28
36
75
877
Aug. 28
70
40
48
250
28
36
70
70
36
28
260
28
36
70
97 i
Aug. 29
44
50
265
38
36
36
28
270
28
36
1008
Aug. 31
44
50
260
30
36
36
30
275
30
36
1063
Sept. 1
42
52
270
30
34
34
30
285
30
36
U02
Oily liquid at b
Fig. HI
Sept. 2
46
54
280
30
34
34
30
295
30
34
liii
Sept. 3
36
38
285
30
36
36
30
295
30
36
liii
Sept. 5
50
54
290
30
36
36
30
295
30
36
liii
Probable Error
±2.5
±10
(a) Average temperature of a
tion machines and cause pressure, which prevents the
ready flow of ammonia gas towards the absorber,
whereby the efficiency of the plant is reduced.
In the case of compression machines, any gases not
ammonia will fill space in the cylinder of the ammonia
pump, and will reduce the efficiency of the pump in
direct proportion to the volume of such gases present.
If the ammonia gas contains io per cent of such
gases, then the efficiency of the pump will be reduced
by io per cent.
More serious is the presence of non-condensing
gases in ammonia at the compression side of the
machine. In both absorption and compression plants,
the gas under high pressure enters the condenser to
be liquefied. Liquefaction depends upon the pres-
sure and temperature in the condenser. The tempera-
ture being largely invariable since it is dependent upon
the temperature of the cooling water, the efficiency
of a given plant depends largely upon the pressure of
the ammonia gas alone.
Pure ammonia gas condenses to liquid ammonia at
lowest pressure at a given temperature. If the am-
monia gas is contaminated with gases of a non-con-
densing nature then the pressure necessary for con-
densation of the ammonia in the gas mixture is in-
creased, according to well-known physical laws. The
increase of pressure is in direct proportion to the amount
of non-condensing gases present. If the ratio of am-
monia to other gases is i to i, then twice as much
pressure is required for its condensation as for the
condensation of pure ammonia.
This applies both to absorption and compression
machines. It becomes serious if the space which is
occupied by the gases in the condenser is small. Double
pipe condensers, which are mostly used, have a very
small condensing space, measuring at an average
12 cu. in. per ft. of pipe. The ammonia in a gas mix-
ture forced into a condenser is liquefied and with-
drawn while the contaminating non-condensing gases
remain, gradually filling the condenser in cumulative
action and paralyzing its efficiency. For this reason
ammonia of high purity will produce superior results.
The non-condensing gases mixed with ammonia
may be air and in this
case they are easy to
detect. An apparatus
for measuring them is
published in Vol. VI.
p. 214, of our Trans-
actions. But there
may be other impuri- j
ties in ammonia,
which, liquid in them-
selves, may produce
non-condensing gases
in ice machines, and
many of these sub-
stances are difficult to
detect by analysis.
Therefore, the con-
sumer must largely
rely upon the reputa-
tion of the ammonia
manufacturer who
stands for the quality
of his goods.
There is another
source from which
non-condensing gases
may develop in com-
pression machines,
and it must be well
understood that not in
all cases is the quality
of ammonia responsi-
ble for the presence of
non-condensing gases
in the machine. The oil used for lubricating the com-
pressor mixes intimately with the ammonia and if it
contains substances, which at temperatures prevailing
in the machine develop permanent gases, then these con-
stituents of the oil act in the same manner as if they were
brought in with t he ammonia charge. Fortunately most
oil is good in this respect . and particularly the cheaper
grades of compressor oil give good satisfaction. How-
ever, there is oil on the market which is undesirable,
and operators of ice machines do well to make sure
of the good quality of the oil they use in their machines.
A simple apparatus for testing oil in this respect
is represented by Fig. IV. It is operated as follows:
Mar., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
207
:'!<:!
With the stopper removed, the bulb tube is filled
entirely with the oil which is to undergo the test,
whereupon the stopper is firmly inserted and the ex-
cess oil removed from the funnel over the stopper.
Upon heating in a metal bath, undesirable oils will
develop gases which will accumulate under the stopper,
while an equivalent volume of oil is forced through
the capillary tube into the funnel
over the stopper and the volume
of gas may be measured by the
graduation on the tube.
If non-condensing gases
accumulate in the machine, it
becomes necessary to remove
them and the operation of doing
this is called purging.
Purging is generally done by
opening a small valve on the top
of the condenser, or absorber,
or both. The gases which always
contain a large proportion of
ammonia may be led by a tube
under water, whereby ammonia
is absorbed, the permanent gases
rising in bubbles to the surface
of the water. If no bubbles form,
all the non-condensing gases are
removed, and purging is com-
pleted. Another way of purging
is to let the gases escape into the
air and ignite them by a torch,
in which case they burn with a
luminous flame which dies out as
soon as pure ammonia flows from
the orifice. With pure ammonia
in the machine, purging may be
done at long intervals of time,
while with impure ammonia daily
purging becomes a necessity.
There is finally a class of im-
purities found in ammonia which
causes J corrosion of iron, from
which ice machines are made.
This occurs more frequently in
absorption plants, where corro-
sion often destroys parts of
machinery, causing leaks, and
subsequent loss of ammonia dur-
ing operation.
Acetic acid, acetonitrile, and
similar compounds belong to
this class of impurities, and they
are frequently found in aqua
FlG- v ammonia. A small amount of
acetic acid can corrode large quantities
by hydrolysis, since the acid always is regenerated.
The chemical action on parts of apparatus is illustrated
by two tubes represented in Fig. V and Va. Both
tubes were used for four years in two absorbers, the
one in pure, the other in impure, aqua ammonia. The
one has lost hardly any of its weight, while the other
■ roded to a thin shell.
of iron
In absorption machines the heating coils in the re-
tort are most seriously affected by impure ammonia.
Fig. VI represents the lower part of a retort con-
taining a double heating coil. The coil is made from
iVa-in. extra strong iron pipe, and weighs about 1200
lbs. If used with pure aqua ammonia, it will last
many years, while with impure ammonia frequent re-
newal becomes imperative. I hold records about
coils of this particular size, which in a single year
lost as much as 100 lbs. of their weight by corrosion
if used with impure ammonia, and I have records of
other coils of the same size which were used for as
much as 10 years with pure ammonia under the same
conditions as the first-mentioned coils and which lost
less than 5 lbs. of their original weight.
How seriously the efficiency of an ice plant can be
affected by impure am-
monia is strikingly dem-
onstrated by the results
which were obtained in
the operation of two new
and identical absorption
ice machines, operated
in parallel and inde-
pendently of one another
by the same steam plant,
by condensing water of
the same temperature,
and by the same set of
engineers,- but charged
with an equal quantity
of ammonia of different
purity. Both qualities
of ammonia were goods
offered in the regular
market and were pur-
chased by the manu-
facturer of the two ice
machines for the purpose
of making a comparative
test of the ammonia.
The operations were con-
ducted under the direc-
tion of the manufacturer
of the ice machines and
by the proprietors of the
plant, who were disinterested parties. Each of the two
ice machines had a capacity of 5° tons and there was
an independent ice- tank for each machine. The test
was run over a period of almost 17 months, beginning
June 6, 1914, and terminating October 31, 1915.
The first charge of each machine consisted of 16,500
lbs. aqua ammonia, 26° Be\, and 3855 lbs. liquid an-
hydrous ammonia. During the 17 months of opera-
tion 375 lbs. aqua ammonia 260 B6. and 775 lbs. liquid
anhydrous ammonia were added to replenish the
charge in Plant No. 1, and on Oct. 31, 191 5- after 17
months' operation, the charge was approximately
of the same strength as at the beginning of the test
run. The machine was operated 24 hrs. per day ex-
cepl between seasons, when it was run in day time only,
vintcr, when it was shut down. Ice was drawn
2o8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 3
at the rate of 55 tons per day during about 8 months
and refrigeration was supplied to the ice-storage room
estimated to be equivalent to 3 tons of ice per 24 hrs.
in the warm season of the year. The plant ran regu-
larly about 13 per cent overrated capacity. A total
of 15,862 tons of ice was pulled, and counting the
refrigerating done as equivalent to 1000 tons, 16,862
tons of ice were produced in 17 months at an expense
for ammonia amounting to 1.27 cents per ton of ice.
Nineteen tons of ice were made for every pound of
ammonia lost in operating the plant.
No serious leaks were observed in the plant. Small
quantities of permanent gases were burned off during
the first weeks of operation, giving a flame about 3 in.
long from a 3/s-in. pipe. No gas was purged off dur-
ing the following four months and in the second sum-
mer a flame of only about l/j in. length could be burned
from the purge tube at intervals of time and then only
for a few minutes.
A sample of aqua ammonia drawn from the machine
after a 17 months' run was clear as water and it is be-
lieved that no corrosion whatever has taken place in-
side the plant. This, however, can be confirmed only
by opening the apparatus, which will probably not be
necessary for several years to come.
The result of this run is remarkable if it is com-
pared with the result in Plant No. 2. This plant was
started June 22, 1914, 18 days later than Plant No. 1.
With the same quantity of ammonia, bought from a
different manufacturer and used for the initial charge,
Plant No. 2 could produce only 42 to 44 tons of ice
while Plant No. 1 had made 57 tons. Upon the ad-
dition of 1000 lbs. anhydrous ammonia, 50 tons of
ice could be made per day in No. 2.
From June 22, 1914, to November 1, 1915, that is,
in about 16V4 mo., 13,183 lbs. aqua ammonia, 260 Be.,
and 3484 lbs. anhydrous ammonia were used in ad-
dition to the initial charge, and at the end of the period
the ammonia charge in the machine was about 1000
lbs. short on ammonia. 11,308 tons of ice had been
made during the period and the cost of ammonia per
ton of ice was 15.16 cents, as against r.27 cents in
Plant No. 1. One and one-third tons of ice were
made for every pound of ammonia lost in operating
the plant.
Serious leaks were observed after a few weeks'
operation in the screw connections of the pipes and
condensers, caused by corrosive action of the ammonia.
Large quantities of permanent gases were burned off
daily during the entire period of operation, giving a
flame of as much as 3 in. diameter, and over 24 in.
long, and this flame would burn from 20 to 30 min.
at a time. The excessive consumption of ammonia
was caused by leaks and purging.
A sample of aqua ammonia drawn from the machine
after 16 months' operation was dark and dirty, and
no doubt considerable corrosion had taken place in-
side the apparatus.
Plant No. 1 had made during the test period an
equivalent to 16,862 tons of ice, while Plant No. 2
made 11,308 tons, a deficiency of 33 per cent, and this
deficiency must be attributed alone to the difference
in quality of the ammonia charge.
The consumption of coal in Plant No. 1 was ascer-
tained to be one ton of Illinois coal to eight tons of ice,
while in Plant No. 2 only 51/? tons of ice were made
per ton of coal, consumed under the boiler.
Similar differences in efficiency were experienced in
many plants, which led to the belief that the quality
of the ammonia charge had an important bearing
upon the operation of ice plants. There were no
methods of analysis known to be delicate enough for
the purpose of differentiating between the quality
of different brands of ammonia, and it seemed to be
of sufficient importance to have methods of analysis
developed even at great cost for the best of the refrig-
erating industry. Upon the request of the American.
Association of Refrigeration, Congress appropriated
S30.000 to be put to the credit of the Bureau of Stand-
ards, which sum was to be used for the development
of methods of analysis of commercial ammonia and
for the determination of physical constants of re-
frigeration.
The composition and testing of commercial liquid
ammonia was admirably investigated by E. C. Mc-
Kelvy and C. S. Taylor, both of the U. S. Bureau
of Standards, Washington. D. C, by experiments
equal in accuracy to determinations of atomic weights.
A progress report on the result of 2 years' work
was presented at the twelfth annual meeting of the
American Society of Refrigerating Engineers in De-
cember, 1916, and published in their journal for March,
1917.
The report describes in detail methods of sampling
and methods of analysis for the quantitative deter-
mination of, first, non-condensing gases; second,
residue on evaporation: third, volatile impurities
containing carbon; fourth, water; fifth, pyridine;
sixth, acetonitrile and ammonium acetate; and seventh,
direct determination of ammonia.
McKelvy and Taylor made by these methods a
series of comparative tests on eleven samples of liquid
anhydrous ammonia made by ten different manufac-
turers and tabulated the results. The eleven sam-
ples were marked by letters of the alphabet from A
to 5. Samples .1 to // represented eight standard
American brands provided in 50- to 100-lb. cylinders.
They were obtained either by purchase in the open
market, or by purchase or donation from manufac-
turers, and are believed to represent fairly well the
materia] now used in the refrigerating industry.
Samples A", L and LL were of German origin, L
having been purchased in 1906. Sample M was an
American product purchased in 1907. Sample 5
was prepared from Sample B by several fractional
distillations, the first of which was made from metallic
sodium.
The results of the comparative tests are given in
Table III, opposite the letter indicating the origin
of the sample. The column headings show the nature
of the test and the manner of expressing the results.
As to the limit of accuracy of the figures given in
Mar., 191S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
209
the table, it was found that in the case of volatile
carbon compounds the results were too low. Fifty-
eight grams of pure ammonia, mixed with 3 mg.
acetonitrile, yielded 95 per cent of the carbon in the
combustion test, while 58 g. of ammonia mixed with
15 mg. acetonitrile yielded only 67 per cent of the
calculated amount of carbon dioxide, owing to incom-
plete combustion in the experiment. For this reason,
the values given in the table for Samples B and K
are fairly correct, while the amounts of carbon dioxide
obtained from other samples were much too low,
probably by 40 to 100 per cent. In the case of pyri-
dine, the limit of accuracy was found to be 1 in 100,000,
rABL
s III-
-COMP
3SITION
op Liquid Anh
YDROUS
Ammon
AS
Volatile
Non-Condensing G
AS
Residue
CCom
In
In
on
pounds
Liquic
Gas
Evapora-
Water
Cc.
Cc.
Composition
tion
G. CO*
Method Method
Per
Per
Ni
O2
H2
By
Per
KOH
CaCi
Sam-
100
100
Per
Per
Per
Weight
100 g.
Per
Per
ple
g.
g-
cent
cent
cent
Per cent
NHs
cent
cent
A
7
69.1
30.9
0.0
0.012 h
0.019
0.006
0.013
26
86.7
13.3
0.0
0.007 (
0.001
B
4
70.8
29.2
0.0
0 . 009 h
o!6o2
0.007
o!642
"9
70.0
30.0
0.0
0.011 I
0.008
C
'6
70.3
29.7
0.0
0 . 008 h
0^051
0.007
o!6io
"8
69.4
30.6
0.0
0.008 I
0.005
D
'6
68.4
31.6
0.0
0.014 h
0.029
0.006
oioio
' \2
72.6
27.4
0.0
0.017 (
0.004
E
6
65.0
35.0
0.0
0.011 h
o!6i9
0.006
oioio
ii
74.0
26.0
0.0
0.010 I
0.006
F
is
67.0
28.7
4.0
0.015 h
o!6ol
0!626
8032
80.1
19.9
0.0
0.022 I
G
6
70.0
27.0
3.0
0.025 h
o!032
o!6o7
o!626
"9
68.0
26.0
6.0
0.100 ;
0.009
H
6
66.7
33.3
0.0
0.062 h
o!902
0.010
0l027
ii
66.7
33.3
0.0
0.134 I
0.010
K
69.0
31.0
Trace
0.276 h
o!6o4
0.011
0!80
19
80.0
20.0
Trace
0.300 (
0.032
L
9
77.5
22.5
0.0
0.533 h
0i497
0.041
0^50
5680
99.4
0.6
Trace
0.540 ;
0.069
LL
is
79.0
21.0
0.0
0.318 h
o.'io3
0.053
0^33
1870
99.3
0.7
0.0
0.230 1
0.040
M
0.040 h
0.051 ;
o!6i4
0.011
S
0.000
0.000
0^008
(h) Evaporatit
>n at ro
om temperature. (/) Ev
aporation at low tempera-
and for acetonitrile and ammonium acetate quanti-
ties less than 5 in 100,000 could not be detected.
In addition to the results in the table, McKelvy
and Taylor point out the following data of interest:
Sample F contained a trace of pyridine and sample
H 0.02 per cent. The German Samples L and LL
contained 0.015 Per cent and 0.005 Per cent, respec-
tively. All others contained less than 0.001 per
cent.
In the samples showing a low residue on evapora-
tion {A to E), the residue consisted of a reddish film
hardly visible. For the other samples at most a brown-
ish drop of oily liquid was left, and only for Samples
A", L and LL could the volume of the results have
been measured. The percentage of iron oxide in
the residue was greater, the smaller the amount of
residue in the sample.
Sample F contained 0.005 per cent ammonium
acetate or acetate-forming substance, and Sample L
a trace. All others contained less than 0.005 Per
cent.
The r< e combustion tests showi
difference in the various samples, but in practically
all of the tests McKelvy and Taylor observed that no
carbon dioxide appeared in the absorber until at least
95 per cent of the liquid had evaporated.
In making this observation, the Bureau of Stand-
ards in 1916 disclosed the fact that small quantities
of volatile carbon compound can be concentrated
into a small volume of liquid anhydrous ammonia by
fractional distillation. The Badische Company observed
the same fact and patented its invention in 19 13.
The same process was discovered and put into
operation in 1892 in these works and has been in
successful operation ever since. While inspecting
our works this afternoon you will have an opportunity
of seeing the first apparatus used in 1892 and the pres-
ent plant comprising 5 compressors and 3 stills capa-
ble of redistilling 25,000 lbs. of liquid anhydrous am-
monia per day of 24 hours. The product corresponds
in quality to Sample B in the table, the volatile car-
bon compounds of which are so small that by burning
100 g. ammonia only 0.002 g. carbon dioxide could
be obtained, which indicates that less than 0.001
per cent volatile carbon compounds could have been
in the ammonia.
Sample A' in the table, which comes nearest to B,
was ammonia made in Germany by the Haber process
and was evidently redistilled since the Badische Com-
pany holds a patent for purifying ammonia from the
Haber process by fractional distillation.
The importance of this investigation is emphasized
if I state that in the test run with the two 50-ton
machines described in this paper, Plant No. 1 was
charged with ammonia which in quality was equal
to Sample B in the table. The aqua ammonia for the
prime charge of this machine was also made by satura-
ting pure distilled water with ammonia of purity B.
Plant No. 2 was charged with aqua ammonia of
unknown purity. The same brand, however, has
given good satisfaction in other instances. But I
have reason to believe that the liquid anhydrous am-
monia in this charge was similar in quality to Sample
H, and from this the conclusion might be drawn that
the difference in efficiency of the two plants was caused
by the difference in purity of the ammonia charges
and more particularly by the presence of volatile
carbon compounds in the ammonia.
It is to be hoped that this progress report of the
Bureau of Standards may soon be followed up with
a complete account. The remaining part of the re-
port will include an investigation and analysis of aqua
ammonia, a most difficult problem, and at the same
time, a problem of the greatest importance for the
operation of absorption ice machines. At the pres-
ent we possess no method of analysis sensitive enough
to ascertain small quantities of impurities in aqua am-
monia, and enormous sums of money are constantly
being lost in the operation of absorption ice machines
on account of impure ammonia.
The only way to minimize these losses at the pres-
ent time would seem to be in using liquid anhydrous
ammonia of known purity and pure distilled water
for charging absorption plants. But attention should
be paid to the quality of distilled water, which rarely
of sufficient purity to answer this purpose.
Here in St. Louis, we are fortunate to have a supply
of city water which upon a single distillation yields
an excellent product for use in making aqua am-
monia. In the city water plant, Missouri River
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 3
water is first purified by sedimentation, after the sus-
pended matter has been coagulated by sulfate iron
and lime. A subsequent filtration by sand filters
removes the last suspended matter and oxidation
with chlorine removes bacteria.
From water obtained by distillation of St. Louis
city water, and liquid anhydrous ammonia of purity
B, my company is manufacturing pure aqua ammonia
for use in absorption ice machines, and aqua ammonia
used in the test run in Plant Xo. 1, which was de-
scribed before, was aqua ammonia of this purity.
Reverting to the question of analysis of aqua am-
monia, it is believed that the quick detection of minute
quantities of volatile substances which render aqua
ammonia unfit for use in refrigerating machines will
hardly be accomplished by chemical analysis. It is
most likely that methods have to be resorted to which
are based upon physical principles and which reveal
actions of such impurities, although they do not dis-
close their identity. In looking over the literature
on the subject, I found a statement by G. Tammann
in his investigation on vapor tensions1 that apparently
the increase of vapor tension of volatile substances
following a decrease in space, which is occupied by
the same vapors, is caused by minute impurities, and
it would seem possible to use this observation for a
method of testing volatile substances for purity.2
This remark is prompted by the observation of A.
Wullner and O. Grotrian3 that the vapor tension of
volatile substances increases if the vapor volume is
decreased.
Wullner and Grotrian found the increase of vapor
tension for water smaller than for other volatile sub-
stances, yet it would be 5-10 mm. if the vapor vol-
ume was reduced from 1/i to l/io of the original vol-
ume.
G. Tammann has repeated these experiments, and
has found that there is no increase of vapor tension
caused by decrease of vapor volume for water, if it
is pure, and he succeeded in making water of sufficient
purity to prove this fact.
For ether and carbon bisulfide he could materially
reduce this irregularity by purifying the substances,
but he could not make them sufficiently pure to show
the same tension at varying volumes.
From this Ostwald4 draws the conclusion that no
substance except water has ever been made of abso-
lute purity.
G. Tammann then suggests that this observation
might be used for a method of testing volatile sub-
stances for purity and Ostwald states4 that one part
benzene in 10,000 parts of water can be detected in
this manner.
It has occurred to me that these observations
may be used for determining volatile impurities in
aqua ammonia in the following manner:
1 ilimoires de V Academic des sciences de Si. Petersburg VII. serie tome
SB, No. 9 (1887). 18.
• Compare Ostwald, AUtem. Chemie. I, 306-309.
' Wiedemann. Annalen. 11 (1880), 600.
• AUtem. Chemie. I, 309.
Two barometers are combined in one apparatus,
one of which is charged over mercury with a solu-
tion of pure sulfate of ammonium and pure water, the
other with aqua ammonia, which is to be tested,
and which previously was neutralized with pure sul-
furic acid to make a solution of ammonium sulfate in
water of the same concentration as the solution charged
into the first barometer; and then the relative vapor
tension in the two
barometers at
various tempera-
tures is determined.
To prove the pos-
si bi 1 i t y of this
method, apparatus
shown in Fig. VII
was constructed,
having two barom-
eters in a narrow
space allowing of
uniform heating of
both barometers.
Two barometers
were made from one
length of glass tub-
ing which was
equally wide at
both ends. The
tube was drawn out
to a point in the
center and both
points were closed.
Therefore both
barometers were
equally wide near
the closed end of
the tube and i cc.
of mercury filled
22 mm. of the
barometer tubes.
For making the test
both tubes were
filled with mercury
and the air was
removed by re-
peated evacuation,
and filling up with
mercury. A 25 per
cent solution of
pure sulfate of
ammonium in
water was prepared
from which air was
expelled by boiling,
and methyl orange
was added to prove acidity. 2.5 cc. = 2.S25 g. of
this solution were introduced into each barometer,
and in Barometer B 0.015 %■ benzene enclosed in a
small flask was also inserted, whereupon the follow-
ing readings were taken at various temperatures
and various pressures.
Table IV shows that 0.003 per cent benzene can
Mar., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
easily be detected in 25 per cent solution of ammonium
sulfate by use of this apparatus:
Table IV
Difference in
1 mm. Indies
Temp.
Barometer
Benzene
Deg. C.
B — A - mm.
Per cent
20
52
0.0106
27
77
0.0071
35
105
0.0051
45
148
0.0038
60
184
0.0030
70
200
0.0027
80
215
0.0026
I am well aware that the apparatus and experi-
ments which I have presented to you are in no way
exact and complete in the way physicists will look
at them, and I would hesitate indeed to present them
for publication in a physical journal. In no way
can they compare with the investigations of H. C.
Dickinson and N. S. Osborne of the U. S. Bureau
of Standards on the constants of refrigeration.
But incomplete as they are, they have served me
as guides in the manufacture of pure ammonia
for use in ice machines, and I find satisfaction in the
assurance that the most painstaking investigations
of McKelvy and Taylor have confirmed the fact that
commercial liquid anhydrous ammonia of such purity
is made that it is more worthy of the designation
"chemically pure" than many other chemicals which
are sold at a high price as chemicals of highest purity.
4320 Washington Boulevard
St. Louis, Missouri
TESTING NATURAL GAS FOR GASOLINE
By G. G. Oberjell
Received July 5, 1917
CASING-HEAD GAS
A very complete description of the methods for
testing natural gas for gasoline is contained in the pub-
lication by G. A. Burrell and G. W. Jones.1
The objections to the various methods have been
well stated in this publication. Owing to the fact that
tests with the portable absorber seem to be more
practical, that method has been preferred in most of
the test cases carried out for the Ohio Fuel Supply Com-
pany. The main objection to the use of the portable
absorber in field testing is the effect of pressure on the
yield.2
In order to meet the requirements for a method that
would give the content and gravity of gasoline in
natural gas, it was deemed advisable to modify the
absorption method so as to meet all conditions of pres-
sure encountered in field testing. The pressure there-
fore chosen was atmospheric.
Tests have shown that the allowable saturations of
oil with gasoline for complete extraction of gasoline
depend upon the gas pressure, the temperature of the
oil, the gasoline content of the gas, and the type of
absorber. The four-coil type of absorber designed by
P. M. Biddison3 gives a greater yield in most cases in
tests with casing-head gases than the absorber with one
coil. Experience has shown that the four-coil type of
1 "Methods of Testing Natural Gas for Gasoline Content," Bureau of
Mines, Technical Paper 87.
1 Proceedings of The Natural Gas Association, 8, 1916.
' Natural Gas Journal, 1916.
absorber when used in testing casing-head gas gives
practically the same yield as the apparatus used in
these experiments, providing a low percentage satura-
tion of oil with gasoline is maintained.
The absorber (Fig. i) used in these experiments was
designed so as to give sufficient contact of oil and gas
in order to completely remove the gasoline. The
absorber is cylindrical in form and made of 22 gauge
galvanized iron. It is 10 in. in diameter and 24 in. in
length. The ends of the absorber should be conical.
The ends are fitted with quarter-inch nipples attached
by a boss. Quarter-inch globe valves or quarter-inch
cocks are attached to the nipples. The dimensions
chosen give the absorber a capacity of about 1 cu. ft.1
Fig. 1 — Cubic-Foot Absorber
The absorber was calibrated by weighing with water
and checked against the meter made by the American
Meter Company and used for determination of heating
values of gases.
METHOD OF OPERATING
One end of the absorber is attached to the gas supply
by means of rubber tubing. The absorber placed in a
vertical position is then purged for 30 min. Connec-
tion with the gas supply is made at the top in case the
gas is lighter than air, or at the bottom in case the gas
is the heavier. In either case the last 1 5 min. for purg-
ing should be made at the top so as to expel small
amount of oil left from the previous test. The valves
1 "Industrial Gas Calorimetry," Bureau of Standards, Technologic Paper
86, 35.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, Xo. 3
are closed with the absorber filled with gas at atmos-
pheric pressure. The temperature of the gas and
barometric pressure are recorded. With the absorber
in a vertical position oil is forced into it by pressure
applied at A. After a small amount of oil is added,
reduced pressure caused by absorption of gas will
generally draw the liquid into the absorber. The re-
»
9
1
Synthetic M
)I5TILLATI0N 1E.5T:
\
&r,
KSOl
Gravity Of Gasoline &Z.\° Be'.
8
Apparatus Used 5howh In Fig. 3
1
•
j
b
0
0
u
— 0
5
./
4-
1
1
3
1
I
30 40 50 GO 70
Per Cent Of Gasoline Recovereo
•ceptacles used in these experiments were made of
glass and had a capacity of 850 and 880 cc, respectively,
having been calibrated at room temperature. The
tube between B and C is filled with oil before the re-
ceptacle is attached or the filling of tube and receptacle
is accomplished by a three-way cock at B. Attempts
to add oil by placing the receptacle at the top of the
absorber are liable to result in loss of gas. After adding
oil the absorber is agitated for 20 min. In case the
gas is very rich in gasoline vapor considerable reduced
pressure results. If such is the case, air is allowed to
enter. The manometer used in flow tests will show if
there is a reduced pressure. This point should not
be overlooked in order to prevent distortion of the
apparatus. After a few minutes of agitation the trouble
due to reduced pressure will be overcome. The oil is
withdrawn and sent to the laboratory for a distillation
test. In order to ascertain time required for purging,
the following test was carried out:
Rate of gas flow 27 cu. ft. per hr.
I onnectxoo for purging At top
Specific gravity of gas used 0.65
Gas Bow began al 9.01 a.m.
Oxygen in exit gas at 9.0.1 am 19.9 per cent
Oxygen in exil gas al 9.06 am 1.7 per cent
1 »\\ gen in exit gas at 9.1 I a.m 0.3 per cent
1 >\\ k<"U in exit gas at 9.16 a.m 0.0 per cent
METHOD OF DISTILLATION
Anticipating losses in evaporation during distillation
of oil samples containing such small quantities of gaso-
line as would be obtained from i cu. ft. of natural gas,
distillation tests were made on synthetic mixtures of
gasoline and mineral seal oil. The results of these
tests are shown graphically in Fig. 2. Practical tests
with the absorber checked against plant yield on natural
gases having a gasoline content of 1.8 pints, 1.6 gallons
and 2.6 gallons, respectively, show that these losses
need not be taken into consideration if the gas and oil
are thoroughly agitated. This is probably due to a
more complete extraction of "wild gasoline," chiefly
pentanes. (See Tests 1, 2 and 3.)
The apparatus used in distillation consists of a 1000
cc. copper flask to which is attached a metal exit tube
(Fig. 3). The condenser is made from glass tubing and
contains 3 bulbs of about 80 cc. total capacity. The
condenser jacket is made from a gallon can, the bottom
of which has been removed. The temperature of the
bath is maintained at 32 ° F. by an ice-water mixture.
The distillate is received in a graduated cylinder (Fig. 4)
surrounded by an ice-water mixture. The receiving
cylinder is graduated in tenths and capable of being
read to V100 cc- The thermometer bulb is placed
2V2 in. below the outlet of the exit tube and 800 cc. of
oil are used in distillation. (If desired, an aliquot por-
tion by weight could be used.) Distillation is carried
on until the exit vapors show a temperature of 3500 F.
I
^^
^
The thermometer is then removed. It is advisable
to run a blank on the mineral seal oil before using for
testing purposes since some of the grades of oil will give
an appreciable amount of distillate if heated to 350° F.
After allowing time for drainage the cylinder is removed
Mar., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
213
and placed in a water bath at 6oc F. The volume at
60 c F. is recorded. The condenser is washed by run-
ning a small amount of alcohol and ether through the
tube and dried with air before a second distillation is
begun.
GRAVITY OF GASOLINE
The apparatus selected for taking the gravity of a
small volume of gasoline was checked against the fol-
lowing instruments: the Tycos Standard Hydrometer
made by Taylor Instrument Company, U. S. Bureau
of Standard Specifications; the Boots Specific Gravity
Bottle, 25 cc. capacity; and the Westphal Balance.
The following methods were used to obtain the
gravity of small volumes of gasoline:
I — Graduated cylinder (Fig. 4) for samples of 4 to
10 cc. volume. A cylinder of dimensions of left arm
of Pycnometer No. 2 (Fig. 5) for samples of 1 to 4 cc.
volume. Such a cylinder can be readily made in the
laboratory. Liquid may be transferred to the pycnom-
eter from the receiving cylinder of the distillation ap-
jmm.
cap///ary
fusing
fmm capi/Ury
O
Fig. 4 — Graduated Cylinder Fig. 5 — Pycnometer No. 2
paratus by means of close-fitting rubber connections.
The open ends of the pycnometer are closed with connec-
tion tubing and glass plugs, the cylinder, tubing and
glass plugs being weighed before gasoline is added. Care
must be taken to use fresh pieces of rubber tubing,
since rubber tubing increases in weight due to absorp-
tion of gasoline vapor. Upon standing the rubber will
gradually lose in weight due to escape of the vapor.
II — Graduated cylinder (Fig. 4) and tube for samples
of 1 to 4 cc. volume. A small tube with elongated tip
and 2 mm. bore was calibrated by weighing with air-
free distilled water at 60° F. The tube, after being
carefully cleaned and dried, is placed in an air bath at
60 ° F. The cylinder containing the gasoline is care-
fully weighed on an analytical balance and then placed
in a water bath at 60° F.
A measured amount of gasoline is forced into the
calibrated tube and then rapidly removed. The
cylinder is stoppered, dried and weighed. From the
loss in weight the gravity of the gasoline is determined.
Results are generally low. The operation should be
repeated with the exception that no gasoline is removed.
Loss in weight during this trial is used in correcting
gravity.
Ill — Pycnometer Xo. 2 (Fig. 5) for samples of 1 to
4 cc. volume. This method is similar to that used by
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THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 3
the Bureau of Mines and the pycnometer is essentially
the same type of instrument as that devised by Dr.
J. A. Culler, Miami University, 1908. The pycnometer
is calibrated by weighing it filled to the etch mark with
air-free distilled water at 6o° F. The dry pycnometer
is filled above the etch mark with gasoline. It is
placed in a water bath at 60 ° F. The excess gasoline
is removed by a roll of filter paper. The instrument is
dried, and weighed.1 From the weight of gasoline and
water the gravity of the gasoline is computed.
Results of tests with 8o° Be\ gasoline show that the
above methods have an accuracy of 0.5° Be\ The
objection to the use of the method is evaporation of the
volatile liquid during the process of weighing. The
objection to the use of the cylinder (Fig. 4) is the error
in reading. The presence of heavy gasoline vapors in
such a cylinder would also introduce error.
COMMENTS ON TESTS
Attention is called to the apparent inconsistency of
the gravity of the gas and the yield of gasoline.1 Pre-
liminary tests on the absorption method with 100 cc.
of gas and 35 cc. of mineral seal oil3 seem to show a more
definite relation to yield of gasoline obtained with the cu.
ft. absorber, the tests having been conducted on gases
in one field. However, there is not enough information
on hand to state this definitely.
Distillation of 100 Cc. op Gasoline Recovered from Cu. Ft. Absorp-
tion Tests, Using the Enoler Flask
Per cent of
Temperature
Distillate
Range — Deg. F.
0-10
82-105
10-20
105-120
20-30
120-134
30-40
134-140
40-50
140-173
50-60
173-196
60-70
196-228
70-76
228-300
Residue i
a Flask = 3 Per cent.
Loss
n Distillation = 21 Per cent.
There are some objectionable features to the use of the
method just described. The absorber is rather bulky.
This objection could be overcome by changing the
size of absorber and working under pressure, providing
the absorber is made rigid to prevent change in volume.
Pressure could be obtained with a small pump, which
could be used also to force oil into the absorber.
If the absorber were fitted with a removable close-
fitting end, it could be used as a case for other instru-
ments. Another objection which would apply to all
laboratory methods is that yields reported on a well
would be lower than those which would be obtained
after the well was put under reduced pressure. How-
ever, it happens that an increase in quantity of gasoline
from a given well due to reduced pressure causing an
increase in yield of gasoline per thousand cubic feet of
gas is compensated to some extent by a decrease in
Volume of gas.
Preliminary tests indicate that alcohol may be used
as the absorbing medium instead of mineral seal oil and
the separation of the gasoline and alcohol made by
dilution with an equal volume of water.
'"The Analytical Distillation of Petroleum," by W. F. Rittman and
E. W. I lean. Bureau of Mines, Bulletin 1S5, 27.
• "The Condensation of Gasoline from Natural Gas," Bureau of Mines,
Bulletin 88, 45.
■ "Methods of Testing Natural Gas for Gasoline Content." Bureau of
Mines, Technical Paper 87.
The cubic foot absorber is intended especially for
casing-head gas testing and has been found to give
trustworthy results. When the method is used for
testing natural gas of lower gasoline content the results
are less accurate.
The above tests and tests by others indicate that the
practical absorber for testing natural gases for gasoline
content would consist of small unit absorbers grouped
in series. A testing outfit in which absorbers and meter
were made of aluminum could be carried by one man.
Preliminary tests at atmospheric pressure with an out-
fit built on this principle and consisting of a four-unit
series absorber resulted in 85-90 per cent recovery of
gasoline from a natural gas having a yield of 1.4 pints
per thousand cubic feet of gas.
The Ohio Fuel Supply Company
Homer, Ohio
THE VALUATION OF LIME FOR VARIOUS PURPOSES
By Richard K. Meade
Received June 8, 1917
The subject of the valuation of lime for various
purposes is one which has received very little attention
in the scientific press. The methods of analysis have
been very carefully worked out but these all follow the
standard procedure for the analysis of silicate and car-
bonate rocks, and required nothing more than the
application of well-known gravimetric separations and
volumetric titrations. The methods differ in no es-
sential from those employed in the analysis of any
calciurit mineral or artificial product decomposable by
acid and containing the same elements as lime. Out-
side of the analytical methods, very little has been
published on the testing of lime. The standard text-
books contain nothing other than analytical methods
and in even the special works on calcareous materials
little attention is paid to the subject. In some treatises
on the manufacture of certain products in whose
elaboration lime is used, there are given special methods
for the analysis of lime to be used in this art. The
American Society for Testing Materials has drawn up
specifications, but these latter are little more than a
classification of various kinds of lime and could hardly
be used to control the general purchase of lime as, for
example, are the cement specifications of the same
organization.
The difficulty with lime is that it is not only a
building material but it is also an important raw
material in many industries, notably the chemical and
metallurgical ones. The requirements are quite differ-
ent in these various industries and the qualities which
the builders ask of the lime are quite different from
those needed by the chemical manufacturer.
Even here again the qualities necessary in one class
of building lime are not required in another, while
in one chemical process one kind of lime is required
and in another an entirely different sort of product
is necessary. Generally speaking, the building trade
is most interested in color, plasticity and possibly
strength; while the chemical manufacturer wishes
purity from carbon dioxide, silica and the oxides of
iron and alumina, and to have either a high or low
content of magnesia as the process may require.
Mar., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
215
Unfortunately there are no standards of physical
properties and the builder grades his lime largely by
means of experience. No color scheme or standard
grade of color has yet been devised nor are there even
any methods- which are generally accepted as reliable
for testing plasticity. On the chemical side of the
question, however, much more has been done, as I
have said, and at the larger chemical works quite re-
liable methods are employed for the valuation of the
lime which they employ. At many of the smaller
works, however, very crude methods of analysis are
employed. It is the purpose of this paper to outline
the methods most generally employed for the chemical
analysis of lime. No originality is claimed for these
methods on the part of the writer and whenever their
source could be traced credit has been given. The
object of the paper is rather to collect these methods
in one place where they will be generally accessible
to the chemist interested in lime.
By way of introduction it may not be amiss to give
the various more important uses of lime in the arts,
the classification of limes according to chemical com-
position, etc., and to designate the properties which
lime should possess to be acceptable in each industry.
CLASSIFICATION OF LIME
The standard specifications of the American Society
for Testing Materials (Report of Committee C-7 for
191 5) divide lime into two grades:
(a) Selected — Shall be well burned, picked free from
ashes, core, clinker or other foreign material.
(b) Run-of-Kiln — Shall be well burned, without
selection.
Quicklime is shipped in two forms:
(a) Lump Lime — Shall be kiln size.
(b) Pulverized Lime — Shall be reduced in size to
pass a '-/i-in. screen.
Quicklimes are divided according to their chemical
composition into four types:
(a) High Calcium (c) Magnesium
(6) Calcium (</) High Magnesium
The following chemical limits are prescribed by the
specifications above referred to:
Table I — Chemical Composition
High- High-
Calcium Calcium Maokksian Magnesian
Run- Run- Run- Run-
Se- of- Se- of- Se- of- Se- of-
lected Kiln lected Kiln lected Kiln lected Kiln
Per Per Per Per Per Per Per Per
cent cent cent cent cent cent cent cent
Calcium Oxide 85-90 85-90 90 90
(min.) (min.)
Magnesium Oxide 10-25 10-25 25 25
(min.) (min.)
Calcium Oxide +
Magnesium Oxide 90 85 90 85 90 85 90 85
Carb..n Dioxide
(max ) 3 5 3 5 3 5 3 5
SOli . - Alumina +
Oxide of Iron
(max.) 5 7.5 5 7.5 5 7.5 5 7.5
Hydrated lime takes the same chemical classifica-
tion as the lime from which it was made.
USES OF LIME
In the building trade, lime is used for three important
purposes: (i) Mixed with sand as a bonding material
in laying brick and stone; (2) for plastering; and (3)
hydrated and mixed with Portland cement to confer
certain properties to mortars of the latter, such as
plasticity and imperviousness to water.
As I have said, the suitableness of a lime for building
purposes depends entirely on physical properties,
although these in turn are, of course, affected by chem-
ical composition. For all of the above purposes a
lime may belong to any of the grades referred to above.
For bonding brick and stone, the important qualities
of lime are the sand-carrying capacity, the crushing
strength and tensile strength. For plastering, se-
lected lump lime or hydrated lime is employed. Good
color and plasticity are, of course, important in lime
for this use. The lime must not "pit" or "pop" and
must not give too great change of volume during
setting — the quicker the latter the better, also hy-
drate must be thoroughly hydrated in addition to the
foregoing properties. Magnesian or dolomitic limes
are generally considered preferable to calcium limes
for plastering.
For use with Portland cement, very impure and off-
color hydrate may be successfully employed. Here
the fineness and completeness of hydration are most
important.
The tests ordinarily employed for building limes,
therefore, are those for chemical composition, sand-
carrying capacity, crushing strength, tensile strength
and setting time. Hydrated limes in addition are
subjected to tests for fineness and constancy of volume.
Large quantities of lime are used in agriculture
both in the form of quicklime and hydrated lime.
Some authorities claim that only calcium lime should
be used for this purpose, while others contend that
magnesium and dolomitic limes are just as efficient.
The question may, therefore, be considered an open
one, depending usually on the attitude of the agri-
cultural department of the state in which the lime is
sold. Generally speaking, the cheapest grades of
lime are used for fertilizer, as color and physical prop-
erties need not be considered and chemical impurities
are only undesirable as they detract from the amount
of calcium oxide present. The value of lime for fertil-
izer depends entirely on the cost per unit of calcium
oxide (or calcium and magnesium oxide if the latter
is considered equivalent to the former). For con-
venience in applying, ground lime is to be preferred
to lump lime, while hydrated lime owing to its extreme
fineness is to be preferred to either lump or ground
lime.
Many sprays used for trees and plants are prepared
from lime. For this latter purpose the value of the
lime depends entirely on the percentage of free calcium
oxide which it contains. Magnesia is of no value here.
In the manufacturing arts, what is wanted in all
cases is a very pure lime, and the value of the latter
depends entirely on the percentage of active or quick-
lime in the latter, that is, the uncombined calcium oxide
(sometimes calcium and magnesium oxides combined).
In the manufacture of caustic soda and of sugar,
magnesia is considered harmful. Following is a list
of the more important chemical industries in which
lime is employed and the class of lime employed by
each.
2l6
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 3
soda ash produced by the "Solvay" or ammonia
process. A high-calcium lime must be employed and
impurities are undesirable aside from their lowering
the unit contents of lime. The valuable content of
the lime is the free calcium oxide.
caustic soda produced by "causticizing" soda ash
with lime. The requirements for lime are the same as
in the manufacture of soda ash.
ammonia — Requirements for lime are the same
as in the manufacture of soda ash.
potassium dichromate — Requirements are the same
as for soda ash.
paper and pulp by the soda process — Require-
ments are the same as for lime used for caustic soda.
calcium carbide — Magnesia and impurities are
decidedly objectionable and the lime should be very
well burned and as pure as possible. The valuable
content is the free calcium oxide.
bleaching powder — Magnesia should be as low
as possible. Impurities are objectionable as they
lower the quality of the powder. The valuable con-
stituent of the lime is the free calcium oxide.
calcium cyanide — Pure high-calcium lime is de-
sired, the value depending on the quantity of free
calcium oxide present.
calcium acetate (acetate of lime) — Value of
lime for this purpose depends solely on the percentage
of free calcium oxide. Magnesia and impurities of
themselves do no harm.
GLYCERINE, LUBRICATING GREASES AND FAT INDUS-
TRIES— Requirements are same as for calcium acetate.
purification OF illuminating gas — Requirements
are the same as for calcium acetate.
purification and softening of water — Require-
ments are the same as for calcium acetate.
sugar — Pure high-calcium lime is required. Mag-
nesia and silica cause trouble in the process and should,
therefore, be present only in small quantities. The
valuable constituent is free calcium oxide.
leather — For tanning, free calcium oxide is the
valuable constituent. Iron oxide is objectionable as
it causes stains.
sand lime brick — A pure high-calcium lime is
desired. Impurities are not objectionable of them-
selves. Magnesia should not be very high. If
hydrate is employed it must be completely hydrated.
paper and pulp by the sulfite process — Require-
ments are for a high-magnesium or dolomitic lime.
Impurities are only objectionable as they detract from
the quantity of the free oxides of calcium and mag-
nesium present, the two latter being the valuable
constituents.
MAGNESIA- — Dolomitic limes alone are required for
the purpose and the value depends solely on the per-
centage oi free magnesium oxide present.
glass — Both high-calcium and high-magnesium limes
are used. The oxide of iron should be low but other
impurities are immaterial.
cold water paints — Hydrated lime is employed
and fineness and color are the main requin
Chemical composition is unimportant.
metallurgy — Both high-calcium and high-mag-
nesium limes are employed. Impurities are objection-
able only when present in large quantity. Generally
speaking, the lime should be burned much harder than
usual for this use.
physical tests
The only physical tests of lime for which standard
methods are available are those for determining (1) the
proper or normal consistency of lime paste, for which
purpose the Chapman apparatus is now pretty gener-
ally employed, (2) the percentage of waste in quick-
lime and (3) the fineness and constancy of volume of
hydrated lime. For conducting these latter tests,
the standard specifications of the American Society
for Testing Materials prescribe the procedure. These
same rules also instruct as to sampling. Their direc-
tions are as follows:
sampling quicklime — When quicklime is shipped in bulk,
the sample shall be so taken that it will represent an average of
all parts of the shipment from top to bottom, and shall not
contain a disproportionate share of the top and bottom layers,
which are most subject to changes. The samples shall com-
prise at least 10 shovelfuls taken from different parts of the ship-
ment. The total sample taken shall weigh at least 100 lbs.
and shall be crushed to pass a i-in. ring, and quartered to pro-
vide a 15-lb. sample for the laboratory.
When quicklime is shipped in barrels at least 3 per cent of
the number of barrels shall be sampled. They shall be taken
from various parts of the shipment, dumped, mixed and sampled
as specified above.
All samples to be sent to the laboratory" shall be immediately
transferred to an air-tight container in which the unused portion
shall be stored until the quicklime shall finally be accepted or
rejected by the purchaser.
sampling hydrated limk — The sample shall be a fair average
of the shipment. Three per cent of the packages shall be
sampled. The sample shall be taken from the surface to the
center of the package. A 2-lb. sample to be sent to the labora-
tory shall immediately be transferred to an air-tight container,
in which the unused portion shall be stored until the hydrated
lime has been finally accepted or rejected by the purchaser.
percentage of waste in QUICKLIME — An average 5-lb.
sample shall be put into a box and slaked, by an experienced
operator, with sufficient water to produce the maximum quantity
of lime putty, care being taken to avoid "burning" or "drown-
ing" the lime. It shall be allowed to stand for 24 hours and
then washed through a 20-mesh sieve by a stream of water
having a moderate pressure. Xo material shall be rubbed
through the screens. Not over ., per cent of the weight of the
selected quicklime nor s per cent of run-in-kiln quicklime shall
be retained on the sieve. The sample of lump lime taken for
this test shall be broken to all pas- a i-in screen and be retained
m screen. Pulverized lime shall be tested as received.
FINENESS OF HYDRATED i.imk -A ioo-g. sample shall leave
1. hie of not over 5 per cent on a standard 100-
mesta sieve and not over 0.5 per cent on a standard 30-mesh
sieve.
VNCY OF VOLUME Equal parts of hydrated lime under
test and volume constant Portland cement shall be thoroughly
mixed togethei and gauged with water to a paste. Only suffi-
cient water shall be used to make the mixture workable. From
this paste a pat about .; in. in diameter and ' ; in. thick at the
center, tapering to a thin edge, shall lie made on a clean glass
plate about 4 in, square This pat shall be allowed to harden
j J his in moist air and shall he without popping, checking,
cracking, warping or disintegration after 5 hrs. exposure to
-tram abovt boiling water in a loosely closed vessel.
Mar., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
217
For the other physical tests for lime the methods
employed for the most part are similar to those used
in testing cement. As a matter of fact, however, such
complete testing of lime is hardly ever done by the
architect or engineer and about the only time that a
complete set of tests is made is in the case of a scientific
investigation. One or two of the larger producers
have made some extended tests of their product along
scientific lines, and here and there an engineering
organization has undertaken this work with a view to
obtaining information on the properties of various
limes. The various government bureaus have also
made and are constantly making elaborate tests.
So far as we know, however, lime is not regularly in-
spected and tested by any large user.
The methods which are employed in such investi-
gations are in general quite similar, as I have said,
to those employed in testing cement although the de-
tails for the most part differ with each operator. The
first step is always to determine the proportions of
lime and water which are necessary to make a paste
of standard consistency. This is now usually done
by means of the Chapman apparatus. This apparatus
is fully described in the Proceedings of the American
Society for Testing Materials, Vol. 13, p. 1045. This
consists of a split cylinder of thin, hard rubber
about 2 in. in diameter by 3 in. high, tapering slightly
towards the bottom. When this is filled with paste
and dropped a short distance (3 in.) the cylinder will
spread and may be measured from the widening of
the slit in the cylinder. Chapman considers 0.40 in.
to be about the correct amount for a lime putty of
normal consistency either with or without sand. All
tests which are to be made of the lime should be made
with a paste of the standard consistency as determined
with this apparatus.
For determining the crushing and tensile strength,
a mortar consisting of standard lime paste and stand-
ard Ottawa sand should be used, the proportions being
lime paste of standard consistency equivalent to
one part by weight of dry lime to three parts of sand.
The crushing test should be made on 2-in. cubes and
the tensile-strength test on the standard cement
briquette. The specimens are, of course, stored in air
and may be broken at any period, generally after 3
months.
For testing the sand-carrying capacity of lime, test
pieces are made up employing varying proportions
of standard lime paste equivalent to a definite quantity
of dry lime and standard Ottawa sand. The test is
made just as is the crushing test.
The Vicat needle is used to determine the time of
set and is employed as in cement testing.
There is no very well-accepted method for testing
hardness. Sometimes a sand blast is used. Very
recently, however, the Bureau of Standards has been
employing the following method: 1000 g. of BB lead
shot are allowed to drop from a reservoir through a
i-in. iron pipe 6 ft. X io3/* in. long on a mortar placed
at an angle of 45° with the vertical axis of the pipe.
The loss in weight of the mortar due to the impact and
wearing action of the shot determines the hardness.
Color can, of course, be obtained by comparison
with known standards. These may be made by mixing
any pure white powder such as ground calcite with
definite amounts of brown coloring matter. There is
no recognized standard, however.
No satisfactory tests have been proposed for plas-
ticity and about the only method of judging this is the
purely empirical one of spreading over a surface by
an experienced operator.
DETERMINATION OF FREE CALCIUM OXIDE OR HYDROXIDE
For determining the free calcium oxide in quick-
lime or free calcium hydroxide in hydrated lime,
the following methods are used in the laboratories of
chemical manufacturers and in many instances the
lime is bought on a unit basis as the result of this
determination.
BY TITRATION" WITH STANDARD HYDROCHLORIC ACID
This is the oldest and simplest method. Weigh 28 g.
of the coarsely ground sample into a liter graduated
flask containing about 250 cc. of recently boiled dis-
tilled water. Boil for 10 min., close with a cork con-
taining a 6-in. capillary tube and allow to cool some-
what. Make up to the mark and mix well. Immedi-
ately after mixing draw off 50 cc. of the milk of lime and
titrate at once with normal hydrochloric acid, using
phenolphthalein as an indicator. Allow the flask to
remain some time to see if the pink color returns. For
the percentage of free calcium oxide, multiply the
number of cc. required by 2.
In the case of hydrated lime use a 1.4-g. sample, place
in an Erlenmeyer flask with 250 cc. of water and titrate
the entire volume after boiling and cooling as above.
In the case of quicklime the larger weight is necessary
in order to get a proper average. The sample should
be quickly ground and placed in a tightly corked bottle
— never in a sample envelope.
scaife method — The chemists for the Scaife Com-
pany modify this method as follows: Weigh 1.4 g.
of the carefully prepared and finely ground lime into
an 8-oz. assay flask, add about 80 cc. hot water, cover
with a beaker, carefully heat and then boil for three
minutes.
Cool, remove cover, add 2 drops phenolphthalein
and titrate with A7 HC1 adding the acid rapidly in a
thin stream while shaking constantly to avoid local
excess of acid. Near the end drop in the acid rapidly
while shaking until the pink color disappears. Note
the reading but ignore any return of color.
Repeat the experiment adding about 5 cc. less acid
than before, call the number of cc. used "A." Grind
up any small lumps with the round end of a thick glass
rod, transfer the pink mixture to a 250-cc. volumetric
flask, dilute to the mark with distilled water, mix, let
settle half an hour.
Titrate 100 cc. slowly with phenolphthalein and
N HC1 until colorless. Call this additional number of
cc. used "B." Then, percentage of available calcium
oxide = 2.1 + 5B.
by titration with oxalic acid — Lunge in his
"Technical Chemists' Handbook" gives the following
method for determining calcium oxide in quicklime:
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 3
"Weigh 100 g. of an average sample carefully taken,
slake it completely, put the milk into a half-liter flask,
fill up to the mark, shake well, take 100 cc. out, run
it into a half-liter flask, fill up, mix well, and employ
25 cc. of the contents, equal to 1 g. quicklime, for the
test. Titrate with normal oxalic acid and phenol-
phthalein as indicator, adding the acid very slowly and
shaking well after each addition. The color is changed
when all free lime has been saturated and before the
CaCOs is attacked. One cc. normal oxalic acid =
0.02805 CaO."
Lunge also give the following method for carbon
dioxide: "Titrate CaO and CaC03 together by dis-
solving in an excess of standard hydrochloric acid and
titrating back with standard alkali. By deducting the
CaO estimated as above the quantity of CaC03 is
obtained."
by sucrose solution — Guilford L. Spencer gives
the following method for determining the calcium
oxide in quicklime in his "Handbook for Cane Sugar
Manufacturers." As this method is related to the
industrial process in which lime is used in sugar manu-
facture it is presumably especially applicable to testing
lime at the sugar works.
"Add sufficient water (30 cc.) to 10 g. of lime,
in a mortar, to form a thick milk. Add an excess of
pure sucrose in the form of a solution of 3 5-4 5 ° Brix
and mix it intimately with the lime, which forms a
soluble saccharate. Transfer the solution and residue
to a ioo-cc. flask, using a sugar solution of the above
composition to wash the last portions from the mortar
and to complete the volume to 100 cc, mix and filter.
Titrate 10 cc. of the filtrate with a normal solution of
hydrochloric acid using phenolphthalein or lacmoid
as an indicator. The burette reading X 0.028 = the
weight of calcium oxide (CaO) in 1 g. of the lime, and
X 100 = percentage of calcium oxide."
solvay method — The following method was de-
vised by the chemists of the Solvay Process Co. and is
very reliable. For carrying it out a special flask shown
in Fig. I will be needed. Boil 4 g. of the lime ground
to pass a 100-mesh sieve in a 250-cc. Erlenmeyer flask
for a few minutes with a little (60 cc.) water to thor-
oughly disintegrate it.
After cooling, transfer to the lime bottle (Fig. I)
filling up to the lower mark (129 cc.) with water, then
to the upper mark (178.6 cc.) with ammonium chloride
solution made by dissolving 250 g. of crystallized
ammonium chloride in a liter of water.
Mix thoroughly by inverting about 30 times. Do
not mix afterwards or results will be too high.
Let settle from 15 to 20 minutes, draw out 50 cc. of
the clear liquid with a pipette and deliver with stirring
into a slight deficiency of normal hydrochloric acid
and about 150 cc. of water.
For 90 per cent lime, deficiency is 30 cc. normal
hydrochloric acid.
For 65 per cent lime, deficiency is 20 cc. normal
hydrochloric acid.
Titrate to the end-point using methyl orange as in-
dicator.
The number of cc. of normal hydrochloric acid
times 2.5 gives the percentage of active (available) CaO.
BY CONVERTING SODIUM CARBONATE TO SODIUM
hydroxide — The chemists of some plants in which
lime is used to causticize soda employ a method making
use of this reaction. The method is as follows:
Weigh s g. of the sample into a 500-cc. graduated
flask and add 200 cc. of approximately normal sodium
carbonate, or 10 g. of sodium carbonate and 200 cc. of
water. Close with a stopper having a Bunsen valve
in it or a 6-in. tube drawn out to a thin point and boil
for one-half hour. Add 10 g. of barium chloride dis-
solved in a little water and make up to the mark with
— 1-3
• Ol»" •
r~
r
7
f
S
'»
f\
176.6
cc.
\
V
— 1
|
I29C
cc.
V
>
,
h
«
1
I
^
1
j
— e.
cold water. Stopper tightly and mix well. Allow pre-
cipitate of calcium carbonate and barium carbonate to
settle. Draw off 100 cc. of the clear solution and ti-
trate with normal hydrochloric acid. The number of
cc. of acid used multiplied by 2.8 is equivalent to the
percentage of free calcium oxide in the sample.
ESTIMATION "I Mil PERCENTAGE OF CAUSTIC LIME
IN Milk 01 LIME BY MEANS OF THE SPECIFIC
GRAVITY 1 HLATTNER)
The method devised by Blattner making use of the
specific gravity of milk of lime which is only suitable
Mar., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
219
for very rough work is also given in Lunge's Handbook
and is as follows: Thin milk of lime is poured into the
cylinder and the reading of the hydrometer is taken
quickly before the lime subsides. For thick milk of
lime employ a somewhat wide cylinder, put the hydrom-
eter in without using any force and turn the cylinder
slowly around, so that it receives a slight shaking until
the hydrometer ceases to sink. The following table
is valid for 15° C:
Table II-
-Amount
OF
Lime in Milk
OF LlM
E
(Calculated from Blattner)
egrees
G. CaO
Lbs Ca
O
Degrees
G
CaO
Lbs
V.ul.k
1 per liter
per eu.
ft.
Twaddell
per liter
per
2
11.7
0.7
28
177
1
4
24.4
1.5
30
190
1
6
37.1
2.3
32
203
1.
8
49.8
3.1
34
216
K
10
62.5
3.9
36
229
1'
12
75.2
4.7
38
242
1.
14
87.9
5.5
40
255
1.
16
100
6.3
42
268
1(
18
113
7.1
44
281
1
20
126 -
7.9
46
294
If
22
138
8.7
48
307
15
24
153
9.5
50
321
2(
26
164
10.3
608-12 Law Building
Baltimore, Maryland
A STUDY OF THE DeROODE METHOD FOR THE
DETERMINATION OF POTASH IN
FERTILIZER MATERIALS
By T. E. Keitt and H. E. Shiver
Received July 25, 1917
Determinations of potash have been made in America
for the past thirty years by a method first proposed
by Lindo1 in 1881 and. modified by Gladding2 in 1885.
The Lindo-Gladding method is familiar to every chem-
ist and does not need repetition here; it has been
adopted by the Association of Official Agricultural
Chemists.3 "The process depends upon the fact that
potassium platino-chloride is insoluble in strong al-
cohol, and the easy solubility of the associated salts,
for instance sodium, in the same reagent.''4 In this
method the earthy bases have to be removed before
precipitating the potash, necessitating the addition
of reagents and their subsequent removal by precipi-
tation and filtration, which does not contribute to
the ease or the accuracy of the determination.
The fertilizer manipulators have contended that
the Lindo-Gladding method does not account for all
of the water-soluble potash. Likewise, it has been
recognized by certain chemists that this method does
not obtain all of the potash.6-6 One of us7 has shown
that there are grounds for the manipulators' conten-
tions that our present method of analysis does not
account for all of the potash present in water-soluble
1 "Original Method for Potash Determination." Chem. News, 44 (1881)
77. 86. 97, 129.
: "Improvement on Lindo Method." U. S. Dept. of Agr., Div. O!
Chem., Bull. 1885, 7, 38.
• A. O. A C , U. S. Dept. of Agr., Bureau of Chemistry. Bull 107.
4 Wiley, "Principle and Practice of Agriculture Analysis," 11 (1895)
540, 554, 555, 570.
' Luntc's "Technical Methods of Chemical Am I Ml (1908)
526.
• Hint?, and Weber, (hem. Anal. Atwrr... 1896; ESrper, Z. an,,
S5, OSS.
'Keitt, "Potash in Mixed I 'Hi Carolina Agricultural
Experiment Station, Hull 173 (1013), II.
form, and that there is another source of error which
compensates for the occlusion. The second source
of error is the diminished volume of the solute due to
the volume occupied by the precipitates formed on
addition of ammonia and ammonium oxalate. Breck-
enbridge,1 Porter and Kenny,2 Bell,3 and Shiver4
have studied certain errors occurring in the official
method, laying particular stress on occlusion and the
solubility of the precipitate. Wiley5 calls attention
to "The remarkable facility with which potash be-
comes incorporated with the precipitates of other
bodies." Hibbard6 states that occlusion "may amount
to from i to io per cent of the original amount of
the potash." Garrigues7 in reporting a new modi-
fication gives some good results on the discrepancies
of the official method, showing among other things
that the loss from occlusion varied from o.n to 0.20
per cent on six samples run by him. One of us5 has
found that more than 0.5 per cent of potash was
occluded by the ammonia precipitate in certain samples.
Robinson8 and Winton9 have studied the character
and magnitude of certain errors in this method, and
the influence of concentration on the accuracy of the
determination, with startling results. Smith10 in a
general discussion on occlusion remarks, "As is well
known, many insoluble compounds which are precipi-
tated in the course of analytical processes possess the
property of carrying down and retaining certain soluble
salts in such a manner that the latter oftentimes can-
not be removed, even by prolonged washing."
Chemists, realizing the need of an improved method,
have suggested many processes11 none of which have
shown sufficient merit to replace the Lindo-Gladding
method. The perchlorate method received special
attention, and for a time threatened to replace the
Lindo-Gladding method, but the latest results may be
summarized as follows: "The perchlorate method
for the determination of potash was found less suitable
than the platinum method. It is longer, more difficult
and more expensive as to reagents."5
A method based on the principle of moist combus-
tion was proposed by DeRoode12 in 1895 and modified
by Vietch13 in 1905, who says, "It is unfortunate that
more attention has not been called to the method
of Moore14 (DeRoode) for in it many of the preliminary
operations are omitted and it is at once the simplest
> "Potash Tests in Mixed Fertilizers ." Tins Jul knal, 1 (1909), 409;
"Potash Tests in Commercial Fertilizers." Ibnl . 1 (1909), 804.
' "Loss of Potash in Commercial Fertilizers." Ibid . 1 (1909), 304.
! "The Estimation of Potash," Chem. News, 79 (1899), 1 JS.
•"The Determination of Potash as Perchlorate," Ibid., 79 (1899),
265.
» Loc. cit.
• "A Study of Determination "f Pol ; ' knal, 9 (1916),
505.
'"The Determination of Potash in Manures," J Am. ( hem 17
(1895). 47.
» "Some Sources of Error." Ibid 16
I in Some Conditions Affecting, etc.," Ibid.. 17 (18''
» "Contamination ol Predpitatei in Gravimetrii Analysis,' 1917
ii Hicks, "A Rapid Modified Chlorplatinati Method etc.,"!
N.M.. 8(191
u "The Detenu 17
189S), 85, 86.
H "The Bstim "•"' , IT (190
Ihi.l . 20 i IK').-
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. Xo. 3
and shortest, and possesses a high degree of accuracy."
However, the method has been allowed to stand un-
perfected in details and unnoticed. This method elim-
inates all of the preliminary "precipitation, filtration,
and incineration, with its accompanying sources of
error due to occlusion, diminished volume and sputter-
ing, besides loss of time and some of the personal equa-
tion due to lessened number of operations. A method
very similar to DeRoode's was suggested by Losche.1
Much work has been done in the laboratory of the
South Carolina Experiment Station using the DeRoode
method as a skeleton, and the final results show a very
high degree of accuracy, also the modified process
obviates the objections of the chemist and the manu-
facturer.
The method is applicable to all commercial fertilizers,
including concentrated salts. The details of the
method follow: 10 g. of the sample are placed in a
500-cc. flask and 300 cc. of water added. The con-
tents of the flask are maintained at boiling tempera-
ture for approximately 30 min., cooled and diluted to
volume. After allowing to stand until the material
has settled, filter and draw out 50 cc, an aliquot
representing one gram. Place the aliquot in a porce-
lain dish and add 3 to 5 cc. of nitric acid to destroy
any organic matter that may be present.2 Evaporate
to dryness over a water bath, take up with hot water
and an excess of hydrochloric acid. Evaporate
again to dryness, take up with hot water, adding several
drops of hydrochloric acid, and enough platinic chloride
to precipitate all of the potash present. Thus all of
the details through the precipitation are carried out
on one bath, in almost one operation, and in a very
short time. Cover the precipitate with the acidulated
alcohol, the method of preparation of which is described
later. Allow to stand for 15 to 20 min., in which time
all iron, aluminum, and magnesium will dissolve;
filter, and wash with the acidulated alcohol solution
until the runnings are colorless, washing free of the
excess of platinic chloride. Next wash well with
ammonium chloride (saturated with KjPtCU). This
washing should be thorough, for the accuracy of the
method is largely dependent upon this operation;
6 or 7 washings usually suffice. The function of the
ammonium chloride wash is the same as in the Lindo-
Gladding method. Wash thoroughly with 95 per cent
alcohol to remove the ammonium chloride; then dry
and weigh the precipitate and calculate results as in
the older method.
The preparation of the acidulated alcohol is as
follows: To each 1000 cc. of 95 per cent alcohol
add 75 cc. of cone, hydrochloric acid, then pass dry
hydrochloric acid gas into the mixture until 1 cc. of the
alcohol neutralizes 2.25 cc. normal potassium hydrox-
ide, '-4 using phenolphthalein as an indicator. The hydro-
chloric acid gas may be prepared by using C. P. sodium
chloride and concentrated sulfuric acid, or by heating
' "The Estimation of Potassium," Chem.-Ztg., 20 (1896), 38.
• Croolccs, "Select Methods in Chemistry Analysis," Second Edition,
188C, p. 33.
' Lot. til.
* Bear and Salter, "Methods in Soil Analysis," West Virginia Agr.
Eipt. Sta., Hull. IBS (1916). 10.
concentrated hydrochloric acid and first passing the gas
through sulfuric acid and then into the alcohol. The
solvent action of this acidulated alcohol on potassium
chloroplatinate is about equal to that of the Lindo
ammonium chloride solution, which is about one-third
that of ordinary 80 per cent alcohol. Or. if expressed
numerically, one gram of pulverized potassium chloro-
platinate was digested for two hours in 500 cc. of
acidulated alcohol, at room temperature. The solvent
action under these conditions was found to be one part
in 60,000. ' The ammonium chloride is made up by
adding to each 1000 cc. of water 200 g. of ammonium
chloride and saturating in the cold with potassium
chloroplatinate. The acids used are C. P. concen-
trated. Whatman's filter papers Xo. 42 (9 cm.) were
used on 130 mm. funnels. Drying was effected in
a Freas electric oven at a temperature of 110° C.
for i'/j hours. Porcelain dishes are used, entirely
replacing platinum dishes which may be liberated for
use in the arts and in the manufacture of munitions.
The following work was done in this laboratory
to test the new method with commercial salts. A
solution containing 10 g. of potassium chloride and
another containing 10 g. of potassium sulfate were
made and analyzed by this method. The potassium
chloride by theory should give 63.20 per cent K20;
the results obtained by analysis were 63.12 per cent
and 63.04 per cent, showing an average of 63.08 per
cent or 99.81 per cent of theory. The potassium sulfate
theoretically contained 54-2° per cent K20; the results
obtained by analysis were 54.08 per cent KjO and 54.08
per cent K20, being identical and 99.78 per cent of
theory.
Some samples collected by the State Board of Fer-
tilizer Control were analyzed These samples are
representative of commercial fertilizers as found on the
open market. The following results were obtained by
(1) the Lindo-Gladding method, (2) the Lindo-Gladding
method plus occluded potash, obtained by repeated
solution and precipitation of the ammonia and am-
monium oxalate precipitates, and (3) the modified
method:
Table I — Comparison of Linoo-Gladding Method, Llndo-Gladdino
: o ^ c <
Plus
Occluded Potash and Modipied
"■So
- - z
XT3-0 £
>» c-0
* s~
S S~
.0 0 « S
■°a 0
•0 0
jlTJ u
*
z°i
*~3
*!i
'.— 0
■O-ot
Sample
lit
a VA
B. O 0 ,.
3"°
No,
C-
2-
0
0
0
58 A
3.15
3.28
3.33
0.18
0.05
S8B
3.35
0.20
0.07
160 A
i'.j'l
2!o9
2.97
0.26
0.08
160B
2.97
0.28
0.08
S47A
5^98
o!22
6.24
0.26
0.02
547B
6.22
0.24
0.00
8S0A
2^68
2!86
2.94
0.26
0.08
850B
2.95
0.27
0.09
12 29 A
iiio
3^22
3.33
0.23
0.11
1229B
3.26
0.16
0.04
The above table shows that the modified method
gives an average of 0.062 per cent more water-soluble
potash than the Lindo-Gladding method plus occluded
potash obtained by repeated solution and precipitation
of the precipitates formed in the flask preparatory to
' Lot. tit.
Mar., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
making the determination as officially directed. Fur-
thermore, the modified method shows an average in-
crease of 0.232 per cent over the Lindo-Gladding method.
There is no doubt that this increased amount of
potash is present in water-soluble form and is not
accounted for by the official method, because one of
us1 has shown that every time the precipitate formed
by ammonia and ammonium oxalate in the flask is
dissolved and precipitated, the filtrate contains potash.
The amount of potash obtained by repeated precipi-
tation and filtration was never as much as the theoretical
when pure salts were used.
In order to ascertain whether all potash is determined
by the new method, the following synthetic solu-
tions were analyzed by the methods compared in
Table I :
Solution 1 contained potassium chloride and ferric
sulfate equivalent to 5.99 per cent K20 and 10.31
per cent Fe203.
Solution 2 contained potassium chloride and tri-
calcium phosphate equivalent to 5.99 per cent K20
and 10 per cent Ca3(PO.j)2.
Solution 3 contained potassium chloride, iron, and
tricalcium phosphate equivalent to 5.99 per cent
K20, 10.31 per cent Fe203, and 10 per cent Ca3(P04)2.
Solution 4 contained potassium chloride, iron,
tricalcium phosphate, and aluminium sulfate equiva-
lent to 5.99 per cent K20, 10.31 per cent Fe203) 10
per cent Ca3(P04)2 and 10 per cent A1203.
These solutions were intentionally exaggerated as
to content of impurities and the determinations
shown are the first and only results obtained, em-
phasizing the ease and accuracy of the method of
determination.
Solution Jj^pU
5.99 5.61 5.643
5.99 5.61 5.633
5.99 5.10 5.129
5.99 5.09
■S aS*- S'Sp go-So
« 5 Q a
5.94 — 0.05 0.33 0.297
5.80 — 0.19 0.19 0.167
5.75 —0.24 0.65 0.621
5.78 —0.21 0.69
Table II shows that soluble iron and aluminium
compounds and tricalcium phosphate retain large
amounts of potash in the Lindo-Gladding method
where these compounds are precipitated and the potash
determined in the filtrate. The indications are that
the relation is a chemical phenomenon, because of the
fact that very little potash is recovered by repeatedly
dissolving and reprecipitating the residue. Iron (10.31
per cent) retained 0.38 per cent K20, only 0.033 per
cent of which was recovered in the filtrate by dis-
solving and reprecipitating three times in 400 cc.
of solution. Tricalcium phosphate (10 per cent)
retained 0.38 per cent K20, 0.023 Per cent °* which
was recovered in three combined filtrates. Aluminium
salts were not used alone with potassium chloride
on account of the similarity of their properties to those
of iron salts, but aluminium sulfate was included in
the fourth solution. A combination of 10.31 per cent
Fe203 and 10 per cent Ca3(P04)2 shows a retention
slightly greater than the sum of the retention of the
salts added to separate solutions. This appears
to indicate a slight additional occlusion by the com-
bined precipitates, which occlusion is doubtless greater
than it appears on account of the diminished volume
due to the larger precipitate. The retention inci-
dent to the use of ferric sulfate and tricalcium phos-
phate amounts to 0.89 per cent, only 0.029 per cent
of which was recovered by three solutions of the pre-
cipitates and their subsequent precipitation. The
addition of 10 per cent A1203 in the form of aluminium
sulfate to the other two impurities increases the ap-
parent retention only 0.01 per cent, but the diminution
in volume by the additional precipitate no doubt
compensated for a greater loss which is not apparent.
The fact that large retention occurs in these precipi-
tates serves to bring out strikingly the results obtained
by the new method which are shown in the fifth column
of Table II. These results are consistently slightly
lower than theory, but are about within the limits
usually allowed for experimental error. The fact
that they are within an extreme range of 0.19 per cent
and the further fact that a result slightly below theory
is to be expected make them quite satisfactory, show-
ing the marked superiority of this method over the
Lindo-Gladding from the standpoint of accuracy.
To further test the new method more samples were
secured from the Fertilizer Control Laboratory and
analyzed by both methods with the following results:
Table III — Comparison op Lindo-Gladding Method with Modipied
Method
Potash Potash Difference
Reported Determined between
by L.-G. by De Roode Columns
Sample Method Method 2 and 3
No. Per cent Per cent Per cent
18 0.90 0.88 —0.02
59 4.34 4.46 0.12
74 4.45 4.57 0.12
90 2.71 2.79 0.08
93 4.60 4.66 0.06
160 0.90 0.93 0.03
247 1.84 1.84 0.00
302 4.75 4.89 0.14
311 4.61 4.85 0.24
313 3.52 3.59 0.07
335 2.88 2.89 0.01
356 1.64 174 0.10
357 2.54 2.71 0.17
386 0.25 0.26 0.01
421 0.95 1.10 0.15
641 1.74 1.97 0.23
694 1.73 1.87 0.09
770 1.38 1.40 0.02
961 0.86 0.93 0.07
54 2.18 2. 19 «01
Table III shows an average gain of 0.085 Per cent
for the modified method over the Lindo-Gladding
method on 20 samples. In every case except one the
new method gave higher results as was to be expected.
In the case of the exception the results were very close.
It is to be expected that the differences between the
methods on different samples will be variable on ac-
count of the varying amounts of impurities present
in different mixed fertilizers. The results by the modi-
fied method are accurate. In the Lindo-Gladding
method a case might arise where diminished volume
due to large precipitation would more than counter-
balance the effect of occlusion. This may be the case
in Sample 18, Table III. As a general rule, however,
the occlusion takes out more potash than the content
TEE JOURNAL OF INDUSTRIAL AM) ENGINEERING ( HEMISTRY Vol. 10, No. 3
of the volume that the precipitates occupy, this being
evidenced by every result obtained except that on
Sample 18.
The new method was used by Mr. T. D. Padgett
of this laboratory on 6 samples with concordant results.
JAllV
[1 has been shown that the DeRoode method sur-
mounts the difficulties encountered in the Lindo-
Gladding method. These same sources of error are
incident to the Anhalt and the Alternate methods to
a greater or less extent.
A few of the outstanding advantages of the modified
method may be summarized as follows: ease of manipu-
lation; small amount of time consumed, being much
less than in the Lindo-Gladding method; a much
greater degree of accuracy; all incineration, with
possible losses from sputtering; precipitation, with
its great loss from occlusion; filtration, not adding to
the accuracy of the determination due to the volume
occupied by the precipitates; and a great part of the
evaporation being dispensed with. Finally, any pro-
cess that eliminates the use of platinum apparatus
without sacrificing accuracy should be welcomed.
By avoiding ignition, only porcelain dishes have been
used in this method, thus placing at the disposal of
the Government large numbers of platinum dishes
now kept by all official and commercial laboratories
for the determination of potash.
Laboratory South Carolina Experiment Station
Clehson College, S. C.
LABORATORY AND PLANT
BLUE AND BROWN PRINT PAPER: CHARACTERISTICS,
TESTS AND SPECIFICATIONS
By F. P. Vkitch. C Frank Sammet and E. O. Reed
Received October 8, 1917
The manufacture of paper for use in blue and brown
printing is an important special branch of paper making.
The frequent handling and folding to which this class
of paper is subjected in all branches of engineering
wink and the value attached to many prints as perma-
nent records necessitate that the paper in addition
to the essential properties, to withstand coating, print-
ing and washing satisfactorily, shall be of exceptionally
high quality and great durability.
The first photograph produced dates back to about
1802, when Thomas Wedgewood published an article
in the Journal of the Royal Institute entitled "An
Account of a Method of I ' dntings upon Glass
and of Making Profiles by the Agencj of Light upon
Nitrate of Silver, with Observations by H. Davy."
In this article it is stated that white paper or white
leather when moistened with silver nitrate undergoes
no change when kept in the dark, but upon exposure
to the light speedily changes to nearly Mack, lilue
print paper was invented in 1840 by Sir John Hersehel,
and in 1001 brown print paper was patented by Van
I
Formerly the best paper obtainable in this country
for blue and brown printing came fi iny and
Prance, and though a number of paper makers have
made such papers for years ii has been exceedingly
diffii nil i" obtain a domi of sufficiently high
quality to be satisfactory in service. It is only recently
that American-made papers that will meet the ac
nying specifications for "Best Quality" and for
"High Quality" papers have come to the attention of
the Bureau.
In lino the Navy Department requested the De-
lllture to investigate the quality of
blue and brown print papers and submit Specifications
under which it could purchase high grade and durable
papers. In this in , than .'000 samples,
including, it is believed, all of the commercial brands
of blue and brown print paper, both foreign and do-
mestic, were examined, and from the data thus obtained
specifications were issued in 191 2 which now serve,
with some modifications, as a basis for the purchase
of these papers by the Navy Department. Up to
that time, so far as can be learned, no complete speci-
fications for blue and brown print paper had ever been
prepared and used in this country. By the aid of these
specifications and with suggestions from this Bureau,
American manufacturers have since made blue and
brown print papers which are equal to, and in some
superior to the foreign-made papers and which
have been found to meet all the accompanying speci-
fications in every particular An important special
branch of paper making has been established in this
country, and if the quality of the paper is maintained.
rs may confidently depend on these papers for
the most exacting requirements.
In a broad sense high-grade blue and brown print
paper is tper of the best quality, preferably
all rag >toi k, so sized as to be resistant in a proper
degree to the absorption of the sensitizing solution
and yet t" coat absolutely uniformly. As this class
of paper is s 0 much handling in both the
:ion and in many cases is valuable
as permanent records, it should possess high physical
ies and be very resistant to chemicals.
al and laboratory tests have demonstrated
that the most reliable indication of the durability
and serviceability of blue and brown print paper is
obtained by the determination of its folding endurance.1
This test does not, however, indicate the resistance
of paper to tearing when the print is being washed
and handled to remove the soluble salts. This informa-
tion is best obtain, ,' ermination of the tensile
strength' of the paper when wet. which gives results
1 Witch. Sammet am! Reed, "The Standardization and Accuracy
of the Tester for Detenniirini the Folding Endurance of Paper." Paper,
No 1.'. SO. 1 I
Reed "A Method for Determining the Strength of Paper
when Wei, TBD JODTUJAL, 8 1916), 1003.
Mar., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
223
conforming with actual service. Paper may comply
in all other respects with the specifications and yet
not withstand thorough washing and handling while
wet. In many instances sheets of paper 10 or more
feet in length are so handled. In these cases wet
strength is a property of the greatest importance,
since an otherwise serviceable paper would be en-
tirely unsatisfactory and its rejection would be neces-
sary.
Table I — Results of Physical Tests of Blue Print Papers
Coated and Uncoated
All Physical Tests Made at 70° F. and 65 Per cent Relative Humidity
Folding
Endur-
Bursting ance
Stock Weight Strength Trans-
Rag Straw 24x36 Aver- verse
L & P Per Per 500 age Strength Double
No. cent cent Lbs. Pts. Factor Folds
19724 Uncoated 100 0 29'A 30.5 1.03 403
Coated, exposed and
washed 28 31.0 1.11 426
19710 Uncoated 50 50 36V: 21.0 0.58 23
Coated, exposed and
washed 37 22.0 0.59 42
19669 Uncoated 65 35 37 27.0 0.73 71
Coated, exposed and
washed 39 28.0 0.72 107
19582 Uncoated 100 0 53Vs 50.5 0.92 955
Coated, exposed and
washed 52 51.0 0.98 1131
19756 Uncoated 75 25 66 47.5 0.72 352
Coated, exposed and
washed 67 49.0 0.73 364
19757 Uncoated 85 15 92 63.0 0.69 367
Coated, exposed and
washed 88'A 65.0 0.73 403
Blue prints are only positive prints, while brown
prints are chiefly used as negatives from which to
make blue prints. The translucency of the paper
used for brown prints is of some importance and can
be determined and specified by use of the translucency
photometer1 devised by this laboratory.
For papers to be used as permanent records only
the best quality rag stock is recommended. In in-
stances where permanency is not essential, but ser-
viceability for a limited period is desired, rag stock
mixed with sulfite or straw will produce a good paper.
A paper should have high folding endurance in both
directions and this property can be attained only
Table II — Results of Physical Tests of Brown Print Papers
Coated and Uncoated
All Physical Tests Made at 70° F. and 65 Per cent Relative Humidity
Folding
Endur-
Bursting ance
Stock Weight Strength Trans-
Rag Straw 24x36 Aver- verse
L & P Per Per 500 age Strength Double
No. cent cent Lbs. Pts. Factor Folds
19741 I ucoated 100 0 40 36.0 0.90 188
Coated, exposed and
washed 37 31.0 0.84 67
.oated 70 30 38'A 38.0 0.99 289
Coated, exposed and
washed 39 34.5 0.88 128
19738 Uncoated 100 0 52>A 43.5 0.83 554
Coated, exposed and
washed 52 35.5 0.68 14"
19742 Uncoated 100 0 55>/i 38.0 0.68 169
Coated, exposed and
washed 52 37.0 0.71 70
19739 Uncoated 100 0 75 50.5 0.67 4
Coated, exposed and
washed 71'/j 46.5 0.65
through the use of high-grade rag stock. The de-
termination and specification of the folding endurance
in the weak (usually the transverse) direction are suffi-
cient, since for practical purposes the results thus ob-
tained are fully as indicative of serviceability and
durability as arc the results obtained by testing the
folding endurance in both directions of the paper.
1 C. P. Sanimtt, "A Photometer for the Measurement of the Trans-
lucency of Paper," Tuis Journal, 9 (1917;, 784.
The stock must be so beaten and sized as to produce
a flexible sheet with a "closed" formation. Wet
strength not only depends on the character of the stock
and the beating, but largely also on the effectiveness
of the sizing and the formation of the sheet. For proper
•coating the paper should not be too heavily surface
sized nor highly glazed. It must, however, be well
sized since a serious defect would be to have the
coating solution penetrate the sheet.1 The best and
Table III — Specifications for Best Grade Unprepared or Prepared
Blue Print Paper — Also Unprepared Brown Print Paper
Extra
Thin Thin Medium Thick
vV eight
Basis 24x36 — 500 (Pounds) 28 40 55 70
17x22—500 (Pounds) 12 17 24 30
Stock
Rag ... (Per cent) 100 100 100 100
(Points) 25 40 50 63
Strength Factor (24x36 — 500) 0.90
Wet Tensile Strength
Longitudinal — Shall be not less
than (Grams) 500
Transverse — Shall be not less
than (Grams) 300
Folding Endurance
Weak direction (usually trans-
verse) shall be not less
than (Double folds) 400 500 800 1000
Thickness
Shall not exceed (Inch) 0.0030 0.0035 0.0050 0.0060
Ash
Shall not exceed (Percent) 2 2 2 2
most durable papers are those in which the essential
characteristics are obtained by the use of high-quality
stock, its proper beating, sizing and careful handling
on the machine.
The durability and serviceability of all grades of
blue and brown print papers are greatly affected by
the method and care with which the paper is coated
with sensitizing solutions. Paper was formerly coated
with sensitizing solutions using a brush or sponge and
subsequently allowing it to air-dry in a dark room.
Undoubtedly there is less injury to the paper when
coated and dried in this manner, but owing to the
great demand for this character of print paper this
Table IV — Specific
1.00
0.90
0.9
600
800
800
400
500
500
i for High-Grade Unprepared or Prepared
Blue Print Paper
Thin Medium Thick
Weight
Basis 24x36 — 500.
Basis 17x22 — 500.
Stock
Bursting Strength
Shall be not less than
Strength Factor (24x36—500) .
Wet Tensile Strength
Longitudinal — Shall be not
less than
Transverse — Shall be not less
(Percent) 100
(Points) 36
(i 90
tha
s) 600
si 400
800
500
800
500
Folding Endurance
Weak direction (usuallv transverse)
Shall be not less th.i u ' Double folds) 300 500 600
Thickness
Shall not exceed (Inch) 0.0035 0.0050 0.0060
Ash
Shall not exceed I Per cent) 2
procedure has been almost universally superseded by
machines for rapid coating and drying. The dura
bility of machine-coated paper is least affected when
iied at a slow speed and dried a a Low tempera-
ture. Rapid drying of sensitized paper at a high
temperature is very injurious to the paper, especially
when coated with brown print solution 1.
| i I . unmet, "The Detection of Fault) Sizing in Mich-Grade
Papers," Bureau of Chemistry, Circular 107.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 3
Brown print paper continually deteriorates with
age, even if properly wrapped and stored, due to the
nitrates in the coating liberating nitric acid which
attacks the fibers. The maximum strength of this
paper is retained only through its immediate use
after coating. Paper stored two or three months or
even for a shorter time, especially in summer or humid
localities, is usually unfit for service. It is almost
Table V — Specifications for Medium Grade Unprepared or Prepared
Blue Print
Thin Medium Thick
Weight
Basis 24x36—500 (Pounds) 40 55 70
Basis 17x22— 500 (Pounds) 17 24 30
Stock
Rag — Shall not be less than. (Percent) 50 50 50
Remainder may be bleached
sulfite of straw
(Points) 32.0
0.80
600
400
150
38.0
0.70
800
500
45.0
0.65
800
500
150
0.0060
Strength Factor (24x36 — 500)..
Wet Tensile Strength
Longitudinal — Shall be not
less than (Grams)
Transverse — Shall be not less
than (Grams)
Fold ing Endurance
Weak direction (usually transverse)
Shall be not less than (Double folds)
Thickness
Shall not exceed (Inch) 0.0035
Ash
Shall not exceed (Per cent) 5
impossible to remove entirely the injurious chemicals
from brown prints even by prolonged washing, but a
thoroughly washed print will be serviceable for a
considerable time.
Most blue print coating solutions are not injurious
to the paper if properly applied and the paper pro-
tected from light, moisture and heat. Blue print
paper is coated for printing at different speeds and at
least three speeds are generally obtainable. These
speeds are variously designated as "slow" or "regular,"
"rapid," and "electric." The speed at which a coated
paper may be printed is dependent on the proportion
of the ingredients of the coating. High-speed coatings
are most unstable and will keep only a short time.
Best prints are obtained by using the "slow" speed
coated paper, and coating of this kind will keep for a
much longer time.
printing, machines combining printing, washing and
drying have been developed. Unfortunately these
machines subject the paper during the printing and
drying to considerable heat arising from the artificial
lights and heating coils employed for drying. The
washing is not as thorough as tank washing since it
is done within a few minutes and with many machines
only the sensitized side is washed.
Table VI — Specifications for Hich-Grade Brown Print Paper
First Grade Unprepared Brown Print Paper Should Equal First Grade
Blue Print Paper
Thin Medium
Weight
Basis 24x36 — 500
Basis 17x22—500
Stock
Rag
( Pounds) 40
( Pounds) 1 7
55
24
Percent) 100
100
(Points) 35.0
45.0
0.90
0.8O
(Grams) 600
(Grams) 400
800
500
Strength Factor (24x36 — 500)
Wet Tensile Strength
Longitudinal — Shall be not less than.
Transverse — Shall be not less than . .
Folding Endurance
Weak direction (usually transverse)
Shall be not less than (Double folds) 300
(Inch) 0.0035
(Per cent) 2
The essential characteristics of blue and brown print
papers are identical except that only all rag paper of
the highest quality is suitable for brown prints.
The relative effects of the two coatings on papers
are shown in Tables I and II.
It will be seen that the bursting strength and folding
endurance of coated, printed and washed blue print
papers are not lower than of the same papers uncoated.
On the other hand the bursting strength, but more
especially the folding endurance of coated, printed
and washed brown print papers are lower than that
of the uncoated papers. The folding endurance is
decreased so greatly that it is clear that brown prints
cannot be durable and that where durability is impor-
tant blue prints must be used.
Three grades of blue print paper are sufficient for
all types of work. The best grade must be of a quality
Table VII — Analyses of Representative Uncoated Blue and Hr
Print Paper
All Physical Tests Made at 70
Weight .
24x36 17x22
Rag
L& P
500 500
Per
No.
Lbs. Lbs.
cent
28547
29>A 13
100
28541
35 15
100
31631
45 19'/.
100
28531
47 20
50
28542
52 22%
100
28513
55 '/. 24
100
28517
60 26
100
31803
62 27
100
28532
66 28 'A
70
28530
92 40
75
and 65 Per cent Relative Humidity
Bursting Bursting
no . Thickness Strength
Animal Starch 1/10000 Average
Inch Pts.
0.7
0.8
0.4
0.9
0.5
0.8
0.6
0.5
4.7
2.9
2.6
3.8
1.8
2.6
2.0
Present
Present
Present
Trace
Present
Present
Present
Present
Present
Present
29.0
38.5
55.5
31.0
42.0
35.0
42.5
76.0
46.5
60.5
Strength
Factor
24x36
0.98
1.10
1.23
0.66
0.80
0.63
0.71
1.23
0.71
0.66
Wet Tensilb
Strength
Long. Trans.
G. G.
566 310
820 526
552 308
742 398
808 629
10004- 570
1000+ 661
947 538
852 548
1000+ 886
Foldino
Endurance
Long. Trans.
Double Folds
1284 469
Care in the process of printing, washing and drying
of blue or brown prints is fully as important as in the
coating of the paper. The most durable results are
obtained by printing by sunlight, immersing the whole
print and thoroughly washing in tanks of running water,
followed by air-drying suspended from racks.
Sun printing is too slow for most commercial re-
quirements and "slow" printing coatings are not used
where a large number of prints are required in a short
time To meet the commercial requirement for rapid
suitable for permanent records and must withstand
frequent handling. High grade must be of good quality
suitable for records lasting a considerable period,
and must withstand frequent handling. Medium
grade may be a paper suitable for drawings of brief
existence which must, however, withstand a fair amount
of wear and tear. Paper not falling in these classi-
fications is not suitable for prints other than those of
a small size and requires no specifications, as the^_use
to which these prints are put is not severe.
Mar., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
225
Table VIII — Typical Results on Various Coatbd and Uncoatbd Papers
All Physical Tests Made at 70" F. and 65 Per cent. Relative Humidity
. Weight
-St
oc*
Bursting
Tensile
- — Stretch —
Wet Tensile
Folding
24x36
17x22
Rag
Ash
Thickness
Strength Strength Strength
Long.
Trans.
. — Strength — .
Endurance
L&P
500
500
Per
Per
Per
1/10000
Average
Factor
Long.
Trans.
Per
Per
Long.
Trans.
Long.
Trans.
No.
Lbs.
Lbs.
cent
cent
cent
Inch
Pts.
24x36
Kg.
Kg.
cent
cent
G.
G.
Double
Folds
28541
35.0
15.0
100
0.8
26
38.5
1.10
7.3
5.0
3.6
6.4
820
526
1815
932
28551
37.5
16.0
100
0.9
27
38.0
1.01
8.2
4.3
3.1
4.9
905
438
1099
424
31471
39.0
17.0
100
Straw
1.0
33
30.5
0.78
7.6
4.4
2.1
5.3
421
223
1226
536
28540
39.0
17.0
63
37
2.4
30
18.0
0.46
5.8
3.4
0.8
1.6
690
386
12
9
31246
41.0
17.5
100
0.9
30
30.5
0.74
7.3
3.1
2.4
6.2
633
273
473
119
31645
41.0
17.5
100
0.9
31
31.0
0.76
6.9
3.5
2.2
4.7
624
274
433
166
31647
42.0
18.0
100
0.7
30
37.5
0.89
8.9
3.0
2.9
6.7
854
320
1684
270
31643
42.0
18.0
100
0.6
30
36.5
0.87
9.2
3.5
2.9
5.0
878
333
1645
403
31641
42.0
18.0
100
0.9
30
31.0
0.74
7.0
3.9
2.9
4.9
634
344
683
249
3 1639 to)
43.5
19.0
100
1.9
30
36.5
0.84
8.9
3.5
2.9
4.3
869
325
1290
309
31629(0)
43.5
19.0
100
1.9
32
37.0
0.85
9.3
3.5
3.3
5.2
836
296
1315
320
31633(a)
43.5
19.0
100
1.7
31
38.5
0.89
8.7
3.3
3.1
5.9
840
309
1244
331
31631
45.0
19.5
100
0.4
35
55.5
1.23
10.3
6.1
4.4
7.5
552
308
3020
2137
31635(a)
45.0
19.5
100
1.8
35
52.5
1.17
10.4
5.1
4.2
6.3
582
275
2648
1775
31776
45.0
19.5
100
0.4
34
55.0
1.22
10.8
5.8
4.4
6.2
625
328
3265
2156
31802
45.5
19.5
100
0.5
35
57.5
1.26
10.1
5.8
3.6
5.7
614
337
3285
2390
31470
48.0
21.0
100
1.0
40
36.5
0.76
8.9
4.9
2.2
5.8
577
280
1160
716
31869(a)
48.5
21.0
100
0.8
40
67.0
1.38
11.1
6.4
4.2
7.2
1000 +
621
2936
2553
31476
49.5
21.5
100
0.6
35
39.0
0.79
9.3
4.4
3.0
5.9
934 •
433
1379
487
28542
52.0
22.5
100
0.5
35
42.0
0.80
6.5
5.4
3.5
7.0
808
629
1439
1308
Sulfite
31644
54.0
23.5
92
8
1.2
39
47.5
0.88
11.9
5.0
2.8
8.4
1000 +
425
2010
1121
31630(a)
54. S
23.5
100
2.0
40
48.5
0.89
11.5
4.9
3.0
7.2
959 +
375
1577
1054
31648
54.5
23.5
89
ii
1.0
40
46.5
0.85
10.8
4.4
3.0
10.3
1000 +
429
1385
1058
28513
55.5
24.0
100
0.8
39
35.0
0.63
8.8
4.6
2.6
5.4
1000 +
570
409
153
31640(a)
56.0
24.0
95
'5
2.1
40
48.0
0.86
11.0
4.9
3.1
9.8
974
418
1542
913
31634(a)
56.5
24.5
100
1.9
40
48.5
0.86
12.1
4.9
3.2
9.0
1001
415
1223
849
31636
56.5
24.5
100
2.1
37
37.0
0.66
9.1
4. I
2.8
7.1
824
363
825
429
31479
57.5
25.0
100
0.5
37
44.0
0.77
10.2
4.7
3.3
8.5
840
408
1402
448
31472
57.5
25.0
100
1.0
50
43.0
0.75
11.3
6.0
2.4
6.2
844
408
2075
1252
31637(a)
58.5
25.5
95
'5
1.9
40
45.5
0.78
10.9
4.8
2.7
7.1
868
370
1519
621
28517
60.0
26.0
100
0.6
43
42.5
0.71
9.2
5.3
2.5
4.9
1000 +
661
265
135
31646
61.5
26.5
100
0.9
50
35.5
0.58
8.1
5.3
2.4
4.8
974
676
201
197
31632(a)
61.5
26.5
100
1.6
52
66.5
1.08
12.0
7.3
4.0
7.0
805
420
3624
2406
31478
61.5
26.5
100
0.8
42
46.5
0.76
10.6
5.0
3.2
5.5
864
447
1219
331
31803
62.0
27.0
100
Straw
0.5
40
76.0
1.23
13.8
7.6
3.9
6.6
947
538
3576
2666
31477
63.5
27.5
100
1.0
45
49.5
0.78
9.8
6.3
3.9
6.6
906
539
1235
717
28532
66.0
28.5
70
30
4.7
50
46.5
0.71
9.0
6.0
2.5
4.6
852
548
717
400
31638(a)
69.0
30.0
100
1.4
50
59.0
0.85
14.0
6.3
3.5
7.1
1000 +
608
2874
1768
28530
92.0
40.0
75
25
2.9
71
60.5
0.66
12.3
7.2
2.9
4.4
1000 +
886
544
423
(a) These
samples were exposed, washed and dried blue prints
all other samples were uncoated.
There should be but one grade of brown print paper.
This should be of the highest quality obtainable.
Brown print paper should be used as soon after coating
as possible.
Specifications for blue and brown print papers,
the practicability and value of which have been demon-
strated by over 5 years' service, are given in Tables
III, IV, V and VI.
EXPLANATION OP CONDITIONS AND TESTS
These specifications are drawn on the basis that
the tests are to be made at 70 ° F. and 65 per cent
relative humidity. Coated paper should be exposed,
washed and allowed to air-dry in single sheets before
testing.
Paper varying in weight from that specified must
have a bursting strength relative to that stated.
Wet Strength: Tensile strength determined on
strips 15 mm. in width and 10 cm. in length, after
immersion in water at 700 F. for 20 minutes.
In Table VII are given complete results on ten
different uncoated blue and brown print papers for
the purpose of showing the relationship between the
stock and sizing and the physical qualities of the
paper.
High-grade rag stock, properly prepared, produces
the best physical qualities. Sulfite stock mixed with
rag stock does not give a high holding endurance and
lacks durability. Straw stock mixed with rag usually
produces a good wet strength and a fair folding en-
durance, but lacks durability.
Other than the quality of the stock used, one of the
most important factors in the manufacture of blue and
brown print papers is the character, quality and amount
of sizing. Analyses of this class of paper have usually
shown a high per cent of rosin or animal size or both.
An excessive amount of sizing is to be avoided as it
prevents the paper from coating properly. Animal
size aids the folding endurance of paper because of
its flexibility, while too much rosin size makes the
paper brittle and the folding endurance is decreased.
The papers which gave the best results on coating
with blue print solution are Nos. 28547, 29541 and
28542. Samples Nos. 31631 and 31803 were difficult
to coat owing to the large percentage of animal size.
For satisfactory coating and durability the paper
should not contain over 3 per cent of either rosin or
animal size.
Table VIII contains typical results obtained in the
examination of various lots of blue print papers, both
uncoated and coated. They show how widely the
quality of the papers varies and how few papers are
of high quality and satisfactory in both dry and wet
physical qualities. No direct relationship between
the physical qualities of paper in either the dry or
wet condition is observable although the same factors
in paper making determine the qualities. A great
many samples exhibiting very good folding endurance
are so low in wet strength as to render them useless
for most blue print work, while several papers showing
a poor folding endurance have a high wet strength.
CONCLUSIONS
Blue prints in many instances are highly important
permanent records which are subjected to most severe
226
THE JOURNAL OF INDUSTRIAL A N D ENGINEERING CHEMISTRY Vol. 10, No. j
handling in service. It is therefore essential that
such papers should comply with strict specifications.
Three types of specifications have been prepared which
will insure the quality of paper suitable for any par-
ticular purpose. Owing to the fact that there are
numerous inferior grades on the market the promis-
cuous purchase of blue print paper without specifica-
tions will likely lead to unsatisfactory service.
Only the highest quality paper should be used for
brown prints since the coating solution seriously in-
jures the fiber in a short time. Where a permanent
record is desired brown prints should never be
used.
It has been found in practical use that "thin" and
"medium" papers. give as good if not better service
than "thick" papers, and it is recommended that both
for utility and economy light-weight papers be used
whenever practicable.
The depth of color, clearness and durability of a
print are largely controlled by the methods of coating,
and care in printing, washing and drying. For the
best results slow-speed coatings should be used and
these should be printed at a low temperature and
thoroughly washed to remove all soluble salts and
then air-dried.
PRECAUTIONS TO BE OBSERVED WITH
PRINT PAPERS
JLUE AND BROWN
I — All coated papers should be used as soon after
coating as practicable; brown print papers will possess
their maximum durability only when printed immedi-
ately after coating.
II — To insure strength and durability of the printed
paper, all coating, printing and drying should be done
at the lowest practicable temperature.
Ill — After printing, the paper should be thoroughly
washed by immersion in fresh running water to remove
all unfixed acids and other chemicals, which if not
removed will cause the print to fade and the paper
to become brittle. Prints for permanent records can
hardly be washed too thoroughly. This applies es-
pecially to brown prints.
IV The coated paper must be kept in a cool, dry
place and be properly wrapped to exclude moisture
and light. This is absolutely essential with coated
brown print papers.
V Prints should never be folded. They should be
kept flat or rolled, in a dry, dark place.
Leather and Paper Laboratory
Bureau of Chemistry
Washinoton. D. C.
A HYDROGEN SULFIDE GENERATOR
By Louis Sattubr
Received l.mu.tr\ 24, 1918
A greal variety of hydrogen sulfidi
have been de cribed However, it still remained a
one which would satisfy the
Moratory wh Ontinually in
a comparatively large volume. The apparatus here
described has given satisfactory service in this labora-
tory. The construction is apparent from the sketch.
By shortening or lengthening the tube connecting
the reservoir C and the mixing bottle B the gas is de-
livered at any desired pressure. Furthermore, the
capacity of the generator can be readily altered to
hold either larger quantities of iron sulfide. A . or larger
quantities of acid, C.
MERCURY
SAFETY
VAEVE
After the aspirator bottle A has been filled with
iron sulfide, diluted hydrochloric acid (about 50 per
cent by volume) is poured into the reservoir bottle
C. By opening stopcocks 1 and 2 the acid is allowed
to flow into the mixing bottle B. This bottle should
be seven-eights filled. Then stopcock 1 is closed
and enough acid poured into C so that when stopcock
1 is again opened there are about 3 in. of acid left in
the reservoir bottle C after B is filled.
The waste acid is removed by closing stopcock 2
and opening stopcock 3. The pressure from the reser-
voir starts the syphon D. A Woulff bottle, £, is used
for washing the gas. This is partly filled with
into which leads a submerged lead coil sealed at the
end and perforated with small holes. Any excessive
gas pressure is taken care of by a safety device con-
sisting of a glass tube which may be lowered to any
depth into mercury.
The generator in this laboratory holds 50 lbs. of
iron sulfide and 14 liters of acid. The cost of ma-
terial was twenty-seven dollars.
Tub- Rockefeller Institute for Medical Research
New York City
Mar., 191S
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
227
DISTINGUISHING MANILA FROM ALL OTHER "HARD"
ROPE FIBERS
By Charles E. Swett
Received December 4, 1917
In the rope industry fibers are classed as "soft,"
hemp, jute, linen, cotton, etc., and "hard," as manila
(musa), sisal (agave), maguey, New Zealand (Phor-
mium tenax) and others. In general, the hard fibers are
lignified. Among the soft fibers jute also is a lignified
fiber, but its physical characteristics place it beside
hemp.
The two hard fibers of preeminent importance are
manila and sisal.
The distinction between manila and sisal is not easy,
except by a practical rope maker and not always by
him, especially when they occur together in rope.
When it is desired to estimate the amounts of the
two present in a given rope the microscope has to be
used. The cross-sections are characteristic but not in
all cases satisfactory. For instance, sisal from East
Africa is sufficiently different from manila to enable one
to separate them, but sisal from Yucatan (henequin)
is not always enough different to make it possible to
say how much may be present.
The sections are not easy to make and when made
may contain thousands of fibers. When it is con-
sidered that the field under magnification to 200 diam-
eters is of the order of one millimeter and that a rope
of 2 or 3 in. of cross-section may have to be examined it
will be understood that some method for differentiating
these fibers other than the employment of the micro-
scope would be of great use.
Such a method has been worked out in this laboratory
and is here described in some detail.
If the sample is treated with a solution of bleaching
powder acidulated with acetic acid, then with ammonia,
manila takes a russet-brown color. All other hard
fibers turn cherry-red. Thus it becomes possible to
distinguish manila from all the others, which is the
matter of chief importance.
SOLUTIONS REQUIRED
i. ether to pour down a strand to remove most of
the spinning oil.
2. bleaching powder solution — A clear solution
of chloride of lime, containing about 5 per cent of
available chlorine, acidulated with acetic acid (30 cc.
of bleaching solution and 2 cc. glacial acetic acid).
Acidulation with an acid stronger than acetic will not
answer, for example, hydrochloric acid will give no
test.
3. water to rinse after the above.
4. alcohol to remove water.
5. STK"N(. AMMONIA.
PRELIMINARY EXAMINATION OF THE SAMPLE
Remove most of the oil by pouring ether down the
strand. Wave through the air for a minute or two to
remove most of the ether; immerse one end of the sample
in the acidulated bleach solution for 20 sec; rinse first
withjwater, then with alcohol and then immerse in
ammonia.
Manila will instantly turn brown.
Sisal, New Zealand, istle, Mauritius, maguey will
assume a cherry-red.
When so applied the test is somewhat fugitive, the
red color degrading in the course of a few minutes so
that it may not be possible to pick out the different
colored fibers from the strand. As applied it enables
one to say whether the sample is all manila, all non-
manila or a mixture. This is all that is required in
many instances.
When it becomes necessary to estimate the percent-
ages of manila and non-manila the procedure is as fol-
lows:
Apply the test as before but instead of immersing the
fibers in ammonia in the last operation, suspend the
treated end of the strand above the ammonia for a
minute or so. As thus practiced the manila does not
assume the brown color as rapidly, but at the end of
2 or 3 min. the color develops and is permanent.
The cherry-red of the non-manila fibers remains for
hours and a separation may be made by picking out the
red or the brown. A reading glass is of assistance.
When the separation is made as above it is desirable
to take the two differently colored strands and apply the
test as first described, i. e., by treating the hitherto
untreated ends with ether, immersing in bleach acetic
solution, rinsing with water and then immersing in
ammonia. This serves as a check and as the separation
will be closely approximate as a result of the fuming
test, the few fibers which may show up as wrongly
placed can be removed with ease.
One desiring to practice this test should first work on
samples of known origin. With practice it seems to be
possible to estimate the manila content of a rope down
to a single fiber. As the test is so quickly applied it is
the writer's practice to take less than a strand for treat-
ment and then go through the sample taking perhaps
20 or 30 fibers at a time.
The difference between the red and the brown is
most evident at the end of 3 or 4 min. after fuming with
the ammonia.
The bleach solution made with one part of chloride
of lime and seven parts of water, then filtered, may be
kept in a stoppered amber bottle away from the light
for a long time. When some is to be used it should be
poured from the stock solution and acidulated with the
acetic acid for present use. Throw away when the
tests are done. It will not keep in an acidulated con-
dition.
Chlorine water will not serve, neither will iodine
solution or bromine water; nor will any acid tried
answer so well as acetic.
Too much emphasis cannot be placed on the fact that
hydrochloric or other strong acid is not suitable to
replace acetic acid as used in this test. This reiteration
is made because, notwithstanding specific instructions,
two competent chemists have assumed that because
the test failed with hydrochloric acid there was nothing
in it. In neither case were the directions followed and
when attention was called to this fact no trouble was
experienced in securing the appearances described.
Laboratory of Arthur D. Little. Inc.
Cambridge, Mass.
228
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 3
CURRENT INDUSTRIAL NLW5
DIESEL ENGINE BLAST PRESSURE CONTROL
An automatic electrical device, developed by Mirrlees, Bicker-
ton and Day of Stockport, for regulating in accordance with
the load the pressure of the air which blows the fuel into the
cylinders of Diesel engines, was described by Mr. H. S. Russel
before the Diesel Engine Users' Association. The main current
passing round a solenoid, controls a finger which moves round
the scale of a pressure gauge and which is calibrated to point
to that blast pressure which is best for the engine for the amount
of power being generated at the moment, its zero or no-load
position being the no-load blast pressure. It is provided with
platinum contact pieces, as also is the indicating finger of the
pressure gauge which is connected to the blast pipe; the two,
therefore, act as a single-pole switch, making and breaking a
relay circuit which in turn makes and breaks the circuit which
operates the throttle valve on the air-compressor inlet. Should
the pressure finger stand lower down the scale than the other
finger the electrical arrangements are such that the throttle
valve, which is normally held closed by a spring, is pulled off
its seat. The pressure in the blast pipe then rises rapidly (the
compressor always having a substantial margin of capacity)
until the pressure finger moves up to and makes contact with
the other finger; when this happens the throttle valve closes and
remains closed until the fingers come together again. By this
device a variation from 550 lb. (no-load pressure) to 950 lb.
(full-load pressure) can be obtained in four seconds, and as
several seconds are required for the fly-wheel to slow down and
the governor admit more fuel the correct pressure is always
on the top of the fuel.— A. McMillan.
HIDES AND SKINS FROM VENEZUELA
There are sources of supply of cattle hides not yet fully ex-
ploited in Venezuela, in spite of the attention which is being
given to developing the meat export trade. Purchasers of deer
skins, alligator and jaguar skins, says the Times Trade Supple-
ment, are desired, as well as purchasers of cattle hides.
In these times when anything capable of being made into
leather is almost sure to repay careful investigation, it would
probably be worth the while of the tanner to ascertain what use
could be made of the skin of the chiguire or "carpincho." This
is a big rodent, about 4 ft. by 3 ft., having a thick skin covered
with a brown coat of short, coarse hair. Millions of these
animals are to be found in the valleys of the Orinoco and its
tributaries and, owing to the damage they do to sugar crops, the
Venezuelan Government is desirous of exterminating them. — M.
GERMANY'S COMMERCIAL METHODS
We read in the Revue Ginirale de I' ElectricitS that the French
Government has learned from an authorized source that, in
neutral countries, in Spain notably, the Germans are plotting
the disorganization of allied enterprises which compete with their
own. They are offering very advantageous contracts to the
greatest number of men belonging to the allied enterprises to
lead those men to abandon abruptly their employment as soon
as peace is declared. At the present time the Germans are
specially busy with the electrical understandings and they are
endeavoring to bring about their stoppage by the lack of ex-
perienced hands. German agents have carried out a complete
investigation in regard to the whole personnel of the said allied
enterprises from laborers to technical staff to whom offers have
been made, to come into effect after the war, of situations much
more advantageous than those they now hold. The contract ensur-
ing the situation is drawn up either in Germany 01 Switzerland and
signed before a Notary Public. Similar attempts at disorganization
are being proceeded with by the enemy in Switzerland. — M.
COAL-MINING MACHINERY FOR ARGENTINA
Owing to the severe lesson learned in Argentina since the out-
break of war in regard to imported coal supplies, the Govern-
ment is making a determined effort to work the coal deposits
that have so far been located. A considerable amount of money
has been allocated for this purpose and already orders have
been placed for part of the necessary equipment and plant.
Manufacturers of coal-mining plant, hoisting machinery,
wire ropes, pumps, fans and iron piping would do well, says the
Times Trade Supplement, to get into communication with the
authorities at Chubut where the best of the coal deposits, so
far discovered, are situated. The mines in which the Govern-
ment is mostly interested arc in the territory of Chubut, situated
124 miles from the nearest railway. A line of rails is, however,
to be laid down to join up the mines with the track. The
quality of the coal is said to be good.
Other deposits are situated in the Provinces of San Juan
and Mendoza. So far, however, it has proved anything but a
simple matter to obtain delivery of even a modest consignment
of apparatus. — M.
UTILIZATION OF NITRE CAKE
In a paper in Rev. des prod. chim. the possibility of using nitre
cake in connection with the sulfites obtained in phenol manu-
facture is considered. By combining nitre cake with the residual
sulfite it should be possible to obtain 86.5 per cent sodium sul-
fate together with 5.2 per cent free sulfuric acid, and about 7
per cent alumina and sodium sulfite. This product should be
of interest in the manufacture of glass. A certain quantity
of phenol should also be recovered at the same time. The
percentage of sodium sulfite may be taken as not less than
50 per cent. If the liquor is divided into two parts, the first
part may be treated with nitre cake to produce sodium sulfate
and sulfur dioxide and the second part may be saturated with
the sulfur dioxide obtained from the first part to produce pyro-
sulfite or metasulfite. The author claims to have actually ob-
tained metabisulfite in this way, and, with efficient cooling, the
yield should be quantitative.
A further important use for nitre cake appears to be in the
manufacture of magnesium sulfate. The hot nitre cake is con-
veyed into a trough containing a carbonated magnesium com-
pound such as dolomite or magnesite, the mixture being thor-
oughly stirred. The cooled mass, which is very spongy owing
to the evolution of carbon dioxide, is broken up, washed with
boiling water, decanted, filtered and evaporated. The sodium
and magnesium sulfates are separated by difference in solu-
bility. It would seem from figures given that this utilization
of nitre cake should be remunerative. — M.
ELECTRO-TECHNICAL INDUSTRY IN JAPAN
Japan has been working hard, says Engineering, 104 (19:7),
684, under favorable conditions during the war, and, among
other branches of her industry, that of the electro-technical
industry has made important strides. As an example may
be mentioned large capacity electric generators of, say, 10,000
k\v . which before the war were always imported from England,
America and Germany, but which are now made within the
country. The aggregate value of electro-technical machines
and appliances annually manufactured in Japan has been tripled
during the war and now amounts to between S15.000.000 and
$20,000,000. The export of electric plant and apparatus also
shows a material increase especially to China and Dutch India.
and Japan already holds the fifth place in the matter of export
of incandescent lamps. — M.
Mar., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
TANNIN AND TIMBER
Communications will be welcomed by the Bureau of Forestry,
Manila, says a contemporary, from firms in a position to exploit
the very large growth of mangrove in the Philippine Islands.
The tannin content of the barks amounts to from 12 to 35 per
cent. A completely successful cutch is said to have been made,
dry, solid and brown in color, from the mangrove bark obtained
in the Archipelago. There are 21 species of mangrove in the
Philippine swamps and the potential cutch production is
tremendous. Mindoro, one of the larger islands about 100
miles from Manila, appears to offer the most inducement to a
firm able to work the mangrove growths for piles, poles and
firewood as well as bark. Firewood cutters already operating
would be willing to sell the bark. There are over 30,000 acres
of mangrove swamps in Mindoro estimated to yield 50,000 tons
of bark convertible into about 17,000 tons of cutch. — M.
ALUMINUM GOODS FOR BRAZIL
According to the Times Trade Supplement there is here a
market for as many articles of light material as can be shipped,
all existing stocks, for some months past, having been completely
exhausted. The dearth of supply is entirely due to the cessa-
tion of shipments of German consignment through neutral
ports which continued for some time after the outbreak of war.
Although some small shipments of aluminum goods were sent
to South America from the United Kingdom, three-fifths of
the imports of this class came from Germany and Austria.
The demand among the Brazilian and in all the Central Amer-
ican countries is for cheap cooking utensils. German goods,
when obtainable, have been invoiced at very low figures against
which it has been difficult for other manufacturers to compete,
and it might be worth while for manufacturers to send out a
full range of samples making the prices as low as possible and
allowing a reasonable amount of credit. The value of German
trade in these goods amounted in normal times, with Brazil
alone, to over $82,500 and with the other countries of South
America, to over $85,000. It is, however, worthy of note that
both the United Kingdom and the United States purchased
these goods from Germany in pre-war days to a considerable
extent. Manufacturers may be interested to know that the
German goods are "spun" not "cast," this being the chief reason
why they can be sold at a cheaper rate. In addition, the South
Americans prefer the dull silvery appearance of the German
goods to the bright, polished, tin-like appearance of the British
goods. The more salable of aluminum hardware articles ex-
ported to Brazil include meat dishes, pudding bowls, colanders,
pie dishes, forks, spoons, stewpans, milk boilers, kettles, sauce-
pans (with or without lids), spirit stoves. — M.
WIRING SUPPLIES
A fully illustrated list has been issued by the Lamp and Wiring
Supplies Department of the British Thomson-Houston Company,
Mazda House, London, and deals entirely with wiring installa-
tion accessories. It covers the standard types of such appli-
ances as lampholders, switches, wall plugs, ceiling roses, cut-
outs, distribution boards, fuse boxes and insulators. Among
the items included are porcelain Goliath Edison screw lamp-
holders designed to meet the requirements of the Admiralty and
other Government Departments; new designs of brass Goliath
holders; standard bayonet and Edison screw holders in both
porcelain and brass-case types; the "Quiklok" cover ceiling rose,
which has been approved and standardized by the War Office
and which, among other advantages over the ordinary ceiling
rose, can be wired on the bench and secured in position on the
•ceiling by a quarter turn of the wrist; interlocking and other
types of combination switch plugs; and new patterns of dis-
tribution fuse boards and insulators. — M.
PURE BISMUTH
According to an article in the Journal of the Chemical Society,
London, the determination of minute traces of impurity in bis-
muth is difficult since the basic salts form amorphous precipitates
which obstinately retain other metals as also do the sulfide
and oxide. The electrolytic method of separation also fails.
The best means of obtaining the pure metal is by crystallizing
the normal nitrate from strong nitric acid. Fairly pure bismuth
nitrate is dissolved in half its weight of 8 per cent nitric acid and
the solution mixed with an equal weight of strong nitric acid.
The crystals which separate at o to ioc C. are washed with ice-
cold nitric acid. The pure nitrate is then converted into the
oxide by heating and this is reduced by fusion with potassium
cyanide. Further purification is effected by melting the metal
under paraffin and removing by means of a glass spoon the first
and purest crystals formed. Purified bismuth melts at27i°C,
and when pressed into wire the melting point is lowered to
195 ° C. and its specific electric resistance is then 1.20. Various
samples of bismuth sold as pure were found to contain from 0.03
to 0.25 per cent of impurities. The method for testing for im-
purities is detailed. — M.
CHROMIUM STEEL FOR MAGNETS
Owing to the commandeering of tungsten for military pur-
poses, says Engineering, 105 (1918), 18, German electricians
found themselves without tungsten for their magnet steels
early in the war and experiments on the use of chromium in
place of tungsten which had already been projected were ac-
celerated. The research has been conducted at the Reichsan-
stalt on behalf of the Verband Deutscher Electrotechniker. The
preliminary report of 19 17 did not give particulars which were,
however, communicated to the members of the Verband on
inquiry. Krupp's Works supplied 37 specimens of steel con-
taining varying percentages of chromium and carbon. They
had been turned into rods and hardened in various ways in the
works and were then aged after the method of Stronhal and Barus
by repeated heating, cooling and mechanical stress while being
tested at intervals in the Reichsanstalt. The unfinished in-
vestigation concerns also the temperature coefficient of mag-
netization and the durability of the steels. It results that on
an average, chromium steels which have undergone suitable
heat treatment do not rank below tungsten steels. The very
best chromium steels, however, are not equal to the best tungsten
steels. Technically, chromium steels would thus appear to be
quite satisfactory while for special researches their further
improvement is desirable. — M.
AN AUTOMATIC CONTROLLER FOR ELECTRICAL
HEATING APPARATUS
The Electrical World gives an account of a small and com-
pact heating controller for use with electrical heating appli-
ances which has been brought out by the Automatic Electric-
Controller Company of Seattle. The device is made in two
types, one for alternating and one for both alternating and
direct current. It consists of a thermostat of copper and iron
riveted together and placed immediately over a heating coil
connected in series with the load. The heat from the coil
causes the thermostat to break the circuit whenever the tempera-
ture rises above a certain point. It can be adjusted to operate
over a wide range of temperature between 90 ° and 1600 C. by
ca using the contact point to move downward and bend the
thermostat, thus increasing the temperature requisite to cause
the latter to break connection. It is claimed that the device
will enable 40 per cent of the heat now used in excess by various
implements to be saved, as the exact temperature necessary
for any operation can be obtained. The device also acts as
a safeguard against excessive current. — M.
23°
THE JOURNAL OF INDUSTRIAL AND ENGINEERING ( EEMISTRY Vol. 10. No. 3
MACHINERY FOR KOREA
The completion of the Seishin Kainei Railway in Northern
Korea, says a contemporary, opens up hitherto unworked fields
of coal, iron and timber. The iron mines in Mosan are now
likely to b< exploited and it is said Hut the Mitsubishi Kuhara
and .Suzuki concerns are all interesting themselves in the develop-
ment. Investigations are now being made into the possibili-
ties of the Kanhoku coal field. The product so far obtained
is not of very good quality but it is hoped that better strata
will be reached. The Suzuki Company has sent experts to ex-
amine the forests on the banks of the River Tumen in order to see if
a large lumber mill would pay. Meanwhile, a state sawmill
has been started in Kainei and a pulp manufacturing plant
has been erected in Shingishu for the purpose of utilizing the
forests on the banks of the Yalu. The timber from this source
is also to be turned to account at a paper mill to be erected
at New Wiju. This scheme involves an expenditure of $5,000,000.
In the first place, a plant will be set up for turning out about
20,000 tons of paper-making material annually and this part
of the program is expected to take two years. Seventy miles
up the River Yalu a hydro-electrically driven pulp mill is pro-
jected while a third part of the developments consists in the
erection of yet another factory capable of manufacturing 30,000
tons of pulp a year. — M.
AUTOCLAVES AND HIGH PRESSURE PROBLEMS
According to a paper by Mr. C. E. Stromeyer, Chief Engineer
to the Manchester Steam Users' Association, one way out of
high pressure difficulties is to discard autoclaves altogether and
to allow the chemical process to take place in a long pipe. The
inlet portion of such a pipe should be coiled into a vessel con-
taining molten or solid lead heated to the proper temperature
or it should be led through vessels with different temperatures;
the end of the coil could be led through a cooling vessel. The
chemicals, usually two fluids, would have to be forced into one
end, cither hot or cold, by two plunger pumps of correct volumes
acting simultaneously and, if the diameter of the pipe be made
sufficiently small to ensure that the critical velocity is exceeded,
thorough mixing is bound to take place. A loaded relief valve
would have to be provided at the outlet end. Several of these
coils are in use and are said to work satisfactorily. It appears
Hi, it they are always made of iron whereby their use is limited
to certain processes. They could, however, be mad. .if lead
provided that precautions be adopted of equalizing or nearly
equalizing the pressure on the outside and the inside. To do
this and at the same time maintain the correct temperature,
it may be necessary to place the pipes in closed vessels ami make
the heating baths of various fluiels having suitable boiling tem-
peratures. Possibly the same substances which are used or
piciilueed in the pipes might be used as heaters. — M.
UTILIZATION OF WASTE BOOTS
\i meeting of the London Section of the Society of Chemical
Industry, a paper em the "Utilization of Cemdemned Army
Boots" was read. The author dealt with the use of waste boot
leathei foi road making, the- manufacture of animal charcoal,
ammonium sulfate, the production ol grease and fatty matters,
manure-, leather-board, clogs, washers, mats, leather pulp,
leather powder, cyanides, glue and size. With regard to the manu-
1 ' turi hi leather-board, the- author -aid that, in his opinion,
although it had been tin; subject of many patents, it had not met
with any measure of commercial success. At the present time,
the manufacture of leathei board for use in insoles of boots and
the soles of slippers and such like, employing this discarded
army footwear for the purp" appears to be more
attractive than in less strenuous times. < >u the question of
using waste leather for the production eif leather pulp, it was
1. it. il that this was probably practicable but it would have a
powerful competitor for this purpose in the feirm of waste scraps,
cuttings and machine turnings of new leather which is more
suitable to work up. The relative prices of the two materials
would decide whether this would be a sound commercial propo-
sition.— M.
VEGETABLE WAX FROM COLOMBIA
A wax obtained from the leaves of the wax palm of the Andes,
Ceroxylon andicolum, used in Colombia for making candles but
not yet exported has been examined recently at the Imperial
Institute, Loudon, and full particulars are given in the current
bulletin of the Institute. The palms occur only in western
tropical South America and are said to be exceedingly abundant.
The sample examined consisted of fine powdered wax of a pale
straw color with a small admixture e)f vegetable matter. The
palm wax when purified is similar in character to carnauba wax
which comes from Brazil, and to candelilla wax imported from
Mexico, except that its melting point (93° C.) is higher than
that of carnauba wax (84 ° C.) and that of candelilla (70° to
720 C.).— M.
ZINC REFINING IN JAPAN
Interesting particulars have reacheel us, says the Eastern
Engineering Journal, regarding the zinc refining industry in
Japan. It would appear that the supply of ore for the Japanese
zinc refineries is by no means assured. The production of zinc
ore in Japan deies not exceed 50,000 tons per annum, while the
existing Japanese refineries need about three times that quantity
if they are to be kept at their full capacity. Further, if
all the projects for new refineries and additional plant are
realized, the requirements of the- industry in the near future
for /iiie- on- will exceed .too.tK.io tons. — M.
SOUTH AFRICAN INDUSTRIAL DEVELOPMENTS
The British Trade Commissioner in South Africa writes that
.1 company has been formed I'm the- manufacture of carbide at
Gerniiston and was expected te> begin producing at tin end of
last October, it is hoped thai the factory will be- able to pro-
eluce some ,t tons "i carbidi i"i day. The same company is
also producing carbon electrodes. A company for detinning
purposes has been established al Cape Town Large quanti
ties of scrap tin have- accumulated in differt m parts of tin- Union
and 11 1 thought that there will be- an ample supply of waste
tin for the company's purpose \ glass bottle factory is to be
reopened at Hatherley, Victoria, as soon as certain technical
difficulties have been overcome. The- recoverj of .nse-uie-. tin
smelting ami tin- refining of antimony are among other imhis-
trie-s which have- also been established in tin- Union. M.
BRITISH BOARD OF TRADE
I'm iiie; the month of December, the British Board of Trade
received inquiries from firms in the United Kingdom and abroad
regarding sources of supply for the following articles. Firms
which may be able to supply information regarding these things
are- requested to communicate with tin- Director of the Com-
mercial Intelligence Branch, Board of Trade. 73 Basinghall St.,
London, E. C.
Machinery and Plant for:
Die casting machines
Making noodles
Distillation of peat and lignite
Covering copper wire with India
rubber insulation
Manufacture of sugar of milk
and dyeing furs
' » toothpicks
Brace-fittings .rustless steel]
Buckles lor trench coats
Buttons
Carbon brushes for dynamos
Garter-fittings (rustless steel)
Metal polish
Pitch coke
Tic fittings
\\ helebone for brushes
Making wooden eoutup
Marking thermometers
M.
Mar.. 1018 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
TRADL ASSOCIATIONS
THE CHEMICAL ALLIANCE
Some 200 manufacturers of chemicals met at the Hotel Bilt-
more, New York City, on Wednesday, February 6, 1918, to
organize the Chemical Alliance and its affairs for the coming
year.
It was at the suggestion of the U. S. Department of Com-
merce that the Chemical Alliance was formed and it was in-
corporated under the laws of Connecticut on July 30, 1917.
When organized it was made up of the chairmen of the sub-
committees of the Committee on Chemicals and the officers were :
President, W. H. Nichols; Vice-President, Horace Bowker;
Secretary, J. D. Cameron Bradley. The sub-committees have
since been discontinued.
The object of the Alliance as at present organized is to carry
on the work begun by these committees and to cooperate with
the Government in solving war problems which affect the in-
dustry. In the words of the constitution of the Alliance,
"The Chemical Alliance, Inc. is established to promote in all lawful
ways the commercial interests of its members, to cooperate with the Govern-
ment in all matters of national concern, and to secure the advantages to be
obtained by mutual cooperation; to acquire and disseminate information
concerning trade conditions at home and abroad, credits and other matters
of interest; to deal with questions affecting the public safety and welfare,
and in general to promote the interests of the chemical industry and all
its branches."
The organization is an alliance of all branches of chemical
industry and industries related thereto, but only manufacturers
are admitted to membership. There are at present nine sections,
but a tenth for Oils, Fats and Greases will soon be established.
The nine sections already formed with the number of members
in each are as follows:
1. Acids— 31
2. Coal and Gas
By-Products — 20
3. Foreign Pyrites — 7
4. Electrochemicals — 9
5. Fertilizers— 61
Miscellaneous
Chemicals — 20
Alkalies— 12
Domestic Pyrites
and Sulfur — 4
Dyestuffs — 10
Horace Bowker, president of the Alliance, in addressing the
meeting, outlined the general plan for the cooperation of the
Alliance with the War Industries Board and emphasized the
fact that the Alliance was not the outgrowth of any Association
but was brought into existence by war needs to serve the Govern-
ment as needed by furnishing information, or men, or both.
Mr. MacDowell, representing the War Materials Committee
of the War Industries Board, described the functions of that
committee and outlined their expectations of cooperating with
the Alliance and availing themselves of its service.
Officers for the general organization were elected as follows:
President: Horace Bowker, The American Agricultural Chemical Co.,
2 Rector Street, New York City.
Vice-President: Henry Howard, The Merrimac Chemical Co., 148 State
St., Boston. Mass.
Secretary-Treasurer: J. D. Cameron Bradley, American Agricultural
1 h. mical Co.. 92 State St., Boston, Mass.
Directors: Horace Bowker, American Agricultural Chemical Co.,
2 Rector St , Xew York City; Henry Howard, Merrimac Chemical Co.,
148 State St., New York City; Win. Hamlin Childs, The Barrett Co.,
17 Battery Place, New York City; E. R. Grasselli, Grasselli Chemical Co.,
Cleveland, Ohio; W. D. Huntington, Davison Chemical Compai
more, Md.; I> w. Jayne, The Barrett Co., 17 Battery Place, New York
I Ledoux, The Pyrites Co., Ltd.. 15 William St., New York City;
K. A. I.idbury, Oldbury Klcctro-Chemical Co., Niagara Kails. N. Y.; C. H.
1 Armour Fertilizer Works, Chicago, III.. Edward Mallinckrodt,
Jr., Mallinckrodt Chemical Works. 3600 N. 2nd St., St. Louis, Mo . urn I!
Nichols, General Chemical Co., 25 Broad St., New York City, J. D. Pennock,
Solvay I'n l Reese, E. I. du Pont de Nemours
Miming! ..!.; John J. Riker, 19 Cedar St., New York City;
A. G. Roscngartcn Powers-Weightman-Rosengarten Co., Philadelphia, Pa.;
ii ..ii. Virgini ■ I arolina Chemical Co., Richmond, Va.
The sections elected chairmen and committees as follows:
1. Acids Section: Chairman: W. D. Huntington, Davison Chemical
Co., Baltimore, Md.; S. B. Fleming, International Agric. Corp., 61 Broad-
way, New York City; J. M. Goetchius, General Chemical Co., 25 Broad St.,
New York City; C.F. Burroughs, F. S. Royster Guano Co., Norfolk, Va.;
J. H. D. Rodier, Grasselli Chemical Co., Cleveland, Ohio; Chas. M. Butter-
worth, Pennsylvania Salt Co., Philadelphia, Pa.
2. Coal and Gas By-products Section: Chairman: D. W. Jayne,
The Barrett Co., 17 Battery Place, New York City; W. R. Addicks, Con-
solidated Gas Co., New York City; C. J. Ramsburg, H. Koppers Co.,
Pittsburgh, Pa.; W. E. MacKay, New England Coke and Gas Co., Boston,
Mass.; A. A. Schlesinger, Milwaukee Coke and Gas Co., Milwaukee, Wis.
3. Foreign Pyrites Section: Chairman: A. D. Ledoux, Pyrites Co.,
Ltd., 15 William St., New York City; C. F. Burroughs, F. S. Royster Guano
Co., Norfolk, Va.; F. H. Nichols, General Chemical Co., 25 Broad St., New
York City; W. H. Mills, Naylor & Co., 120 Broadway, New York City.
4. Electrochemicals Section: Chairman: F. A. Lidbury, Oldbury
Electro-Chemical Co., Niagara Falls, N. Y.; C. D. Cohen, American Cyan-
amid Co., 511 Fifth Ave., New York City; F. J. Tone, Carborundum Co.,
Niagara Falls, N. Y.
5. Fertilizers Section: Chairman: C. G. Wilson, Virginia-Carolina
Chemical Co., Richmond. Va.; C. F. Burroughs, F. S. Royster Guano Co.,
Norfolk, Va.; W. D. Huntington, Davison Chemical Co., Baltimore. Md.;
C. H. MacDowell. Armour Fertilizer Works, Chicago, 111.; A. C. Read,
Read Phosphate Co., Savannah, Ga.; Albert French, Internat. Agric. Corp.,
61 Broadway, New York City; Porter Fleming. Southern States Phos. &
Fert. Co., Augusta, Ga.; William Prescott, American Agric. Chem. Co.,
2 Rector St., New York City; Frederick Rayheld, Swift & Company,
Chicago, 111.
6. Miscellaneous Chemicals Section: Chairman: A. G. Rosengarten,
Powers-Weightman-Rosengarten Co., Philadelphia, Pa.; G. P. Adamson,
General Chemical Co., 25 Broad St.. New York City; Wm. Henry Bower,
Henry Bower Chemical Mfg. Co., Philadelphia. Pa.
7. Alkalies Section: Chairman: J. D. Pennock, Solvay Process Co.,
Syracuse, N. Y.; E. H. Hooker, Hooker Electro-Chemical Co., 40 Wall St.,
New York City; N. E. Bartlett; E. Sargent; EH Winkler, Columbia Chem-
ical Co., Pittsburgh, Pa.
8. Domestic Pyrites and Sulfur Section: Chairman: C. H. Mac-
Dowell, Armour Fertilizer Works, Chicago, 111.; W. N. Wilkinson, Union
Sulphur Co., 17 Battery Place, New York City; H. P. Nash, Ladenburg-
Thalmann Co., 25 Broad St., New York City; C. G. Wilson, Virginia-
Carolina Chemical Co., Richmond, Va.
9. Dyestuffs Section: Chairman: C. L. Reese. E. I. du Pont de
Nemours & Co., Wilmington, Del.; H. A. Metz, Central Dyestuffs & Chem.
Co., Newark, N. J.; M. R. Poucher, du Pont Chemical Co., Wilmington,
Del.; R. W. Hochstetter. Ault & Wiborg, Cincinnati. Ohio; August Merz,
Heller & Merz. Newark, N. J.; H. D. Ruhm, Marden, Orth & Hastings Co.,
■61 Broadway, New York City; I. F. Stone. National Aniline Co., New York
City; F. M. Fargo, Calco Chemical Co., Bound Brook. N. T ; A. R. Curtin,
Middlesex Chemical Co.; J. M Matthews. Grasselli Chemical Co., New
York City.
DYESTUFF CONVENTION
On Tuesday, January 22, a large assemblage of manufac-
turers of and dealers in dyestuffs gathered in Rumford Hall,
Chemists' Club, New York City, to discuss the advisability of
organizing an association to be devoted to American dyestuff
interests.
Mr. H. G. McKerrow outlined the preliminary steps which
had been taken in bringing about the meeting, and suggested
that specific actions were not essential at this time, but rather a
decision as to whether or not such an association is desirable.
The following temporary officers were chosen:
Chairman: Frank Hemingway, Frank Hemingway, Inc., New
York.
irer: C. 1'. Jenkinson, National City Hank, New
York
1 v.- C. C. Bennett, Color Trade Journal. New York.
11 taking the chair, Mr. Hemingway called attention to
the fact that while standardization of dyestuff s was an importanl
topic it constituted onlj one oi many important functions of such
an association as is contemplated. He urged thai thl policj of
tin 1 nidation should not b« loo open in regard to membership,
and proposed tin appointment "I a large committee to determine
tin qualifications for membership. The importance of coopera-
252
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 3
tion between American, British and French interests was clearly
outlined and the speaker concluded with a tribute of appreciation
of Mr. McKerrow's work in the preliminary steps which resulted
in the gathering.
Mr. McKerrow spoke at length concerning the purpose and
possibilities of such an association, discussing the questions of
standardization, the need of arbitration in the great mass of now-
pending disputes, of adequate tariff protection, and of fair dealing
in the industry.
The meeting was then addressed by Benjamin M. Kaye, an
attorney who has participated successfully in the organization of
several trade organizations, who pointed out that of 500 national
associations in commercial lines there was none to represent the
dyestuff industry, and that this industry was in need of such or-
ganization on account of the character of German competition
which would have to be met after the war.
On motion of L. A. Ault, of Cincinnati, each one present rose
and stated his business connection. A lively discussion followed
as to whether the association should include both manufacturers
and dealers. The chairman suggested that it might be well to
divide the membership into two classes: active members, the
manufacturers, and associate members, the dealers. The further
suggestion was made that the associate members have no vote.
The opinion of the meeting seemed to be that a physical mixer of
dyestuffs should not be considered as a manufacturer, inasmuch
as he adds nothing to the amount of dyestuffs produced. To
meet this question fairly the dealers retired to another room
in the building, and in their absence the manufacturers decided
that only straight-out American manufacturers should be eligible
for membership, further denning the terms as follows: "an
American citizen whose plant is in America and not controlled
by outside capital." Thereupon each manufacturer stated the
location of his plant. The manufacturers adopted unanimously
the principle of active members with voting power, and associate
members without the ballot privilege. The question of differ-
entiation between the coal-tar and the natural dyestuff manufac-
turer was postponed for later consideration.
D. W. Jayne of The Barrett Company gave an interesting
account of the proposed Chemical Alliance.
Just before adjournment of the morning session Mr. McKerrow
reported that the dealers in their meeting requested that a com-
mittee of the manufacturers be appointed to confer with a com-
mittee of the dealers. This request was acceded to, and the
chairman appointed J. M. Matthews, L. A. Ault and August Merz.
Dr. Matthews reported at the afternoon session that the
joint committee of the manufacturers and dealers recommended
that the association consist of active members — manufacturers
with voting power, and associates — dealers, machinery manu-
facturers, etc., with no vote, but with a representative on the
directorate. Furthermore, that associate members should have
control over the qualifications of associate members, and that if
an arbitration board should be appointed the associate members
should have a representative upon such board. The report was
unanimously adopted.
The chair appointed the following committee on organization:
J. M. Matthews, L. A. Ault. A Mere, \V. S. Woodward, T. N.
Hyndman, H. G. McKerrow. S. R. David.
Dr. Wallace Pierce of the V. S. Conditioning and Testing
Laboratory addressed the meeting on the subject of standardiza-
tion. He considered this matter perfectly practicable, and laid
stress upon the need of accurate sampling. It was pointed out
that on pure compounds coloriuu trie methods are satisfactory,
and the use of the spectroscope and microscope in the work of
standardization was illustrated. Emphasis was put upon the
fact that the standard is a unit and not an ideal
An interesting talk was given by H 11 wood Hendrick on the
early efforts of dye manufacturers in this country, pointing out
the good that might have been accomplished if in those days
a truer spirit of cooperation had prevailed.
The convention was addressed by A. E. Parker on the sub-
ject of patents in relation to the dyestuff industry, and by Brad-
ford Webster on "Arbitration."
On Wednesday morning the convention heard the address of
Grinnell Jones of the U. S. Tariff Commission, which follows:
THE TABIFF COMMISSION AND THE DYE INDUSTRY
By Grihkbu. Jonbs
It is not necessary before this audience to discuss the his-
tory of the tariff law of September 8, 1916, which raised the
duties on dyes and other coal-tar products. I shall merely re-
mind you that the legislation creating the United States Tariff
Commission forms a part of this same bill. This law charges
the Commission with the duty of gathering the facts needed
for the consideration of questions of tariff policy and requires
that all information at its command shall be put at the disposal
of the President and Congress, whenever requested. The Com-
mission recognizes that the dyestuff industry' presents one of the
most important and complex problems which it will have to
consider and is planning to make a report to Congress on this
industry.
Last August the Commission sent a questionnaire to many
of the leading textile mills asking for a statement in regard to
the effect of the dyestuff shortage of 1915 on their business and
the extent to which their needs have been met by the growth
of the American dyestuff industry. These consumers were
also asked to give certain statistical information bearing on the
question and to state their opinion in regard to the wisest
policy for the country to adopt on the question of the tariff on
dyes. Returns have been received from 77 textile manufac-
turers and a summarized statement of the replies will be pub-
lished very' soon. The Commission is now seeking information
from the manufacturers of dyes, intermediates, and other coal-
tar products.
The Underwood tariff law levied an import duty of 30 per
cent ad valorem on dyes, except indigo, alizarin, and dyes de-
rived from anthracene and carbazol, which were on the free list.
The act of September 8, 1916, placed an additional duty of 5
cents per pound on the dyes formerly dutiable at 30 per cent ad
valorem and imposed a duty of 30 per cent upon the dyes for-
merly on the free list. By the same act coal-tar crudes were
put on the free list and intermediates were made dutiable at
15 per cent plus 21 . cents per pound. These specific duties
of 5 cents in the case of dyes and certain other finished products,
and 2'/» cents in the case of intermediates, were called special
duties. The law further provides that these special duties shall
remain in force only 5 years, and that they shall thereafter be
gradually reduced by one-fifth annually. The law, however,
contains another provision, which reads as follows:
' • » • • But if_ at the expiration of live years from the
date of passage of this Act, the President finds that there is not
being manufactured or produced within the United States as
much as sixty per centum in value of the domestic consumption
of the articles mentioned in Groups II and III (intermediates
and finished products) of section five hundred, he shall by procla-
mation so declare, whereupon the special duties imposed by this
section on such articles shall no longer be assessed, levied, or
collected."
The President of the United States has requested the Tariff
Commission to ascertain the facts on which executive action
under this clause must be based. It has seemed wise not to
wait for the expiration of the five-year period before beginning
a systematic study of the development and progress of this in-
dustry in the United States.
The schedule which has recently been sent to all manufac-
turers known to us is designed to ascertain the facts needed for
Mar., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
233
the application of the 60 per cent clause, as well as to secure
certain other information which will be helpful to the Commis-
sion and Congress in determining the wisest future policy. The
Commission is taking a census of the coal-tar products for the
year 19 17, asking for the quantity and value of the production
of each intermediate, dye, or other finished product.
It is, of course, well known in a general way to those familiar
with the dye industry that the development of indigo, alizarin,
and the vat dyes derived from anthraquinone and carbazol
has not kept pace with the development of the azo dyes. Since
these branches of the industry are the very ones which under the
present law do not get the benefit of the special duty of 5 cents,
it is of great importance that the Commission have for the con-
sideration of Congress definite statistical information in regard
to the development of the different branches of the industry.
For this and other reasons we are asking for detailed information
in regard to the production of each separate dye, not simply
for grand totals. We hope to publish the totals in as great de-
tail as can be done without revealing the operations of individual
concerns. For example, in the cases of aniline and Bismarck
Brown there will be so many producers that the total produc-
tion for the country can be published without revealing the
operations of any individual concern. It is believed that this
information will be of interest and value not only to Congress
but to the producers themselves. In many other cases the
publication of the total would reveal the operations of individual
concerns. In all such cases the dye or intermediate in question
will be grouped with others of a similar character so as to cover
effectually the details. In the case of dyes sold under a trade
name, whose chemical nature is kept as a trade secret, we are
asking that you give us confidentially sufficient information in
broad, general terms, to enable us to classify properly each such
dye. It is especially important that we be able to distinguish
clearly between dyes dutiable at 30 per cent plus 5 cents per
pound and those dutiable at 30 per cent only.
You will notice that under the present law it is necessary to
ascertain both production and consumption of dyes in the United
States. It would be impossible to secure complete returns from
consumers themselves. It therefore becomes necessary to re-
gard the consumption in the United States as equivalent to the
sales of American manufacturers plus imports minus exports.
Although the law requires a comparison of the value of the domes-
tic consumption and production, we are asking for the quantity
as a check on the values and also because the quantity is for
many purposes a better indication of the growth of the industry
than the value.
One of the difficulties which we foresee is the lack of a gen-
erally accepted standard of quality and strength of dyes. If,
as a result of the deliberations of this association, a generally
recognized standard is adopted, the future work of the Com-
mission will be greatly facilitated.
We recognize that it will not be easy to bring together the
information called for on the schedule, but rely with confidence
on the cooperation of the industry toward enabling the Com-
mission and Congress to deal intelligently with an important
public question. Although we have sought and secured the
helpful cooperation of a number of representative manufac-
turers, both large and small, in the preparation of this schedule,
we realize that it is capable of improvement. We ask you to
do the best you can to supply the information in the form called
for this year. We shall welcome constructive criticism which
will help us to prepare a better schedule for later use. In
making suggestions a clear distinction should be drawn between
changes which can be made under the present law and changes
which would require an amendment to the law.
The work which the Commission is doing on the special law
of September 8, 1916, is not confined to the questionnaire just
described. We are also considering very carefully the possi-
bility of improving the law by amendments.
For example, the new act does not repeal all of the provisions
of the old law which are in conflict with the intent of the new
law. The list of intermediates mentioned by name is capable
of much improvement. Such important intermediates as Mich-
ler's ketone and dinitrophenol are not mentioned, whereas the
relatively much less important nitrotoluylenediamine and mono-
chlorphthalic acid are included. Very little attention appears
to have been paid to intermediates for medicinals or photographic
chemicals or flavors. Many suggestions have been made to
the Commission in regard to changes in the wording of the law.
We have prepared a list of such of these suggestions as seem
worthy of serious consideration. We shall send a copy of this
list to anyone who cares to offer evidence or opinion in regard to
the advisability of the proposed changes and we shall welcome
any additional suggestions.
The Commission will be glad to arrange for a conference
with representatives of the dye industry in the near future.
If such a conference appears to be desirable, the Commission
will be glad to confer with the officers of this Association, or
with any special committee appointed for the purpose of mak-
ing all necessary plans and arrangements.
An interesting discussion of various phases of the tariff question
followed, and it was agreed that all manufacturers would endeavor
to supply the Commission as promptly as possible with the data
requested for the preparation of its report to Congress.
The committee on organization reported, recommending that
it be continued with power until the first annual meeting, in
order that the details of membership, incorporation, committees,
etc., might be carefully considered. The powers asked by the
committee were as follows:
I — To prepare and file a certificate of incorporation.
II — To prepare by-laws for submission at the annual meeting.
Ill — To arrange the time and place of the annual meeting.
IV — To entertain and pass upon application for membership.
V — To confer with the Tariff Commission and report at the annual
meeting.
The recommendations of the committee were all adopted, and
the convention adjourned to meet on March 6, 10 a.m., at
the Chemists' Club.
AMERICAN DRUG MANUFACTURERS ASSOCIATION
The seventh annual meeting of the American Drug Manu-
facturers Association was held at the Waldorf-Astoria, New
York City, January 29-30, 191 8. The meeting was well at-
tended and was thoroughly representative of the American
industries engaged in the manufacture of drugs, medicinal
chemicals, biological products, plasters, and surgical dressings.
The membership of the Association embraces practically all
of the producers of the above supplies of the entire country.
These producers have been confronted with many problems,
such as embargoes upon their crude materials and upon then-
shipments of finished products, as well as a shortage of coal
resulting in many cases in the closing of factories. In common
with other industries, they have stood up as best they could
under these circumstances, while at the same time yielding then-
skilled help, chemists and others, to the ranks of the Army and
Navy. How best to meet such conditions and at the same
time produce better products in far greater quantities are ques-
tions which have been earnestly discussed among the members.
■ The Association feels that in view of the nature of the products
produced embargoes should not apply to its industry and that
priority order should be granted to them. It has been difficult
in the past to bring this about and the Association has felt that
the nature of its products was understood neither by the public
at large nor by the transportation officials. One of the im-
portant steps suggested at the meeting, therefore, was a move-
234
III). .l"i RNAL Of INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 3
inent in the direction of publicity. By this is meant proper
publicity. The members of this Association produce what
may be called the legitimate drugs and medicines actually used
1 ibi '1 by physicians and surgeons in their daily practice.
Xhej 'I" not manufacture what are commonly known as
"patent" medicines. Proper publicity would therefore naturally
be of an educational nature, tending to inform the public and the
officials as to the products produced and the method of using them.
The Association has established a committee known as the
Committee on Standards and Deterioration, and made up of
from its membership. It is their object to study the
standards that are now in use, hoping to improve them, and to
study the deteriorations that occur, hoping to prevent them.
This Committee may be expected to produce results, since it is
made up of practical men and provided with ample funi
quite unusual features for a committee of scientists.
The Association has a very active legislative committee and
its work is of importance to the members, keeping them advised
of the many laws that are being enacted, proclamations issued,
regulations promulgated, new taxes imposed, etc. This com-
mit t< -e is one of the strongest features of the entire Association,
and its importance should not be overlooked.
The Association passed a resolution urgently requesting the
Committee of Revision of the U. S. Pharmacopoeia to establish
alternative standards for some drugs which, owing to the war,
cannot be obtained of present V S. P. quality.
The Association passed a resolution reaffirming its opposition
to any patent legislation dkcriminating against medical, chemical
or pharmaceut ii al di 1 overies.
Inasmuch as drug manufacturers of the country are making a
united effort to cooperate with the Government in every
thought best to maintain the Association at its
highest point of efficiency, and therefore all officers were re-
elected.
CHLMI5T5 IN WAR SLRVICL
GOVERNMENT RECOGNIZES THE IMPORTANCE OF
CHEMISTRY IN THE WAR
Adequate chemical control of manufacturing plants engaged
in the supply of war material is now receiving the careful con-
sideration of the War Department. The experience of both
Great Britain and France teaches the necessity of conserving
the supply of trained chemists, at no time large, in order that
the supplies upon which the winning of the war so largely de-
pends may not be curtailed.
Provision has now been made through an order of the Adju-
tant General of the Army by which manufacturers of material
necessary to the prosecution of the war, who have lost the ser-
vices of chemists through the first draft, may again obtain the
services of these men for war work.
It is announced, also, that provision has been made by which
manufacturers threatened with the loss of their trained chemists
in the present draft may retain these men. Only those chem-
ists whose services are necessary to war work will be considered
and the evidence submitted by the manufacturer must be con-
clusive.
Manufacturers thus affected should apply to the Chemical
Service Section, N. A., New Interior Building, Washington,
D. C, for the regulations governing the transfer of men already
drafted, or the possible reclassification of men not yet called.
This request must come from the manufacturers; applications
from the men will not be considered.
The following communication with accompanying question-
naires will make clear to the manufacturers the procedure to
be observed in requesting transfer of men already drafted or re-
classification of men not yet called:
1 <i Pica of the Chief of the Chemical SERVICE Section
1 108 New Interior Bun 1
Washington, D. C.
By an order of the Secretary of War the Adjutant General
of the Army has authorized the Chief of the Chemical Service
Section of the National Army to initiate such measures as are
try to secure deferred classification for chemists whost
ire essential to war industries. Under the Selective
1 1 illations such action is limited to a letter of advice
to the Local and District Exemption Hoards transmitted through
the \. inn. nil General's oilier, substantially as follows
"Tin' Chemical Service Section of the War Department has invest!
latus of your company in connection with the production of war
material and considers it important that the efficiency of your organisation
be maintained, fn this connection the services of
at a technical expert in have been invest!
it is believed that his continued employment in war industries would be
to the best interests of the Government. You are therefore advised to
apply to the local exemption board for deferred classification in his case
on the ground that he is a necessary highly specialised technical expert of a
necessary industrial enterprise. Such action, of course, should be taken
only with Mr 's consent. If he prefers to enter the
military service, please advise this otlice of that fact in order that his
services may lie utilized where most needed."
Under the same order of the Secretary of War the Chief of
the Chemical Service Section will initiate action for the return
to civil industries of any expert chemist whose service in the
industry from which he was taken is of more importance to the
Government than are his services in a military capacity. Ex-
cept in the cases of members of the Reserve Corps, the action
taken will consist of a recommendation to the Adjutant General
of the Army that the man concerned be discharged from the
National Army. National Guard or Regular Army, as the case
may be, re-enlisted or re-commissioned in the proper branch
of the Reserve Corps and placed upon the inactive list. In the
cases of members of the Reserve Corps, the action will consist
of a recommendation that the man concerned be placed upon
the inactive list.
In order that this office may act intelligently, you are asked
to fill out the questionnaire herewith enclosed.
Chemical Service Section, N. A.
Name of Ma
Address
(Please u
ufacturer.
FORM B
: typewriter in filling i
Full name of Chemist (Age)
Address
A: (To be filled in by manufacturer, not the chemist)
Information regarding chemist.
1 . Is he willing to receive deferred classification
Ho
2. Serial No Liability No
Questionnaire Classification Class Paragraph Date.
Title and address of l.oeal Board
Has appeal for reclassification been mad.
Result
Length ol lime chemist has been wrllr your Company. . . .
Proportion of total hours of the services of the chemist
production* of war materials
Education (above grade of high school'1
Experience
Compauy
Duration of employment
Mar., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
7. Nature of materials in the production* of which said chemist is engaged:
8. Relation of above materials to the war:
9. Statement of the importance of the chemist to the above war work
by the officer in charge of the department:
Note — This is to be addressed to Chief of Chemical Service Section.
N. A., New Department of Interior Building, Washington, D. C.
FORM C
(Please use typewriter in filling in this blank)
Name of Manufacturer
Address
Full name of Soldier (Age)
Camp address
A: (To be filled in by manufacturer, not by soldier)
Information regarding soldier:
1. Is the soldier in the Regular Army, National Army or Reserve Corps?
2. If the soldier is in the Regular Army or National Army does he desire
a discharge with re-enlistment in the Reserve Corps (inactive list)
in order to re-enter your employ?
3. If the soldier is in the Reserve Corps does he desire to be placed upon
the inactive list in order to re-enter your employ?
4. Length of time soldier was with your company
5. Proportion of total hours of the services of the soldier would be spent
on production* of war materials
6. Education (above grade of high school)
Experience:
Company
Duration of employment
Nature of materials in the production* of which said soldier will be
engaged :
9. Relation of above materials to the '
10. Statement of the importance of the soldier to the above war work by
the officer in charge of the department:
Note — This is to be addressed to Chief of Chemical Service Section,
N. A., New Department of Interior Building, Washington. D. C.
American Chemical Society
Washington, D. C.
So many hundreds of letters are being received from firms and
individuals that it is necessary to print the following, which
covers most inquiries.
DEFERRED CLASSIFICATION
Individuals can obtain deferred classification only through
the Local Boards or by appeal to the District Boards.
Manufacturers engaged in the production of materials neces-
sary for the war may apply by letter to the Chemical Service
Section, National Army, Room 1108, Interior Building, Wash-
ington, D. C, for the return to them of necessary trained chemists
now in the army and not already transferred to Chemical Service.
They may also apply through the Chemical Service Section for
deferred classification of trained chemists necessary to the con-
trol of their operations who are not yet called. Applications
from the men themselves will not be considered. Only those
1 hi mi ts whose services are necessary to war work will be con-
sidered. The evidence submitted by the manufacturers must
i»- conclusive.
STUDENTS IN CHEMICAL COURSES
Students taking a regular chemical course may lie enlisted
in the Engineers Reserve Corps and placed on the inactive list
• Under production is to be included research, development and con-
trol work necessary to manufacturing operation.
in order to complete their college course. The dean or president
of the institution must certify, however, that their standing is
such as to warrant the conclusion that they will graduate with
a record equal to the first third of the graduates of the previous
ten years. This does not apply to students in biological and
physiological chemistry as the Chief of Engineers has ruled that
such come under the Surgeon General's Office, rather than under
the Engineering Department. Students wishing to take ad-
■ vantage of this opportunity to receive their degrees before en-
tering the country's service, should address the Chief of Engi-
neers, War Department, Washington, D. C, asking for the
necessary blanks to be filled out for this purpose.
TRANSFERS TO CHEMICAL SERVICE
Transfers to Chemical Service are made by the War Depart-
ment on request from some division of the army for the particular
chemist needed. After the approval of the commanding officer
and the Chemical Service Section, the man is transferred.
Remember that the Secretary has no power to transfer you la chemical
service. He simply brings your name and qualifications before
those who have.
No one can predict how great this requirement for chemists
will be. At present, although nearly a thousand chemists are
serving in a chemical capacity, some 300 men, properly classified
as chemists, remain in the camps. Accordingly, if you enlist
as a chemist before you are called, you will deprive another
chemist actually in the army of his opportunity to render chemical
service. The industries which supply the army and navy with
the sinews of war need chemists and are being seriously handi-
capped by the depletion of their chemical personnel. Cards
giving age, training, experience, etc. (obtained from question-
naires tiled with the Bureau of Mines) , of all men with chemical
training known to be in the army, are kept in the office of the
Society. These cards are constantly consulted by those in com-
mand needing chemical assistance. Men are chosen not to give
the individual an opportunity to serve in a chemical capacity,
but to find the man especially qualified for the work in hand.
Accordingly, you may or may not be selected. Men with plant
experience, research, physical and organic chemists, some anal-
ytical chemists, etc., have been in demand. On the other hand,
there has been almost no chance to place pharmaceutical chem-
ists, agricultural or food chemists, as the army apparently has
little need for this form of chemical service and the Government
itself is not manufacturing in these lines.
GOVERNMENT POSITIONS OTHER THAN IN THE ARMY OR NAVY
Chemical positions in the Government service other than those
by enlistment in the army and navy are obtainable only through
the Civil Service Commission. They do not necessarily exempt
the encumbent from military service.
COMMISSIONS
Commissions seek the man. A number of chemists have been
commissioned, but in almost every instance it has been by pro-
motion from the ranks for recognized ability, or the particular
man has been sought to fill a special place of responsibility or
trust for which he was known to be especially fitted. The place
was not made for the man, but the man was found for the place,
sometimes after long search. A commission carries authority
with it and is not lightly awarded whether in the engineering,
medical or chemical branches of the service.
IMPORTANT TO ALL CHEMISTS OF DRAFT AGE
Information regarding individuals is obtained from the ques-
tionnaire on file iii tin- Bureau of Mines, Washington, I' C,
If you have not Tilled out our of these questionnaires, write to
.11 of Mines, asking that "in- lie sent you for this purpose.
236
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, Xo. 3
When once in the army keep me informed by post-card of
your military address and any change in that address, even
should you be sent to France. Although you may not be chosen
early among those needed for' chemical service, the demand for
chemists is constantly increasing, and your country may call
you at any time where you are best trained to serve.
It is my duty to help place you where you can serve our country
best as the need arises. It is your duty to keep me informed of
your address and to accept any service to which the War De-
partment may assign you, even though you may prefer to fight
in the ranks in France.
February 15. 1918 Charles L. Parsons, Secretary
NOTL5 AND CORRL5PONDLNCL
SPRING MEETING OF THE AMERICAN CHEMICAL
SOCIETY
After consultation with the Advisory Committee and other
members of the American Chemical Society, the Directors have
voted to omit the Spring Meeting of the Society, which was to
have been held in St. Louis this coming April. It is felt that
the transportation conditions are such that unnecessary travel
should be avoided, and also that the chemists of the country
are so busily engaged in meeting war needs that their work should
not be interrupted for the purpose of conference at this time.
The Annual Meeting of the Society will be held in Cleveland,
Ohio, in September.
Washington, D. C. Charles L. Parsons, Secretary
January 29, 1918
WAR RISK INSURANCE FOR CHEMISTS IN MILITARY
SERVICE
All chemists in the military service are urged to take out
war risk insurance, even if they are assigned to chemical ser-
vice or are later released from the army for service in the war
industries. This is a form of insurance arranged by the War
Department at a very nominal rate, which gives adequate pro-
tection against death or injury.
RAMSAY MEMORIAL FUND
After the death of Sir William Ramsay in July 1 9 1 6, a memorial
meeting was held in London to commemorate his thirty-five
years of service in physical and chemical sciences, education,
and public welfare. The gathering of distinguished men, under
the chairmanship of Lord Rayleigh, decided
1 — To raise a substantial fund as a memorial to Sir William; and
2 — To use such fund for the establishment of
(a) Ramsay Research Fellowships, tenable wherever necessary facilities
might be available, and
(6) Ramsay Memorial Laboratory of Engineering Chemistry at the
University of London, where Sir William served twenty-six
of his most fruitful years of activity.
A committee of prominent men in the physical and chemical
sciences in Great Britain, including the leaders of the Coalition
Government and Ambassadors then accredited to the Court
of St. James, was later organized. Through this general or-
ganization, committees were organized in Australia, Canada,
Chile, Denmark, Holland, India, Italy, Japan, New Zealand,
Spain, Switzerland, and the United States. Correspondence
with nun of science indicates the formation of national com-
mittees also in China, France, and Sweden, and perhaps
Russia.
The sum set out to be raised was £100,000. To date some-
thing over £300 have already been contributed by residents of
the United States.
The merits of the objects of this fund arc obvious. The
recognition of a man who made so many valuable contributions
to our knowledge and who won so many Friends through his
wonderful friendly sympathy and erudition appeals especially
to American men and women,
The Committee expects some generous contributions and will
welcome the receipt of other large gifts, but it hopes especially
to have a great number of small subscribers. The receipt of
checks, postal orders, or cash, for one dollar or over, sent to the
Ramsay Memorial Fund Association, 50 Hast 41st St., New York
City, will be promptly acknowledged.
UNITED STATES COMMITTEE FOR THE RAMSAV MEMORIAL FUND
Walter Hines Page,
Vice President
Charles Baskerville,
Cha
Wm. J. Matheson,
Treasurer
Leo H. Baekeland
Wilder D. Bancroft
Marston T. Bogert
Chas. F. Chandler
Francis W. Clarke
Wm. D. Coolidge
John H. Finley
Edward C. Franklin
Frank Hemingway
Chas. H. Herty
Charles James
George F. Kunz
F. Austin Lidbury
Arthur D. Little
C. E. K. Mees
R. A. Millikan
Richard B. Moore
Wm. H. Nichols
William A. Noyes
Henry F. Osborne
Charles L. Parsons
Ira Remsen
Theodore W. Richards
Edgar F. Smitn
E. G. Spilsbury
Julius Stieglitz
Milton C. Whitaker
Editor of the Journal of Industrial and Engineering Chemistry:
I am deeply interested in the appeal made by the Committee
on the Ramsay Memorial which is to appear in this issue of your
journal. Knowing Sir William as well as I did, I cannot imagine
a more graceful compliment than that every member of the
chemical fraternity should have some part in this work. It
would afford me great pleasure if every member of the American
Chemical SocrETY should promptly remit something to the fund,
realizing that the matter of taking part in it is of more conse-
quence than the amount of the subscription.
New York City WILLIAM H. NICHOLS
February 15, 1918 President, American Chemical Society
CHEMICAL RESEARCH IN THE VARIOUS COUNTRIES
BEFORE THE WAR AND IN 1917
Dr. Bernhard C. Hesse recently suggested to me that he and
probably others would be interested in information regarding
the effect of the war on the relative chemical activities of the
various nations. I am able to supply information on this sub-
ject only in so far as this activity is reflected in the publication
of papers and is measured by the number of abstracts published
in Chemical Abstracts. In peace times such figures would be a
fair gauge of chemical research throughout the world; at the
present time they are, of course, affected by the fact that much
chemical work in the warring nations is kept secret and also
by the fact that Chemical Abstracts is having great difficulty in
getting abstracts of the papers published in Germany and Austria.
Nevertheless the figures in the accompanying table are not with-
out considerable meaning. With tin exception of the Japanese,
German and Austrian literature the field of chemistry was covered
thoroughly by Chemical Abstracts both in 19 13 and in 1917;
the Japanese journals were only partly abstracted in 1913 and
the German and Austrian literature was covered with only a
fair degree of thoroughness in 1017. Inability to get the German
and Austrian journals is the reason for the incompleteness in
191 7. I believe that the figures in the table give a fair representa-
tion to Germany and Austria, however, because the 191 7 volume
of Chemical Abstracts contains in addition to abstracts of most of
the current papers (obtained from British, Dutch, Spanish and
lUrnals with abstract sections), a considerable number of
abstracts of papers published in 191 6, due to the fact that a
Mar., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
large shipment of 1916 German and Austrian journals was re-
ceived early in 1917.
The table speaks for itself.1
Number of Number of Per cent Per cent
Abstracts Abstracts of Total of Total
Countries in 1913 in 1917 in 1913 in 1917
United States 3940 4602 21.1 43.9
Great Britain 2741 1560 14.7 14.9
France 2481 794 13.3 7.6
Germany 6539 2065 34.9 19.7
Austria 539 112 2.9 1.1
Italy 905 305 4.9 2.9
Russia 474 264 2.5 2.5
HoUand 328 276 1.8 2.6
Norway 15 19 0.08 0.18
Switzerland 226 114 1.21 1.08
Belgium 185 7 0.99 0.06
Sweden 110 64 .0.58 0.62
Japan 71 166 0.38 1.58
Spain 34 26 0.18 0.24
Denmark 41 20 0.21 0.19
Other countries 52 89 0.27 0.84(a)
Total 18,681 10,483
(a) The increase here is due chiefly to the fact that Chemical Abstracts
is now covering certain South American journals not abstracted in 1913.
Three points of special interest are : ( i ) The United States and
Germany have exchanged places, Germany having been first
by a big lead in 19 13 and the United States second, and vice
versa in 191 7; it is to be noted that the lead of the United
States in 1917 was greater than the lead of Germany in 19 13.
(2) Great Britain has maintained her relative position with
almost no variation. (3) The number of papers published in
the neutral European countries has fallen off considerably.
It will be interesting to see to what extent the various countries
will return to their ante bellum positions when the war is over.
The effect which the entrance of our country into the war will
have on publication here will also be of interest. No marked
change was to be noted in 1917; in 1918 I look for further ex-
pansion of industrial journals and for contraction of journals
devoted to pure science.
Columbds, Ohio E. J. CRANE
January 31, 1918
LICENSES REQUIRED FOR EXPLOSIVES AND THEIR
INGREDIENTS
Editor of the Journal of Industrial and Engineering Chemistry:
An Act of Congress (Public Document No. 68, Sixty-fifth Con-
gress) to prohibit the manufacture, distribution, storage, use and
possession in time of war of explosives, and the ingredients
thereof, provides that a license from the Bureau of Mines is
necessary for every person, firm and corporation, to purchase,
possess, sell or use any explosive or the ingredients thereof.
Any violation of this Act is punishable by a fine of not more
than $5000, or by imprisonment of not more than one year, or
both fine and imprisonment.
Selling to a person who has not a license is punishable by a
fine of $1000.
The Bureau of Mines has published the following list of
articles requiring licenses under this Act.
As the readers of your journal are undoubtedly interested
in this subject, I am taking the liberty of calling it to your atten-
tion for such publicity as you are able to give it.
In most places the county clerk has been designated as the
licensing agent. In Greater New York licenses may be obtained
from John R. Healy, Room 1100, Municipal Building, Manhat-
tan, or John F. Dixon, 365 Jay Street, Brooklyn. Application
must be made in person. Duly authorized officers of corpora-
tions or companies must make application for the company or
corporation.
The following commodities are those for which licenses are
required :
1 Abstracts of papers that could not be certainly associated with a
particular country, as, for example, some of the Communications of the
Eiihlh International Congress vf Applied Chemistry, were not counted.
EXPLOSIVES
Ammonium nitrate
Blasting powder
Caps — blasting, detonating, percussion — all classes
Detonating fuse, or cordeau detonant
Detonators
Dynamites
Electric blasting caps and electric detonators
Fireworks and flashlight powders
Fulminates
Fuse of all varieties
Guncotton
Gunpowder and gunpowder mixtures (except small arm or shot gun cart-
ridges)
Nitrocellulose and nitroglucose
Nitroglycerine (except in official U. S. Pharmacopoeia solution or in form
of pills or granules containing not more than >/«• grain each)
Nitro-glycol, -mannite, -starch, and -sugar
Permissible explosives
Ammonium picrate
Picrates
Picric acid
Smokeless powder (except small arms and shot gun cartridges)
Trinitrotoluol
Trinitrocresol
Trinitronaphthaline
Tetranitroaniline
Tetranitromethylaniline
INGREDIENTS
(List approved January 5, 1918)
The purchase, possession, sale or use of any one of the in-
gredients herewith listed below in amounts of one ounce or over
requires a Federal Explosives License.
Bichromates — ammonium, potassium, sodium
Chlorates — barium, potassium, sodium, strontium
Chromates — ammonium, barium, calcium, chrome green, chrome yellow,
lead, potassium, sodium
Nitrates — ammonium, barium, copper, ferric, lead, magnesium, nickel,
potassium, silver, strontium
Nitric acid — -aqua fortis, fuming, nitric acids of all grades and strengths,
mixed acids
Perchlorates — perchloric acid, potassium
Perborates — magnesium, sodium, zinc
Permanganates — calcium, potassium, sodium
Peroxides — barium, calcium, magnesium, oxon (cubes and cartridges),
sodium, strontium, zinc
Phosphorus
New York City
January 15, 1918
J. R. Healy
Federal Licensing Agent
THE INDEXES TO CHEMICAL ABSTRACTS
The comparative lateness of the appearance of the 1917 Index
to Chemical Abstracts is such a keen disappointment to
the Editor that he would like the privilege of stating to the
members of the American Chemical Society that this is not
due to a change of policy. The subject index is considered
to be the most important part of the journal and more
work is being put on it than ever before, but the work is
still planned so that normally the index will appear at
least as soon as the early part of January. In the
case of the 1917 index a combination of unfortunate cir-
cumstances, among which are the fuel famine (it struck us in
December during the most crucial week) and the traffic conges-
tion (one package of copy was over two weeks in traveling be-
tween the printer's office and ours), caused most of the delay.
Getting the annual index into the hands of the members by
the first of the year, as has been done during the past few years,
is a very strenuous task, but one in which we have come to take
special pride.
A word regarding the Decennial Index is due the members
also. Inquiries which are received show that many are anxious
for the completion of this index. The task, with all the pre-
cautions that are necessary for accuracy, completeness, consis-
tency, and convenience in use, has proved to be a much more
time-consuming one than was ever anticipated. We just want
to say that the work is being pushed as rapidly as circumstances
involved in the nature of indexing, especially subject indexing,
our regular work of issuing the journal and the annual indexes,
and the policy of not sacrificing quality for speed will permit.
One of the things in a subject index most important to be avoided
is the scattering of like entries; the proper codrdination can be
accomplished only in case a limited number of experienced
workers handle parts of the task. As a matter of fact, it proved
to be desirable for the associate editor and editor, working to-
gether, to examine every one of the hundreds of thousands of
238
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 3
entries (the organic names excepted) with the abstract
them and all are being gone over again for such revisions as can
be made, only after all the entries have been assembled under
the various subject headings. It takes many weeks just to
handle the cards. \Vc have indexed subjects, not merely words,
and abstracts, not merely titles: the difference is very great.
The second volume of authors, which has been in course of
printing since last September, will appear soon. As an example
of a source of delay in the case of this part of the index, atten-
tion is called to the fact that many times it has been necessary
to write letters to authors or to abstractors to whom the original
papers are available in order to straighten out discrepancies
in the spelling of authors names.
Columbus, Ohio E. J. CRANE
January 31, 1918
THE UTILIZATION OF NITER CAKE
Under ordinary conditions the disposal of niter cake is a
troublesome problem. The best practice has been to add small
amounts to the charge of salt and sulfuric acid for making muri-
atic acid.
Sometimes this addition is in solid form and sometimes the
niter cake is stored in a cast-iron tank as it is discharged from the
nitric acid retorts and is run into the muriatic pots as wanted.
Before 19 14, so far as I can learn, niter cake alone was very
seldom used for muriatic acid manufacture. Since that time it
has often been impossible to secure a sufficient supply of sulfuric
acid and considerable amounts have been and are being made in
this way. On the whole, notwithstanding the fact that heat
economy is secured by the use of the material direct from the
retorts, I am inclined to think the use of cold niter cake the best
practice. I have made several thousand tons from this material
in this way without serious difficulty.
A patent owned by the General Chemical Company provides
for grinding and mixing the materials, but this is quite unneces-
sary, expensive and, in damp weather, troublesome.
Muriatic acid made from niter cake always contains more
sulfuric acid and unless carefully watched, this may run up to 1
or even 2 per cent. If the workmen about nitric acid plants
were careful, the cake need not contain more than 27 per cent
free acid, but they are not, and large experience has shown that
about 32 per cent is better practice. For the same reason, cake
should be free from nitric acid and iodine, but practically all
muriatic acid made from cake contains both. While most niter
cake is free from all but a trace of these undesirables, every little
while a clock watcher will dump his fire before iodine shows in
the condensing tubes and the resulting cake will be bad. For
these reasons I am convinced that where practicable it is desirable
to keep the muriatic made from niter cake entirely separate from
that made from salt and sulfuric.
This method of working up niter cake is insufficient to take care
of the product even in time of peace. In war time what to do
with niter cake becomes a serious problem. Near the coast it is
dumped in the rivers without any unnecessary display. I be-
lieve that not less than 50,000 tons monthly are now thus disposed
of near New York. In inland location-, the fish wardens arc apt
to get wise and raise a row.
The du Fonts have succeeded in finding a large number of
new uses for niter cake and have organized an agency for disposing
of il which has been 1 ery successful, notwithstanding which they
could probably find a supply for new customers,
It is thus evident that the time is ripe for a process for
organizing the disposal of this material in a separate department
of the plant where it may lie resolved into salt cake or Glauber's
salt and free acid and utilized.
it may be objected that salt cake is not a readily marketable
product and to some extent this may lie true, but the market for
this product lias greatly enlarged during the last decade and is
steadily improving
My proposal (Application No. 170,607 for U. S. Patent,
granted but not yet issued; is to dissolve the cake in water to a
solution having a specific gravity of 1.35 and to blow cold air
through the solution in proper receptacles well insulated to pre-
vent inflow of heat. The sodium sulfate separates as Glauber's
salt in small crystals which are dumped into a centrifugal and
washed with a Glauber's salt solution. A very pure salt cake
containing less than one-fourth of one per cent free acid may be
readily obtained, and a mother liquor containing only a small
amount of sodium bisulfate with much free sulfuric acid. This
is evaporated, either in a glass apparatus, which I have recently
invented, or in Duriron puns, and the resulting mixture used in
place of a part of the sulfuric acid in nitric acid making.
For this work ordinary ice apparatus will be found unsuit-
able. Too much time is required to withdraw the heat, and the
crystals arc large and enclose mother liquor. I find that although
the use of cold air is theoretically less efficient, it is better suited
to this purpose. The agitating action is also essential in securing
a rapid separation since this solution, like water and all watery
solutions, is a poor conductor of heat.
This method of separating crystals is in principle somewhat
like the granulation of sugar, and in the massecuite produced the
size of crystal may be regulated as in sugar-making. It is clear
that this method may often be applied with advantage to other
salts. There seems to be no reason why the majority of these
salts may not just as well be prepared of regulated crystal size
and with great improvement in purity.
Lafayette College Edward HaRT
Easton, Pa.
January 9, 1918
READJUSTMENTS AT THE MASSACHUSETTS INSTITUTE
OF TECHNOLOGY TO MEET WAR CONDITIONS
Within two months after the declaration of war by the United
States, the Massachusetts Institute of Technology had arranged
to allow- its advanced classes to anticipate the work of the fol-
lowing year by taking special courses during the summer. A
considerable number of juniors availed themselves of this op-
portunity and in consequence will be graduated early. The
chemists, of whom there is a great need in war work, will be
graduated in April Seniors in other courses who were in good
standing when they left to enter the service have been given their
degrees.
The present junior class, through a readjustment of its pro-
gram of studies, will drop out practically a term of senior work,
will study throughout the summer, and. if they enter the service,
will receive their degrees in October. Thus they will be ready
for service eight months earlier than they would be normally.
Then, too, the Institute is to admit on February 4th, at the
beginning of the second term, a special class of freshmen who
will be admitted without entrance examinations, the certificate
of the master of the preparatory school that they are mature
enough for the work of the Institute being considered sufficient.
The response which is being made to this offer of the Institute
fully justifies this setting aside of tradition as to time and con-
ditions of entrance. It is expected that this new class will be
composed of unusually line students eager to begin their higher
education without delay, in order to be ready as soon as possible
to do their part in me I ring demand for technically
trained men
DIRECTIONS FOR ASSISTANT EDITORS AND
ABSTRACTORS
The Editor of Chemical Abstracts has recently published a
revised edition of the pamphlet entitled ■■Directions for As-
sistant Editors and Abstractors," which gives in a concise
form rules on the preparation of abstracts, forms, spellings,
nomenclature, etc., which have been adopted in the publica-
tions of the American CHEMICAL S iciBTY, and have come to be
Mar., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
regarded as representing the usage approved by the Society.
The material has been prepared with a great deal of care, and
after consultation with those who are interested in the cause
of good chemical nomenclature in this country. The rules agree
very closely with what is considered the best usage in Great
Britain. Copies of the Directions can be obtained by address-
ing Chemical Abstracts, Ohio State University, Columbus, Ohio.
(G0 — Gi0) (I)
"Per cent pheno. = — (T0 — TJ0 ) —
2-73 0.0003367
or, Per cent phenol = 0.366 (T0 — Tso)
Per cent phenol = 0.585 (T0 — Tso) — 2780 (Ga — G,0) (II)-"
Page 17, right-hand column, 5th line from the bottom should
read: "3 to 4° C," in place of "3 to 400 C."
Page 18, right-hand column, 25th line from the top should
read: "201 ° C. (corr.)" in place of "197 ° C."
G. W. Knight, C. T. Lincoln, el al.
ESTIMATION OF PHENOL IN THE PRESENCE OF THE
THREE CRESOLS— CORRECTION
In the article printed under the above title [This Journal,
10 (1918), 9] the following corrections should be made:
Page 1 1 , right-hand column, 4th line from the bottom should
read: "2.73° C," in place of "2.75 ° C."
Page 12, left-hand column, 6th to 10th lines from the top read:
1. 00
"Per cent phenol = (T0
2-73
1. 00
Tso) — (Go— GTO)
0.0003367
or, Per cent phenol = 0.366 (T0 — Tso) — 297o(G0 — Gso) (I)
in the case of o-cresol + p-cresol + phenol mixtures; and,
Per cent phenol = 0.585 (T0 — T50) — 2780 (G„ — Gso) (II)
in the case of o-cresol + m-cresol -+- phenol mixtures" in place of
ELECTRIC FURNACE SMELTING OF PHOSPHATE
ROCK, ETC.— CORRECTION
The following corrections should be made in the article
printed under the above head in This Journal, 10 (1918), 35.
Page 37, 2nd col., nth line from bottom should read: "7800
tons phosphate rock @ $4.50 per ton. . . .$35,100.00."
Page 37, 2nd col., 7th line from bottom should read: "8
laborers @ $2.00 per day (330 day year). . . .$5,280.00."
Page 37, 2nd col., 3rd line from bottom should read: "Power
@ $25.00 per H. P. Y $100,000.00."
J. M. Carothers
WASHINGTON LLTTLR
By Paul W
Metropolil
Embargoes, idle Mondays and transportation delays have
added materially to the burden of those in Washington who are
trying to be helpful in speeding up the production of chemicals
and in assisting the government to secure its ever-increasing
requirements of the so-called war chemical supplies. There
has been no retardation, however, of the activities of the many
prominent chemists and of those importantly connected with
chemical industries, who are busily engaged in Washington.
Research is being conducted and various projects carried into
effect which, if they could be made public, would give ample
basis for spectacular display in newspapers and doubtless would
surprise the great majority of the country's chemists. For
military reasons, however, the more important things which are
being done by chemists in Washington must not be discussed.
The care that is being taken to maintain secrecy in connection
with some activities is indicated by the fact that the corre-
spondent of This Journal has been requested by a high official
not to mention in this correspondence the names of certain
: prominent chemists who are being called into consultation here
or who have been assigned to war work in Washington.
Following its first annual meeting in New York, February 6,
The Chemical Alliance, Inc.', has been able to get down to re-
sult-getting work, which was not possible to the same degree
[ prior to a definition of all its policies and a systematic outline
of its work.
Chemicals imported during the year just closed were valued
at $144,235,400. This compares with $125,813,205 for the year
1 1916. During December 1917, the value of all imports of
I chemicals was 514,1136,740. This is a decided increase over
December of 1916, when the total value of all chemicals imported
was Sx ,487, 809.
All chemicals exported during 191 7 were valued at Si 93, 255,160.
This is a substantial increase over 1916, when the aggregate
value of all chemicals exported was --1 '15.286,008. Exports of
[dyes and dyestuffs more than doubled. In 191 7 the value was
66,107,361 as compared with £7,953,986 in 1916 and $2,510,650
in 1915. Sulfuric acid exports in 1917 fell slightly below those
of the year preceding. The 1917 exports were 63,542,930 lbs
■ compared with 66,463,501 His. in [916. The total value of all
acid exports in 1917 was 552,695/140 as compared with
■45,015,464 in 1916. The principal increase in the d ll
ted to any single country was to the United Kingdom.
Nt Wilson has appointed, on recommendation oi Secre-
tary of the Treasury McAdoo, the following members of the
Assay Commission Representative Wm. A Ashbrook, Johns-
town, Ohio; Dr. \V. P. Hillebrand, Bureau of Standards, Wash
inton, Dr. Marcus Benjamin, Washington; Will 11. Rounds,
Sioux Palls, South Dakota; Kenneth M Simpson. San Francisco;
iank Building, Washington D. C.
Louis A. Fischer, Washington; Dr. Geo. F. Kunz, New York;
John L. McNeill, Durango, Col.; W. P. Morris, New Hampshire;
L. V. Bassett, Rock Mount, Salem, 111.; Samuel Newhouse,
Salt Lake City; Calvin Page, Portsmouth, N. C; A. C. Weiss,
Duluth; J. H. O'Neil, Boston; L. W. Nieman, Milwaukee;
Martin H. Glynn, Albany; Roy W. Keehn, Chicago; S. B.
Amidon, Wichita, Kan.; Robert P. Oldham, Seattle.
Arrangements have been made by the United States Geo-
logical Survey to secure weekly reports as to output from all
by-product coke manufacturers in the country. From these
reports, the Survey is compiling weekly a statement showing
to what per cent of capacity plants are being operated. The
reports also show the factors limiting production. The last
report shows that the plants of the country were operated at
70.6 per cent of capacity. Failure to secure coal caused a loss
of 23.8 per cent; repairs to plants, a loss of 2.8 per cent; car
shortage and other causes, 2.8 per cent.
Published reports that ample ammonia will be available for
ice making next summer forced from the Food Administration an
admission that the ammonia shortage is acute and that it is
likely to become necessary to commandeer it.
Volunteer chemists are addressing millers and bakers through-
out the country on the technical phases of milling requirements
and how best to utilize wheat substitutes in "Victory" bread and
other war-time doughs. The work is under the direction of the
United States Food Administration.
Cancellation of the car-load rate on hydrofluoric and hydro-
fluosilicic acids from Newell, Pa., to Columbus, Ohio, has been
asked by the Baltimore and Ohio Railroad in an application to
the Interstate Commerce Commission. The same carrier also
has asked permission to increase car-load rates on sulfuric and
muriatic acids from Moundsville, W. Va., to points in Mary-
land, Pennsylvania and West Virginia. Carriers handling
imported nitrate of soda, iron pyrites, chrome and manganese
ores have requested increased rates from the seaboard to various
of the consuming centers
Exceeding in importance any othei circumstance affecting the
fertilizer industry is the inability to secure transportation of
phosphate rock. Shortage has become so acute that several
sulfuric acid plants will lie forced to elose. owing to their inability
to stotr acid which ordinarily is mixed immediately on manu-
facture with the phosphate. Even a more serious side to the
phosphate rock situation is the fact thai fertilizer shipments are
being delayed. Since 5,000,000 tons, out of a total movement
of 7,000,0a ' inns of fertilizer i,mu 1 mow before the end of March
in order' to lie available foi tins year's use th < quences of
;, ,,i tin timeari certain to be fai < ichin After one
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. 3
day's idleness on the part of fertilizer factories, the Fertilizer
Committee of The Chemical Alliance was able to secure their
exemption from the fuel order.
Difficulty is being experienced in the administration of the
federal explosives act, due to a very general lack of knowledge
as to just what the bill provides. Trade in ingredients is giving
the most trouble.
The government has under consideration the erection of an
acetic acid plant. While some sites in the United States are
being considered in this connection, it is regarded as probable
that arrangement will be made to secure the erection of a large
addition to an existing plant in Canada. Shreveport, La.,
has been considered as a possible site for the plant. An un-
limited amount of natural gas is available near that Louisiana
city. If an entirely new plant is erected, it is estimated that its
cost will be $6,000,000.
Garabed T. K. Giragossian is greatly in fear that infringers
upon his plan to produce energy without expense are going to
rob him of the fruits of his work. Mr. Giragossian wrote a
lengthy letter to the Speaker of the House of Representatives
preparing Congress, apparently, for a delay in placing his work
before the Commission. An extract from the letter is as follows:
"I wish that the Government and the public as well should be the
judicial tribunal to conclude as to the originality of my work prior to the
verification of my claim as designed. Thus I expect that the scientific
commission's finding will include the originality of the work under the in-
structions of the Government given beforehand. Then nobody can, at
least morally, challenge and charge the commission with partiality, favoritism
etc., in rendering their certificate and thus obscure my achievement.
"I cannot believe that the spirit of our Congress will tolerate or for-
give that I should divulge the secret of my work to any person or com-
mission so long as there exists a legal opportunity by which infringers
can drag me into court in order to contest the originality of my work,
or so long as there may be the faintest possibility that my work may be
the prey of patent sharks, or that infringers may have a legal loophole
to pounce upon me and to snatch the fruit of my lifelong struggle.
"I am at the disposal of our Government at any time. If I may be
commanded to select the authorized commission I am willing to do so
when I am notified and given legal, unequivocal, and tangible assurance
that I will be recognized as the original discoverer of my work as pre-
scribed above. It is inconceivable that our Congress will tolerate the
delay of the advent of this work on account of the fantastic claims or
palmistic phraseology of willful obstructors and impostors."
The bill concerning the Garabed discovery was agreed to in
conference without difficulty and has been signed by the Presi-
dent.
Representatives of the Bureau of Chemistry are holding meet-
ings with mill, grain and elevator men throughout the country
to demonstrate methods of preventing explosions of grain dust.
One of the hitches in the effort to reach an agreement with
Norway regarding the commodities which were to be exported
to meet the Norwegian requirements arose over calcium carbide,
calcium nitrate, ferrosilicon and molybdenite. While Norway
needs calcium carbide as an illuminant and calcium nitrate 'as
a fertilizer, each of these chemicals would be of important use
to Germany in the making of munitions. In the same way,
Norway is in great need of ferrosilicon and molybdenum for its
domestic use, but as these materials are of first importance in
the manufacture of implements of war, the United States War
Trade Board drew stringent conditions under which these and
other products were to be furnished to Norway. The provisions
were more drastic than Norway was prepared to accept.
OBITUARIL5
CHARLES CASPARI, JR.
Charles Caspari, Jr., whose death took place last October,
was born in Baltimore in 1850. His father, a former pupil of
Wohler, had for political reasons fled from Germany in 1848,
but inspired in his son an intense longing for a German university
career. This longing was never satisfied: when still quite young
the boy was thrown upon his own resources, yet lived to prove
once more that a distinguished career may result far less from the
advantages, financial and educational, by which one may be
surrounded in youth, than from such gifts, natural and acquired,
as ambition, perseverance and a trained reason. In his effort
to prepare himself for a scientific career, he used every available
minute that could be spared from the monotonous work upon
which his livelihood as a drug
clerk depended: he studied in
omnivorous fashion; he per-
fected himself in methods of
analysis; he prepared every-
thing that he was likely to be
called upon to dispense; he got
into communication with all who
could assist him and answer his
questions; and, in order to
clarify and coordinate his
knowledge, he wrote articles and
even textbooks and treatises of
formidable scope. He thus be-
came a writer of clear, fluid
English, accurate and concise.
With intense pride in his pro-
fession, he would not tolerate for a moment anything that
savored of slovenliness in technique. At nineteen he was
graduated from the Maryland College of Pharmacy; ten years
later he became Professor of Pharmacy in that institution and
held this post until his death When appointed Food and Drug
Commissioner for Maryland, he began at once a course of con-
structive administration, the aim of which was not prosecution,
but instruction and inspiration. Outside his own State, also,
he soon attracted notice, and one by one responsibilities were
placed upon him. For twenty-eight years he was a powerful
influence in the American Pharmaceutical Association. His
work upon the successive editions of the Pharmacopoeia, of the
National Formulary of the National Dispensatory, was of great
value.
Dr. Caspari was extraordinarily modest and unselfish; he was
straightforward, truthful and unafraid. For anything that sug-
gested display or insincerity, he had nothing but contempt.
He feared no one, for he demanded of himself a higher standard
of craftsmanship than he could expect from others. For honest
failure he felt sympathy, and — a true friend — forgave many
failings and enjoyed apparently above all else the pleasure of
adding, as he had opportunity, to the happiness of those about
him. He was one whom it was a privilege to have known, and
a blessing to have known well.
Wvatt W. Randall
( 7
I ^ -
Caspari. Jr.
JOSEPH PRICE REMINGTON
Dr. Joseph Price Remington, Dean of the Faculty in the
Philadelphia College of Pharmacy and a member of the Amer-
ican Chemical Society of many years' standing, died at Phila-
delphia, January 1st, in his seventy-first year.
Prof. Remington was best known to the scientific world by
the fact that since 1901 he has been the chairman and the vital-
izing force of the Committee of Revision of the United States
Pharmacopoeia. Under his energetic yet judicious control,
tliis work, which sets the standards and gives the method of
preparation of crude drui;s and compounded medicines for the
druggists and the physicians of the country, has achieved a
position as the most accurate and complete of the Pharmaco-
poeias of the world. A comparison of the U. S. Pharmaco-
poeia with those of the most advanced European countries is
Mar., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
241
entirely in favor of our national work, and the pharmaceutical
and medical journals of Europe have conceded this with prac-
tical unanimity.
The passage of the National Food and Drugs Act in 1906 gave
additional force to this publication by making it the legal stand-
ard in all questions of purity and strength of such articles enter-
ing into the preparation of foods and medicines as came within
its scope. The whole administration of the food and drug
adulteration regulations of the Bureau of Chemistry at Wash-
ington and of the various state food commissions was therefore
based upon the purity and strength standards of the U. S.
Pharmacopoeia. The added responsibility thrown upon the
Committee of Revision during the last decade in view of this
important connection imposed new labors in conducting exten-
sive correspondence and investigations, all of which Prof. Rem-
ington undertook with unflagging zeal. At a memorial meeting
held in Philadelphia on January 4th, Dr. Wiley testified in strong
terms to the constant support Prof. Remington had given at
all times to the Government officials in their work of the enforce-
ment of the Food and Drugs Act and the raising of the standards
of these products so essential to the Nation's health.
Hardly less important to the profession of pharmacy and
medicine was his connection with the U. S. Dispensatory, which
is an encyclopedic commentary upon the drugs and medicines
which are in current use or known to science, and is a recognized
authority in the courts and in the U. S. Patent Office. Of this
work he had been since 1880 the pharmaceutical editor and the
responsible supervising head.
He also published in 1885 his "Practice of Pharmacy," a very
complete textbook which has had a very large circulation and
which has gone through a number of editions.
Prof. Remington was born March 26, 1847, in Philadelphia,
the son of a well-known physician. After completing a high school
education he entered a wholesale drug house where he spent
four years, during which time he attended the Philadelphia
College of Pharmacy, graduating in 1866. He then spent
three years under Dr. E. R. Squibb, of Brooklyn, N. Y., the
founder of the present firm of E. R. Squibb & Sons, where
he had exceptional opportunities for becoming a skilful chemical
analyst and also learned manufacturing methods. Following
this he spent three years in the chemical works of Powers &
Weightman in Philadelphia. This was certainly laying a sound
foundation for his subsequent career and explains the broad
grasp he had in after-life of both chemical and pharmaceutical
subjects.
In 1874 ne succeeded Prof. Procter, whose assistant he had
been for several years, as Professor of Theory and Practice
of Pharmacy in the Philadelphia College of Pharmacy, a con-
nection only to be severed by
death after forty-four years of
continuous service.
He was a pleasing and popular
lecturer and made many warm
friends among the thousands
who were his pupils during this
long period of years.
Besides his active member-
ship in the American Chemical
Society and the English Chem-
ical Society, the American Philo-
sophical Society and the Acad-
emy of Natural Sciences of Phila-
delphia, and the Chemists' Club
of New York, he had been
elected to honorary membership
in many pharmaceutical and medical societies in this country
and abroad and had taken part as delegate in international
pharmaceutical and medical congresses.
To those who had the privilege of intimate personal contact
with Prof. Remington, the loss now experienced is a great
one because of his cheerful disposition, his unfailing courtesy
and kindly consideration for all who were brought into contact
with him. To the writer it means the breaking of a close friend-
ship extending through forty years. He is glad to be privi-
leged to extend this inadequate tribute to his memory.
Samuel P. Sadtler
Joseph Price Remington
PERSONAL NOTLS
Dr. Glenn V. Brown, professor of chemistry at Bucknell Uni-
versity, has been granted leave of absence and is now connected
with the Jackson Laboratory of the du Pont Company.
Dr. W. L. Evans, a captain in the Ordnance Department,
is organizing a large staff for research work and routine tests in
the War Department.
Mr. Burton G. Wood, formerly of the Monsanto Chemical
Works of St. Louis, is now chief chemist of the Intravenous
Products Company of St. Louis, manufacturer of organic arsenic
products.
Chancellor Samuel Avery, of the University of Nebraska,
has been given leave of absence in order that he may go to
Washington to accept the position of chemist with the National
Council of Defense.
The United States Civil Service Commission announces
open competitive examinations for metallurgical chemists, sala-
ries $1600 to $2400 a year, and assistant metallurgical chemists
at $1000 to $1600 a year, for men only. Applicants should
apply at once for Form 1312, stating the title of the examination
desired, to the Civil Service Commission, Washington, D. C.
On account of the urgent needs of the service, applications will
be received until further notice.
Mr. Russell Hayworth, formerly with the Citizens Gas Com-
pany, of Indianapolis, is now with the Ordnance Department
as engineer of tests, Curtiss Manufacturing Company, St.
Louis, Mo.
Mr E. Colonna de Giovellina, former instructor in chemistry
at the Vancouver Academy, and who had been appointed re-
search chemist of the Whalen Pulp and Paper Mills, Ltd., has
been ordered to report to the First Depot Battalion of the
Canadian Expeditionary Force.
Dr. J. I. D. Hinds, of Lebanon, Tennessee, has been appointed
chemist of the geological survey of Tennessee. Dr. Hinds
succeeded Dr. Paul C. Bowers, who has been called to Wash-
ington for government service.
Mr. A. G. Stillwell has accepted a commission as Captain in
the Ordnance Reserve Corps and is now stationed in Washing-
ton, assigned to research work in the Toxic Gas Division. Be-
fore leaving New York Mr. Stillwell incorporated his business
under the title, The Stillwell Laboratories, Inc. His former
assistant, Mr. E. C. Moffett, is now manager and will carry on
the work.
Prof. Chas. H. LaWall, of the Philadelphia Section, of
the A. C. S., has been appointed Dean of the Philadelphia
College of Pharmacy, succeeding the late Dr. Joseph P. Rem-
ington. He has also been nominated for the Chair of Theory
and Practice of Pharmacy in the College.
Mr. G. W. Roark, assistant chemist in the Chemical Section
of the Agricultural Experiment Station at Iowa State College,
Ames, Iowa, has been appointed chief chemist of the Federal
Chemical Company's plants and will have his offices at Louis-
ville, Kentucky.
Dr. J. A. Wilkinson, formerly associate professor of chemistry
at Iowa State College, Ames, Iowa, has been appointed Captain
in the Design Section, Gun Division, and is now located at
Washington, D. C.
THE JOURNAL OF INDl STRIAL AND ENGINEERING I HEMISTRY Vol. 10, No. 3
1 11 Philip A. Shafer, of Washington University, has been
called to the national service.
The Short Course in Ceramic Engineering at the University
of Illinois closed its two weeks' program on Saturday, January
19th. The program of lectures was carried through as planned
and those in attendance at the course expressed themselves as
thoroughly satisfied with the results oi thei] attendance. In
addition to the lectures given by members of the University
staff, the following lectures from outside contributed largely to
making the Course a successful one Mr. A V Bleininger, of
ih. Pittsburgh Laboratory of tin- U. S. Bureau oi Standards;
Prol C. B. Harrop, of the Department of Ceramic Kngineering,
at 1 ilno State University; and Mr. Dwight T. Farnham. In-
dustrial Engineer, of St. Louis, Mo.
Mr. A. E. Blake, for several years research chemist at Mellon
Institute, Pittsburgh, Pa., has been appointed sales engineer
for the Surface Combustion Company of Long Island City,
N. Y., and is in charge of the new office for the Pittsburgh
district at 547 Union Arcade, Pittsburgh, Pa.
1 >r. Frank Austin Gooch, professor of chemistry and director
of the Kent Chemical Laboratory of Yale University, will re-
tire at the end of the present year. Dr. Gooch will be suc-
ceeded by Prof Bertram Borden Boltwood, since 19 10 professor
of radio-chemistry.
Mr. Albert Sauveur, professor of metallurgy and metallog-
raphy of Harvard University, has been granted a leave of absence
so that he may continue his research work for the French gov-
ernment.
Prof. Sterling Temple of the department of chemistry of
the University of Minnesota has gone to Washington, where
he is to engage in work in the Ordnance Department.
Prof. E. V. McCollum, head of the department of chemistry
of the school of hygiene and public health of Johns Hopkins
University, delivered the Packard lecture before the Ameri-
can Pediatric and Rush Societies of Philadelphia on February
12. The subject of the lecture is "Growth."
Prof. Charlotte Fitch Roberts, since 1894 head of the de-
partment of chemistry at Wellesley College, died on December
5, 1917, in her fifty-eighth year.
Dr. F. H. Thorp has been appointed lecturer in industrial
chemistry at the Massachusetts Institute of Technology.
At a conference of cereal chemists and representatives of the
U. S. Food Administration held in the Chemists' Building, New
York Citv. onFebruary 12, 1918, Dr. J. A. LeClerc, of the Bureau
of Chemistry, Washington, D. C, gave a report of work which
has been going on in the Bureau for the past five years on the
use of wheat substitutes in breadmaking.
Mr. Robert J. Anderson, formerly chief chemist for the Cleve-
land Metal Products Company, is now engineer of tests of ord-
nance material, War Department, and is stationed at the Brier
Hill Steel Company, Youngstown, Ohio.
Mr. R. S. Dean has been made acting head of the department
of metallurgy at the University of Pittsburgh.
Dr. H. S. Adams is now superintendent of the New Brunswick
laboratories of E. R. Squibb X: Sons.
Mr. Harry Eastwood, formerly assistant engineering chemist,
City of Chicago, is now with the Milton Manufacturing Com"-
pany, Milton, Pa. He is also engineer of tests for the Ordnance
Department.
Mi. Raymond E. Kirk, former instructor in chemistry at Iowa
State College, Ames, Iowa, has been appointed chief inspector
for the V . S A. and is now with the Atlas Powder Company,
Webb City, Missouri.
Dr. William II. Warren, formerly of Wheaton College, Norton,
Mass., has been appointed Captain in the Quartermaster Re-
serve Corps and is now in Washington.
Dr. David Klein, State Food Analyst of Illinois, has received
a Captain's commission in the Sanitary Corps of the United
States Army.
Simmons College announces the appointment for the second
half of the college year of Mrs. Kenneth L. Mark as instructor
in chemistry.
Mr. Ellwood Hendrick, of New York City, has joined the
staff of Metallurgical and Engineering Chemistry as consulting
editor.
Dr. Gorham \V. Harris has been appointed temporary head
of the chemistry department of Simmons College.
I>r. I.. F. Goodwin has been appointed professor of industrial
chemistry and chemical engineering at Queen's University,
Kingston, Canada. Dr. Goodwin served with the Second
Battalion Canadians in France and Flanders. He was also em-
ployed as technical adviser to the British War Office for
nd then transferred to Ottawa where he served for a
year in a similar capacity to Sir Sam Hughes, then Minister of
Militia and 1 >i
Dr. Katharine Blunt, of the Home ICcouomics Department of
Chicago University, has been granted a leave of absence for the
winter quarter. She has been called to Washington by the Food
Administration as one of the members of the committee of uni-
versity instructors appointed to plan the introduction of con-
servation courses into universities and colleges.
The Manitoba Chemical Society was organized at Winnipeg
on January 15 to provide facilities for the exchange of ideas
and discussion of chemical subjects and to afford a medium
for recommendations to the authorities in regard to chemical
problems of national interest. The following officers were elec-
ted: J. W. Shipley, secretary; E. L. C. Foster, treasurer; M. A.
Parker, F. J. Birchard, H. S. Davis and F. Pugh members of
the executive committee.
Mr Ilk Richardson gave an illustrated talk on "A Chem-
ist's View of the Native Industries of China" at a joint meeting
of the New York sections of the American Electrochemical
Society, the Society of Chemical Industry and the American
Chemical Society, held at the Chemists' Club on March 1.
Mr. Emil Illich, of the chemical laboratory of the National
Lead Company, has joined the aviation corps and is now sta-
tioned at Camp Grant, Rockford, III.
Mr. William Simonson, of Cincinnati, aided by Cincinnati
capitalists, is organizing a company for the manufacture of
nitrates, ammonia and dyestuffs. The chemical will be manu-
factured by a process invented by Mr. Simonson, claimed to
greatly reduce the cost of production. It is understood that
the projectors of the enterprise are considering the location of
the plant at or near Muscle Shoals, Ala., where the Government
is building its S30,ooo,ooo nitrate plant.
The following committee has been appointed to raise $2,000,-
000 for a new chemistrv building for Cooper Union: Y. G
Bloede, H. C. Enders, J. C. Olsen, Alfred Spice, P. C. Walsh, Jr..
Maximilian Toch, H. A. Metz, S. A. Samuels and E. R. Hewett,
Treasurer, Cooper Union, New York City.
Dr. John E. Teeple has resigned the position of chief of the
Chemical Section of the U. S. Signal Corps, which position he
has held during the past month.
It is reported that Prof. W. A Kouantz, a research chemist in
the College of Pharmacy of the State University, Iowa, has dis-
covered a method by which pure phenacetin, meeting all require-
ments for medicinal use, can be produced at less than half its
present cost.
Doncko L. Milie, an Austrian, until recently general manager
of the chemical department of Madero Bros., was arrested and
held in bail for examination on February :i accused of fraudu-
lently substituting salicylic acid for quinine which had been
ordered for military hospitals in Italy. Following this arrest, on
F'ebruary is. recen its took charge of the Madero Bros.' business
when an involuntary petition in bankruptcy was filed in the
Federal District Court, New York, by three creditors.
Dr. Isaac Strauss, who is said to be connected with a chem-
ical company that manufactures toluol, is detained at Ellis
Island.
Miss Helen Updegrapf, Newark, Del., a graduate of Cornell
University, has been appointed assistant chemist at the Dela-
ware College Experiment Station. Newark, succeeding Prof.
A. C. Whittier, resigned.
Mar., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
INDUSTRIAL NOTES
■ of Applications Made to the Fed
1911
Pat. No.
986,148
1913 1,059,983
1,078,135
13,848
1913
1914
Rrii
1905 782,729
1913 1,081,897
1909 924,664
1910 978,889
1913 1,053,396
1913 1,056,548
1913 1,057,154
1906 812,554
1908 892,166
1904 777,201
1906 821,776
1913 1,081,592
1914 1,116,398
Patentee
Ehrlich & Berthe
Ehrlich & Berthe
Khrlich & Berthe
Korndorfer & Reuter
Emil Fischer
Ehrlich & Berthe
Karl Irmhoff of Bredeney.
near Essen on the Ruhr,
Ger.
Karl Irmhoff of Bredeney.
near Essen on the Ruhr.
Ger.
Karl Irmhoff of Bredeney,
near Essen on the Ruhr.
Ger.
Ger.
Karl Irmhoff of Bredeney,
near Essen on the Ruhr,
Ger.
Alfred Einhorn, Munich
Farbw. vorm. Meister, Lu- Derivatives of oxyarylar-
cius & Bruning, Hochst sinic acids
on the Main
Farbw. vorm. Meister, Lu- Alkali compounds of dioxy-
cius & Bruning, Hochst diaminoarsenobenzene
on the Main
Farbw. vorm. Meister. Lu- Preparation from alkali
cius & Bruning, Hochst salts of the 3,3-diamino-
on the Main 4,4-dioxyarsenobenzene
Farbw. vorm. Meister, Lu- Derivatives of diaminodi-
cius & Bruning, Hochst oxyarsenobenzene
on the Main
C. Merck, Darmstadt C-C-Dialkylbarbituric acid
Farbw. vorm. Meister, Lu- Medicinal preparation
& Bruning, Hochst
on the Main
Dermatological Laboratories, Philadelphia
Takamine Laboratory, Inc., N. Y.
Farbwerke Hochst Co., N. Y.
Diarsenol Co., Inc., Buffalo
Dermatological Research Laboratories, Phila-
Takamine Laboratory, Inc., N. Y.
Dermatological Research Laboratories
Takamine Laboratory, Inc., N. Y.
Dermatological Laboratories. Philadelphia
Takamine Laboratory, Inc., N. Y.
Diarsenol Company, Inc., Buffalo, N. Y.
Abbott Laboratories, Chicago
Takamine Laboratory, Inc., N. Y.
Diarsenol Co., Inc., Buffalo
Farbw. vorm. Meister. Lu-
cius & Bruning. Hochst
on the Main
Sewage treatment apparatus Pacific Flush-Tank Co.,
office at Chicago)
N. Y.
Treating sewage
Sewage purification
Process of drying sludge
Settling-tank
Pacific Flush-Tank Co.,
office at Chicago)
(Principal
(Principal
Pacific Flush-Tank Co., N. Y. (Principal
office at Chicago)
Pacific Flush-Tank Co.,
office at Chicago)
Y. (Principal
Y. (Principal
Alka
esters of para- Rector Chem. Co., Inc., N. Y.
> benzoic acid
Process of preparing prin-
ters' overlays and under-
lays
Alfred Gutmann Actien- Sand blast machine
gesellschaft fiir Maschin-
enbau of Altona, Otten-
sen, Germany
Alfred Gutmann. Actien- Means for removing dust
gesellschaft fur Masch-
inenbau
Farbw. vorm. Meister, Lu- Medicinal preparation
cius & Bruning, Hochst
on Main
Farbwerke Hochst Co., N. Y.
The Abbott Laboratories of Chicago
Calco Chemical Company, Bound Brook, N\ J
R. P. Andrews Paper Company, Washington.
D. C.
Hoeval Manufacturing Corp., N. Y. (Ex-
ring Corp.,
Buffalo
Diarsenol Co., Inc
P. Ehrlich & A. Bertheii
Farbw. vorm. Meister, Lu- Dihydrochloride of diamino Diarsenol Co., Inc., Buffalo
cius & Bruning dioxyarsenobenzene
1907 T.M. 61 ,678 P. Beirsdorf & Company Tooth paste and tooth Lehn and Fink (exclusive)
Hamburg powder
1906 T.M. 50,868 Heinrich Bohr and Com- T. M. for pocket knives Boker Cutlery & Hdwe. Co., 101 DuaneSt.,
pany, Selingen, Ger. New York (exclusive)
1906 T.M. 54,700 H. Boker & Co. Scissors and knives Boker Cutlery & Hdwe Co., 101 Duane St.
New York (exclusive)
A certain named chemical The Abbott Laboratories of Chicago
product
1904 T.M. 42,942 L'ngarische Gummiwaren Rubber and asbestos pack- Another Packing Co. of Philadelphia
Fabriks Acktienger-Buda- ing
pest, Hungary
Langenscheidtsche Verlags- Pocket dictionary of Greek David McKay. Philadelphia
1903 T.M. 40, 115 E. Merck of Darmstadt
1911 Copyright
registration
3,163, class
A, XXC
.... Copyrights
for German
periodicals
and books
1 ,008,864
buchhandlung (Prof.
Langenscheidt), Sch6
berg, Berlin
1911
12,707 Max Riiping
' original patent No. 709.799 1 19021
' 931,579
Hulsberg & Cie. m.
Berlin, Germany
Hulsberg & Cie, m
Berlin, Germany
995,394
837,017
868,294
Diedrick A. M. Doublet,
Einsbuttel near Hamburg
Robert Zahn, Planen, Ger.
Treibachcr Chemise he
Werke Gesellschaft. m. h.
II. of Treibach, Austria-
Hungary
nd English languages
1 iion of wood, etc.
Method of impregnating
wood
Sand blast blower
Jacquard embroidering ma-
1 Sine
Pyrophoric mass
Clinton darby Levy, 2 Duane St., New York
Leobcke, Von Bernuth Co.,:
Ave . New York
1 mbi I 1 v<>" Bernuth Co,
in Madison
Ho
.. ,1 M.muf. Corp.. X. Y.
Robert Rumen Importing Co., Gregory Ave
& Hackensack Plank Road, Weehawken,
N. v.
Lindsay Light Co.. Chicago
Pyrophoric alloy
I 111,1 .IV I 1 111 I 1, , t In I'M
1901 680,395
Carl Auer von Welsbai
Robert Schmidlin, Hochst Farbwerke vorm. Meister, Process of producing phenyl- E. 1 <lu Pont de Nemours 1
Main Lucius & Bruning glycin and its homologues Del
Johanness Pdecer, Frank- Deutsche Gold and Silbcr Process of making indoxyl B. I. du Pont de Nemours i
, Willi
Willi
iiiKton,
ington,
(a) This is a list of the applicatii
Schcide Anstatt vorm.
Rocsslcr, Frankfort on
Main
re been made to date. Addil
hey occur.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 3
List op Applications Mads '.
*B Fbdbral Trade Cohmis
Year
Pat. No.
Patentee
1906
818,992
Oscar Bally & Max Henry
Isler, Mannheim
Badische
Fabrik
on the
1905
787,859
R. H. SchoII, Karlsruhe
Oscar Bally, Mannheim
Badische
Fabrik
on the
1911
1,003,268
Richard Just and Hugo
Wolff, Ludwigshafen on
the Rhine
Badische
Fabrik,
1905
796,393
Oscar Bally, Mannheim
Badische
Fabrik
1904
753,659
Rene Bohn, Mannheim
Badische
Fabrik
1903
739,145
Rene Bohn, Mannheim
Badische
1913
1,055,701
Rene Bohn, Mannheim
Badische
Fabrik
1903
724,789
Rene Bohn, Mannheim
Badische
Fabrik
1913
1,063,173
Christian Rampini, de-
ceased, by Wm. E. Mar-
land, administrator
Badische
Fabrik
1908
906,367
Oscar Bally, Mannheim
Hugo Wolff, Ludwigshafen
Badische
Fabrik
1910
961,612
Max Henry Isler and Hugo
Wolff
Badische
Fabrik
1902
711,377
Max Bazlen, Ludwigshafen
Badische
Fabrik
1909
931,958
Louis Haas, Heidelberg
Badische
Fabrik
1905
795,755
Max Bazlen
Badische
Fabrik
por Licenses under Enemy Controlled Patents Porsoant to the "Trading with
Enemy Act" (.Concluded)
Assignor Patent Applicants
Anilin & Soda Anthracene dye and process E. I. du Pont de Nemours Co.
of Ludwigshafen of making the same
Rhine
Anilin & Soda Anthracene compound and E. I. du Pont de Nemours Co.
of Ludwigshafen, process of making the
Rhine same
Anilin and Soda Anthracene dye and process E. I. du Pont de Nemours Co.
Ludwigshafen of making the same
Anilin & Soda Anthracene coloring matter E. I. du Pont de Nemours Co.
and process of producing
the same
Anilin & Soda Anthracene derivative and E. I. du Pont de Nemours Co.
process of making the
1 Co.
Anilin & Soda Anthracene dye
E. I du Pont de Nee
Anilin & Soda Pigment and 'process of E. I. du Pont de Nemours Co.
making the same
Anilin & Soda Blue dye and process of E. I. du Pont de Nemours Co.
making the same
Anilin & Soda Producing aminoanthraqui- E. I. du Pont de Nemours Co.
nones and derivatives
thereof
Anilin & Soda Anthracene dye and pro- E I. du Pont de Nemours Co
cess of making the same
Anilin & Soda Anthracene compound and E. I. du Pont de Nemours Co.
process of making it
Anilin 8: Soda Solid alkaline hydrosulfites E. I. du Pont de Nemours Co.
and process of making the
Anilin & Soda Sulfur dye and process of E. I. du Pont de Nemours Co.
making the same
Anilin & Soda Process of making stable E. I. du Pont de Nemours Co.
dry hydrosulfites
Manufacturers of chemicals and various other products
who use acetate of lime in their processes, are being asked to
answer a somewhat lengthy questionnaire which is being sent
out to producers of acetate of lime under government direc-
tion. The questionnaire is the direct result of the recent action
of the government in seizing the entire output of that commodity
and which consumers will be able to obtain for their private
uses only through a government permit. Inability of the govern-
ment to obtain sufficient quantities of the acetate has led to
this action, the material being vitally needed for the making
of military explosives.
American scientists have placed a new medical discovery at
the disposal of the Allies in Europe. It is expected that the
new product, phenolsulfonephthalein, will be a vital factor in
minimizing diseases among our troops in France. It is reported
that the drug was discovered by the chief of the department
of chemistry of Johns Hopkins University, and after tests in
the physiological department and by the pharmacologists of
that institution, was found to be the most efficient of all diag-
nostic agents for tracing defects in the functioning powers of
the kidney.
A plant for the manufacture of alcohol, to cost not less than
$3,000,000, is in process of erection adjoining the West Virginia
Pulp and Paper Company plant, at Luke, Md. The entire
output is to go to the United States Government, which is fur-
nishing the funds to build.
It is reported that a chemical plant costing $1,000,000 is to
be constructed by the Federal Government at Mechanicsville,
N. Y., to utilize the by-products of paper manufacturing plants
of the West Virginia Pulp and Paper Company. The Govern-
ment is to manufacture acetone, which is to be used to mix
with varnish for coating aeroplane wings.
It is reported that a Spanish firm is manufacturing wool from
cork, which it is claimed may be substituted for natural wool
in the manufacture of mattresses, pillows and quilts. The
material is stated to be cleaner and lighter than wool. It is
first treated with chemicals to remove any resinous substances
and to render it flexible and less likely n> break.
The Oil, Paint and Drug Reporter states that more sulfuric
acid was produced in the United States in 1917 than in any
previous year, and that a moderate estimate shows that the in-
crease in the production of acids of all strengths in 1917 over
that in 19 16, stated in terms of 60 ° Be. acid, amounted to at
least 600,000 tons.
According to advices from headquarters of the du Pont
de Nemours Powder Company, the production of potash at
Columbus Marsh, Ney County, Nevada, is to begin at once.
Preliminary drillings on the marsh gave brines carrying 3V1 per
cent soluble potash, and it is hoped to increase this by tapping
the bottom of the prehistoric lake at a depth of 4,000 ft.
The Great American Chemical Products Company. Xew
York, N. Y., the company which is being formed by druggists
throughout the country, has begun the operating of four pre-
liminary plants in the Greater Xew York district, and will
shortly operate two more, at Buffalo and Bound Brook.
Plans have been completed for the plant of the Collinwood
Chemical Company, Collinwood, Tennessee, the new company
which will manufacture alcohol and acetate of lime for the gov-
ernment. The plant will cost in the neighborhood of $2,000,000
and will have a daily capacity of 2700 gals, of wood alcohol,
52,000 lbs. of acetate of lime and 12,375 bushels of charcoal.
The plant, which will be finished September 1 and will cover
twenty-five acres, will produce a quantity of tar, creosote, wood
preservative and wood oils, in addition to the alcohol, charcoal
and acetate of lime. The product which the government will
take is to be manufactured into war munitions.
The big German dye factories at Ellesmere Port, on the
Mersey River, England, were recently sold to Col. Brotherton,
of Leeds, England. The concerns involved were the Badische
Anilin und Sodafabrik, the Farbenfabriken vorm. Fr. Bayer &
Company, and the Actiengesellschaft fur Anilinfabrikation
of Berlin. The plant was built nine years ago to conform with
the British patent laws and is described as presenting the most
modern ideas in construction of a chemical works. It is ideally
located for deep water transportation, ocean-going steamers
being able to dock outside of the works. It conforms largely
to the construction of similar works on the Rhine River in
Germany.
A resolution has been introduced in the House by Represen-
tative Mason, of Illinois, which will prove of interest to the chem-
ists of the country, as it provides for an investigation to show
whether chemical processes are being used to foist upon the
country food that is without nutritive value. After citing
these charges the resolution authorizes the Secretary of Agri-
culture to make a full and complete investigation to cover the
following subjects:
First, what cereals are treated chemically or otherwise so as
to deprive them of any of their food values before they are used
in bread, biscuit, crackers, cake, pastry, and so forth.
Second, what, if any, of the cereals that haVe been treated
chemically or otherwise in a manner to reduce their food values
are ground in the mills of this country and mixed with wheat,
corn, rye, barley, buckwheat, or other cereals before the same
are sold to the consumer.
Third, what, if any, of the by-products of the cereals are
treated chemically or otherwise in a way to deprive them of
their food value or in a way that makes their use deleterious
to public health and are used in the manufacture of bread or
other food products.
Fourth, what, if any, mineral oils are being used as a substi-
tute for animal fats and whether the use of such products is a
fraud upon the consumer and whether the same is deleterious
to the public health.
Mar., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
24S
Turkey is developing its textile industry, and new textile
plants aggregating a capital stock of Si, 000,000 have been
started there within the last few months.
The Harden, Orth and Hastings Corporation, of New York,
have acquired control of the Buttercup Oil and Car Company,
Louisville, Ky. The latter is one of the largest producers of
cottonseed oil in the country, and its already large and diversi-
fied output of such products will be increased by the new
owners.
In an address before the Delaware Section of the A. C. S. at
Wilmington, on February 8, Mr. C. M. Barton, vice president
of the duPont Nitrate Company, stated that his concern
has developed a process for extracting potash from nitrate
ores and has made large profits from it. The Company is draw-
ing on Chilean nitrate ores for the purpose and has communica-
ted the process to allied interests producing nitrate ores in
Chile, enabling them to increase their output of potash greatly.
The recently organized Dyestuffs Association of America
has appointed the following committee to consider the various
points of tariff recommendations for a conference with the Gov-
ernment Dye Commission: J. Merritt Matthews, August
Merz of Heller & Merz, R. T. Dicks of Dicks, David Co., and
H. G. McKerrow of E. F. Drew & Co., all of New York; L. A.
Ault of the Ault & Wiborg Co., Cincinnati; and C. B. Althouse
of the Althouse Chemical Co., Reading, Pa.
At the suggestion of the War Trade Board, upwards of fifty
representatives of the leading crushers and importers of castor
oil and castor beans held a meeting in New York on January 12.
The meeting was held for the purpose of forming an associa-
tion to cooperate with the Government in securing adequate
supplies of castor oil for the lubrication of aeroplane motors.
Large quantities of this oil have already been absorbed by the
Government, but, to insure the necessary supplies in the future,
the organizing of factors in the trade for the purpose of controll-
ing the industry was deemed necessary. The following com-
mittee of five members was chosen for the task of organizing
the association as a membership corporation: A. C. Trask,
of Marden, Orth & Hastings Corporation, chairman; Leonidas
J. Calvocoressi, of Ralli Bros., Irving R. Boody, of Balfour
Williamson & Co., Frederick A. Marsh, of Baker Castor Oil Co.,
and Howard Kellogg, of Spencer, Kellogg & Sons Co.
GOVERNMENT PUBLICATIONS
By R. S. McBride, Bureau
NOTICE — Publications for which price is indicated can be
purchased from the Superintendent of Documents, Government
Printing Office, Washington, D. C. Other publications can
usually be supplied from the Bureau or Department from which
they originate. Commerce Reports are received by all large
libraries and may be consulted there, or single numbers can be
secured by application to the Bureau of Foreign and Domestic
Commerce, Department of Commerce, Washington. The regu-
lar subscription rate for these Commerce Reports mailed daily is
$2.50 per year, payable in advance, to the Superintendent of
Documents.
NATIONAL MUSEUM
Mineral Industries of the United States: Coal Products,
an Object Lesson in Resource Administration. C. G. Gilbert.
Bulletin 102, Part 1. 16 pp. Paper, 10 cents. Published
November 17, 191 7.
Mineral Industries of United States: Sulfur, an Example
of Industrial Independence. J. E. Pogue. Bulletin 102,
Part 3. 10 pp. Paper, 5 cents. Published November 7, 1017.
SMITHSONIAN INSTITUTION
Administration and Activities of Smithsonian Institution.
A. H. Clark. Publication 24.50. From Report for 1916.
22 pp.
The Earth, Its Figure, Dimensions, and Constitution of Its
Interior. Articles by T. C. Chamberlin, H. F. Reid, J. F.
Haytord and F. Schlesinger. Publication 2457. From Re-
port for 1916. 30 pp.
I Petroleum Resources of United States. R. Arnold. Pub-
lication 2459. From Report for 1916. 15 pp.
Present Problem of Evolution. M. Caullery. Publica-
tion 2462. From Report for 1916. 15 pp.
PUBLIC HEALTH SERVICE
The Standardization of Anti-typhoid Vaccine. G. W. McCoy.
Hygienic Laboratory Bulletin no, Part 1. Published No-
vember 191 7.
A Colorimetric Method for the Estimation of the Cresol or
Phenol Preservative in Serums. E. Elvove. Hygienic Labora-
tory Bulletin no, Part 2. Published November 191 7.
Toxicity of Certain Preservatives Used in Serums, Viruses
and Vaccines. J. P. Leake and H. B. Corbitt. Hygienic
Laboratory Bulletin no, Part 3. Published November 1917.
Observations on the Significance of Anti-sheep Amboceptor
in Human Serum, with Reference to Complement Fixation
of Standards, Washington
Test for Syphilis. M. H. Neill. Hygienic Laboratory Bulle-
tin no, Part 4. Published November 1917.
Public Health Laboratory Specimens: Their Preparation and
Shipment. H. E. Hasseltine. Public Health Reports, 32,
2016-2032 (November 30, 1917). This paper has been pre-
pared for the purpose of furnishing brief, concise instructions
relative to the preparation and shipment of specimens for
laboratory examination in order that the best results may be
obtained.
Arsphenamine (Salvarsan): Licenses Ordered and Rules
and Standards Prescribed for Its Manufacture. Public Health
Reports, 32, 2071-72 (December 7, 1917). The Federal Trade
Commission, on November 30, 1917, issued orders for licenses
to manufacture and sell the product heretofore known under
the trade names of "salvarsan," "606," "arsenobenzol," and
"arsaminol" to the following named manufacturers: Derma-
tological Research Laboratories, of Philadelphia; Takamine
Laboratory, Inc., of New York; and Farbwerke Hoechst Co.
(Herman A. Metz Laboratory), of New York. The drug will
be manufactured and sold under the name of "arsphenamine."
The rules and standards, prescribed by the United States Public
Health Service, were promulgated by the Federal Trade Com-
mission, November 22, 1917.
Appropriations for City Health Departments. P. Preble.
Public Health Reports, 32. 7 pp. Published December 7, 1917-
Summary of expenditures of 330 cities in the central and eastern
United States for public health work.
Mitigation of the Heat Hazard in Industries. J. A. Watkdjs.
Public Health Reports, 32. n pp. Published December 14,
1917.
Industrial Efiiciency. F. S. LEE. Public Health Reports, 33.
7 pp. Published January n, 1918. "The bearings of physio-
logical science thereon: A review of recent work."
WATERTOWN ARSENAL
Report of Tests of Metals and Other Materials Made in
Ordnance Laboratory at Watertown Arsenal, Mass., Fiscal
Year 1916. 132 pp. Cloth, 75 cents.
INTERNAL REVENUE COMMISSIONER
Alcoholic Medicinal Preparations. Treasury Decision 2544.
6 pp. This is a revision of Treasury Decision 2222, covering
a list of alcoholic medicinal preparations for sale of which special
tax is required.
246
THE JOURNAL OF INDUSTRIAL AM) ENGINEERING ( HEMISTRY Vol. 10, Xo. 3
Distilled Spirits. Treasury Decision 2576. 3 pp. This
covers instructions relative to ale and use ■>! distilled -pints
for other than beverage purposes under the Food-control act of
August i". 1917, and the act of October 3, 1017
GEOLOGICAL SURVEY
Gold, Silver, Copper and Lead in Alaska in 1016. A. H.
Brooks. From Mineral Resources of the United States, 1916,
Part I. 13 pp. Published November 20, 1017. Mines Re-
port. A summary of the production statistics for these metals
will appear later.
Gold, Silver, Copper, Lead and Zinc in New Mexico and Texas
in 1016. C. W. Henderson. From Mineral Resources of the
United States, 1916, Part I. 28 pp. Published November
23, 1917- Mines Report. (See summary latei
Gold, Silver, Copper, Lead and Zinc in California and Oregon
in 1016. C. G. Yale. From Mineral Resources of the United
States, 1916, Part I. 53 pp. Published December 3. 1917.
Mines Report. (See summary later.)
Gold, Silver, Copper, and Lead in South Dakota and Wyoming
in 1016. C. W. Henderson. From Mineral Resources of the
United States, 1916, Part I. 14 pp. Published November
21,1917. Mines Report. (See summary later.)
Gold, Silver, Copper, Lead and Zinc in Arizona in 1016.
V. C. Heikes. From Mineral Resources of the L'nited States,
1916, Part I. 37 pp. Published December 21, 1917. Mines
Report. (See summary later
Gold, Silver, Copper, Lead and Zinc in the Eastern States
in 1016. J. M. Hru.. From Mineral Resources of the United
States, 1916, Part I. 9 pp. Published December 18, 1917.
Mines Report. (See summary later. I
Gold, Silver, Copper, Lead and Zinc in Montana in 1916.
V. C. Heikes. From Mineral Resources of the United States,
1916, Part I. 32 pp. Published December 22, 1917. Mines
Report. (See summary later.)
Mica in 1916. W. T. Schaller. From Mineral Resources
of the United States, 1916. Part II. 18 pp. Published November
28. 1917. The total value of tin- domestic mica (muscovite)
produced and sold in 1916 was $594,391. the highest value re-
corded by the United States Geological Survey. The value
of the sheet mica produced in [916 was exceeded by the produc-
tion in 1900, 1909, 1910 and 1913. Except for 1912, 10:4 and
1915 the quantity of sheet mica produced was the smallest
since 1904.
The run-of-mine mica is sold either in bulk it s,> much per
ton or on 1 ontract at a fixed price per ton The prices paid
represent the value of the mica as it is taken from the mine and
not the value of the finished cut mica ready foi the trade. The
finished cut mica brings a much higher price, as it is ready to
be used and has had a considerable amount ol money spent on
it It is obviously inconsistent to add tOgethei the value of
mica of two greatly different classes, vet this procedure is the
only one that can at present be followed. The total production
for the United States in 1916 of cut sheet mica was ,15, 1 74 lbs..
valued at in average price of Si jo per lb The total
production of uncut sheet mica, which includes an estimated
percentage of the sheet yield of run of-mine mica, was 350,689
lbs , valued at $113,792. or an average price of onlv So 2 1 per
lb. Vet this uncut mica needs only to be cut in order to have
its value materially increased
The figures of production of mica in the l'nited States, as
reported to the l'nited States Geological Survey, do not show
any noteworthy change in the quantity (9,102 short tons'
I m the two years 1915 and 1916, as compared with the
quantity (9,821 short tons) produced in the two years immedi-
ately preceding 1014. In 1914 the production was 1.0..S short
toiis Neither was there am significant change m the same
years in consumption that is. production plus imports minus
exports. About So to 90 per cent of the total domestic con-
sumption of mica is mined in the United States, the remainder
imported from Canada and India, either direct or
through England. The imports have decreased, those for
1912 and 1913 amounting to nearly 2.500 short tons and those
for 1915 and 1916 amounting to about 1,500 short tons. In
1914 the imports were 611 short tons. In round numbers
11,000 short tons of mica were consumed in 1915 and 1916,
as against 12,000 short tons in 1912 and 1913 In 1914 appr.
niately 5,000 short tons wen consumed.
Fluorspar and Cryolite in 1916. E. F Btrchard From
Mineral Resources .if the l'nited States, 1916. Part II. 17 pp.
Published December 14, 191 7. The total quantity of domestic
fluorspar reported t" tin Survey as -old in 1916 was
short tons, valued at $922/154, an increase in quantity of 18,794
short tons and in value of $158,179, representing nearly 14 per
cent of the quantity and nearly 21 per cent of the value of the
product marketed in 1915. The average price per ton for the
whole country, all grades of fluorspar, gravel, lump, and ground
considered, was approximately S5 92 in 1916, compared with
$5.58 in 1915. an increase of about 6 per cent. This value
represents the selling price on board cars or barges at railroad
or water shipping points
As usual, the bulk of the fluorspar sold was in the form of
gravel spar, the quantity in 1916 amounting to 133.651 short
tons, or nearly 86 per cent of the total Two grades of spar,
gravel and lump, showed important increases in 1916 over all
preceding years, but ground spar did not show as large an out-
put as in 1915, the decrease in quantity having been more than
29 per cent in 1916. The general average price of domestic
fluorspar declined steadily from 191 2 to 1915. largely as a re-
sult of improvements in methods of milling and handling large
quantities of spar in the Illinois-Kentucky district, and this
price was lower in 1915 than at any time in the last 10 years;
but in 1916. as predicted in this chapter in Mineral Resources
for 1915. an increase in price was to be expected. The average
price of all grades of spar increased in 19 16, the ground spar
A the gravel and lump 45 and 43 cents per ton, respec-
tively.
The imports of fluorspar mt" the L'nited States entered for
consumption in 1916 were 12.323 short tons, valued at
compared with 7.107 short tons, valued at $22,878, in 1915.
This represents an increase of about 72 per cent in quantity and
per cent in value. The price assigned to the imports
in 1916 averaged $4 .38 a ton, a- compared with $5.19 a ton in
1915. an increase of Sin, a ton. or about 37 per cent The
imports of fluorspar in 1010 were equivalent to about
cent of the domestic production of gravel spar, as compared with
nearly 6.3 per cent in 1015 The average reported price of
imported spar at duck, exclusive of the duty, was equivalent to
about 82 per cent "i the average price of domestic gravel spar
at mines or nearest shipping points in 1916. compared with 05
per cent in 1915 According to the prices reported, including
the dutj . but excluding freight charges, the average
cost of imported spar to the consumer was £3 88 a tern ill iqio.
compared with $5 .34 lor domestic gravel spar at the mines or
mills, ui 1015. the cost of the imported material, including the
duty of $1 50 a ton, was $4 69, compared with $4. so for domestic
gravel spar The freight charges on domestic spar to points
where it is consumed are generally higher than on fon
from the docks to eastern steel plants, so that a slight advantage
in price still may be enjoyed by the imported spar at eastern
steel plants Foreign spar is. however, not generally of so high
grade as the mechanically treated -par from Illinois and Kentucky
and since fluorspar is , .t value chiefly according to its
purity, purchasers should find that the purer American spar is
more efficient and consequently cheaper in the end. Recently
difficulties in getting supplies of fluorspar from American mines
Mar., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
when needed, on account of freight embargoes, lack of cars,
difficulties of transportation on Ohio River, and labor troubles,
have led steel manufacturers to accept readily whatever foreign
spar was available.
No cryolite is produced in the United States, the entire supply
used in this country being imported from Greenland.
The quantity of cryolite reported to have been imported for
consumption in the United States in 1916 was 3,857 long tons,
valued at $165,222, as compared with 3,940 long tons, valued
at $82,750, in 1915. The average price per ton declared in
1916 was apparently $42.84, as compared with $21 in 1915.
Cryolite is imported free of duty.
The annual imports of cryolite, beginning in 1894, are shown
in a table, according to the records of the Bureau of Foreign
and Domestic Commerce. They range from a minimum of
36 long tons in 1910 to 12,756 long tons in :8g4, but are mostly
between 1,000 and 6,000 tons a year. There are wide varia-
tions in average price per ton reported during this period, such
as $10.58 in 1898 and $65.08 in 1910. The latter figure may be
an error, as there seems to be no especial reason for so high a
value in 1910, unless the shipment may have consisted of the
white grade of cryolite. In 1916, in keeping with the increased
prices of most mineral products due to the demands of war and
especially of those dependent upon ocean transportation to
centers of consumption, the price rose to $42.84 a ton or more
than 100 per cent as compared with that of 19 15.
Sand and Gravel in 1916. R. W. Stone. From Mineral
Resources of the United States, 1916, Part IT 13 pp. Pub-
lished December 21, 191 7. The quantity of glass sand produced
in the United States passed the 1 ,000,000- ton mark in 1905;
in 1916, for the first time, it exceeded 2,000,000 tons. There
has been a tendency in the last few years for the average price
per ton to decrease, the lowest price being 85 cents in 1915,
but there was a strong recovery in 1916 to 97 cents.
It is believed that the production in 1917 will be considerably
greater and that the average price per ton will exceed $1, as
an increased output is promised by larger demands and new
uses for glass. As a structural material glass has an increasing
use — for example, in the larger window area demanded in new
office, factory, and school buildings.
The effect of the war in Europe on the molding-sand industry
in the United States is very apparent. Reports of production
made to the United States Geological Survey show an increase
of 30 per cent in 19 16 over 19 15. This great increase was
caused by the demand for vast supplies of machinery and muni-
tions for shipment abroad and also for manufacturing and mining
machinery for domestic use, all of which required molding sand
for casting the metal. The production in 1916 exceeded 4,500,000
tons for the first time and the average price per ton, 69 cents,
was the highest yet recorded.
The total production of grinding, polishing, and blast sand in
1916 was 1,370,354 short tons, valued at $889,651. This was
an increase of about 40 per cent in quantity and 100 per cent in
value over the production of 1915.
Pennsylvania was the largest producer of fire or furnace
sand, which is a highly refractory silica sand used for lining and
patching reverberatory and other furnaces, cupolas, and ladles
used to contain molten metal. It is also used for making runners
for pig-iron casting. Although the quantity produced in 1916
as reported to the Survey was less than in 1915, the total value
was mure than double thai of the earlier year. The average
price per ton in 191.5 was about ,54 cents; in 1916 it was 90 CI ni
and considerable quantitie brought well over $1 ■ > ton
The grand total of sand and gravel produced in tin I nited
States in 1916 shows :m increase of more than 12,000,000 short
tons and in value of more than $6,600,000.
Zirconium and Rare-Earth Minerals in 1916. W. T. Schaller.
From Mineral Resources of the United States, 19 16, Part II.
Published December 22, 19 17. In 1869 a small output of zircon
and in 1883 a much larger quantity was reported to have been
mined. Small quantities were produced from 1903 to 1907,
and then intermittently to 191 1. For the last five years no
production of zircon in this country has been reported to the
United States Geological Survey. In view of the large pro-
duction of natural zirconium oxide from Brazil it seems doubtful
whether for present purposes there will be an active demand for
zircon. This report also discusses in detail the occurrence and
uses of cerium, yttrium, and lanthanum.
Magnesite in 1916. C. G. Yale and H. S. Gale. From
Mineral Resources of the United States, 1916, Part II. Pub-
lished January 16, 1918. The production of magnesite in the
United States in 19 16 far exceeded that of any preceding year.
The increase was due to the larger demand for refractory mag-
nesite products and to the decline in imports. Though more
magnesite was used in the United States in 1916 than in 1915,
the use of the mineral has now been greatly curtailed by its
relative scarcity and high cost. Owing to its use in the steel
and copper industries, magnesite is an important though a minor
war commodity, and the need for it in these industries is so
great that its lack has at times been viewed with serious ap-
prehension.
The most important development of the year 1916 was the
opening in eastern Washington of large deposits of a coarsely
crystalline magnesite that is like marble or dolomite in texture
but is essentially magnesite in composition. Early in 1917
this material was being shipped at the rate of several hundred
tons a day, and calcining furnaces were in course of erection
to prepare magnesia for use in making refractory material and,
it is said, also for use in cement mixtures. Coming at a time
when the sources of supplies abroad are cut off, the discovery
of these deposits appears to be most fortunate. The deposits
are large and it appears that they will afford a supply of uni-
form character by relatively cheap methods of mining. It is,
perhaps, too soon to say just how well the material is suited
for refractory or other uses, but the present indications are
that it is proving to be very satisfactory.
The crude magnesite produced and sold or treated in the
United States in 1916 amounted to 154,974 short tons, valued
at $1,393,693, as compared with 30,499 tons, valued at $274,491.
in 1915. In 1916 California produced 154,259 tons, valued at
$1,388,331, and Washington 715 tons, valued at $5,362.
Mineral Springs of Alaska. G. A. Waring. With a Chapter
on the Chemical Character of Some Surface Waters of Alaska
by R. B. Dole and A. A. Chambers. Water Supply Paper
418. 109 pp. Paper, 25 cents. This short report brings
together the available analyses of Alaskan surface waters in
order that they may serve as a nucleus for amplifying the rather
meager knowledge now at hand regarding the chemical composi-
tion of streams in a subpolar region.
Annual Report of the Director. G. O. Smith. 176 pp.
This is tin thirty-eighth annual report and covers the fiscal
year ending June 30, 1917. A brief review of the important
activities of tin- service is given, liui principally the report deals
with administrative drlails.
Anticlines in the Southern Part of the Big Horn Basin, Wy-
oming: A Preliminary Report on the Occurrence of Oil. D. F.
HEWBTT and C. T. LupTon. Bulletin 656. 188 pp.
Oil and Gas Possibilities of the Hatchetigbee Anticline,
Alabama. <» B. Hopkins. Bulletin 661-H, from Contribu-
tion i" Economic Geology, 1917. Part 2. 33 pp Published
December 1 t, 1917. "The object of the present work is to show
more in detail the location and extent of this anticline, to point
248
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. j
out in a general way the areas that are most deserving of tests
with the drill, and to give those interested in exploratory drill-
ing for oil and gas information regarding the geology of the area,
the character of this fold, and the occurrence and depth of
possible productive oil sands."
COMMERCE REPORTS— JANUARY, I0l8
' South China provinces, which years ago had ceased to culti-
vate indigo, are now raising more than enough for their own
needs. (Pp. 3 and 197)
New large plants are to be erected in Norway for the produc-
tion of carbide, cement and steel, chrome leather, and super-
phosphate. (Pp. 10 and 36)
All the tin, copper, zinc and nickel ores smelted in Swansea,
Wales, are imported, the only mineral product of Swansea being
coal. The British government has subsidized the importation
of zinc concentrates from Australia. (P. 38)
Mineral products of South Africa include diamonds, asbestos,
coal and ores of copper, tin, gold, silver, chromium, iron and
tungsten. (P. 51)
A company has been organized in Sweden for the utilization
of the enormous peat deposits by the Wielandt process of dis-
tillation, by which a coke is produced which is excellent for do-
mestic use, as well as for electric iron smelting. By-products
include ammonium-sulfate, wood alcohol, acetic acid, tar, motor
fuels, lubricating oils, creosote, hard and soft paraffin and pitch.
(P. 65)
Coal veins are to be worked in Sweden, which are too thin to
pay in normal times. As the coal ashes contain about 4.4 lbs.
vanadium per ton of coal, it is hoped to recover this vanadium
for steel production. (P. 66)
Cultivation of Ceara rubber in East Africa is increasing.
The "ceara" plant, unlike the "Hevea," can be tapped only
for five or six years. The rubber is coagulated by acid and
is shipped without washing. The rubber is valuable, though
inferior to Para. (P. 68)
New industrial enterprises in Sweden include the recovery
of waste fats for soaps, etc., electrolytic production of aluminum,
and the manufacture of dyestuffs on a large scale. (P. 87)
The capital stock of all the large German dye companies
has been greatly increased, in order to provide capital for the
enlargement of the nitrogen plant of the Badische Anilin and
Soda Fabrik. (P. 88)
The orange-oil industry of Jamaica has increased greatly in
recent years. The oil is extracted by hand, by a simple de-
vice for pricking the oil cells of the rinds. The oranges are then
used as stock food. (Pp. 90-4)
The Italian government has taken over all stocks of alcohol
and of raw materials such as molasses, damaged cereals, refuse
figs, etc. (P. 108)
In Italy, miners' safety lamps, chiefly portable electric, are
required in the sulfur mines, on account of accumulations of
hydrogen sulfide. Numerous cases of poisoning by hydrogen
sulfide occur. (P. 133)
A large white lead factory has been erected in Australia to
use the stack process. A basic sulfate white lead plant is also
in operation. (P. 151)
Practically all the musk of commerce, used so extensively
as a basis of perfumes, is obtained from Tibet from the ab-
dominal sac of the male musk deer. Among efforts to synthesize
musk, that of Baur was most nearly successful in imitating the
odor, although his compound, produced from benzene and a
tertian.' butyl alcohol, is entirely different in composition from
true musk. (Pp. 156-8)
The manufacture and sale of oleomargarine is now permitted
in Canada. (P. 179)
Pig iron is now being produced from iron sands of New Zea-
land. (P. 184)
Essential oils produced in large quantity in Spain are spike,
rosemary, thyme, fennel, sage, juniper, pennyroyal, and geranium
rose. There are several large steam distilleries, as well as hun-
dreds of small producers. The best grades of oil are refined
by vacuum distillation. (P. 189)
Increased cultivation of castor beans in Trinidad is urged to
meet the greatly increased demands for use as airplane motor
lubricant. (P. 248)
In London, grease and oil are being removed from parts of
motor busses, trunks, etc., by means of hot 3 per cent caustic-
soda, instead of by kerosene as formerly. Oil so recovered can
be again used as motor oil. Grease and oil recovered from waste,
rags, etc., is used as fuel in Diesel engines. (P. 264)
The National Institute of Industrial Chemistry, at Monte-
video, Uruguay, is now successfully operating a factory for the
manufacture of a large number of chemicals. (P. 358)
The total aggregates of rubber plantations in 1 916 was about
2,000,000. Even with maximum anticipated production, a
shortage of rubber is expected within a few years. (P. 377)
Molybdenum ore is now being shipped from South China to
Canada and the United States. (P. 390)
Special Supplements Issued in January
Portugal — 116
Venezu
Ja — 48a
Malta— 20a
British Inc
British West Indi
a— 226
China-
-52A.i
Canada — 23 d
French West Indi
ss— 28a
Dutch East Indies — 53a
St. Pierre Miqielson — 37a
Japan —
-30C
Braril — 406
Australia —
Colombia — 426
British
South Africa — 666
Paraguay— 45a
British West India — 67a
Uruguay — 476
Tunis — 79a
Statistics
5p Exports
TO TBB UNITBD STATES
Trinidad — Sup. 226
Portugal-
-Sup. 116
Corundum
Balata
Antimony
Creosote oil
Mangrove bark
Beeswax
Sodium cyanide
Copra
Ergot
Leather
Divi-divi
Glycerin
Paper stocks
Gold
Gum copa
Venezuela — Sup 48*
Hides
Tartar
Balata
Logwood
Hides
Chicle
Asphalt
Rubber
Copaiba
Petroleum
Manganese
ore
Copper ore
Qubbkc — Sup 23d
Albumen
Mercury'
Sulfur ore
Divi-divi
Hides
Aluminum
Cork
Rubber
Asbestos
Sugar
Wood alcohol
Colombia-
-Sup. 476
British India — Sup.
Ammonium sulfate
Balsam
506
Bone black
Divi-divi
Nux vomica
Calcium carbide
Dyewoods
Senna
Calomel
Gold
Indigo
Turmeric
Creosote
Hides
Formaldehyde
Ipecac
Hides
Chloride of lime
Indigo
Lemon grass oil
Magnesite
Platinum
Coconut oil
Soda ash
Rubber
Castor oil seeds
Sodium cyanide
Silver
Copra
Rubber
Toluot
Sugar
Chrome ore
Mangrove
extract
Copper ore
Explosives
Burma — Sup. 50r
China — Sue S7h
Hides
Grease
Iron and steel
Antimony
Paraffin
Cutch
Leather
Albumen
Teak
Barite
Cantharide
Rubber
Dolomite
Camphor
Lac
Paper stock
Aniline dyes
Japan — Sup 55f
Graphite
Indigo
Antimony ore
Sulfur ore
Galls
Bronze powder
Wood pulp
Licorice
Alum
Zinc ore
Musk
Glycerine
Brazil— Sup. 406
Rhubarb
Gum camphor
Castor oil
Benzoate of soda
Indigo
Balsam
Turmeric
Menthol
Copaiba
Gold
Sulfur
Cream of tartar
Hides
Vegetable warn
Glycerine
Pi*: iron
Copper
Cyanide
Bean oil
Crucibles
Ipecac
Cottonseed oil
Gold
Potash
Rape seed
oU
Gold leaf
Hides
Peanut oil
Hides
Manganese ore
Soya bean
oil
Iridium
Platinum
Wood oil
Manganese ore
Wolframite
Linseed
Matches
Mica
Vegetable
tallow
Vegetable oils
Monatite
Zinc ore
Fish oil
Rubber
Graphite
Sugar
308
Agar-agar
Beeswax
Acids
Tungsten ore
Carnauba wax
Ammoniutr
sulfate
Zinc dust
Mar., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
BOOK RLVILW5
The Distillation of Resins. By Victor Schweizer. Trans-
lated by H. B. Stocks, F.I.C., F.C.S. Second English Edition.
Scott, Greenwood & Son. Price, $2.52.
The true title for this book would better read: "Elementary
Treatise on the Distillation of Rosin, Manufacture of Illumina-
ting Gas from Rosin, Rosin Oils, Lubricants, Resin Soaps and
Resinates, Varnishes, Lamp Blacks and Pigments, Printers'
Inks, Typewriter Ribbons and Carbon Papers." There are
•one or more chapters on each subject, and necessarily, each
chapter is very limited.
The title page shows the book to be the second English edi-
tion, and one might readily draw the conclusion that a great
deal of material and many cuts had been retained from the former
edition, which must have been published many years ago, as
much of the material contained in the book may be regarded as
almost obsolete. The book contains a short, concise description
■of the oleo and gum resins.
Another chapter is devoted to colophony and its properties.
Chapter 5 is devoted to the manufacture of illuminating gas
from resins, an obsolete and expensive method for the manu-
facture of illuminating gas.
The apparatus described for the manufacture of rosin oil is
crude and is more nearly comparable with what one might ex-
pect to put up for small laboratory experimental operations,
rather than for large manufacturing work.
On page 88, in speaking of the lime to be used in the manu-
facture of "Patent Lubricants," the author makes the statement:
"The lime used must be pure. This is easily tested by slaking
it. Pure lime rapidly absorbs large quantities of water, soon
breaks up, evolves much heat and forms a very soft powder."
On page 89, in speaking of "Patent Lubricants," the author
says: "Fillings are also added in many cases to cheapen the
product or to increase its consistency, but these are inactive
bodies having no lubricating power of their own."
Chapter 10, on the manufacture of resin soaps and resinates,
is crude in the extreme, and gives only an elementary or experi-
mental idea of the true processes.
In describing the operations used for burning oils in lampblack
chambers, the author makes the following statement on page 131 :
"Occasionally a sudden break in the satisfactory working may
occur * * * * This is always to be traced to a quick change in
the barometric pressure, which can be proved by consulting a
barometer at intervals."
One might make numerous other criticisms.
For instance, the illustrations on pages 38 and 181, Figs. 10
and 64, are identical in every respect, and each one covers about
a half page.
It is to be doubted whether any modern ink manufacturer
would be successful by using the methods or formulas recom-
mended in this book. The same would apply to typewriter
ribbons. The following statement appears on page 195, in speak-
ing of the material used: "Choose a thin but closely woven ma-
terial of which both warp and weft must be silk (cotton tape is,
however, usually employed)."
A further statement that may be questioned appears at the
I, bottom of the same page. It reads: "As, moreover, most coal-
| tar dyes are soluble in glycerine, which must always enter into
the composition of a typewriter ink, the maker has a fairly free
hand in his choice of a dye." Several points of this statement
could be sharply questioned.
The reader of this book may profit in that he will gain a very
elementary, although in some respects certainly an incorrect,
knowledge of the manufacture of a large number of things, about
each one of which a book several times the size of this volume
could be written. . _ _
A. B. Davis
The Chemistry of Farm Practice. By T. E. KeiTT, Chemist of
South Carolina Experiment Station, and Professor of Soils,
Clemson Agricultural College, S. C. John Wiley and Sons,
Inc., New York, 1917. xii + 253 pp. 81 figures. Price,
Cloth, $1.25.
This book furnishes the knowledge of the fundamentals of
chemistry required for intelligent agriculture and applies this
knowledge to the art of agriculture and to the problems of the
agriculturist. Its scope has not been limited to the study of
soils, fertilizers and manures, although these subjects are given
careful consideration. It also discusses in as non-technical
language as possible such subjects as feeds, nutrition, sanitary
water, boiler water, and insecticides, subjects in which not only
the farmer, but the suburban resident is interested.
As a textbook, it should prove useful in high schools, in
farming communities and in' short courses in agricultural col-
leges where instruction in the chemistry of farm practice should
be given. As in such cases it would not be possible to give the
usual formal course in general chemistry, followed by technical
agricultural chemistry, the essential principles of chemistry
have been given in the first few chapters, a combined textbook
being thus provided.
There are some inaccuracies in statement incidental to a first
edition, for example:
Page 3. "An atom does not remain free or uncombined."
Page 16. "Two molecules of hydrogen chloride are expressed
2HCI **** A molecule of sulfuric acid is H2SO4."
Page 26. "The stronger bases attack metals such as aluminum
and zinc, producing thereby water as one of the products of the
reaction."
Page 27. "What is left of the acid after its hydrogen is re-
moved is the acid radical."
Page 27. "There are four classes of salts * * * * (1) Nor-
mal Salts (2) Acid Salts * * ♦ * * (3) Basic
Salts * * * * (4) Neutral Salts."
Page 30. "Persulfuric acid, HzSiOs."
Page 30. "H2SO2, hyposulfurous acid."
Page 30. "Sodium hyposulfite, NazSOa."
Page 36. "The three compounds of carbon *********
are carbon dioxide, carbonates and the carbohydrates."
The author has done his work well and the book will serve a
useful purpose.
W. A. Withers
An Introduction to Theoretical and Applied Colloid Chemistry.
By Dr. Wolfang Ostwald. Authorized translation by Dr.
Martin H. Fischer, Eichberg Professor in the University of
Cincinnati. John Wiley & Sons, Inc., New York, 1917-
Price, $2.50.
This book contains a series of lectures delivered on this side
of the ocean during the winter of 1913-1914 and attempts "to
give a general survey of modern colloid chemistry as a pure
and as an applied science and in a form readily intelligible to the
general reader," making "its first appeal to such readers as have
heard little or nothing of colloid chemistry."
first lecture— Fundamental Properties of the Colloid
State. Colloids as Examples of Dispersed Systems. Methods
of Preparing Colloid Solutions.
second lecture — Classification of the Colloids. The
Physico-Chemical Properties of the Colloids and Their De-
pendence upon the Degree of Dispersion.
third lecture — The Change in State of Colloids.
fourth lecture — Some Scientific Applications of Colloid
Chemistry.
fifth lecture — Some Technical Applications of Colloid
Chemistry.
THE JOURS M. OF INDUSTRIAL ASD ENGINEERING CHEMISTRY Vol. 10, No. 3
The author adheres to the lecture form, which may make the
book seem a little weak to those who attended the lectures
themselves, actually saw the experiments and felt the influence
of the lecturer's personality. The broad field is, however, ably
covered by well chosen typical examples and experiments and
the book will fulfill its purpose as a "propaganda sheet for
colloid chemistry."
The translation is excellently done.
REMARKS OF THE ADVOCATUS DIABOLI
Throughout the book the author maintains his own views on
most points, without presenting divergent views adequately
or at all. His claim that a book of this type is new, is rather
naive. He does not always apportion credit or priority properly,
but seems to be more familiar with the work of contributors
to the Kolloid Zeitschrift (of which he is editor) than with the
work of certain authors, published in the English language.
Tn an addendum to the preface the author says: "If this volume,
born of two continents, is thus sent into the world from the
trench and from the midst of artillery- fire, I hope that I shall not
therefore be charged with cheap coquetry. Convinced as I
am of the justice of my Fatherland and its power to carry matters
to a victorious conclusion, equally convinced am I that the bond
of science which is common to all people can never be destroyed,
and certainly not by war; and that it is this bond which must
finally serve to bind together and so to protect all mankind
from such experiences as the present."
Just before this he says: "War is a temporary and pathological
phenomenon appearing in the organism of mankind; it is a
means to an end; and there exist treasures, like science and art,
unshatterable and everlasting."
And just to think that this was all written from Champagne
in March 191 5, when the very artillery he speaks of was wreck-
ing the Cathedral at Rheims!
Jerome Alexander
The Chemistry of Colloids. By Prof. Richard ZsiGMONDY.
Translated by Ellwood B. Spear, Associate Professor of
Inorganic Chemistry, Massachusetts Institute of Technology.
John Wiley & Sons, Inc., New York, 1917. Price, 83.00.
This is an authorized translation of Prof. Zsigmondy's
"Kolloidchemie-ein Lehrbuch" published in 1912, with which
arc included several chapters by the translator, entitled "In-
dustrial Colloidal Chemistry," and a chapter on "Colloids in
Sanitation" by Prof. John F. Norton.
In the preface to the German edition mot included in the
translation) the author gives the purpose and scope of his book,
which may be briefly summarized as follows:
The rapid development of colloid chemistry has brought to
light a great many isolated facts demanding coordinations and
generalizations which, unless care be exercised, may actually do
violence to the facts themselves. The author, therefore, rather
than aiming at completeness, takes up with great thoroughness
earches and facts of general significance, especially those
bearing on electrical properties and on the theory of peptization.
The general section includes a terse but comprehensive in-
troduction, a chapter on Classification ably upholding Zsig-
mondj 's views, a chapter on the Properties of Colloids, and one
on Theory (especially of peptization). In the special section
the inorganic colloids are treated with much greater complete-
ness than are the organic colloids. The translation is in the
main well and conscientiously dour, and the book will certainly
be welcome and useful to everyone interested in colloid chem-
istry.
REMARKS oF Tin: ADVOCATUS Dl
Certain errors in the German original are unfortunately
perpetuated by the translator; thus S/illard instead of S/ilard,
Lysalbinnic instead of Lysalbinic; on page t -.odium st<
spoken of as being a crystalloid in alkalim solution, whereas
alcoholic solution is meant and is actually referred to in the
section on soaps, p. 188.
There are quite a few misprints and some rather serious
and inexcusable errors in translation: Zsigmondy's own "star
dialyzer" is illustrated on p. 35 with the caption "Stern's
dialyzer" and is so referred to later on, on p. 136, which is quite
surprising, as Zsigmondy himself read the translation; on p. 81,
electrolytic solutions instead of solutions of electrolytes; on p.
115, Fig. 19, emulsion instead of emulsin; p. 143, Fig. 23, letter-
ing in text at variance with that in diagram (01 omitted from
diagram < ; p. i.si. benzopurple instead of benzopurpurin; p. 162,
reference to Graham omitted, others therefore mismarked, etc.
Again while using the preferential spelling gelatin, the trans-
lator inconsistently uses the less desirable pepsine, sulfide,
chlorine, cathion, etc., instead of pepsin, sulfid, chlorin, cation,
etc. Although Zsigmondy's "Zur Erkenntnis der Kolloide" is
very frequently referred to and in fact largely contributed to
the make-up of this book, no mention is made of the English
translation, although this was published by the same publishers
under the title "Colloids and the Ultramicroscope."
In conclusion, the added chapters are hardly up to the high
standard of the German original.
Jerome Alexander
Allen's Commercial Organic Analysis. Vol. IX. Fourth Edi-
tion. P. Blakiston's Son & Co., Philadelphia, Pa. Price,
S5.00, net.
The new edition of this valuable treatise has just been re-
ceived and brings up to date the articles appearing in the pre-
ceding eight volumes Not only have the articles by original
writers been revised, but materia! appears from the pens of eleven
new collaborators. The subject matter covers a wide range
of organic compounds and products, with concise methods
for the detection and estimation of impurities and adultera-
tions. In addition, this volume contains a complete index
of all volumes of the set. This book is a timely addition to our
chemical literature and should be in the library of all those
interested in the subjects treated.
Allex Rogers
Standard Methods of Chemical Analysis. A Manual of Ana-
lytical Methods and General Reference for the Analytical
Chemist and the Advanced Student. Edited by Wil-
fred W. Scott, Research Chemist. General Chemical Com-
pany xxxi + 898 pp. Illustrated. Second Edition, Re-
vised 1">. Van Xostrand Co.. New York, 1917. Price,
$6 o,..
The first edition of this l>c>ok was published early in 1017
and was reviewed in This Journal, 9 (1917), 917. A few-
changes have been made in the text, and new tables added.
Those faults to which attention was called in the former review-
have been corrected, for the most part, but the Editor has not
had opportunity to read over the entire book and correct certain
very obvious misprints These, however, do not seriously
affect the value of the book and it will doubtless continue to
have a good sale
W. T. Hall
Laboratory Guide of Industrial Chemistry. By Allex Rogers.
Second Edition. D. Van Xostrand Co., New York. Price,
i, net.
The first edition of this manual was reviewed in This Journal.
1 1 100.) , so The new edition has been well revised. 54
pages of ne« material added, ami the price increased from
1 o $2 . OO.
The book Is. a- .1 whole, thoroughly practical and teachable.
The chapters on Leather and Soap Manufacture are especially
\ aluable, a- would be expected bv anyone knowing of the author's
success in teaching these subjects at Pratt Institute.
Ralph H. McKee
Mar., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
251
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British Standard Specifications for Cast Iron Pipes and Special Castings
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Chemical Constitution of the Proteins. R. H. A. Plimmer. New Ed.
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Chemical Physiology: Directions for a Practical Course. W. Cramer.
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Chemistry: Elements de chimie. Metalloides. F. G. M. Classe. 3rd
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Chemistry: Handbook of Chemistry and Physics. Cleveland Rubber
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Commercial Algebra. G. Wentworth. 12mo. 266 pp. Price, $1.12.
Ginn & Co., Boston.
Cotton and Other Vegetable Fibers. Ernest Goulding. 8vo. 241 pp.
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Engineering: American Stationary Engineering. W. E. Crane. 12mo.
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MARKET REPORT-FEBRUARY, 19 IS
WHOLESALE PRICES PREVAILING IN THE NEW YORE MARKET ON FEB. 15
INORGANIC CHEMICALS
Acetate of Lime 100 Lbs.
Alum, ammonia, lamp 100 Lbs.
Aluminum Sulfate, high-grade Lb.
Ammonium Carbonate, domestic Lb.
Ammonium Chloride, white Lb.
Aqua Ammonia. 26°. drums Lb.
Arsenic, white Lb.
Barium Chloride Ton
Barium Nitrate Lb.
Bary tes, prime white, foreign Ton
Bleaching Powder. 35 per cent 100 Lbs.
Blue Vitriol Lb.
Borax, crystals, in bags Lb.
Boric Acid, powdered crystals Lb.
Brimstone, crude, domestic Long Ton
Bromine, technical, bulk Lb.
Calcium Chloride, lump. 70 to 75% fused Ton
Caustic Soda. 76 per cent 100 Lbs.
Chalk, light precipitated Lb.
China Clay, imported Ton
Feldspar Ton
Fuller's Earth, foreign oowdered Ton
Fuller's Earth, domestic Ton
Glauber's Salt, in bbls. . 100 Lbs.
Green Vitriol, bulk 100 Lbs.
Hydrochloric Acid, commercial. 20 B Lb.
Iodine, resublimed Lb.
Lead Acetate, white crystals Lb.
Lead Nitrate Lb
Litharge. American Lb
Lithium Carbonate Lb
Magnesium Carbonate. U. S. P Lb.
Maguesite. "Calcined" Too
Nitric Acid. 40« Lb.
Nitric Acid. 42° Lb.
Phosphoric Add. 48/50% Lb.
Phosphorus, yellow Lb.
Plaster of Paris Bbt
Potassium Bichromate, casks Lb.
Potassium Bromide, granular Lb.
Potassium Carbonate, calcined. 80 C 85% Lb.
Potassium Chlorate, crystals, spot Lb.
Potassium Cyanide, bulk, 98-99 per cent Lb.
Potassium Hydroxide. 88 © 92% Lb.
Potassium Iodide, bulk Lb.
Potassium Nitrate Lb.
Potassium Permanganate, bulk Lb.
Quicksilver, flask 75 Lbs
Red Lead. American, dry Lb.
Salt Cake, glass makers' Ton
Silver Nitrate Or.
Soapstone, in bags Ton
Soda Ash. 58%, In bags 100 Lbs.
Sodium Acetate Lb.
Sodium Bicarbonate, domestic 100 Lbs.
Sodium Bichromate Lb.
Sodium Chlorate Lb.
Sodium Cyanide Lb.
Sodium Fluoride, commercial Lb.
Sodium Hyposul6te 100 Lbs.
Sodium Nitrate. 95 per cent, spot 100 Lbs.
Sodium Silicate, liquid. 40* Be 100 Lbs.
Sodium Sulfide .60%. fused, in bbls Lb.
Sodium Bisulfite, powdered Lb.
Strontium Nitrate Lb.
Sulfur, flowers, sublimed 100 Lbs.
Sulfur, roll 100 Lbs.
Sulfuric Acid, chamber 66 ° Be1 Ton
Sulfuric Acid, oleum (fuming) Ton
Talc. American white Ton
Terra Alba. American, No. I 100 Lbs.
Tin Bichloride. 50" Lb.
Tin Oxide.
Lb.
White Lead, American, dry Lb.
Zinc Carbonate Lb.
Zinc Chloride, commercial Lb
Zinc Oxide. American process XX Lb.
0
4.00
2»/«
11
15' . ©
19'A 0
I6> ,4 ©
65.00 ©
9'/i 0
40.00 ©
2.50 ©
9 ©
7>/i 0
13'A 0
27.50
5.50
OEOANIC CHEMICALS
Acetanilid. C. P.. In bbls Lb.
Acetic Acid. 56 ,>rc cent, in bbls Lb.
Acetic Acid, glacial, 99>/i%. in carboys Lb
Acetone, drums Lb.
Alcohol, denatured. 1 80 proof Gal.
20.00
1.50
1.15
45.00
3.00
9'/s
30.00
15.00
1
30.00
3.00
1.25
1.70
2.50
1.35 © 1.36
83' 1
3.75
4.00
125.00
10.00
2.90
45.00
75.00
15.00
4.10
135.00
lO'/i
35.00
56>/j
12.50
2.95
17
3.00
25 Vi
3.00
4.60
1.35
50.00
80.00
18.00
9'/.
IO'/i
Alcohol, sugar cane, 188 proof Gal
Alcohol, wood. 95 per cent, refined Gal.
Amyl Acetate Gal.
Aniline Oil. drums extra Lb.
Benzoic Acid, ex-toluol Lb.
Benzol, pure Gal.
Camphor, refined in bulk, bbls Lb.
Carbolic Acid. U. S. P.. crystals, drums Lb.
Carbon Bisulfide Lb.
Carbon Tetrachloride, drums. 100 gals Lb.
Chloroform Lb.
Citric Acid, domestic, crystals Lb.
Creosote, beech wood Lb
Cresol. U. S. t Lb.
Dextrine, corn (carloads, bags) Lb
Dextrine, imported potato Lb.
Ether, U. S. P. 1900 Lb.
Formaldehyde. 40 per cent Lb.
Glycerine, dynamite, drums included Lb.
Oxalic Aud in casks Lb.
Pyrogallic Acid, resublimed. bulk Lb.
Salicylic Acid, U. S. P Lb.
Starch, cassava Lb.
Starch, corn (carloads, bags) pearl 100 Lbs.
Starch, potato. Japanese Lb.
Starch, rice Lb.
Starch, sago flour Lb.
Starch, wheat Lb.
Tannic Acid, commercial Lb.
Tartaric Acid, crystals Lb.
4.85
C
5.00
1.35
a
1.37
5.10
a
5.25
26
a
28
5.50
a
5 75
35
a
40
85
a
86
54
a
57
7Vi @
8
15'/
a
16
63
a
65
75
a
78
1.90
a
2 00
18
a
20
7'
©
8>
18
'9
20
3.15 a
3.25
1.05 a
1.15
6.30 ©
6.45
IO'/i a
11
8 ©
10
6'/i a
7'
5 0
6
55 a
60
75 0
77
OIL8, WAXES, ETC.
Beeswax, pure, white Lb.
Black Mineral Oil, 29 gravity Gal.
Castor Oil. No. 3 Lb.
Ceresin, yellow Lb.
Corn Oil. crude 100 Lbs.
Cottonseed Oil. crude, f o. b. m<U Lb.
Cottonseed Oil. p. s. y 100 Lbs.
Menhaden Oil. crude (southern) Gal.
Neat's-foot Oil. 20" Gal.
Paraffin, crude. 118 to 120 m. p Lb.
Paraffin Oil, high viscosity Gal.
Rosin. "F" Grade, 280 lbs BbL
Rosin Oil. first run Gal.
Shellac. T. N Lb.
Spermaceti, cake Lb.
Sperm Oil. bleached winter. 38* Gal.
Spindle OD. No 200 Gal.
Stearic Acid, double-pressed Lb.
Tallow, acidless Gal.
Tar Oil. distilled Gal.
Turpentine, spirits of Gal.
METALS
No. 1. ingots Lb.
Antimony, ordinary Lb.
Bismuth. NY Lb.
Copper, electrolytic Lb.
Copper, lake Lb.
Lead. N Y Lb.
Nickel, electrolytic Lb.
Platinum. re6ned soft Ox.
Silver Ox.
Tin. Straits Lb.
Tungsten (WOi) Per Unit
Zinc. NY Lb.
FERTILIZER MATERIALS
Ammonium Sulfate 100 Lbs.
Blood, dried, f. o.b Chicago Unit
Bone. 3 and 50. ground, raw Ton
Calcium Cyanamid Unit of Ammonia
Calcium Nitrate. Norwegian 100 Lbs.
Castor Meal Unit
Fish Scrap, domestic, dried, f. o. b. works Unit
Phosphate, acid. 1 6 per cent Ton
Phosphate rock. f. o. b. mine: Ton
Floi ida land pebble. 68 per cent Ton
Tennessee. 78-80 per cent Ton
Potassium "muriate." basis 80 per cent Ton
Pyrites, furnace site, imported Unit
Tankage, high-grade, f. o. b. Chicago Unit
18.65
©
17V
0
20.25
—
0
2.87
0
8
0
38
o
27", <
1.58
28'/.
13»
'l 0
i." •
3.30
0 3
35
23'/. 0
—
nominal
6
. 0
7
55
0
108.00
56
86"
• @
nominal
90
J0.00
a 26.00
8
a
7.40 a 7.50
6.50 © 6.55
30.00 0 32.00
nominal
nomin.U
18.00
nominal
3.25 0 3.50
5.50 a 600
345.00 © 330.00
nominal
6.40 * 7.10
Tfte Journal of Industrial
and Engineering Ghemistry
Published by THE AMERICAN CHEMICAL SOCIETY
AT BASTON. PA.
Volume X
APRIL 1, 1918
No. 4
Editor: CHARLES H. HERTY
Assistant Editor: Grace MacLeod
Advertising Manager: G. W. Nott
ADVISORY BOARD
H. E. Barnard, H. K. Benson, F. K. Cameron, B. C. Hesse, A. D. Little, A. V. H. Mory, M. C. Whitaker
Published monthly. Subscription price to non-members of the American Chemical Society, $6.00 yearly; single copy, 60 cents
Price per single copy to American Chemical Society members, 50 cents. Foreign postage, seventy-five cents, Canada, Cuba and Mexico excepted
Entered as Second-class Matter December 19, 1908, at the Post-OfBce at Easton, Pa., under the Act of March 3, 1879
All communications should be sent to The Journal of Industrial and Engineering Chemistry.
Telephone: Vanderbilt 1930 35 East 41st Street. New York City
Subscriptions and claims for lost copies should be referred to Charles L. Parsons, Box 505, Washington, D. C.
ESCHENBACH PRINTINO COMPANY, EaSTON, Pa.
TABLE OF
Editorials :
The Chemistry Rainbow 254
The Parting of the Ways ■ 254
What's in a Name? 255
Camp Followers 255
Organization within the Dyestufi Industry 256
Wood Waste 256
Important Notice 256
Product Patents 257
Original Papers:
Sulfite Turpentine. A. W. Schorger 258
The Effect of Incomplete Distillation on the Yield of
Products in the Destructive Distillation of Birch
R. C. Palmer 260
The Influence of Moisture on the Yield of Products
in the Destructive Distillation of Hardwood. R.
C. Palmer and H. Cloukey 262
The Effect of Catalyzers on the Yield of Products in the
Destructive Distillation of Hardwoods. R. C.
Palmer 264
Some Experiments on the Pulping of Extracted Yellow
Pine Chips by the Sulfate Process. Otto Kress
and Clinton K. Textor 268
The Production of Nitric Acid from Nitrogen Oxides.
Guy B. Taylor, Julian H. Capps and A. S. Coolidge. 270
Influence of Time of Harvest, Drying and Freezing of
Spearmint upon the Yield and Odorous Constituents
of the Oil. Frank Rabak 275
Carbonation Studies. II — The Carbonation of Dis-
tilled Water. Harrison E. Patten and Gerald H.
Mains 279
Examination of American-Made Acetylsalicylic Acid.
Paul Nicholas Leech 288
The Determination
Potassium Iodate.
of Arsenic in Insecticides
George S. Jamieson
by
Laboratory and Plant:
Notes on Sodium Cyanide.
W. J. Sharwood 292
A Comparison of the Proximate and Mineral Analysis of
Desiccated Skim Milk with Normal Cows' Milk.
Bverhart P. Harding and Hugo Ringstrom 295
An Improved Automatic Pipette-Washing Device.
Aubrey Vail Fuller 297
CONTENTS
Addresses:
Methods of Gas Warfare. S. J. M. Auld 297
The Consumption and Cost of Economic Poisons in
California in 1916. George P. Gray 301
The Debt of Preventive Medicine to Chemistry.
George W. Goler 303
William H. Nichols Medal Award:
Introductory Address. Charles H. Herty 305
Presentation Address. William H. Nichols 305
Acceptance of Medal. Treat B. Johnson 306
The Development of Pyrimidine Chemistry — Medal
Address. Treat B. Johnson 306
Message from Prof. Bogert 312
Current Industrial News:
The Ekenberg Peat Process; Norwegian Iron Industry;
Magnetic Separations and the Rarer Metals; New
Source of Alcohol; New Rust Prevention; Transvaal
Deposits of Chrome Ore and Magnesite; New Oil
Nuts; Catalytical Bleaching of Oils; Gas-Heated
Isothermal Room; Magneto Ignition; Detachable
Engines for Ships; Synthetic Materials; Insulating
Material; Laminated Belting; British Board of Trade. 312
Scientific Societies:
Tentative Standard Methods for the Sampling and
Analysis of Commercial Fats and Oils 315
Saving Fats from Garbage 320
American Institute of Mining Engineers 321
American Electrochemical Society 32 I
Calendar of Meetings 32]
Notes and Correspondence :
Revised Statement from the Chemical Service Section;
Preparedness Census; Government Control of Pla1
inum: Platinum Resolution by the Argentine Chem-
ical Society; Licensing of Fertilizer Industry Ordered;
Researeli Information Committee; DyestufFi
snciatiiui ; Fcioil in Wai Tinit ; Meeting War Condi-
tions at Rensselaei Polytechnic Institute 321
Washington Letter 325
Unveiling 01 mi: Portrait of Herman Frascb 326
Personals 327
1. Notes 329
Government Publications 331
NEW Publications
Market Report 334
2 54
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. Xo. 4
EDITORIALS
THE CHEMISTRY RAINBOW
After all, the hammer is a strictly constructive tool
if used with constructive intent. It has been fre-
quently used in these columns, but always with the
hope of aiding to some extent the erection of that
great structure of national equipment of men and re-
sources which constitutes the contribution due from
this mighty nation to the welfare of the human race
in the present world conflict. It is helpful, however,
to get away from the sound of the hammer occa-
sionally and to note what progress has been made—
not for the sake of indolent satisfaction, but to gain
Strength and soundness of judgment for more vigorous
blows. For this reason there are recorded here,
without regard to sequence, the following notes:
1 — The Chemical Service Section of the Xational
Army has reached France and is now located in its
research laboratory, a remodeled factory building
placed at its disposal by the French Government.
Major Hamor writes that all are well.
2 — Platinum has been commandeered by the Govern-
ment. The campaign begun at Kansas City a year
ago is ended. The metal can now hold up its head
with justifiable pride, because of its functional meta-
morphosis from vainglorious adornment of the nouveau
riche to the more appropriate r61e of catalyst in acid
manufacture. What about that scrap platinum, odds
and ends, lying about your laboratories? Every little
bit helps.
3 — Toluol has been taken over and is being made
available in gradually increasing quantities. (This
is not one of the bright tints in the rainbow.)
4 — The recovery of spruce turpentine, a new in-
dustry, proceeds apace.
5 — Work is now in full swing on the compilation of
statistics for the census of chemical imports other
than dyestuffs. A publication is here assured which
has finally enlisted the hearty, sympathetic and
enthusiastic support of many departments of the
national government. The lines of its conception
and the thoroughness of execution of the work insure
a publication which will furnish the world a model
of its kind.
6 — Lieutenant Colonel Wm. H. Walker has been
promoted to a Colonelcy and, attached to the Ordnance
Department, is now at the head of one of the most
important undertakings of the Government. May his
"pep" never grow less!
7 — Professor M. T. Bogert has donned the khaki
and as Lieutenant Colonel will head the Chemical
Service Section of the Xational Army on this side.
8 — Practically all of the chemists in the National
Army have now been transferred from camp to the
laboratories of the Government or the industries,
where their highest service to the country can be
rendered.
9 — The membership of the American" Chemical
Society continues to grow so rapidly that Secretary
Parsons has within the past month ordered a further
increase in the issue of each of the journals.
10 — A new championship series is on! Talk about
running up big scores — the Delaware Works of the
General Chemical Company boasts in the March
number of The General Chemical Bulletin that in pro-
portion to the size of its executive and technical
staff it has a larger membership in the American
Chemical Society than any other plant. Reading
the tabulated score we notice that runs were made
by two superintendents, one assistant superintendent,
and four foremen, in addition to the chemists of the
staff. Some scoring machine that! On with the
game! Spring is here and baseball is in the air. Away
with the hammer! Let's try the bat awhile. We
hereby apply for the position of "official scorer" in
this new form of sport.
Already we have exceeded the number of primary
colors in our chemistry rainbow. What difference
does that make? Let the physicists revise their
listings of the tints. All together for America!
THE PARTING OF THE WAYS
The Chemists" Club of Xew York is an unique
institution. Nowhere else in the world have chemists
such an organization with such complete club house
accommodations. In addition to its resident member-
ship it carries on its roll a large number of non-resident
members. Visiting chemists have given up the hotel
habit and nightly tax its housing facilities to the limit.
Outside of Washington it is probably the greatest
center of activity in chemistry in this country to-
day.
For these reasons the Club cannot be considered a
purely local affair, but rather a national institution,
and being such it must measure up to the national
standard of straight-out Americanism. We are on
the threshold of nation-wide suffering and loss
such as this country has never before known.
The day of wrath is soon to come in our land, and
with the Trustees of the Club rests the responsibility
of setting our house in order in anticipation of that
day whose coming no human being can now pre-
vent.
It is natural that the Club should number among
its members many German chemists, for such have
constituted an important group among the working
chemists in America. With the exception of one
recent unfortunate undertaking the German element
in the Club has, for the most part, quietly absented
itself from the club building, thereby lessening the
chance of friction which might so easily develop in
these days. So unobtrusive, too. and so kindly has
been the attitude of those who still frequent the Club
Apr., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
that nothing but equally kindly personal feelings have
Fbeen engendered by such association. We are not
moved in this writing by any personal animus, but
do wish to emphasize the fact that men's emotions
are changing with the gradual lengthening of the
casualty lists, that, with the news, certain to come
in the near future, of Hun atrocities practised upon
American soldiers, feelings will be aroused which will
brook no companionship nor association with those
whose allegiance lies with that country whose ruthless
ambition has plunged the human race into a world
war.
Within the walls of the Club building there now
frequently gather chemists enlisted in our army, or
connected in a civilian capacity with the military
branch of the Government. No restraint should be
placed upon their intercourse by the presence of alien
enemies. In the rooms of the Club many important
committees meet. Should a watchful eye be needed
in an American club? In the library works of ref-
erence need to be consulted. Should this room be a
common meeting ground for Americans and Ger-
mans? Should any of its laboratory space be rented
to an alien enemy while there are American chem-
ists unable to secure quarters in its building because
of the limited number of rooms available for laboratory
purposes?
In forbidding the employment of German waiters
in the dining room the Trustees have taken one
highly desirable step, particularly in view of the
recent incident, narrated to us, of an American
chemist recognizing in the waiter of a Wil-
mington hotel dining-room his former German uni-
versity professor of chemistry. It is no time to take
chances: that is one of our outstanding national
failings, and again and again we pay the penalty.
The Trustees should make the Club an American
institution throughout. To do this would require
dropping from its membership list every alien enemy
and sympathizer, and dismissing from its service
any employee whose allegiance or heart-interest lies
with those with whom we are at war.
Why should the vote of an alien enemy be in any
degree determinative of the policies of the Club or the
personnel of its officers? Yet as members, even though
absenting themselves, this power is conferred in pro-
portion to their number.
If it be argued that the elimination of alien enemies
would not fully remedy the evil because of the possible
presence of naturalized citizens who masquerade be-
hind their naturalization papers, our only reply is —
hunt these down with every agency the country
furnishes and with all celerity forbid them the doors
of the Club.
Finally, if it be argued that this drastic action
would seriously impair the finances of the Club, we
would reply that the argument would admit of only
one interpretation, namely, that the Club had sold its
birthright. On the other hand should this policy
really prove a serious strain on the finances of the
Club, and this fact become known, we are confident
that there would be a rush of new non-resident mem-
bers from among loyal American chemists which would
tax the energies of the membership committee and
more than make good any deficiency in the Club's
finances.
We are at the parting of the ways. If the Chemists'
Club is an American institution — make it truly such.
WHAT'S IN A NAME ?
The answer to this question in so far as it applies
to acetylsalicylic acid (popularly known as aspirin)
is the difference between eighty-eight cents, the price
the druggist must pay for every one hundred tablets
of Bayer aspirin, and forty cents, the cost of an equally
pure American product. Naturally, this difference
in cost is passed on to the individual consumer.
That no scientific justification exists for this differ-
ence in cost is clearly shown in the contribution by Dr.
Paul Nicholas Leech, of the Chemical Laboratory of
the American Medical Association, page 288 of this
issue.
On the other hand, the excess profit fully warrants
the extensive and shrewdly-worded advertising cam-
paign now in progress, a campaign which must eventu-
ally fail, because in the first place, it is contrary to the
prevailing spirit of modern advertising, the motive of
which is constructive rather than destructive, and,
in the second place, it appeals merely to the temporary
ignorance of the public at large, and has no basis in
fact.
We have been informed that the Custodian of Alien
Enemy Property has taken charge of the stock interests
of alien enemies in the company conducting this prop-
aganda. Surely the Custodian will not care, even
in a trustee capacity, to continue as a participant in
a misleading campaign whose sole purpose is the per-
petuation of a monopoly hitherto enjoyed under full
patent protection.
CAMP FOLLOWERS
It was to be expected that along with the great
development of the chemical industries which has
characterized this war period the "camp follower"
would appear. The army of industrial chemists has
won victory upon victory. For the first time in our
history the details of the campaigns have been widely
heralded by the daily press; much publicity has been
given to large earnings. Popular interest has attached
to the doings of the chemist.
To take advantage of such a state of mind is the
normal activity of certain promoters who are ever
alert to fleece the unwary public whenever "a good
thing" appears. There is nothing novel in this situa-
tion. The oil industry has known its meaning, so
too the mining world has been particularly susceptible
to such influences. Stock companies have been
organized with enormous authorized capital, pro-
spectuses issued on fairy-like propositions and shares
offered to the public at ridiculously low figures. The
256
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 4
bait is usually so apparent that it would seem no one
would bite — and yet some always do. The losses are
pocketed, and shame and regret serve as cloaks to
conceal the rawness of the deal.
At present chemical industry is afflicted with a
transfer of such activities to its field. The mails are
being flooded with literature, even the daily papers
are yielding their advertising columns to the announce-
ment of get-rich-quick chemical processes whose im-
possibilities are too apparent ever to delude chemists.
There are those, however, to whom it does not occur to
turn to a chemist for advice before investing in a so-
called chemical enterprise.
Here is an opportunity for public service which the
chemist must embrace, a service of exposure due the
public and due the continued healthy growth of
chemical industry. We may have something more
specific to say on this matter in a later issue if. mean-
while, the duly constituted authorities have not
dispersed these money sharks, here dignified by the
term "camp followers."
ORGANIZATION WITHIN THE DYESTUFF INDUSTRY
Efforts made during the past two months to organize
the dyestuff industry developed the fact that two
distinct interests were involved, the manufacturers
and the dealers. At the preliminary meeting it was
evident that a strong desire existed among the manu-
facturers to confine the membership to this class alone,
but a compromise was effected whereby the dealers
were admitted to associate membership without
voting power. Thinking it over, the manufacturers
decided that this policy was not sound and
that the membership should be confined to manu-
facturers. The second meeting, held on March 6,
developed a most unusual situation, the dealers in-
sisting that they be included in the organization,
while the manufacturers said, "Nay, nay." Of course
the manufacturers' fight was won from the outset.
No one could compel them to be part of an organiza-
tion whose composition was not to their liking.
Unfortunately for the dealers the two main argu-
ments put forward in behalf of their contention were
neither good strategy nor popular propaganda. First,
the plea for general harmony implied that, lacking
such harmony, the dealers would be forced into
Teutonic arms after the war is over, a position no
body of loyal Americans could contemplate at the
present time with any degree of satisfaction on the
one part or admiration on the other. Second, the
threat that, unless admitted, the dealers might as a
safeguard to their own interest oppose before Congress
a tariff sufficiently high to protect the American
against the German industry was so amazing t hat it
suggested that, although some of the leading dealers
may not have been conscious of the fact, Ger-
man agents may have been the real promoters of
this argument. The joke is that those who put for-
ward the latter argument failed to realize the fact
as we see it that sentiment in Congress favoring the
thorough guarding of the American dyestuff interest
exceeds even that of the country at large, for Congress
has fully grasped the idea that the dyestuff industry
is not only an economic necessity as a key industry,
but, more important still, that it constitutes an in-
valuable reserve for high explosives manufacture.
Perhaps, after all, these arguments were simply
childishness.
WOOD WASTE
In this issue we have segregated a number of con-
tributions dealing with wood as the raw material of
certain lines of chemical industry. The topic is
especially timely in view of the need of acetic acid
for the aviation program, spruce turpentine for muni-
tions, and paper for the daily chroniclers of the stirring
events of the war.
There is now in progress within the organization
of the American Chemical Society a campaign for the
constant discussion of national wastes, and the subject
of wood waste is certainly a preeminently suitable
topic. According to A. D. Little, "two-thirds of the
tree is at present wasted either as litter in the field
or as mill waste." According to the same authority
6.48 per cent of the tree is stump, the name carrying
with it the idea of sheer waste.
Is it too great a tax upon the imagination to con-
ceive a vision of the mounting financial liabilities of
this war converted into actual assets through the
focussing of the thought and attention of chemists
upon the subject of national wastes? By no means.
IMPORTANT NOTICE
In the March issue of This Journal, page 237,
there was published a communication from J. R.
Healy, Federal Licensing Agent for Greater New York,
regarding "Licenses Required for Explosives and Their
Ingredients." Mr. Healy pointed out the necessity,
under the recent Act of Congress, of securing licenses
from the Bureau of Mines or authorized agents and
gave a list of explosives and ingredients of explosives
requiring license, the latter when purchased in amounts
of one ounce or more
We are informed by dealers that many orders for
these products, especially the ingredients of explosives,
are being received without license attached. Endless
trouble is therefore accumulating for all concerned.
For this reason wc urge upon all who are responsible
for the ordering of chemicals a careful reading of the
notice in the March issue.
To those who have been accustomed to order
potassium chlorate, lead nitrate, etc.. without any
thought save the cost of the article, the trouble in-
volved in securing licenses may seem like a further
evidence of red tape, but chemists above all others
will at once recognize the al cessity of such
a law at this time.
// explosives or ingredients c plosives are to be
purchased licenses must lie secured.
Apr., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
PRODUCT PATENTS
By E. P. McElroy
Once in every so often somebody of a guileless turn
of mind asks me what a "product patent" is and it
rather peeves me, for one can't define the non-existent.
There is not, never was, and likely never will be a
"product patent:" a patent on a product as a product.
The law does not authorize any such patent. We
who concern ourselves with patents, like other special-
ists, have an argot of our own, and our words and
phrases are not always what they seem. We are
much interested in certain legal relationships between
a process and its product; and we chatter considerably
of product claims, and even of product patents, when
we are really talking about claims for a composition
or for an article. And the innocent bystander, taking
our vocabulary for his own, goes away with the im-
pression that a patent can be had on some disembodied
ghost of a "product;" and then he comes around and
bothers me with his mental nebulosities.
The statute under which we work says nothing
about a product, but it does define as patentable
"any new and useful art, machine, manufacture or
composition of matter." Four statutory classes are
established and anything patentable must be' included
in one of these four classes. An "art" is a process or
method: a way of doing things; and it always results
in a product. This product may be a machine or a
manufacture or a composition of matter. It is not
patentable unless it is one of the three. Conversely,
any machine, or any manufacture or any composition
of matter is a product; it is a product of some "art."
A process may be novel and the product old, as in a
new way of making flapjacks; or both the process and
the product may be new. In the latter event the
process and the product may be, and usually are, the
result of the same mental inventive act; but since they
are in separate statutory classes they are, legally,
different inventions and must be separately patented;
either as different claims in the same patent or as
claims in separate patents — the product of course
being claimed as what it is, as a machine or a manu-
facture or a composition. Being separate inventions,
each must stand on its own legs; and the patentability
of the one is in no way affected by the patentability
of the other. No matter whether the product is a
machine, or an article or a composition, to be patent-
able it must be novel in and of itself, and irrespective
of any novelty in the process by which it is produced.
A composition may be a mechanical mixture or a
chemical compound; and it may be novel because
things are brought together which were never brought
! her before, or because they are assembled in a
Dew way (as in a coated granule) or because, though
old in make-up, the composition is in a new condition
or state; because it has some different form, or char-
acteristic, or property. It does not matter wherein
the novelty resides as long as the composition is new
and useful. But if it is new, then the novelty must
be capable of being pointed out in some way; there
must be a test or a characteristic which can be utilized
to show that the alleged new composition is indeed
new; it may be because it is pink, or is soluble in al-
cohol, or has a particular melting point or almost
anything. If there is no test and no characteristic
which will differentiate it from an old thing which the
public has the right to use, then it is the same as the
old thing. As a matter of common sense, if the new
thing cannot be differentiated from the old thing then
there is no difference. And it cannot be made differ-
ent by talking about its past history; by reciting differ-
ences in the process by which it is made. That par-
ticular experiment in patent law was made by the
Badische at the time of the alizarine synthesis when
it claimed "artificial" alizarine as a new composition.
The Supreme Court remarked, in effect (Cochrane vs.
Badische, in U. S. 293), that if the new artificial
alizarine was exactly the same thing as the old natural
alizarine then it was exactly the same thing and calling
it "artificial" did not make it different. Of course,
sometimes we have to characterize substances by ad-
jectives which look a little process-y because they
happen also to be past preterits of verbs, as in talking
of a boiled ham or a fried egg or wrought iron, but
this does not militate against the general proposition
that a thing to be patentable must be differentiated
from old things by stating its properties or its charac-
teristics; and that it must be new in itself and not new
because of the process by which it was made, i. e.,
it is not made novel by being a "product."
I regret to say that the nebulous-minded gentle-
men with their misconception of "product patents"
instead of merely infesting my office, are getting into
print and into Congress. And in this there is a certain
danger. Mrs. Malaprop was a very pleasant lady;
but it was not safe to entrust any business to her.
In the present mood of Congress and the people, a
proposition to revise the multiplication table, if backed
by a good patriotic showing, might slip through.
And these gentry wish to abolish "product patents"
feeling in some vague way that this will hurt Germany
and help us. I do not see how it will do either; but
I am somewhat hampered by my inability to grasp ex-
actly what they mean by a "product patent" anyway.
If they mean "product" in its legitimate ordinary
sense, then the proposition is an absurdity because it
is to abolish all patents save patents on processes.
For everything that man can make is a product, and
it is a product of a process of making: perhaps a
patentable process and perhaps an unpatentable one;
but still a process.
However, being something of a mind-reader, albeit
my education in this line was somewhat neglected,
1 surmise that what is actually meant is the abolition
of patents on the products of really-and-truly chemical
processes. If this be so, it leaves intact two more of
our statutory classes since a machine and a manu-
facture are commonly products of mechanical or
THE JOURNAL OF INDUSTRIAL AND ENGINEERING ( III.MISTRY Vol. 10, Xo. 4
physical methods; but it makes the fourth class, the
composition of matter, look like the remnants of the
shell-shot cathedral at Rheims, with patentability
hanging on by an eyelash. It is not abolished — not
all of it; just most of it. Some compositions will be
patentable and some not- — those whose pedigree is
in any way tainted with the "chemical." A little
chemistry will damn a thing quite as effectually as
a great deal since courts will not draw distinctions
between much and little, that being purely a "question
of degree." The alibi of the guiltless inventor would
have to be absolute, and there might be some difficulty
of proving it in the absence of any universally accepted
definition of "chemical." At present neither I nor
anybody else can write an impeccable definition of the
word, one which would stand fire in court I do not
even know, for example, whether dissolving sugar in
water is a "chemical" process.
Shifting the anathema to "chemical compound"
does not help any, since if a chemical compound is
something resulting from chemical action (which is
as good a definition as any) we come out the same
hole we went in, with the additional burden of de-
fining a "compound." In a general way I know
what a compound is; we all do. It is a body composed
of two or more elements united in definite proportions,
which, however, is just as true of type metal as of
aniline; or, for that matter, of any good uniform grade
of cast iron.
I fear me that any attempt to sort out the chemical
goats from the physical sheep in the composition of
matter class would prove like the task of hunting polar
bears in purgatory — "apt to be arduous in detail and
disappointing in result." There are too many hybrids,
goatish sheep and sheepish goats. It would be simpler
to abolish the whole class at one fell whack. But I
do not understand anybody wants to do this. So
far as I understand, the chemist is the only chap it is
meant to ostracize; and even he may escape if he does
not have intelligence to know what is happening when
he stews two things together.
Despite the present popularity of class legislation,
being a hidebound Republican I do not like it; and as
a chemist I object to being the class if the legislation
is discriminatory against me. To deprive the chemist
of his reward for his labor by taking away his "product"
claim (whatever that "product" claim may be) is the
same to him as depriving the machinist of his claim
to his machine or the weaver to his new article in
the way of a fabric. It is not good equity ; and moreover
it is not good sense. The object of the patent laws
is to promote the progress of science and the useful
arts, and that they have fulfilled their mission is be-
yond a peradventure. Why stop now and stop in a
single science? For 125 years (to be exact, since
Feb. 21, 1793) the chemist has been as much entitled
to look forward for reward for what he did as any-
body else; he read his title just as clear as did the
machinist. Maybe I am biased, and very likely I am,
but I can't, for the life of me, see wherein there is any
legal or equitable difference between the standing of
the chap who puts together an alkyl radical and an
aryl radical to make a new drug or a new dye and the
man who puts together levers and keys to make a new
typewriter. That the product of one is sold in a bottle
and the product of the other in a box is not material.
Any argument that seeks to discriminate between them
is as lop-sided as a crane; and I don't like being on the
wrong side of the lop. It is at least as much an ob-
ject to the public to encourage the chemist by patents
as it is to encourage the machinist. Both are human
and, commonly, poor, and neither is going to strain
his ingenuity working nights unless he sees a patent
ahead.
Running through all this "product patent" talk
like a rotten streak in a mushy banana, is the idea
that the chemist who creates a new drug or dye that
becomes a public necessity as soon as its creation and
existence are known to the public is guilty of creating
public necessities to his own profit, and he ought to
be discouraged; or if he won't be, then he should not
be allowed to make the profit — which sounds like a
curious piece of mental perversion, worthy of the
gentleman who habitually stood on his head to peel
the apple dumplings; but I am not gilding the lily any
in reproducing it — far from it; I am merely condensing
and Englishing certain actual arguments which have
been made.
Wasbington, d. c.
February 18. 1918
ORIGINAL PAPERS
SULFITE TURPENTINE
By A. W. Schorgbr
Received February 5, 1918
During the recovery of the sulfur dioxide, in the
manufacture of pulp by the sulfite process, a small
amount of oil collects on the surface of the liquor in
the separator and is known as sulfite turpentine.
The oil varies in color from pale yellow to black and
is frequently strongly impregnated with sulfur dioxide.
Various mills have reported a recovery of 0.36 to 1 . o
gal. of turpentine per ton of pulp. The species of
wood employed in order of their importance are spruce,
balsam, and hemlock. It has been reported that no
oil is obtained from cooking hemlock.
The United States produced 1,027,000 tons of
sulfite pulp in 1909 and Canada produced 470,94s
tons in 19 16. The present annual production in the
two countries exceeds 1,500,000 tons. Granting a
ry of only 0.5 gal. per ton, there should be
available annually about 750.000 gal. of this turpen-
tine.
Klason1 appears to have r.rst called attention to
' Btr., »» (1900), 2H1; ci. Kondnkow and Schindelmeiscr. Ckcm.-Ztt..
30 (1906), 722; Kertesz, Ibid., 40 (191-
Apr., 1918 TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
259
the fact that the oil so obtained consists mainly of
^-cymene and not of terpenes. The only reference
found to the American oil is the statement of Herty
and Graham1 that sulfite turpentine consists mainly
of cymene.
Cymene does not appear to be employed for any
specific purpose. Verley2 used it as the basis of a
synthetic violet-like perfume. Dinesman3 prepares
thymol by a method unlikely to compete with the
natural product; 2-Br-/>-cymene is transformed to the
3- or 5-sulfonic acid. After elimination of the bro-
mine by long heating in an autoclave with zinc dust
and ammonium hydroxide, the cymene sulfonic acid
is fused with potassium hydroxide to obtain thymol.
In a previous paper4 the writer has shown that by
the action of aluminum chloride on cymene there are
formed diisopropyl, benzene, toluene, m-xylene, and
i-methyl-3,5-diisopropyl benzene. The yield of tol-
uene may amount to 40 per cent of the weight of the
cymene, but this reaction cannot be employed eco-
nomically except when very unusual prices prevail
for toluene. Cymene also yields toluene by "crack-
ing" processes.6
EXAMINATION OF THE OIL
Oils from three widely separated mills were dis-
tilled, using a 12-in. Hempel column with the follow-
ing results:
.- ■ — — Distillate .
Compo- Up to 175"- 176°- 177°- 178°- Resi-
sition of 175" 176° 177° 178° 182° due
Obtained Wood Per Per Per Per Per Per
from Per cent cent cent cent cent cent cent
Niagara, Wis.. Spruce 100 1.11 7.76 84.03 6.65
Erie, Pa Spruce 90
Balsam 10 7.66 15.18 39.60 33.66 ... 3.74
Berlin. N. H.. Spruce 65
Balsam 35 0.43 2.57 22.00 19.00 35.00 8.81
The older oils when distilled usually give off con-
siderable hydrogen sulfide. The distillation data
indicate that the cymene content is greatest when all
spruce is cooked.
IDENTIFICATION OF CYMENE
Characteristic of cymene is the barium salt (C10H13.-
S03)2Ba.3H20, sparingly soluble in water from which
it crystallizes in shiny plates. The salt is best pre-
pared as follows: To 50 g. of cymene in a flask are
added 100 g. of fuming H2SO4 (10 per cent free S03).
Shaking develops considerable heat and the solution
is complete in about 10 min. The liquid is cooled,
poured into a separating funnel, and about one-third
of its volume of cold water added. On rotating the
funnel carefully two layers are formed, the upper con-
sisting of cymene sulfonic acid, and the lower of dilute
sulfuric acid free from sulfonic acid. The cymene
sulfonic acid should be dissolved in about 5 liters of
boiling water, neutralized with barium carbonate,
and the BaSOj filtered off. After removal of the salt of
the 2-sulfonic acid, the filtrate contains the salts of
the 3-sulfonic acid and disulfonic acid that can be
separated with alcohol.6 The yields of the three
1 Tins Journal, 6 (1914), 803.
'German Patent 101,128 (1897).
■German Patent 125,097 (1901).
< J. Am. Chem. Soc, 39 (1917), 2671.
' Rittman, KritMi Patent 13,100, September 13, 1915.
• Claus, Ber., 14 (1881), 2140.
salts from 50 g. of cymene were 79.9 g., 14.6 g., and
4.2 g., respectively.
When 35.4 g. of the anhydrous barium salt of the
2-sulfonic acid were heated with an equal weight of
PCU and the amide formed by heating with ammonia
in the ordinary way, the yield of the cymene sulf-
amide was 18.93 g- (70.7 per cent of theoretical).
The amide, recrystallized from water, melted at 1140.
The cymene was also oxidized to ^>-oxyisopropyl
benzoic acid, m. p. 1 55 °. As good results are ob-
tained when only half of the amount of KMn04 given
by Wallach1 is used. This method is somewhat
tedious and the yields are poor.
Cymene has been found to react readily with chloro-
sulfonic acid and when an approximately pure cymene
is present this offers a superior means of identifica-
tion. With the terpenes chlorosulfonic acid reacts
with explosive violence. An equal volume of chlor-
sulfonic acid is gradually added, with constant shak-
ing, to the cymene. The mass foams considerably,
but the reaction soon completes itself with only a
slight rise of temperature. The chlorosulfonic acid is
separated by pouring into a separating funnel con-
taining water, extracted with ether, and the ether
extract washed with water to remove inorganic acids.
After evaporation of the solvent the cymene chloro-
sulfonic acid is transformed to the sulfamide by heat-
ing with -concentrated ammonia on the steam bath.
The sulfamide is recrystallized from hot water, using
a little animal charcoal. The method is rapid and
the yields are excellent.
SULFAMIDE OF />-OXYISOPROPYLBENZ0IC ACID Ten
grams of cymene sulfamide were oxidized by heating
on the steam bath with 30 g. of potassium perman-
ganate in 2 liters of water. The manganese sludge
was filtered off, the filtrate evaporated to dryness
and extracted with hot 95 per cent alcohol. The alco-
hol was evaporated and the residue extracted with
hot commercial absolute alcohol. On cooling, the potas-
sium salt of />-oxyisopropylbenzoic acid sulfamide was
deposited as warty masses. The salt was dried at
no° for 48 hrs. and the potassium content determined
as follows:
0.4950 g. salt gave 0.1403 g. K2SO4.
SOj.NHs
Calculated for CJH«(OH).C.HJ < : K = 13.18. Found: K = 13.13.
COOK
CARVACROL FROM CYMENE
The annual importation of thymol has been about
6000 lbs.2 In their physiological and antiseptic
properties thymol and carvacrol appear to be very
similar. A number of iodine compounds,3 such as
"aristol" and "annidalin," prepared from thymol, are
reputed to possess very strong antiseptic properties.
A similar compound,4 "iodocrol," prepared from carva-
crol, has been made in this country for several years.
The 2-sulfonic acid of cymene can be easily pre-
pared, but the fusion with alkali as carried out on a
1 Ann., 264 (1910), 10.
J Hood, U. S. Department of Agriculture, Bulletin 372.
mger and Vortmann, Ber , 22 (1889), 2316; 23 (1890), 2754;
Haver & Co., German Patent 49,739.
< I S, Patent 561,531 (1906); cf. Bayer & Co., German Patent 53,752
(1889).
26o
THE JOURNAL OF INDUSTRIAL AXD ENGINEERING ( HEMISTRY Vol. 10. Xo. 4
small scale gave very poor yields of carvaerol. It is
very probable, however, that satisfactory yields could
be obtained from larger apparatus capable of more
careful control.
carvacrol — The calcium and barium salts of cymene
sulfonic acid were made in the manner described above.
The calcium salt is much more soluble than the barium.
The sodium salt was prepared by decomposing a
weighed amount of the barium salt with sodium car-
bonate in aqueous solution and evaporating to dry-
ness after filtering off the barium carbonate.
The fusion was carried out by placing the sulfonic
acid salt in a nickel dish on a sand bath and adding
the alkali dissolved in a minimum amount of water,
and gradually raising the temperature of the fused
mass to about 3000, with constant stirring. This
temperature should not be exceeded. The melt was
dissolved in water, acidified, and distilled with steam.
The carvacrol was extracted with ether and weighed
after evaporation of the solvent. The yields of car-
vacrol are given in the following table:
Yields of Carvacrol from
Cymene Sulfonic
Acid
Temp
of
usion
Wt.
'
Wt.
Yieid
~ Theo-
No Kind
Grams
Kind Grams
Fusion
Gms.
retical
1 (CioHu.SOiHCa 2HtO
10.00
KOH
30
300°
J 4^
41.0
2 (Cn>Hij.SOj)!Ca.2H:0
10.00
KjCOj
30
500'
0
3 (CioH».SOj)j.Ba.3H.O
10.00
XaOH
30
350°
0
4 CioHu.SOiNa
7.64
KOH
30
300°
0.61
a.6
5 CioHu.SOjNa
7.64
XaOH
30
350°
0
6 (CioHis.SOjhCa.2HiO
10.00
KOH
30
290°
1.10
is!i
8 CioHu.SOiNa
7 64
KOH
7.5
300°
0.91
18.8
9(a) ( CioH,i.SOjHCa.2H.O
10.00
KOH
8.8
300°
3.16
52.9
10(a)(CioHi..SOihCa.2H;0
10.00
KOH
8.8
300°
1.68
28.9
1 1 (a)(CioHu.SO,):Ca 2H:0
10.00
NaOH
6.4
290°
0.74
12.4
(a) Crucible covered dun
ng the fusion.
Other fusions conducted under different conditions
gave only small yields of carvacrol and served to show
the great difficulty of duplicating results. This is
illustrated by Fusions 9 and 10 made under identical
conditions.
identification of carvacrol — The carvacrol ob-
tained was identified as follows: 2.5 g. of the phenol
were dissolved in dilute KOH and made up to 1.5
liters. Six grams of KNO. were then added and after
it had dissolved the solution was strongly acidified
with sulfuric acid. In a short time the carvacrol
nitrite rose to the surface in a flocculent condition.
The nitrite crystallized very readily, using hot 50
per cent alcohol, but after several crystallizations
the compound was still impure and melted at about
I47°-
It was found that the nitrite was insoluble in petro-
leum ether and this property afforded an easy means
of purification. The carvacrol nitrite was dissolved
in a minimum amount of chloroform which was slowly
dropped, with stirring, into a considerable volume
of petroleum ether. The precipitate was finally
crystallized from alcohol. The pale yellow needles
melted at 153-4°. When heated slowly they melted
at 1 50-1 5 20.
SUMMARY
Sulfite turpentine, consisting largely of cymene,
can be used for the production of carvacrol and toluene.
PORBST SlvRVICK
Porbst Products Laboratory
Madison, Wisconsin
THE EFFECT OF INCOMPLETE DISTILLATION ON THE
YIELD OF PRODUCTS IN THE DESTRUCTIVE
DISTILLATION OF BLRCH
By R C. I'almek
Received October 17. 1917
OBJECT OF TESTS
In most hardwood distillation plants a certain
amount of the wood comes out of the retorts after distil-
lation as "brands" or "bones," that is. pieces incom-
pletely charred. When a plant finds it necessary for
economic reasons to use wood that has been insufficiently
seasoned or wood excessively wet with rain or snow, it
is difficult to complete the distillation in the required
24 hours. Under such conditions the amount of brands
is likely to be large, amounting to as much as 8 or 10
per cent of the charge. Usually the brands are re-
distilled, although they are not considered as new raw
material. There is no agreement among operators
as to what yields are obtained by distilling the wood
in two stages, that is. whether there is actually any
gain or loss in products by this procedure. To the
knowledge of the author, the literature reveals no data
on this point. A few experiments were therefore made
to determine just what effect incomplete distillation
had on the yield of products in the destructive distilla-
tion of hardwood and how yields from stopping the
distillation and then redistilling the residue compared
with the yields from a single operation.
EXPERIMENTAL PROCEDURE
Yellow birch cord wood reduced to pieces about 2*/i
in. by 21 ,■■'. in. by 16 in., not very well seasoned, was
distilled in a semi-commercial laboratory retort holding
about 50 lbs. of wood. The temperature in the empty
retort was raised to about 340° C. and a specially con-
structed basket containing the wood was then quickly
introduced. The start of the distillation was then
similar to the start of a commercial distillation where a
new charge is placed in a retort immediately after
drawing out the hot charcoal from a run that has just
been completed. The distillations were carried on
according to the best practice of temperature control,
that is, regulating the fire so that the rate of rise of
temperature in the retort was decidedly decreased after
the tar began to be formed. One run was made in
which the distillation was normally carried to comple-
tion. In two other runs the fire was turned off when it
was obvious from the amount of distillate, temperature,
etc., that the distillation was not complete. Different
stopping points were selected for the different runs.
As the distillation had not reached the point of marked
exothermic reaction in these runs it was checked very
quickly after the fire was turned off.
After cooling to room temperature the retort was
opened and all brands were separated from charcoal.
Any stick which was brown in color, or which could not
be readily fractured by a moderate blow with a hammer,
was considered a brand. All the brands from incomplete
distillations were allowed to remain out of doors during
a heavy rain until they had absorbed water to about
31 1 per cent of the dry weight and were then completely
distilled as if they were normal wood.
Apr., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY 261
The crude pyroligneous acid liquor from each run distillation. The acids are the first of the valuable
was weighed, measured and separated in a clear products to be formed1 and it is especially interesting
acid and settled tar, and the clear acid liquor was then to note that the formic acid is formed more rapidly
analyzed for total acid (calculated as acetic), acetic than the acetic. The total amount of formic acid is
acid, formic acid, wood alcohol and dissolved tar. obtained when more than 45 per cent of the wood is
results leIt as brands. The charcoal curve does not begin at
The results of the tests in percentage of the dry IO° Per cent brands because a stick was not considered
weight of wood distilled are given in Table I. Runs ?harcoal untl1 * had increased in carbon content to
2 and 3 which were made on fresh wood and Run 4 SUch an eXtent that Jt COuld be readily fractured by a
which was made on the brands obtained in Runs 2 and moderate blow with a hammer. The tars do not begin
3 have been combined by calculation to show the total t0 come over untl1 after there ls some charcoal in the
yields obtained by the complete distillation of the retort- The dissolved tar (tar soluble in the pyro-
original wood. The yields from this calculation and ligneous acid) comes over before the oily tar which
the yields from Run 1 indicate the effect of a two- settles out of the Pyroligneous acid. The wood alcohol
stage distillation compared to a single normal opera- 1S the last valuable product to begin to be formed but
■ • it starts just prior to the appearance of the oily tar.
This fact is of special interest in view of the experiments
Table I — Yield from the Distillation of Birchwood at Different , , 0 T, , , ... . ,
stages of Completion(o) on temperature control.- It shows why the point
Tar — — — - Ace- For- Wood when settled tar begins to come is of value in determin-
Run Char- Set- Dis- To- Total tic mic Alco- b
No. coal Brands tied solved tai Acid Acid Acid hoi mg when to begin to practice control, that is, because
1 Complete distillation.. 42.30 0 5.52 5.28 10.80 5.52 4.92 0.44 1.41 ,.t,„ „i..l.| nrppprlpc tVip tar in nrrW nf fnrmarinn Tr
2 wood incomplete 17.66 48.00 i .93 291 4.84 4.53 3.92 o.48 0.885 tne aiconoi precedes tne tar in order oi iormauon. it
3 wood incomplete. 10.77 62.96 0.87 1.73 2.60 3.44 2.99 0.36 0.447 aiso sh0ws why it is not detrimental to the yields to
4 Brands from 2 and 3 . J J
completely distilled . . 54.50 o 4.99 4.29 9.28 2.96 2.56 0.30 1.45 push the distillation rapidly at the start, the reason
run.".'...' 44.49 o 4.174.69 8.86 5.59 4.86 0.59 1.46 being that only a small amount of the acid and none of
brand"' dlsuiiedelds are give" ™ per *"* °f "* dry ™eight °f the w°°d °r the alcohol is formed during the first part of the distilla-
tion.
As will be noted, the distillation in two steps gives The practical appiication of the curve lies in the
from 20 to 25 per cent less. tar. fact that it shows the losses in valuable products when
The yield of acetic acid is about 2.4 per cent lower the distillation is at any degree of completion. It may
for the double operation. The total acid, calculated be noted that even with JQ per cent brands> which may
as acetic, is practically the same. This is due to the be considered the maximum usually obtained in the
fact that while the acetic acid yield is somewhat lower commercial plant- the loss 0f aicohol is only s.o per
the yield of formic acid is about 30 per cent higher for cent and acetate 2 s per cent The charCoal loss is,
the two-step operation. The distillation in two steps of coursej high) being abotlt I2-- per cent.
gives about 4 per cent more charcoal and 2.8 per cent
. . . „ ., • ,, , , . -^ • SUMMARY
more alcohol. Considering all the products it is ap-
parent that, except for the tar. there is no appreciable Semi-commercial laboratory distillations were made
loss or gain in valuable products recovered when brands with birch in which the distillation was stopped before
.. .-,, A completion. The brands obtained were redistilled.
are redistilled. v , . , , ,. .,
The results showed that the combined effect of the distil-
AMOUNT AND ORDER OF FORMATION OF PRODUCTS AT . „ „„„„ „■ ,j„
lation in two steps gave practically the same yields
DIFFERENT STAGES OF DISTILLATION c , - .. ...... „„ „„„,
of valuable products as when the distillation was com-
An examination of the yield data obtained by stop- pieted in one step,
ping the distillation in order to make brands gives an Considering the maximum yield of brands allowable
indication of the order in which the products are formed in a cornmercjai piant as 10 per cent of the original
in the destructive distillation of hardwood. The yields charge the data show that the loss of products is only
of each product in the incomplete runs calculated in s Q pef cent WQod alcohol and 2-- per cent acetate of
percentage of the total obtained in a single distillation Hme when the distniation is stopped at that point,
are given in Table II. When the same data are shown Analysis of the data is of interest from a scientific
graphically, the percentage of total production being standpojnt [n showing the order in which the products
given as one axis against the per cent of wood left as afe formed in the destructive distillation process. The
brands as the other, the results presented are of both acids are the first of the valuable products to be formed,
scientific and practical interest. The foriruc acjd js formed more rapidly than acetic
Table II— Proportion of Total Production when Different Amounts acid, the total yield of formic acid being obtained when
of Brands are Left in the Retort(u) , . , . . u_„„j„ t«l,„ t.,-
Tar , Wood about half of the wood remained as brands. L he tar
Run Char- Set- Dis- Total Acetic Formic Aico- soiubie in the pyroligneous acid is the next volatile
No. coal Brands tied solved Total Acid Acid Acid hoi ov»».w ~ t-j o
1. 1000 0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 product to be formed. This is followed by the oily
32::: till 8:82 ft? li.\ S:! 21:S S:? «:? ":! tar which settles out of the pyroligneous acid. Wood
(a) The yield from a. single complete distillation (Run 1) is taken as a]cohol is the last of the Valuable products to begin to
be formed but precedes the oily tar in order of formation.
From a scientific standpoint the data are of interest -j-j^ cact js 0f spec;ai interest in view of experiments
in throwing some light on the order and amount of the , Gas is actually thc first pruuuct formed,
different products formed at different stages in the * this journal, 7 (1915), 663.
262
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 4
in temperature control which showed that in order to
obtain the maximum yield of wood alcohol it was very
necessary to control the distillation just before the tar
began to be formed.
Forest Products Laboratory
Madison, Wisconsin
THE INFLUENCE OF MOISTURE ON THE YIELD OF
PRODUCTS IN THE DESTRUCTIVE DISTILLA-
TION OF HARDWOOD
By R. C. Palmer and H. Cloukey
Received October 17, 1917
OBJECT OF WORK
In the destructive distillation of hardwood it has
been considered for a long time the best practice to
season the wood for at least 12 months before using
it. The reason for this practice lies chiefly in the in-
crease in operating expenses, due to an excessive
dilution of the crude liquor. It is also the opinion
of some operators that besides increasing the volume
of liquor, green wood gives lower yields of products
than dry, especially of acid. Other operators do not
hold this view. In discussing the importance of using
seasoned wood Klar1 says "the yields of acetate of
lime are inversely proportional to the water content
of the wood carbonized — while the yield of alcohol is
increased if changed at all."
There exists then no agreement among operators as
to the influence of an excess of moisture on the yields.
Many plants are now using wood with a higher moisture
content than formerly because of changes in economic
conditions of wood supply.
In making commercial experiments and demonstra-
tions in controlling the distillation in order to secure
the maximum yield of products, it became apparent
that former experiments in controlling dry wood should
be extended to determine the influence of moisture
under controlled conditions.
In view of these conditions and the possible in-
fluence of moisture in temperature control, the experi-
ments described in this paper were made. The tests
also included a study of the effect of moisture under
conditions comparable with uncontrolled as well as
controlled plant conditions.
EXPERIMENTAL PROCEDURE
distillation- — As it was thought that different
species might be affected differently, the three standard
distillation species, beech, yellow birch and hard
maple, were studied separately. The material was
ordinary cord wood from a commercial plant con-
taining wood seasoned for about 18 months and wood
seasoned from 4 to 6 months.
The tests were all made in a laboratory retort2
holding about 50 lbs. of wood. In all previous work
in the same retort it was the usual practice to start
the distillation from a cold retort. By this method
any excess moisture present was always distilled over
before it could play any part in the destructive distil-
lation reaction and no effect of moisture could be noted.
In these tests the empty retort was first heated to
1 "Technologic dcr Holivcrkohlung," 1910 edition, p. 77.
> Forest Service Bulletin 1S9, and This Journal, 7 (1915), 663.
what would correspond to the end temperature of a
commercial distillation, at which time a specially con-
structed basket containing the wood was quickly
introduced into the retort. In this way the distilla-
tions were comparable to continuous daily plant
practice. Destructive distillation had always com-
menced in parts of the charge, while the water in
another part continued to distil over.
Uncontrolled and controlled distillations, were made
for both green and seasoned wood of the three species.
In former laboratory tests, in which the importance
of control features was established, the procedure was
based on the temperature-percentage distillate rela-
tion. In continuous plant practice it is not possible
to determine the proportion of the total distillate at
any stage of the distillation, so it was thought im-
portant to determine if the time-temperature relation
would not serve as well. There seems to be no doubt
but that it can, as the curves drawn for these relations
were found in these tests to be quite parallel. In
uncontrolled distillation the maximum fire was kept
under the retort until the tar-point was well established
and the fire was then checked so that the distillation
was completed largely by means of the exothermic
reaction. In the controlled runs, as soon as the first
indications of tar were noted in the distillate, the fire
was checked and the firing so regulated that after
that point the rate of rise in temperature was ap-
preciably lower than in the uncontrolled runs.
analyses — The yields of settled tar and charcoal
were determined by actual measurement. The yields
of acetic and formic acids, dissolved tar and wood
alcohol were determined by analysis of the clear
pyroligneous acid.
For acid and dissolved tar determinations ioo cc. of
pyroligneous acid were distilled until no further
distillate came over and the temperature, measured
in the residue, reached 140 ° C. The residual tar was
then washed with 30 cc. of water and the distillate
added to the first, the distillation being stopped when
the temperature in the residue reached 1500 C. The
residue was dissolved tar.
A 25 cc. portion of the distillate was titrated with
norma! XaOH to give total acid, calculated as acetic.
Another 25 cc. portion was diluted with 100 cc. water
and placed on the steam bath with an excess of mer-
curic oxide and allowed to remain for about 2 hours, or
until it was evident that there was no further re-
duction of the oxide. The flask was shaken occa-
sionally. The whole was then distilled from phos-
phoric acid. Titration of the distillate with N/10
NaOH gave acetic acid. The difference between the
total acid and acetic acid determinations was taken
as the formic acid, the formic being oxidized by the
mercuric oxide. Phenolphthalein was the indicator
in both titrations.
Wood alcohol was determined by distilling from a
500 cc. sample of the pyroligneous acid. The distillate
was made alkaline with strong XaOH and 65 per cent
distilled from it. After again being sure that the
distillate was alkaline a third distillation of 60 per
cent was made. About 2 cc. of HSS04 were added to
Apr., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY 263
this distillate and a fourth distillation of 60 per cent acetic and formic acids — The acetic and formic
made. The final distillate was weighed and the acid results are very important from a commercial
specific gravity determined at 15.50 C. in a stand- viewpoint. The effects of moisture and control are
ardized pycnometer. The amount of alcohol was then different for different species.
determined by consulting the tables of Dittmar and The beech with higher moisture gave decidedly
Fawsett.1 more total acid whether controlled or not, but when
No analyses were made of the settled tar so the not controlled the increase in acid was largely formic
yields of acid are proportionately lower than in plant acid, while when controlled the increase was nearly
practice, where the tar is washed for recovery of soluble all acetic acid. When the drier beech was controlled
products dissolved in it. the acid yields were appreciably decreased instead of
results increased.
The results of distilling the wet and dry wood under In order to obtain the maximum yields of acetic
controlled and uncontrolled conditions are given aci<i from beech the experiments show quite con-
separately for the different species in Table I. The clusively that the wood should not be seasoned too
results for the mean of equal weights of beech, birch long and the distillation should be controlled as care-
and maple are also given in the table. The data fully as possible.
represent in every case the mean yield from at least Birch shows somewhat the same tendency as beech
two runs. to give higher yields of acetic acid from the wetter
In Table II the same data are figured on a relative wood but the differences are not nearly so great. The
Table I — The Yield of Products from Beech, Birch and Maple with Dtfferent Amounts of Moisture and Under Different
Conditions of ControlCo)
. Beech . . Maple .
Dis- For- Dis- For- Wood
Mois- Char- Settled solved Total Total Acetic mic Wood Mois- Char- Settled solved Total Total Acetic mic Alco-
Condition ture coal Tar Tar Tar Acid Acid Acid Alcohol ture coal Tar Tar Tar Acid Acid Acid hoi
Dry — Not controlled.. . 24.90 39.45 5.21 4.91 10.15.5.52 4.62 0.69 1.74 21.32 38.66 5.80 6.98 12.78 5.43 4.92 0.38 1.77
Dry — Controlled 22.25 42.00 4.93 4.89 9.82 5.04 4.12 0.73 1.78 22.80 42.35 5.16 4.77 10.13 5.49 4.61 0.68 1.92
Wet— Not controlled... 31.80 38.72 5.45 5.03 10.48 6.23 4 98 1.03 1.80 32.80 39.20 6.12 5.05 11.17 5.37 4.54 0.66 1.88
Wet— Controlled 32.27 39.85 5.01 5.64 10.65 6.25 5.63 0.54 1.91 27.03 38.92 4.87 4.91 9.78 5.59 5.17 0.33 1.83
. Birch . Mean, Equal Portions Beech, Birch and Maple
Dry— Not controlled .. . 20.82 38.88 5.96 5.64 11.60 5.02 4.28 0.59 1.62 22.31 38.98 5.66 5.84 11.50 5.32 4.54 0.55 1.71
Dry— Controlled 21.10 42.30 5.04 4.62 9.66 5.42 4.83 0.48 1.73 22.05 42.20 5.04 4.83 9.87 5.32 4.52 0.63 1.81
Wet— Not controlled... 30.17 40.25 5.93 4.26 10.19 5.62 4.97 0.52 1.58 31.59 39.39 5.83 4.78 10.61 5.74 4.83 0.74 1.75
Wet — ControUed 26.78 42.30 5.52 5.28 10.80 5.52 4.92 0.44 1.41 28.69 40.36 5.13 5.28 10.41 5.78 5.24 0.44 1.72
(a) The yields are all given in per cent weight of the oven-dry wood distilled.
Table II — The Relative Yield of Products from Beech, Birch and Maple with Different Moisture Contents and Under Different
Control Conditions(o)
, Beech ■ ■ . Maple .
Dis- For- Dis- For- Wood
Mois- Char- Settled solved Total Total Acetic mic Wood Mois- Char- Settled solved Total Total Acetic mic Alco-
Condition ture coal Tar Tar Tar Acid Acid Acid Alcohol ture coal Tar Tar Tar Acid Acid Acid hoi
Dry— Not controlled 74.8 94.0 95.7 87.1 95.4 88.4 82.1 67.0 91.1 65.0 91.3 94.8 100.0 100.0 97.2 95.2 54.6 92.2
Dry— Controlled 69.0 100.0 90.5 86.7 92.2 80.7 73.2 70.9 93.2 69.5 100.0 84.3 88.4 78.3 98.2 89.2 100.0 100.0
Wet— Not controlled 98.3 92.2 100.0 89.2 98.5 99.6 88.5 100.0 94.2 100.0 92.8 100.0 72.4 87.4 96.9 87.8 97.1 97.7
Wet— Controlled 100.0 94.9 92.0 100.0 100.0 100.0 100.0 52.4 100.0 82.4 91.9 79.6 70.3 76.5 100.0 100.0 48.5 95.4
. Birch — * Mean, Equal Parts Beech, Birch and Maple
Dry— Not controUed 69.0 92.0 100.0 100. 0 100.0 89.3 86.1 100.0 93.7 70.7 92.4 97.1 100.0 100. 0 92.1 86.7 74.4 94.5
Dry— Controlled 69.9 100.0 84.6 81.9 83.3 96.5 97.2 81.4 100.0 69.7 100.0 86.5 82.7 85.9 92.1 86.3 85.1 100.0
Wet— Not controlled 100.0 95.2 99.5 75.5 87.9 100.0 100.0 88.2 91.3 100.0 93.3 100.0 82.0 92.3 99.3 92.2 100.0 96.7
Wet— Controlled 88.8 100.0 92.6 93,6 93.2 98.2 99.0 74.6 81.6 90.8 95.7 88.0 90.4 90.5 100.0 100.0 59.4 95.0
(a) The yield from the condition giving the highest result is taken as 100 per cent,
basis, taking the highest yield of each product as effect on formic acid is not especially marked. The
ioo per cent. control of dry birch gave good increases in acetic acid,
Moisture and control do not affect the tar and in fact almost as much as the control of the wood with
charcoal yields in the same way for the three species. higher moisture content. The data do not show
Without control the wood containing more water that there is much preference between controlled and
gives more tar for beech but less tar for birch and uncontrolled distillations, if wet wood is being dis-
maple, and when the distillations were controlled the tilled. Considering all factors, however, the results
wetter wood gave more tar for beech and birch but would indicate that, as far as acetic acid is concerned,
less for maple. there is no advantage in seasoning birch too long.
Control itself gave less tar for all species in the In the case of maple also the wood with higher
case of dry wood but more for beech and birch and moisture is to be preferred for best acetic acid yields,
less for maple in the case of the wood with a larger provided the distillation is controlled, the results being
per cent of water. The charcoal yields are always almost as striking as with beech. If dry wood is dis-
increased by control but the effect of more water is tilled the uncontrolled distillations give the highest
different for the different species. For higher moisture yields of acetic acid.
beech gave lower yields of charcoal. Birch gave higher Considering the three species the best yields of
or the same charcoal yields and maple gave more acetic acid are evidently obtained from carefully
when not controlled but less when controlled. The controlled distillations of wood that has seasoned only
relative difference, due to different conditions, are about 6 months. These conditions gave nearly 15
shown more clearly in Table II. per cent more acetic acid than either controlled or
■ Trans. Roy. Soc. Edin.. S3 (quoted in Smithsonian Physical Tables). uncontrolled I 8 months old WOOd.
264
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 4
It is of interest in this connection to give the results
of a commercial temperature-control test lasting about
three weeks. The plant was of about 50 cords per
day capacity, distilling wood composed of about three-
quarters maple and one-quarter birch. Approximately
1 1 00 cords were distilled during the test. The wood
had not been seasoned for more than 8 months
and could be considered very comparable with the
wet wood used in the laboratory tests described in this
paper. The yield of acetate of lime in the commercial
test was increased about 12 per cent over former un-
controlled practice. As the plant had been using
wood of the same quality prior to the test, the results
of these experiments in the laboratory, comparing
wet uncontrolled with wet controlled runs for birch
and maple, indicate that the increase in acetate was
due largely to the maple. The increases obtained in
the plant and in these tests check surprisingly well.
wood alcohol — The influence of moisture on the
wood alcohol is almost as pronounced as on the acids.
The beech, with the higher moisture, gave decidedly
the highest yield of wood alcohol when controlled
and even the uncontrolled wet beech gave a little more
alcohol than either the controlled or uncontrolled dry
beech. The alcohol results, therefore, also indicate
that beech should not be seasoned too long and that
the distillation should be carefully controlled.
In the case of maple, both uncontrolled and con-
trolled wet wood gave higher yields of alcohol than the
dry uncontrolled runs, showing that moisture also
favors the alcohol in this species. However, decidedly
the highest yield was obtained from the dry con-
trolled distillation, verifying former experiments.
Considering both alcohol and acetate, the data would
indicate that for best results from maple the wood
should be only moderately seasoned and the distilla-
tion carefully controlled.
The alcohol results for birch showed that without
doubt this species should be well seasoned for the
highest yields, as the wetter wood gave much smaller
amounts of alcohol. The dry controlled birch gave
the highest yield. Since the acetate yield for the dry
controlled birch was so nearly the same as from the
wood with higher moisture, although slightly lower,
it would seem, considering both products, that birch
should be well seasoned and the distillation carefully
controlled for the best returns. Birch, then, seems
to be different from beech and maple as regards the
influence of moisture on the more valuable products,
such as alcohol, acetic acid and charcoal.
SIM \i A k v
I — Semi-commercial laboratory destructive distilla-
tions were made with beech, birch and maple. One
lot was seasoned for about iS months and another lot
about 6 months. The results showed that moisture
had a decidedly favorable influence on the yields of
acetic acid when the distillations were controlled after
the exothermic reaction had begun. The data indi-
cate that beech and maple should be distilled only
after moderate seasoning in order to secure the highest
yields of acetic acid, provided the distillations are
Carefully controlled. The yields of acetic acid from
birch which had been well seasoned were so nearly
the same as from the wood which had been seasoned
only about 6 months that there is no preference for
this species, provided the distillations are controlled.
II — If the recovery of formic acid should become
important in the distillation of hardwoods, the experi-
ments showed that the highest yields were obtained
from rapid (uncontrolled) distillations of wet wood,
this being particularly true of beech.
Ill — A commercial temperature-control test using
wood seasoned for only about 8 months gave prac-
tically the same increases in acetate as obtained in the
laboratory tests.
IV — Former experiments showing the value of
temperature control in increasing the yield of wood
alcohol have been verified in these tests. Additional
data on the influence of moisture shows that an excess
tends to give still higher yields of alcohol in the case
of beech and the same tendency is shown to a lesser
degree for maple. With birch, however, the drier
wood is preferred for the highest alcohol yields and
although moisture favors the alcohol to a slight extent
with maple as compared to uncontrolled dry distilla-
tion, the controlled dry maple runs gave decidedly
the highest yields of alcohol for that species.
V — An excess of moisture in general gives lower
tar and charcoal yields, but beech is the exception
for tar and birch for charcoal.
Forest Products Laboratory
Madison. Wisconsin
THE EFFECT OF CATALYZERS ON THE YIELD OF
PRODUCTS IN THE DESTRUCTIVE DISTILLA-
TION OF HARDWOODS
By R. C. Palmer1
Received October 17, 1917
PURPOSE OF WORK
The purpose of the work was to study the influence
of various reagents or catalyzers on the formation
of wood alcohol, acetic acid. etc. (i) during the pri-
mary reaction occurring in the destructive distillation
of wood and (2) during any secondary reactions that
take place between the original products.
SCOPE OF WoKK
The experiments conducted so far have been pre-
liminary and include a study of the effect of hydro-
lyzing acid catalyzers in an attempt to induce the
maximum splitting off of acetyl or formyl groups from
the cellulose or ligno-cellulose and the hydrolysis of
these groups to acetic and formic acids or the decom-
position of intermediate products, such as carbohy-
drates, into these products. Any influence on the
formation of other products was. of course, noted.
Phosphoric acid was selected as a catalyzer in these
preliminary tests as being the most adaptable. It
could be readily injected into the wood in solution
and was non-voiat ile, being transformed into the meta-
phosphoric acid at the maximum temperature of the
destructive distillation of wood.
Maple and beech reduced to chips about 1 in. by
1 Acknowledgment is made to Mr. II. Cloukey for making a number
of the .m.i]\ sis
Apr., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
26;
Vj in. by 2 in. in a pulpwood chipper were used.
All tests were made in the autoclave, holding about
5 lbs. of wood, previously described in the report of
tests on the effect of pressure on the yield of products,
and the manner of making the tests was in general
similar to that described in that paper.1
Preliminary experiments were also made on the
distillation of wood in the presence of, or saturated
with, wood tar, in a study of the possibility of split-
ting off methyl groups from the tar to form methyl
alcohol.
DETAILS OF METHOD
The catalyzer was brought into intimate contact
with the wood by placing the chips in enough of a
water solution of the acid to completely immerse them
and the solution brought to the boiling point to drive
out the air in the wood. The chips were then cooled
in the solution, causing a penetration of weak acid
into the wood. The excess liquid was drained off
and the chips weighed immediately after no more
liquid dripped from them. The amount of catalyzer
present was then calculated from the weight of solu-
tion absorbed, knowing previously the strength of
the solution. Titrations were made before and after
treating the chips with catalyzer solution in enough
of the tests to show that no appreciable selective ab-
sorption took place. In the case of acid solution the
Table I — Distillation of Maple i
Max. Temp. Pyro. Acid
Run Catalyzer Retort Bath Pressure Less
No. Per cent Degrees C. Lbs. Moisture Charcoal
I 0 312 470 0 35.05 39.15
2 7.59 332 465 0 41.27 44.90
3 7.92 323 470 60 40.57 46.20
4 2.72 324 470 90 40.20 45.95
5 23.75 320 470 60 40 80 44.05
(a) Results are all in percentage of the dry charge.
chips were always apparently wet to the center.
With the wood tar or creosote only a few of the largest
chips were not completely penetrated by this method.
The chips, after treatment, were allowed to dry in
some cases and in others were distilled immediately.
Some runs were made putting the wood in a cold re-
tort and others putting the wood in the retort pre-
viously heated to a temperature higher than the de-
structive distillation point.
The different control data were taken and analyses
made as in previous work, including the (i) moisture
content of the charge, (2) weight, of distillate and char-
coal, and (3) percentage of total acid, acetic acid,
formic acid, settled and soluble tar, wood alcohol.
and acetone, in the distillate.
RESULTS
The results in general are not very concordant,
but several striking effects have been noted, indica-
ting that when conditions are favorable the yields of
primary products may be affected in a very marked
degree by the presence of catalyzers. Not enough work
has been done, however, to establish all the factors
that influence the part the catalyzer plays in the de-
composition reaction so that the results can be readily
duplicated. The influence of various reagents thai
would poison the action of the catalyzer has not been
worked out.
1 This Journal, • (1914), 890.
maple — The results with maple chips, using phos-
phoric acid as a catalyzer, are given in Table I.
Run i was made without any catalyzer at
atmospheric pressure for comparison with catalyzer
runs and the yields are about the same as previous
tests in the same apparatus.
The experiments with maple showed no striking in-
crease in the valuable products, although several of
the other products showed decided differences when
the wood was distilled in the presence of the acid. In
Runs 3 and 4 the lower yields of acid are undoubtedly
due to the effect of pressure, as noted in previous work.
The catalyzer apparently seemed to have had a detri-
mental rather than a beneficial effect on the acid yield
in this series.
The yields of wood alcohol are quite variable.
Bearing in mind that in previous work with this ap-
paratus the alcohol yields were somewhat lower than
commercial yields and also lower than laboratory
yields in a larger retort,1 several of the runs showed
decidedly more alcohol than the standard in the auto-
clave but not higher than controlled laboratory runs
in the larger retort. The highest yield in the series
was 2.18 per cent (Run 2) as compared with 1.37 per
cent from the standard, an increase of 60 per cent.
Whether the manner of distillation was responsible
for the higher yields or the catalyzer was playing an
Presence of Phosphoric AciD(a)
Gas
Dis-
-Tar-
Acetic
Acid
Acid
Alcohol
ture
5.81
4.56
0.79
1.37
41.35
5.05
4.52
0.40
2.18
45.35
4.65
4. 12
0 41
1.29
39 80
4.55
3.98
0.43
1.46
36 . 00
5.30
4.20
0.84
1.81
34.00
solved Settled
22.66 5.36 3.14
13.85 1.85 Neg
13.40 1.17 Neg.
14.03 0.45 Neg.
15.15 0.72 Neg.
important part in the reaction cannot be determined,
although the data would indicate the latter.
The distillation of wood in the presence of an acid
catalyzer has a marked effect on the tar, on the char-
coal, and on the pyroligneous acid (including only
the water formed by destructive distillation). The
tar which usually settled out of the pyroligneous acid
is apparently practically destroyed and the tar nor-
mally dissolved in the acid liquor is reduced at least
50 per cent in most of the runs distilled at atmospheric
pressure. Previous work showed that pressure alone de-
creased the tar very much, so it was to be expected that
distillations under pressure in the presence of the acid
catalyzer would give even smaller yields of tar. Part
of the tar can, no doubt, be accounted for by the higher
yields of charcoal which averaged about 44.5 per cent
compared to a normal of about 40 per cent, although
since no appreciable amount of tar coke was noted in
the retort any coking of the tar must have taken place
in the charcoal or, in other words, the tar was decom-
posed practically in the wood at the moment of forma-
tion. Pari of the tar can also probably be accounted
for in the pyroligneous acid which was increased from
35 to 40.5 per cent, as during the analyses of the dis-
tillates, especially after neutralization with alkali,
much larger amounts of creosote oil than usual were
1 See apparatus described in tes
T (1913
1 temperature control. This Journal.
266
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 4
noted in the distillate. No qualitative or quantita- Runs 7, 8, 9 and 10 all showed decidedly more alco-
tive study has been made of this oil, but the yields hoi, the increases being 88, 80, 60 and 51 per cent,
and properties compared to normal creosote will be respectively, based on the assumed yield of 1.37 per
thoroughly investigated. cent. Apparently the alcohol yield increases with
The increase in charcoal and oils in the acid liquor an increase of catalyzer up to 5 per cent catalyzer,
does not, however, account for all the tar, especially the yield falling off slightly with higher percentages of
since the gas yield is lower than normal, so it is ap- catalyzer. This is shown in Table III.
parent that some other factors are entering into the The yields of alcohol from Runs 7, 8 and 9 are all
reaction. appreciably higher than the highest yields obtained in
beech — The results with beech chips using phos- the larger retort,
phoric acid as the catalyzer are given in Table II. In (b) Pressure Higher than Atmospheric — Runs
this series a more comprehensive study of variables 11 to 14, inclusive, were all made under constant
was attempted. pressure (no lbs.) and moisture (about 60 per cent)
Run 6 was made without a catalyzer at atmospheric conditions, but with variable amounts of catalyzer,
pressure. Unfortunately, no previous work has been The yield of acids apparently bears no relation to
done with beech in the autoclave with which the yields the amount of catalyzer. In this series, however, the
from this run, which was made as a standard, can be first marked effect of hydrolysis on the yield of acid is
compared. The results are quite different from pre- noted. Run 12 gave 16.05 per cent total acid and
vious work with beech in the large retort, which gave 13.82 per cent acetic acid, an increase of 128 per cent
1.87 per cent alcohol and 5.87 per cent total acid total acid and 169 per cent, or 2.7 times the acetic
compared with the autoclave run of o. 99 per cent alco- yield from Run 6, the standard. What conditions re-
hol, 7.03 per cent total acid and 5.13 per cent suited in such a remarkable yield cannot be determined
acetic acid. We will assume an alcohol yield of 1.37 until further work is done. The yield of formic acid
per cent instead of 0.99 per cent standard, since this was also higher than normal but the proportional
was the yield obtained from maple chips in the auto- increase was less. This may be due to the fact that
clave. This assumption can be reasonably made be- the maximum formation of formic acid takes place
Table II— Distillation op Beech in Presence op Phosphoric AciD(a)
Max. Temp. Pyro. Acid . Tar .
Run Catalyzer Retort Bath Pressure Less Dis- Total Acetic Formic Wood Mois-
No. Per cent Degrees C. Lbs. Moisture Charcoal Gas solved Settled Acid Acid Acid Alcohol ture
6 0 320 470 0 35.80 40.30 19.05 7.70 4.79 7.03 5.13 1.47 0.99 39.15
7(6) 4.79 325 470 0 35.91 40.70 16.43 1.92 Neg. 6.76 5.20 1.20 2.58 138.90
8(6) 4.96 321 470 0 39.38 44.85 15.77 2.11 Neg. 6.60 6.45 0.11 2.20 84.70
9(6) 9.73 325 450 0 36.57 40.25 16.25 2.25 Neg. 6.96 6.70 0.19 2.47 135.90
10(6).... 2.63 333 465 60 34.73 44.55 26.62 1.25 Neg. 6.68 5.12 1.19 2.07 143.70
U 1.25 326 470 110 41.72 44.90 11.85 1.09 0.29 4.56 4.33 0.20 1.44 58.25
12 2.45 331 465 110 39.77 46.45 13.75 1.52 Neg. 16.06 13.85 1.72 2.00 59.30
13 4.85 327 465 110 41.26 44.20 14.54 0.70 0.20 3.58 2 43 0.88 1.33 58.50
14 20.78 326 465 110 37.81 45.20 16.79 0.90 Neg. 6.55 5.33 0.93 2.37 58.10
(a) Results are all in per cent of dry charge. (6) Charged from hot retort, carbon equals 5 per cent for Runs 7. 8 and 9.
cause beech and maple gave practically the same more readily than the formation of acetic acid, the
alcohol yields in the larger retort, and this yield is yield of formic acid, therefore, representing more
more plausible than the lower figure. nearly the maximum possible yield. In the hydrolyza-
(a) Atmospheric Pressure — Runs . 7 and S were tion of hardwood with sulfuric acid for the production
made under the same conditions except moisture con- of sugars, the proportion of formic to acetic acid is
tent, and in Runs 7 and 9 the only variable was the often much higher than by ordinary destructive dis-
amount of catalyzer. In all of this group the total tillation, indicating that the decomposition of the sugars
acid yields were slightly less than the standard, but or whatever is the source of the formic acid takes place
the acetic acid yields were 25 and 30 per cent higher, more readily than the formation of acetic acid. The
respectively, for Runs 8 and 9. Run 7, however, yields of total acid are not higher than normal in any
gave practically the same acetic yield as the standard. of the other runs of this group. In fact, Runs n and
Other work has shown that the presence of an excess 13 gave exceptionally low yields of acid,
of water in beech wood tends to give more formic acid, Table hi
which may account for the fact that Run 7 with the £un „„ . ,Ca,t^yzcr„J „ Yicld °J 5lcoholJ
J ' No. Per cent of dry wood Per cent of dry wood
higher moisture content gave more formic acid. The 6 0 0.99 (assumed 1.37)
data also indicate that as the amount of phosphoric 7 4:79 1%
catalyzer is increased, as in Run 9 compared with 2-47
Run 7, the tendency is to form less formic acid, the The alcohol yields for this group are all higher
moisture content being the same in both cases. Run than the actual normal, but only Run 12, which gave
10 practically belongs to this group, except that it was the high acid yields, and Run 14. with 20. S7 per cent
run at 60 lbs. pressure, all other conditions being the of catalyzer, gave appreciably more than the assumed
same, and it may be noted that this run with the normal of 1.37 per cent alcohol. Run 12 gave 46
higher moisture content showed the same tendency to per cent more and Run 14 about 73 per cent more
give a high formic acid yield, as in Run 7, the yields alcohol than the assumed normal.
of acetic and formic acids being practically the same for The same tendency as noted in the case of maple
both of these runs. to give higher yields of charcoal and pyroligneous acid,
Apr., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
267
lower yields of soluble tar and negligible yields of set-
tled tar, using H3PO4 as catalyzer, was also noted on
all of these runs with beech, although the effect on
the charcoal and pyroligneous acid was not so marked
as with maple, especially when the distillations were
made from a hot retort. Larger amounts of soluble
creosote oil than normal were also noted during the
analyses of the pyroligneous acid.
In the distillations from a hot retort the deposition
of a very finely divided carbon in the outlet pipe was
noted in several runs, amounting to as much as 5
per cent of the dry weight of the charge. This
material was probably the result of decomposi-
tions of tar. No microscopic or chemical examina-
tion was made of the material, but this is now being
done.
THE DISTILLATION OF WOOD AND TAR MIXTURES
A series of runs were made distilling beech chips which
had previously been saturated with crude beechwood
creosote. The results are given in Table IV. The
runs were all made from a hot retort. In Runs 15,
16, 17 and 18 the conditions were practically con-
stant, except for pressure.
The yield of total acid varied considerably in these
runs but was not higher than normal in any case.
from that added to the charge it was necessary to make
the assumptions given in the table, knowing in general
the effect of pressure alone on the tar formed from
the wood.
In distilling the wood and creosote under pressure
difficulty was experienced in maintaining the pressure
to the end of the distillation and it was always neces-
sary to relieve the pressure when about two-thirds
of the total distillate had been recovered, but a large
volume of the distillate always came over during the
blowing-off of the pressure. Coking always took
place when the pressure was relieved, not before, and
although the decreasing of the pressure should have
lowered the temperature, the temperature in the
retort did not fall until enough time had passed
after the pressure was gone for coking to take
place, showing the exothermic character of the coking
reaction.
The fact that methoxy groups can be split off from
the tar by distillation under pressure was indicated
by a change in the physical properties of the oil.
Fractional distillation of the tar before and after the
runs showed that the tar from which methyl groups
had been apparently split off contained high boiling
fractions whose specific gravity decreased with in-
Tablb IV — Distillation of Beech in Presence op Wood Creosote and Mixtures of Creosote and Acids
Wood Alcohol
Per
From
Equal
Ac-
Es-
Pyro. Wood
cent
Per
Parts
tual
tima-
Acid Char-
Tar Re-
Cent
Wood
Per
ted
Per cent
Temperature
Less coal
covered
Tar
and Tar
cent
from
un Catalyzer
Retort Bath
Pressure
Mois- Esti-
Wood
Total
Based
Dry
Tar
0. Tar Acid
Degrees C.
Lbs.
ture mated
Gas
Oil(i>)
Coke(c)
Acid
on Wood
Wood
Only
Moisture
>... 103.0 None
327 475
0
25 . 80 44
24.20
72.70
7.07
6.72
1.37
1.37
0
7.60
>. .. 106.5 None
313 440
30
31.30 44
20.70
58.10
37.95
5.35
2.83
2.87
1.46
7.80
'... 120.2 None
321 440
60
32.10 44
21.90
44.10
39.70
5.56
3.12
3.40
1.75
7.80
!... 112.2 None
334 470
90
31.09 44
24.36
39.65
51.00
6.50
3.47
3.66
2.10
11.26
H,POi
>... 99.2 2.55
321 470
60
32.23 44
21.77
62.95
49.20
6.87
1.03
1.03
10.12
(a) Results are all in per
cent of dry charge. (6) Estimated from assumption
that tar formed by distillation of wood =»
15 per
cent at 0 lb.; 8 per
cent at 30 lbs.; 5 per cent at 60 lbs.; 3.5 per cent at 90 lbs. for Runs 15, 16, 17 and 18, respectively, and 1.25 per cent for Run 19. (c) Estimated from as-
sumption that wood charcoal = 44 per cent.
The yield of alcohol, however, increased with pressure,
the increase following a definite curve. The yield at
90 lbs. pressure for equal parts of wood and creosote
figured in percentage of the dry weight of the wood
was 153 per cent or 2V2 times as much as the yield ob-
tained at atmospheric pressure with equal parts of
wood and tar. Taking the yield from wood alone
under these conditions as 1.37 per cent alcohol, as
obtained in Run 15, the yield from tar alone was 2.1
per cent. Analyses of wood tar1 have given 11.08
per cent methoxy group for crude creosote (195-255°
C). The results indicate then that the distillation
at 90 lbs. pressure will split off about 20 per cent of
these groups as methyl alcohol. Higher pressures
would probably give better yields, but the use of higher
pressures is restricted because of the loss of tar as
coke. Since 70 per cent of the increase in alcohol is
obtained at 30 lbs. pressure the lower pressures are
more desirable because of the higher recovery of oil.
The original tar contained 77V2 per cent oil and 22V2
per cent pitch, so the recovery of oil was 75 per cent
for the run at 30 lbs. pressure. As it was not possible
after distillation to differentiate between the tar formed
by the distillation of the wood and the tar recovered
1 Pieper, Humphrey and Acree, This Journal, 9 (1917), 566.
crease in boiling point, a most unusual property for
wood tars. These fractions are being examined for
acid phenols, which are likely to be present after
splitting off the methyl groups from the phenol
ethers.
Acetone determinations made in these studies
showed that in no case was more than 0.5 to 1 per
cent of the alcohol acetone and in Run 20, which gave
the highest yield of alcohol, only 0.12 per cent of the
alcohol was acetone. It should also be mentioned
that in all of the tests with acid catalyzers the
acetone yield was seldom over 1 per cent of the
alcohol and generally less than 0.5 per cent of the
alcohol.
wood tar and phosphoric acid — The effect of the
acid catalyzer on the tar formed in the normal dis-
tillation of wood has been noted above, the settled
tar, which is the source of wood creosote, being prac-
tically destroyed. The effect of a combination of
creosote and an acid catalyzer at once suggested itself
as an additional means of splitting off methyl alcohol,
and Run 19, using tar and phosphoric, was made to
study that effect. The chips were first treated with
acid and then allowed to dry out to about 10 per cent
moisture and were then treated with creosote. The
268 THE JOURNAL OF INDUSTRIAL AND ENGINEERING < EEMISTRY Vol. 10, No. 4
results anticipated were not obtained as the alcohol SOME EXPERIMENTS ON THE PULPING OF EX-
yields were no greater than normal. It would seem TRACTED YELLOW PINE CHIPS BY THE
then that the action of phosphoric acid on the tar is SULFATE PROCESS
probably much more severe than splitting off of meth- ">' O"o Krkss and Clinton k. textob
oxy groups, and is more likely the immediate forma- Received September 4. 1917
tion of hydrocarbon gases and coke. The work along introduction
this line is being extended, making tar-phosphoric Some time ago the Forest Products Laboratory was
acid distillations at lower temperatures to sec if the asked to determine whether longleaf pine chips, after
destructive effect can be less: the extraction of rosin and turpentine, would be suit-
Several distillations were made using sulfuric acid able for the manufacture of kraft paper. This suggested
as a catalyzer along the lines suggested by German ltself inasmuch as commercial kraft is being made
Patent 185,934, but instead of getting increased from lonKIeaf Pine and the removal of rosm should be
yields of acid and alcohol it was found that, especially an advantage provided th. no other factors
under pressure, the acids were decreased and no alco- entering. Extracted chips are only used as fuel under
hoi at all was formed. Indications were obtained the boilers at the extraction plant and any excess over
that the S02 formed by the reduction of the sulfuric fuel requirements is a complete waste. If they can be
acid acted very detrimentally in the destructive dis- converted into a by-product, the waste will be a source
tillation reaction. of ,ncome whereas its disposal is now an expense.
DESCRIPTION OF TF.ST MATERIAL
CONCLUSIONS
In preparation for extraction, the raw wood, hogged
The general conclusions to be drawn from these to the proper size, is placed in iron extractors, which,
preliminary tests are: in this particular case, are not designed for pressure
I — Under the proper conditions a very high yield extraction, and steamed about 3 hrs. for recovery
of acetic acid may be obtained by the destructive of crude turpentine. After this preliminary steaming
distillation of wood, by using phosphoric acid as a treatment, the extractor is filled with hot gasoline, 58
catalyzer. Two and seven-tenths times as much acid to 6o° Be. and extracted for approximately 5 hrs.
as normal was obtained in one run. Two solvent drops are taken off and the chips are then
tt ti,„ j;-+;h.,+.-,.., „f „.™j ■„ n,„ „,„„ „t washed with fresh solvent, this wash being used on the
11 — 1 he distillation of wood in the presence of °
,,--j,j j.j next extractor. The solvent solution containing the
phosphoric acid showed a pronounced tendency to . . &
j , v. , t r rosin and pine oil is evaporated first for recovery of
give more wood alcohol. Increases varying from v p -
,„ . _„ „__+ „rQ„ „v+„;__j solvent, then for pine oil, while the residue of rosin is
40 to 90 per cent were obtained. ' *
run into barrels for shipment.
Ill— The distillation of mixtures of wood and tar After th(, solution of gasoline and pine oil is all re-
under pressure showed that the methoxy groups in moved from the extractor and after draining for one
the tar can be readily split off, forming wood alcohol. hour tQ remove as much as possible o{ the above mix-
Nearly 20 per cent of a possible theoretical was ob- ture> the extractor is steamed for 5 hrs. to recover sol-
tamed at 90 pounds pressure. The work is being ex- vent The first parl of the steaming occurs with wet
tended to include a study of many other catalyzers steamj while the ,ast half is with superheated steam.
and variables. _,, ... ,
The average yield per ton of wood extracted on a
The recovery of the metaphosphoric acid residual car weight basis is:
in the charcoal, which is readily soluble in cold or hot Rosin 250 pounds
water, could in all probability be made practically Sudlp^Sf!"? -gi'ionl
quantitative by simple leaching. Just what recovery
can be made is being studied. The total amount of chips handled at the plant with
which the Laboratory cooperated on these experiments
The experiments described are only preliminary is 400 tons per day, of which 300 tons are burned under
laboratory investigations, and no attempts will be the boilerSi leaving IOO tons available per day.
made to commercialize the ideas developed until _, T , ,
, ., 11 Tir-ii. .u The Laboratory received a shipment of 1,000 lbs.
further work is done. \\ lth the quantitative recov- , ., ... ,. . r , ,
c , . . ., .. . . ... of "spent wood chips, as thev come from the extractor,
ery of phosphoric acid its use as a catalyzer would be , ,, . ... J . . ,,
„„+•,„!„ „-„ *• 1,1 1 .u r .• c 1.1. j and 5°° lns- of fresh chips which had not been ex-
cntirely practicable and the application of these ideas - _, . , , ,
, , ., ...... r .. . . tracted. We were informed that the original chips
would seem to open up the possibility for the destruc- , • , ., ,
.• j;„4.mi .• c 11 r r j im. contained 12 to 13 per cent moisture, while the ex-
tive distillation of small forms of wood waste. The . . .. . , „
„ ■ , .. , ,., c .u j- i'ii c j tracted chips contained iS to 19 per cent moisture,
commercial practicability of the distillation of wood „,. , . , , . , , . , , ..„ , ,
- . • . , , , . .. , These chips had been treated slightly differently from
and tar mixtures would be 111 the same direction and , ,. ... . .,
, „ , ., , , , , ... the ordinary run of chips, as in the usual practice satu-
depend on the recovery of more valuable constituents . . . . ... , . ' , ,
c .. •■ „ .. . . ,, , , , , , rated steam is admitted to the extractor for ten minutes
of the oil as well as a high yield of wood alcohol. ... . .. .
p.,.. . „ ,• „.• . v. j , .. ., ,- preliminary to opening the digester. This treatment
Patent application has been made by the author for . .. .
.. , , . , , ',.,,. is given to avoid danger of hre.
the protection of these ideas, the patents being dedica-
ted to the public. PROCEDIRK
Fokbst Pkoddcts i.A„„K,ToRv preparation of thk wood- The chips from a super-
Madisdn. Wisconsin ficial examination showed a large percentage of dust and
Apr., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
269
small slivers, which in any chemical pulping operation
would consume cooking chemical and give practically
no yield of pulp.
A 10-lb. sample of the extracted chips was screened
through a series of screens, with progressively smaller
openings and the amount passing through each screen
weighed. The data from this test are shown in Table I.
Unfortunately, such screening does not show the
proper results as the chips are all of great length in
comparison with their diameter. This means that
only such slivers as struck the open mesh of the screen
head-on passed through that particular screen. The
as used in commercial practice for soda and kraft
pulping with the exception that the bottom of the di-
gester is steam jacketed. Only a small amount of
steam was admitted to the jacket to counteract any
excessive condensation. Further, the digester is fitted
with a pump to circulate the cooking liquor during the
digestion. The relief line from the digester leads to
a, cooling coil in a condenser for the purpose of separat-
ing and condensing all volatile products. The digester
is manipulated in a way similar to those in commercial
operation. After the cook was blown and washed,
yield determinations were made. The pulp was then
Table I — Screening Tests on a 10-Podnd Sample (Bone-Dry Weioht) Unextracted Chips
Number of fract
Through size
On size screen
Size of screen opening 0.4.V
Weight of fraction (moist). lbs 0.5870
Percentage (bone-dry) 91.1
Weight of fraction (bone-dry), pounds 0.5.15
Percentage (moist) 5 . .18
Percentage (bone-dry) 5.35
0.271"
1.5700
91.1
1 .43
14.39
14.30
V."
No. 8
0.099"
4.9350
89.7
4.43
45.20
44.30
No. 20
2.4255
91.9
2.325
22.20
23.25
0.930
8.35
8.30
0. 191
1 .92
1.91
0.0705
0.71
0.71
No. 100
0l0555
0^0505
0.61
0.61
0.1440
IM.M
1.32
1.31
(o) Screens marked No 8. No. 20. No. 40. No. 60, No. 80. No. 100 indicate the number of meshes to the inch
proper screening of the chips is extremely important,
as small slivers will give practically no yield of pulp,
but will consume cooking chemicals during the pulping
operation.
The ordinary chip screen as used at the Laboratory
for screening pulp chips was far too coarse to properly
screen this material and so a flat screen was made of
wire having 12 meshes to the inch, with openings about
screened, using a 6-plate diaphragm screen with slots
0.009 bich wide. The pulp after thickening and beating
was run into the form of paper or board over a 15-inch
Pusey and Jones, Fourdrinier machine. .The papers
were run unsized and uncolored as all the pulps are
run at the Laboratory for testing purposes in the form
of waterleaf sheets. Further, having no cylinder
machine at the time these tests were made, the boards
0.08 inch diameter. In many cases, slivers with small were made by winding up the paper on the first press
enough diameter to pass through the screen, would not of the Fourdrinier machine, which, of course, gives
be removed unless they happened to strike the screen poor lamination. The results of the tests are given in
opening head-on. By means of this flat 12-mesh Table II.
Ta
BLE II-
-Pulping T
:sts on Extracted Chips
Usinc
the Kraft
Process
0 v
0*-»
c.=.s
C * U
a,
Wood
Cook
ing
g
Duration of Cook
S
a
upq
<A
0
a 5
£i a
72
s
S
P
6
Z
0
0
J
'5
a.
a
I.iqu
S
X
0
H
■v
0
ft
3
312
5-g
aft
3
Oft
— 3
>
■J) M
>
ft
J5 S
uft
>
-a
'J
0
b
H
ft
6
0
t°
2 a
Hi
<
M
"a
WJ"13"
<
1
<
a
U
Z
%
aji
X-|
z
i
U vi
z
Extracted
247
76
84.7
87.5
13. 13
3.47
80
4.00
1.00
3.0
36.3
0.53
35.47
No
Yes
42.5
43.0
0.74
0.74
4.34
3.99
0.72
0.80
3.45
3 25
5175
5060
726
622
Extracted
248
76
88.5
87.5
13. 14
3.35
80
4.18
1 . 18
3.0
36.6
1.1
35.5
No
Yes
44.5
44.0
0.77
0.72
4.33
4.04
0.79
0.78
3.60
3.30
5012
4970
614
525
Extracted
249
76
84.0
86.0
11 .70
3.64
80
3.9
0.9
3.0
42.2
8.2
34.0
No
Yes
43.0
43.0
0.68
0.61
5.11
3.87
0.57
0.67
2.95
2.50
4340
3995
352
273
Extracted
250
76
84.0
85.0
15.83
4.75
80
3.8
0.8
3.0
35 . 3
0.5
34.8
No
Yes
43.0
43.0
0.65
0.63
4.42
3.61
0.63
0.75
3.00
3.30
5440
5020
414
359
Extracted
251
70
84.97
86.3
13.65
4.08
80
3.9
0 9
3.0
36.4
1 .2
35.2
No
Yes
38.5
38.5
0.69
0.64
4.03
3.52
0.66
0.70
3.30
3.05
4995
4810
447
377
Extracted
252
67.6
57.85
58.6
13.52
4.02
80
4.35
0.85
3.5
41.15
2.02
39. 13
No
Yes
38.5
38.5
0.60
0.61
4.15
3.37
0.63
0.69
3.20
2.60
4670
4250
33S
260
Extracted
253
65.8
83.26
86. 1
11.09
2.60
100
2.75
1.25
1.5
43.8
Not sc
reened
This
vas not run as
paper,
but wa
s made
into
board
Fresh wood
254
63.7
86.45
88.65
1 I . 50
2.78
80
4.4
0.9
3.5
33.2
2.02
31 .2
No
Yes
38.5
38.5
0.62
0.60
4.17
3.49
0.57
0.66
2.85
2.80
4720
4510
363
312
Fresh wood
255
70.8
88.10
88.50
1 I 48
2.79
80
4 8
0.8
4.0
41.4
13.5
27.9
No
yea
41.0
40.5
0.38
0.38
5.44
4.57
0.29
0.34
1.80
2.10
3340
2980
64
42
Fresh wood
256
68.4
1 30 . 3
80.4
8.46
2.23
100
2.4
0.9
1.5
51.15
Not screened
This
cook
od coo
was too raw a
nd ira
s not r
in ove
the
' Bone-dry pulp in
per cent
of bone-dry wood cook
cd.
2 Bone-dry sc
reenings in per
cent of bone-dry wo
ked.
screen, 24 per cent by weight of the material screened
was removed. Cooks 247 to 250 gave very low yields
(about 36 per cent), and this is probably due to the
presence of considerable material that was not screened
out preparatory to pulping. For later cooks, the chips
were rescreened, various percentages being removed,
as shown in Table II.
The cooks were made in a 63-gallon upright steel
digester similar to the customary stationary digester
DISCUSSION
One of the most important problems in considering
the feasibility of utilizing extracted yellow pine chips
in the manufacture of paper pulp is the proper screening
of the chips. This phase of the problem could not be
satisfactorily studied for lack of proper screening ap-
paratus and the shipment of wood was far too small to
carry on any extensive experiments along these lines.
As has already been mentioned, dust, shives, and slivers
THE JOURNAL OF INDUSTRIAL AND ENGINEERING I II EMI ST RY Vol. 10, Xo. 4
of wood of small diameter are practically valueless for
pulping purposes as they give no appreciable yield of
pulp but consume cooking chemicals. The extraction
plant handles 400 tons of chips per day, of which
300 tons are burned under the boilers for fuel purposes.
This would make possible the rejection of 75 per cent
of the wood for fuel purposes, while in our experiments
36.3 per cent of the original wood represented the maxi-
mum amount of screenings rejected. The cost of screen-
ing is small and this matter should receive further
study. There is no question that if we had screened
out 75 per cent of the fines and only pulped the com-
paratively coarse chips better and higher yields of
pulp would have been obtained. Further, the ex-
tracted chips were apparently burnt by the steaming
for removal of the oils and rosin, as could readily be
seen by the clean fracture obtained in many cases on
breaking the chip.
Rather surprising yields of oils were obtained by
condensing the relief gases from the digester. The
yield of oil on the extracted chips averaged about 2.3
gallons per ton of bone-dry chips. For cooks 254 to
256, made on the fresh wood, an average of about 6.7
gallons of oil were obtained per ton of bone-dry chips.
The wood during transit and in storage at the Labora-
tory had probably lost some turpentine and other
volatile oils, which will probably explain the discrep-
ancy between these results and those obtained at the
extraction plant.
Cooks 247 to 254 were made on the extracted chips
varying the conditions of pulping as can be seen from
a study of Table II. No special difficulties were ex-
perienced in pulping the extracted chips and the rather
low yield of pulp we believe can be remedied to a large
extent by the selection of only the larger chips through
better screening.
The strength of the paper was low when compared
with that which has been made at the laboratory from
longleaf pine round wood. This weakness, we believe,
was partly due to the small size of the chips in which
the smaller slivers will readily overcook and to the
apparent burning of the chips by the steaming treat-
ment.
Cook 253 was run with the object of preparing a
pulp suitable for the manufacture of a container board.
Cooks 254, 255 and 256 were run on the fresh wood.
In these cooks apparently insufficient alkali was used
to saponify all the rosin and at the same time success-
fully pulp the wood. Cook 255 represents a raw cook,
while cook 256 was so raw that it was not passed over
the paper machine. Cooks 254 to 256 are of very
limited interest, as they represent pulping tests made
on chips of so high an oil and rosin content that com-
mercially they would be extracted before pulping.
While the above experiments indicate that a com-
mercial grade of kraft pulp might be made from long-
leaf yellow pine extracted chips, it is evident that the
best results will be obtained if the chips are carefully
selected by means of a proper screening system, by
using the largest chip for extraction compatible with
maximum recovery of the oils and rosin, and by avoid-
ing as far as possible the burning of the chips in the
preliminary steaming for removal of turpentine and
rosin.
Forest Products Laboratory
Madison, Wisconsin
THE PRODUCTION OF NITRIC ACID FROM NITROGEN
OXIDES1
By Gcrv B. Taylor, Julian H. Capps and A. S. Coolidge
Received February 14, 1918
Practically all processes for the fixation of atmos-
pheric nitrogen wherein the ultimate product desired
is nitric acid involve recovery of nitrogen oxides. The
arc and ammonia oxidation processes produce these
gases largely diluted with air or nitrogen. Converting
the nitrogen oxides into concentrated nitric acid re-
quires an extensive equipment and is a considerable
item in the cost of manufacture.
The usual industrial procedure is to pass the gases
containing nitrogen peroxide (NOj) with an excess
of oxygen through a series of large packed towers
and absorb the nitrogen oxides in water. The strength
of the circulating acid varies in each tower, the first
producing acid of 30 to 50 per cent concentration, de-
pending on the concentration of NO2 in the gas, while
the last is almost entirely water. The diluter acids
are moved up from tower to tower as their concentra-
tion increases so that the whole of the product is con-
centrated as far as practicable. This acid is further
concentrated, when required, by means of distillation
from sulfuric acid.
While the use of water as an absorbent produces
nitric acid direct, it has certain disadvantages. The
tower space required is very large and storage tanks,
pumping lines and auxiliary equipment for handling
the dilute acids must be made of special material to
resist attack. The acid produced must nearly always
be concentrated further. Also it is practically im-
possible to absorb all the nitrogen oxides by any sys-
tem of towers of reasonable size and number. In
some plants a tower circulating caustic soda or sodium
carbonate solution is installed at the end of the sys-
tem to recover the last traces of acid.
There have been a large number of patent claims
for processes involving the working up of nitrogen
oxides. Alkaline solutions are mentioned frequently
both for the production of nitrates and nitrites. It
has also been proposed to recover the nitrogen oxides
in concentrated form from alkaline solutions with
regeneration of the alkali. Proposals* for freezing
out NtO« do not seem commercially practicable.
Patents' are held on a process for concentrating nitric
acid by means of liquid nitrogen peroxide. An elec-
trolytic process for concentrating dilute acid is pro-
posed in a patent* held by the Salpetersaure Industrie
Gesellschaft wherein NO evolved at the cathode is
led into the anode space for re-oxidation. Classen'
1 Published with the permission of the Director of the U. S. Bureau of
Mines.
1 W. Ramsay. British Patent 26.981 (1907); P. A Guye, U. S. Patent
1,057,052 0910).
' M. Moest. D. S. Patent 1.180,061 (1907); L. Friedrich. British Pat-
ents 319 and 40J (1911).
« British Patent 18,603 (1906).
• British Patent 18.065 (1915).
Apr., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
suggests the use of catalyzers, nickel or cobalt oxides
and nitrates, for promoting the oxidation of NO to N02.
Among the more prominent methods proposed for
the recovery of nitrogen oxides is that of absorption
in rather concentrated (90 per cent) sulfuric acid
with subsequent removal of the oxides of nitrogen
by heat or denitrifying agents. The concentrated
gas thus obtained is reabsorbed in the presence of air
in water to form nitric acid.
In some experiments in this laboratory on absorb-
ing nitrogen peroxide in sulfuric acid containing chromic
acid, it was found that nitric acid was produced di-
rectly and if the absorbing liquid is maintained at
150° C, the acid issues from the system as a mist
which, when precipitated, is 95-100 per cent HN03.
Such a process has two drawbacks: the necessity for ab-
sorbing in a hot solution and the electrolytic recovery of
chromic and sulfuric acids from chromium sulfate. A
number of experiments were made in an attempt to
produce a strong mixed acid by electrolysis of solu-
tions of N02 in concentrated sulfuric acid. If the
nitric oxide from the oxidizer in the presence of excess
of air is cooled and allowed sufficient time to react
wholly to NO2, then its reaction with concentrated
sulfuric acid may be written:
zN02 + H2SO4 = HNO3 + HNOSO4
Theoretically upon electrolysis this reaction may
take place:
HNOSO, + 2H0O =
HNO3 + H2S04 + Ho + 2 faradays
This reaction is an ideal one since it also removes
water by reaction and concentrates the acid. The
power required is not great. In attempting to realize
the reaction experimentally platinum electrodes were
used and alundum thimbles as diaphragms. It was
found that at low concentrations of nitrososulfuric
acid, equivalent to 10 per cent HNO3 in a mixed acid,
a current efficiency of 50 per cent could be obtained
for a short time. However, as the concentration of
nitric acid in the solution increased, the efficiency
dropped to a small value. Even when using 95 per
cent sulfuric acid in the cathode chamber, nitric acid or
nitrososulfuric acid diffused through the diaphragm
and was reduced to NO and some free nitrogen. The
nitrogen represents a loss of acid which might be pre-
vented with efficient diaphragms. However, elec-
trolysis of solutions containing the equivalent of nitric
acid ordinarily used in nitrating acids did not work
at all.
ABSORPTION BY WATER
The chemical reactions involved in the conversion
of nitric oxide, which is produced by both the arc and
ammonia oxidation processes, to nitric acid are es-
sentially as follows:
2 NO + O, Z£±. 2N02 (1)
2 N02 + H20 ^±1 HN03 + HN02 (2)
3 HNOi ^± HNO3 + 2 NO + H20 (3)
The NO arising from Equation 3 reacts with oxygen
and the cycle is repeated. A full discussion of these
reactions is given by F. Foerster and M. Koch.1
' Z angew. Chem.. 21 (1908), 2161.
The reaction expressed by Equation i begins to
proceed in the direction from left to right when the
gases are cooled below 600°, but will not go nearly
to completion even in a large excess of oxygen until
200° is reached as shown by calculation from the
equilibrium formula. However, it has been shown
by Foerster and Blich1 that this reaction has a nega-
tive temperature coefficient so that the gases must
be cooled as far as practicable before entering the ab-
sorption system. It has also been shown that this
reaction occurs in distinctly measurable time.2 Hence,
it has been found necessary to allow the gases to pass
into a large empty chamber or oxidation tower in order
that the nitric oxide may react completely to nitrogen
peroxide before the gases enter the absorption system.3
An absorption system proposed by Moscicki4- [British
patent 17,355 (1911)] in which the gases are passed
horizontally and at right angles to the acid flow inserts
an empty oxidation space between successive units.
EXPERIMENTAL
The experiments described in this report were made
with a small experimental plant used in experiments
to determine the efficiency of metallic gauzes as cata-
lyzers for ammonia oxidation. It may be stated
at the outset that it was fully appreciated that the
results obtained could not be strictly carried over
to an industrial operation on a thousandfold larger
scale, especially as to the ratio between tower space
and capacity, but it was thought that the relative
importance of acid concentration in the several towers,
temperature, speed of passage of the gases and cir-
culation of the absorption liquid, oxygen excess re-
quired, etc., could be obtained, and that many de-
tails might be worked out that would be of value in
operating a larger system. Such details are gener-
ally regarded as legitimate industrial secrets and are
almost never published. There is practically no in-
formation of a detailed nature available in this country
dealing with gases as rich as those produced in am-
monia oxidation on any sort of an efficient absorption
system.
The apparatus consisted essentially of an ammonia
saturator for securing a mixture of air and ammonia,
an oxidizer utilizing a platinum gauze, 3X6 in., for
producing nitric oxide and an absorption system con-
sisting of a cooler and five stoneware towers. The ab-
sorption system is shown diagrammatically in the ac-
companying sketch. The gases from the oxidizer
passed through an iron pipe into the Pyrex glass tubes
of the cooler. These 3/.,-in. tubes were arranged
in two sets of three U-tubes each, in parallel. The
cooling water was continuously passed through the
housing box which was 30 X 24 X 24 in. Each U-tube
was provided with a drain for condensate and liquid
sealed with a test-tube. From the condenser the gases
passed to Oxidation Tower o and then in turn to
> Z. angew. Chem., 23 (1910), 2017.
« W. Holwech, "Uber die Reaktion zwischen Stickoxyd und Sauerstoff,"
Ibid., 21 (1908). 2131.
■ E. K. Scott, "Production of Nitrates from Air, with Special Reference
to a New Electric Furnace," J. Soc. Chem. Ind., 84 (1915), 113. An ex-
perimental absorption system with oxidation tower is described.
« E. K. Scott, "Manufacture of Synthetic Nitrates by Electric Power,"
Ibid.. 36 (1917), 774.
272
THE JOURNAL OF INDUSTRIAL AND ENGINEERING < HEMISTRY Vol. 10, No. 4
the bottom of the coke-packed Towers 1, 2, 3 and
These towers are of the following dimensions:
Height 6 ft.
Diameter inside 10 in.
Ca
•ity
ft.
- II 4" ,
1 4(1 ,
1.90 (
Tower packed with coke >'/■-' ft. at .SO percent free space.
Reaction space above coke and in connecting pipe
Reaction space provided by the Oxidation Tower II. b
pipe connecting to Tower 1
Reaction space in each coke tower
Total reaction space in the system (not counting space above
coke in Tower 4) = 10.60 cu. ft.
The coke was irregular in size, most pieces 1 to 2 in. N"o accurate estimate
could be made of the absorbing surface.
The desirability of having such an oxidizing tower
as o for the oxidation of NO was demonstratt'1 in
small scale laboratory experiments. Nitric oxide
from a small oxidizer containing an excess of oxygen
was cooled to room temperature by means of a Liebig
condenser. By means of suitable stopcocks the cooled
gas could be passed through a 7-liter glass vessel into
a small glass coke-filled tower or by-passed around
the vessel. Forty per cent nitric acid was circulated
rapidly through the tower and the efficiency of ab-
sorption determined by samples, as will be di
later. In the following tabl of the gas
were taken with the reaction space in circuit and then
immediately thereafter with the space cut out si 1 that
all other conditions were the same.
Liters
Total \i"i
Removed
before Tower
Pet •<-iii
Bffi
of To
Pet o
1.8
i.a
Out
1.8
These results show clearly that at the higher velocity
the reaction space increased the efficiency of the tower.
The wet walls of the reaction space absorb acid and
hence the gases enter the tower less concentrated
than in cases where it was not used, but this fact
does not affect the general conclusion that the oxida-
tion space is useful.
The rest of the system needs little explanation.
The acid was circulated by sucking up through glass
lines into the feed bottles with a filter pump. Each
bottle was provided with an automatic glass valve
which closed under suction. The distributor at the
top was a type manufactured by M. A. Knight in
which acid overflows through 8 small holes arranged
in circle.
mi rutin .1] 0P1 RATION
Air was metered and passed through the ammonia
saturator so as to make a mixture containing 8 to 1 1
per cent ammonia. Auxiliary air. also metered, was
added at the point .1 just below the oxidizer. By con-
trolling the relative volume of air and the composi-
tion of the ammonia-air mixUire. any desired
excess could be obtained in the absorption system.
The performance of each tower was determined
by taking gas samples from the sample holes C. At
B a sample was taken, where the gas was still hot and
before any condensation could have taken place.
which represented the total acid entering the sys-
tem. The samples were taken into evacuated glass
bottles of 1 or 2 liters capacity. Each bottle was
provided with a ground glass stopper carrying a capil-
lary stopcock. After taking the sample, a measured
volume of water containing hvdrogen peroxide was
introduced into each bottle to absorb the acid and
sufficient to bring the resulting nitrogen-oxygen mix-
Apr., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
273
ture to atmospheric pressure. The volume of the
bottle, minus that of the introduced reagent, gave
the volume of gas, which, together with its anal-
ysis, furnished the necessary data required to cal-
culate the volume of nitrogen present. The acid
was titrated with N/y NaOH. Since nitrogen does
not react and is constant throughout the system,
it is evident that it may be used as the reference
point and the efficiencies calculated from a knowl-
edge of grams of acid per liter of nitrogen. It was
not found practicable to base any conclusions on
measurements and analyses of the acids produced
in each tower since the packing held up an indefinite
quantity, and the runs were not long enough to re-
duce this source of error. The plant was operated
6 or 7 hrs. per day.
Run 1 — Preliminary run to make acid for future experiments. Acid was
added to first tower and the rest allowed to build up. Samples were
taken to determine relative effects of velocity of gas and oxygen con-
centration.
Cooler — water cooled.
Acid circulated through towers continuously 6 to 15 liters per hour.
Run 2 — Dec. 5, begun 2:00 p.m., closed 4:20 p.m.
Dec. 6, begun 9:45 a.m.. closed 4:15 p.m.
Cooler — air cooled.
Rate acid circulation — towers flooded every 30 min. with 4 liters.
Strength of acid condensed in cooler — 5 per cent HNO3.
Strength of acid condensed in Tower 0 — 30 per cent HNOj.
Run 3 — Dec. 7, begun 10:50 a.m., closed 4:10 p.m.
Dec. 8, begun 9:30 a.m., closed 4:00 p.m.
Dec. 10, begun 9:40 a.m., closed 4:10 P.M.
Dec. 11, begun 9:30 a.m., closed 4:00 p.m.
Cooler — air cooled.
Rate acid circulation — tower flooded every 30 min. with 4 liters.
Strength acid condensed in cooler — 7 per cent HNO3.
Strength acid condensed in Tower 0 — 32.5 per cent HNOa.
Run 4— Dec. 14, begun 10 a.m., closed 3:25 p.m.
Cooler — water cooled.
Rate acid circulation — 8 liters per hour continuous.
Strength acid condensed in cooler — 5 per cent HNOa.
Run 5— Dec. 12, begun 10 a.m., closed 2:15 p.m.
Cooler — 10 to 1:15 p.m., air cooled; 1:15 to 2:15, water-cooled.
Rate acid circulation — towers flooded every 30 min. with 4 liters.
Run r. -Dec. 13. begun 10:30 a.m., closed 4:00 p.m.
Cooler — air cooled.
Rate acid circulation — tower flooded every 30 min. with 4 liters.
Run 7 — Dec. 17, begun 10 a.m.. closed 3 p.m.
Cooler — air cooled.
Rate circulation — tower flooded every 30 min. with 4 liters.
7 per cent XaOH solution in Tower 4.
Run 8 — Dec. 19, begun 9:45 a.m., closed 1:45 p.m.
Same as Run 7, except 30 per cent NaOH solution in Tower 4-
80 to 90 per cent of acid absorbed by alkali is in form of nitrite.
The following tables contain the full data of all
experiments. The date, time, and cubic feet per
hour, and percentage of the total acid absorbed are
given at the moment of taking the samples. In
general, six samples were taken at once giving the
total acid per liter of nitrogen entering the system,
entering each tower, and leaving the last tower.
The temperature of the gas entering each tower and
the specific gravity of the acid in circulation at the
time were recorded. The specific gravity was taken
roughly with a hydrometer at the temperature of
the acid running from the tower. In general, the
acid from the first tower was 8 or io° lower than the
entering gas, in the other towers 2 or 3 ° lower.
DISCUSSION OF RESULTS
Run 3 having demonstrated that the strength of
the acid could be built up in Tower 1 to about 50
per cent without materially increasing the acid loss
from the system, it was considered sufficient in other
cases to take samples with the acid concentrations in
the several towers approximating what they would
be toward the end of a run or the time when the acids
would be moved up to the next tower.
The circulation of the acids through the towers
, was carried out in such a way as to be sure that the
coke packing was always thoroughly wet. This was
done in most cases by periodical flooding, i. c, run-
ning in 4 liters of acid at the top in 10 min. at 30-
min. intervals. After flooding in this manner it
was found that the absorption capacity of the first
tower did not change for an hour or more. In general,
about 10 liters were placed in the jar for each tower
at the beginning of a run. The volume of the cir-
culating liquid increased as absorption took place
in Towers 1 and 2. Tower 1 received part of the acid
indicated as having been removed by Tower o by
the gas analytical results, due to condensation in the
connecting pipe. The volume of acid in circulation
in 3 and 4 decreased, which will be explained later.
temperature — Unfortunately, all our experiments
were made under winter conditions and not much
information was secured on the effect of tempera-
ture, which is probably the most important factor in
determining the size of an absorption equipment
necessary to handle a given quantity of gas. The
small size of the plant did not permit of building up
temperatures on short runs. All experience, how-
ever, goes to show that the absorption should be
carried out at as low temperatures as practicable.
The effect of running the cooler air- and water-cooled
is interesting. When water-cooled most of the water
carried by the gas is condensed out with but little
acid. The gases enter Tower o at room tempera-
ture, about 25°, where they warm up by the reaction
going on between nitric oxide and oxygen. Prac-
tically no acid was obtained from Tower o under
these conditions. When the cooler was air-cooled,
most of the water carried by the gas was condensed
in Tower o together with considerable acid. Arti-
ficial cooling of the gas in the reaction space (Tower o)
would be advantageous.
oxygen excess — When the oxygen in the system
was near the theoretical requirement, there was no
marked increase in the acid loss. However, it is
probably best not to let the concentration of oxygen
in the exit gas fall below 5 per cent.
production and efficiency — The first three towers
(o, 1 and 2) absorb about 85 per cent of the acid
input, the last two only about 10 per cent. At a gas
velocity of about 2.5 cu. ft. per min. doubling the
number of towers would probably not recover the
other 5 per cent.
On a basis of 10 per cent ammonia in the air mix-
ture fed to the oxidizer and go per cent efficiency of
oxidation, 25 per cent auxiliary air must be added
after oxidation to secure an oxygen concentration in
the exit gas of 5 per cunt. This excess may be secured
in industrial operations from the operation of the acid
lifts, but it would probably bo advantageous in add
THE JOURNAL OF INDUSTRIAL AND ENGINEERING ( HEMISTRY Vol. 10. Xo. 4
Towb
R 0
Tower 1
Tower 2
Tower 3
Tower 4
Exrr
a
'<
So
3i
aga
ZoO
Op
1&
3 0
ZoO
1 fi
1 I I-
■z~ So
<
O
6.
NOi per Liter
of Nitroseu,
Gram
cid Absorbed.
Per cent
emp.Hntering
Gas, Deg. C.
<
0
— 0
5 t
ZoC
i ¥■
2 E So
< d„-
■aP fa
:- Sc
<
O
5S§ I8
SO -o
~'i <
t B
-'?
-2. =
5 a
ZoO
■1
I
Date
Time
0
S
<
X
< i-
X •< H
<s>
< i-
w
- <
.- ID
o
<
Oct.
2:
p.m
176
0.2435
9.0
0.2210
65.8 35
1.225
0.0612 14.5 27
1.08
0.0261
4 2 23
1.03
0.0157 ...
'..0
Oct.
24
145
0.2125
7.5
0.1965
55.8 32
1.29
0.0780 24.0 22
1.11
0.0270
4.'; 21
1.03
0.0166 3.0
21 1.01
0.0103
H.5
4 '.
Oct.
25
340
0.2540
6.0
0.2385
42.0 35
1.29
0.1320 30.0 24
1.11
0.0558
8.6 20
1.04
0.0342 5.3
20 1.02
0.0205
7.0
8.1
Oct.
25
P.M
137
0.3160
7.0
(i 2940
37.9 38
1.30
0.1742 34.1 27
1.135
0.0662
7.9 21
1.04
0.0414 3.4
19 1.02
I, 0306
1.6
9.7
Oct.
26
2:30 p.m
107
0.2845
10.4
0.2550
37.4 36
1.30
0.1485 37.2 27
1.155
0.0426
6.4 22
1.05
0.0245 3.6
21 1.025
0.0144
4 "
5.9
Oct.
26
4:00 p.m
172
0.2295
7.0
0.2140 21.0 36
1.30
0.1650 49.5 28
1.165
0.0516
10.1 25
1.055
0.0284 4.7
25 1.025
0.0177
i.ii
7.7
Ron No. 2
Dec.
5
3 :40 p.m
137
0.2890
21.5
0.2270
52.0 40
1.24
0.0765 17.0 24
1.14
0.0275
3.5 23
1.05
0.0174 1.3
22 1.01
0.0137
2.9
4.7
Dec.
6
1 1 :00 a.m
147
0.2997
22.3
0.2322
41.4 41
1.26
0.1089 18.6 26
1.16
0.0531
3.1 25
1.06
0.0437 1.3
23 1.015
0.0398
0
13.3
Dec.
6
1:15 p.m
143
0.2664
18.0
0.2196
43.5 42
1.275
0.1022 23.7 30
1.16
i) niv,,
6.2 24
1.065
0.0231 2.5
21 1.015
0.0164
4.2
'..1
Dec.
6
3:50 p.m
145
0.2745
16.8
0.2286
35.2 43
1.285
0.1314 33.7 38
Ron No. 3
1.18
0.0394
5.3 24
1.07
0.0246 3.3
22 1.02
0.0156
S.O
5.7
Dec.
7
1 1:50 A.M
134
0.2205
25.7
0.1638
48.2 35
1.24
0.0576 17.5 24
1.13
0.0189
3.3 21
1.05
0.0117 1.6
17 1.005
0.0081
9.5
5.7
Dec.
1 :50 P.M
125
0.1935
18.6
0.1575
50.6 36
1.245
0.0597 18.9 23
1.14
0.0230
5.9 19
1.05 5
0.0117 2.3
17 1.01
0.0072
10.4
3.7
Dec.
7
3:45 P.M
142
0.2628
19.6
0.2115
46.5 39
1.26
0.0891 21.7 25
1.145
(MMJll
1.055
0.0186 2.7
19 1.01
0.0115
6.4
4 4
Dec.
g
10:40 A.M
160
0.2007
18.4
0.1638
44.1 35
1.27
0.07.51 24.4 22
1.15
0.0263
5.8 20
0.0147 3.6
18 1.01
0.0075
7.3
5.7
Dec.
8
12 M
138
0.2070
19.8
0.1661
41.4 39
1.27
0.0803 25.1 25
1.16
o 0283
6.4 23
1.06
0.0152 2.6
20 1.015
0.0097
9.0
4 7
Dec.
8
3:40 P.M
152
0.2173
18.0
0.1782
31.6 43
1.285
0.1098 35.0 27
1.175
0.0335
6.0 23
1.07
0.0204 3.9
21 1.02
0.0119
8.0
5 J
Dec.
HI
11:20 a.m
150
0.2151
19.2
0.1737
34.2 39
1.295
0.1004 32.4 23
1.185
0.0306
6.7 22
1.07
0.0161 3.1
20 1.02
0.0095
7.8
4.4
Dec.
10
3 :05 P.M
128
0.2050
19.9
0.1642
29.9 38
1.30
0.1030 33.9 25
1.205
0.0333
8.4 22
1.075
0.0163 3.1
20 1.02
0.0099
8.3
4 B
Dec.
11
10:10 a.m
131
0.3213
.... 37
1.31
25
1.21
.... 22
1.08
18 1.02
0.0171
2.0
5.3
Dec.
11
10 20 A.M
140
0.2646
. ... 37
1.3 1
25
1.21
.... 22
1.08
18 1.02
p.0095
3.5
3.6
Dec.
11
10:35 A.M
151
0.3006
.... 37
1.31
....
1.21
.... 22
1.08
18 1.02
0.0096
5.8
3.2
Dec.
11
2:05 p.m
114
0.3294
.... 40
1.31
25
1.23
. ... 22
1.09
18 1.02
0.0166
1.8
3 r>
Dec.
1 1
2:20 P.M
121
0.3222
.... 40
1.31
25
1.23
.... 22
1.09
18 1.02
0.0177
2.0
5.5
Dec.
11
2:40 P.M
124
0.3222
.... 40
1.31
25
1.23
.... 22
1.09
18 1.02
0.0201
1.8
'..2
Dec.
11
3:50 p.m
152
0.2412
20^6
0.Y9J5
17.8 41
1.32
0.1485 42.3 24
Ron No. 4
1.24
0.0465
10.8 20
1.09
0.0205 2.1
17 1.02
0.0140
6.3
5 S
Dec.
14
11:15 a.m
149
0.2808
5.8
0.2646
58.1 30
1.27
0.1012 22.6 25
1.165
0.0378
5.6 21
1.06
0.0220 1.9
20 1.00
0.0169
3.0
6.0
Dec.
14
2:10 p.m
146
0.2637
6.5
0.2456 45.0 32
1.29
0 1272 33.6 26
1.17
0.0393
5.8 23
1.06
0.0239 3.3
19 1.00
0.0153
5.4
5.8
Ron No. 5
Dec.
12
11 A.M
265
0.2403
20.2
0.1917
34.5 40
1.285
0.1084 25.5 21
1.195
00477
8.2 17
1.075
0.0279 5.3
17 1.015
00150
7.5
6 3
Dec.
12
12:45 p.M
265
0.2286
15.5
0.1935
23.3 48
1.280
0.1399 36.5 22
1.21
0.0562
10.3 18
1.075
0.0330 5.3
17 1.015
0.0209
7.4
9.1
Dec.
12
2:10 P.M
265
0.2232
10.5
0.1998
30.7 36
1.295
0.1309 35.4 23
Ron No. 6
1.225
0.0522
10.2 17
1.085
0.0295 4.3
17 1.02
0.0198
7.:
8.9
Dec.
13
1 1 :45 a.m
67
0.2582
23.7
0.1975
53.6 24
1.30
0.0587 17.8 19
1.195
0.0126
3.3 1'.
1.075
0.0042 0.4
16 1.02
0.0031
1') 5
1.2
Dec.
13
2:00 p.m
71
0.2700
23.0
0.2080
45.8 26
1.30
0.0842 22.3 22
1.20
0.0239
6.5 23
1.075
0.0066 2.4
18 1.02
0.0036
6.9
!.3
Dec.
13
3:40 p.m
62
0.2970
20.4
0.2367
44.6 30
1.305
0.1040 24.4 22
Ron No. 7
1.20
0.0315
6.0 19
1.075
0.0135 2.4
18 1.02
0.0066
5.0
2.2
Dec.
17
10:40 A.M
144
0.2763
.... 36
1.295
25
1.18
.... 20
1.06
0.0134 ...
18 NaOH 0.0055
5.0
2.0
Dec.
17
11:55 A.M
142
0.2510
0.0182 ...
. . NaOH 0.0068
6.4
2.7
Dec.
17
2:10 p.M
116
0.3590
'.'.'.'. 38
i.'ii
'.'.'.'. '.'.'.'. 23
i."i9
'.'.'.'. 19
i.06
0.0298 ...
18 NaOH 0.0139
1.2
3.9
Dec.
17
2:50 P.M
134
0.3140
.... 40
1.31
24
1.195
.. . 20
1.06
0 0340 ...
17 NaOH 0.0141
2 0
4 5
Run No. 8
Dec.
19
10:20 A.M
140
0.2592
.... 36
1.315
21
1.21
.... 26
1.07
00141 ...
22 NaOH 0.0050
':. 4
1.9
Dec.
19
11:45 A.M
136
0.2443
.... 38
1.315
26
1.22
.... 23
1.07
0 0215 ...
19 NaOH 0.0060
6.0
2.4
Dec.
19
1:35 p.m
264
0.2313
.... 42
1.315
27
1.24
.... 23
1.08
0.0432 ...
22 NaOH 0.0109
7.0
4.7
most of the air required before the gas enters the re-
action space preceding the first absorption tower.
Under the conditions of the tests our plant had capaci-
ties as follows, based on 0.285 g- HNO3 per liter of
nitrogen:
Cubic feet gas per minute 1.25 2.5 4.0
Efficiency of absorption — percent... 98 95 91
HNOi recovered in 24 hours— lbs.... 23 44.5 68
The last two towers were very inefficient. This
was due largely to the great dilution of the nitrogen
oxide when they reached this part of the system.
Part of the loss is due to the formation of an acid
mist which, of course, is unabsorbable. The d<
in volume of the circulating liquid in the last two
towers cannot be accounted for by evaporation and
is caused by this formation of mist.
EXPERIMENTS WITH A COTTRELL PRECIPITATOR
About a year ago, in making small scale experiments
in the laboratory on the catalysis of ammonia oxida-
tion, in which the acid make was determined by ab-
sorption in gas washing bottles, the occurrence of a
mist throughout these bottles was noted, which
caused certain losses from the absorption train even
when alkali was used in the last bottles. At that
time a fume precipitation apparatus was secured
and a few successful experiments made. Press of
other work caused these experiments to be discon-
tinued. This equipment was installed in our experi-
mental plant after making the experiments described
above, by removing the connecting pipe between
Towers 3 and 4 and substituting the 3/Vin. glass tube
shown in the figure.
The high-tension current required was obtained
from a transformer such as is used in wireless teleg-
raphy, capable of giving a maximum of 15,000
volts. The current was rectified with a kenotron fur-
nished by the General Electric Company. A plat-
inum wire was placed in the center of the glass tube
and connected to the anode of the kenotron. A coil
of copper wire was wrapped around the tube and con-
nected with the inside wall with platinum wire. This
coil and one terminal of the transformer were grounded.
The voltage was regulated by a variable resistance in
circuit with the primary of the transformer. This
arrangement worked perfectly and stopped all mist
even at considerable velocities of flow through the
tube.
It was found that when all the mist issuing from
Tower 3 was stopped no further mist was formed in
Tower 4. Under conditions of operation obtaining
in Run 3 where the total acid loss was about 5 per
cent, it was found that during the first hour of opera-
Apr., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
275
tion, circulation acids at concentrations near end of a
run, the acid obtained from the precipitator was
about 2 per cent of the total acid input. The quan-
tity of mist decreased steadily to about 0.5 per cent,
where it remained constant. The quantity of mist
varied widely under different conditions, all of which
have not been determined. It has been observed
in a full-sized plant that sometimes there was consid-
erable mist issuing from the absorption system and
at other times none at all. No correlation was es-
tablished with different conditions of operation.
We found in our experimental plant that the mist
was increased by increase of the gas velocity, reduc-
tion of the oxygen excess, and increase of the acid
strength in Tower 3. For example, at a velocity of
150 cu. ft. per hour with a slight oxygen deficiency
samples were taken of the exit gas with the precipi-
tator turned on and ten minutes after turning it off.
In the second case the acid in the exit increased from
0.0174 to 0.0248 g. per liter corresponding to an in-
crease in the end loss of from 6.5 to 9.3 per cent.
The acid recovered from the precipitator contained
very little nitrous acid, being almost wholly nitric
of 15 to 25 per cent strength. No evidence was se-
cured of any increased absorption capacity of Tower
4 by the high potential discharge.
Of the three chemical reactions involved in absorb-
ing nitrogen peroxide in water to form nitric acid,
that represented by Equation 1 above requires ap-
preciable time, and hence is the controlling one. In
order to give this reaction sufficient time all the re-
action space practicable should be provided. Atom-
ized sprays are used in some cases for absorbing gases
by liquids, and have been suggested as of possible
application here. Removal of all packing material
would increase the reaction space for the oxidation
of NO, and efficient liquid absorption surface would
be provided by the sprays. The Cottrell precipita-
tor satisfactorily solves the problem of recovering any
mist that would not settle out. Experiments along
this line are projected.
ACKNOWLEDGMENT
The experiments described are part of the inves-
tigation being carried out by the Bureau of Mines on
the oxidation of ammonia under the direction of the
chief chemist, Dr. Charles L. Parsons.
Bureau op Mines
Washington, D. C.
INFLUENCE OF TIME OF HARVEST, DRYING AND
FREEZING OF SPEARMINT UPON THE YIELD
AND ODOROUS CONSTITUENTS OF
THE OIL1
By Frank Rabak
Received October 11, 1917
The cultivation of spearmint is conducted exten-
sively for the production of the volatile oil, which
is used largely for the flavoring of chewing gum. The
efficacy of the oil for this purpose depends much
upon its composition as regards the odorous constit-
1 Published by permission of the Secretary of Agriculture
uents, the exact nature of which is not clearly under-
stood.
The constituents which serve at least in part
to produce the peculiar, yet much liked flavor of the
oil and of the products flavored with the oil, are per-
haps ester-like or alcoholic in character.
It is stated by Schimmel & Co.,1 that Russian
, spearmint oil is strikingly different from American,
German and Hungarian oils in that, in addition
to carvone, which perhaps constitutes the major
portion of these oils, an alcohol which has been iden-
tified as linalool has been found to be present in con-
siderable quantities.
Elze,2 in an examination of German spearmint
oil, states that the carrier of the odorous principle
of the oil is the acetic acid ester of dihydrocuminic
alcohol.
More recently, Nelson,3 working with an Amer-
ican spearmint oil, though unable to confirm the
presence of dihydrocuminic acetate, reported the
presence of the acetate of the alcohol dihydrocarveol.
This ester is stated to possess the characteristic odor
of spearmint.
Investigations of spearmint oil therefore, with a
view to the identification of the constituents to which
the characteristic odor is attributable, indicate that
esters or alcoholic compounds play an important part
as carriers of the aroma and flavor. Granting that
the odor-bearing constituents are ester-like or alco-
holic in character, a study of the plant was under-
taken at Arlington Farm, Va., to obtain information
regarding the effect of time of harvest, drying of the
plant, and frost action upon the constituents as well
as upon the yield and physical properties of the oils.
Experiments were conducted through a period of
years in which the plants were harvested and dis-
tilled at three distinct stages of growth, viz., budding,
flowering and fruiting stages. The plants were dis-
tilled in both fresh and dried conditions and the oils
subjected to examination and compared both as re-
gards yield of oil and physical and chemical composi-
tion. At the same time, the leaves and flowering
tops were separated from the fresh material at the
different stages of growth and distilled in order to
obtain information regarding the distribution of the
oil in the plant and composition of the oil from the
plant parts as compared with the whole fresh herb.
An experiment was also conducted to determine the
effect of frost action upon the yield and quality of
the oil.
A comparison of the yields of oil from fresh and dry
herb at different stages of growth during the seasons of
1908, 1909, 1910 and 191 1, together with the dates
of harvest and distillation are given in Table I.
No definite relationship exists in the yields of oil
from the fresh herb at any stage of growth during the
several seasons. The yields apparently vary with
the season. Yields of oil during the seasons of 1908
1 Schimmel & Co.. Spearmint Oil. Semi-annual Report of Schimmel &
Co., pp. 45-»6, April 1898.
'"I chtr Krauscminzol," Chtm.-Zlg., 32 (1910), 1175.
' "A Chemical Investigation of American Spearmint Oil," U. S.
Department of Agriculture, Bureau of Chemistry. Circular 92, 1912.
276
THE JOVRSAL OF INDUSTRIAL AND ENGINEERING < EEMISTRY Vol. io, No. 4
.1: I — Yield op Spearmint Oil prom the Fresh and from the Dry Herb at Different Stacks of Growth During Pour Successive Years
(All yields of oil calculated on basis of fresh herb)
Materia!. Date
Herb:
Budding July 24
tag Aur. 3
Fruiting Sept. 9
Di Eerb
Budding
Flowering
Fruiting
(i in
0.22
ii [9
July 7
July 15
fufj >6
lulv 9
July 19
July 29
0.14
0.097
0.14
July 14
Auk '/
Sept. I !
July 29
Aug. 25
Sept. 23
July 7
July 24
Aug. 28
Aug. 3
Aug. 3
Sept. 29
0.23
0.26
0.21
0.187
0.205
0.127
and kjii were noticeably higher than during 1909
and 1 910, from which it is apparent that seasonal
conditions play an important part in affecting the
yields of oil from the plants. The yield of oil from
the fruiting plants is uniformly low as shown by the
average, while the flowering stage produces the high-
est yields during most seasons.
The yields of oil from the dried plants during any
of the stages of growth are lower in practically all
cases than that of the fresh herb. As in case of the
fresh herb, the flowering stage again shows highest
average yield of oil while the fruiting stage shows the
lowest yield. The yields of oil from the dried plants
will, of course, be affected by the length of time al-
lowed for drying, and weather conditions during the
drying period. The average percentage of moisture
in the plants during the three years, 1909, 1910 and
191 1, was as follows: Budding stage, 71.6; flowering
stage, 70.7; fruiting stage, 62.2 per cent.
In order to make a comparison of the yields of oil
from the leaves and flowering tops of the plants at
Table III — Physical Properties, Acic
Ester and Alcohol Content of Spearmint Oil Distilled
Stages of Growth During Successive Years
different stages of growth, the results were tabulated
together wilh the yields from the whole fresh herb
at the three stages of growth.
Table II — Comparison of the Yields of Spearmint Oil prom thb
Fresh Herb, Leaves, and Tops at Different Stages op Growth
Duxuiva Three Successive Years
Yield of Oil. Per cent
Stage of Growth 1909
Whole Herb:
Budding
Flowering 0. 15
Fruiting 0.24
Leaves:
Budding 0.21
F'lowering 0 . 25
Fruiting 0.15
Tops:
Budding 0.28
Flowering 0.31
Fruiting 0.27
An examination of Table II shows that the yield
of oil from the whole herb is lower than either that
from the leaves or flowering tops during any of the
stages of growth, due doubtless to the presence of
stems in the whole herb. The yield of oil from the
flowering tops is uniformly higher than from the
leaves. The tops during the fruiting stage show the
Fresh and Dry Herbs in Various
1910
1911
Average
0.11
0.19
0.07
0.23
0.26
0.21
0 isn
0.200
0 . 1 73
0.08
0.20
0.05
0.24
0.22
0.41
0.176
0.223
0.203
0.08
0.14
0.05
0.42
0.48
0.41
0.260
0.310
0.243
Acid Ester
and A
-Cohol Content
Esters
Calcd. as
Acetate of
Alcohol
Alcohol
Calcd. as
IYSICAL
Rotation
Solubility in
Free Acid
Specific
50 mm.
80 Per cent
i as acetic)
(C.oHuO)
Year
Material
Color. Odoi and Taste
Gravity
Tube
Refraction
Alcohol
Per cent
Per cent
Per cent
1908
Fresh Herb:
Pale greenish yellow, pleasant
characteristic odor, slightly
bitter pungent taste
0.9255(a)
—25. 1
1
3 clear in excess
0
3.8
9.1
Flowering. . . .
Dark yellowish green, pleasant
odor, slightly bitter and pun-
gent taste
0.9288(a)
—24.5
l.4880(M
1
25 clear in excess
0
4.6
8.54
Fruiting
Light yellowish green, faint
i ha! nili'i 1st i< odor, very pun-
gent taste
0.9290(a)
—21 .7
0
75 cleat in excess
0
8.7
13 4
1909
/ n h Herb:
Yellowish red, faint pleasant
odor, bitter pungent taste
0.9316(e)
— 16.3
1.4891(c)
1
2 turbid in 1 5
0.32
8.6
12.0
Flowering. . . .
Dark green, agreeable flowery
odor, bitter aromatic pungenl
or more vols
taste
0.9289(c)
— 16. 1
1 . 4864(c)
1
turbid in 2 or
0.26
12.4
Fruiting
Straw, pleasant ntild odor, bit-
more vols
ter pungent taste
0.9343(f)
— 17.4
1.4873(c)
"
8 turbid in 1 5
0.28
7.3
10.9
Dry Herb:
or more vols
Budding
Yellowish, unpleasant odor, bit-
ter pungent taste
0.9279(e)
— 17.0
1 . 4888(c)
0
8 turbid in 1 5 or
k 04
7.0
11.7
Flowering. . . .
Golden yellow, strong minty
more vols
odor, hitter pungent taste
0.9331(c)
— 17.5
1 . 4868(c)
II
X clear in excess
0.56
10.8
12.7
Fruiting
Dark straw, strong fatty aro-
matic odor, bitter, very pun-
gent taste
0.9254(c)
— 16.5
i 1846
1
turbid in 1 5
0.21
9.1
15.6
1910
/ rr h Herb:
Budding
Yellowish green, pleasant char-
acteristic odor, pungent bit-
or more vols.
ter aromatic taste
0.9312(d)
—22.8
1.4895(d)
0
f> clear in excess
0.14
7.6
16.0
Flowering...
Dark golden yellow, strong aro-
matlc characteristic odor, very
pungent bitter taste
0.9252(d)
—20.3
1 482.M.J)
0
4 turbid ill 2 2
n t,i)
13.4
18.4
Fruiting
Pale brown with green tint fra-
grant flowery odor, bitter.
or more vols
slightly pungent taste
0.9303(d)
i 1800(d)
0
o turbid in '• or
1 5
15.9
214
Dry Herb:
more vols
Budding
Dark golden yellow, less char-
acteristic herb-like odoi
pungenl bitter aromatic taste
— 18.2
1. 4725t.il
0
4 turbid in 10
10.8
15.7
Flowering
Pale brown, herb like strong aro-
matic odor, very pungent bit-
ter taste
1 .4788(d)
or more i.J-
31.8
28.2
Fruiting
Pale brown, herb-like aromatic
odor. strou>; aromatic very bit
lei and pungent taste
0.9159(d)
1 .4745HJI
0
4 turbid in o
or more vols.
0.36
22.0
30.5-
(o) At 22° C. (6) At
24° C. , A. 1 C, (d) At 23° C.
Apr., 191S
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
277
highest average oil content. It is evident from
these results that the greatest portion of oil in the
spearmint plant is found in the flowering tops which
comprise a large portion of the plant as compared
with the leafy structure.
PHYSICAL AND CHEMICAL PROPERTIES OF OILS FROM
FRESH AND DRY PLANTS
The physical and chemical properties of the oil
from the fresh herb in 1908, the fresh and dry herb
in 1909 and the fresh and dry herb in 1910 during the
budding, flowering and fruiting stages were deter-
mined and tabulated in Table III. The physical
properties determined were the color, odor, taste,
specific gravity, rotation, refraction and solubility
in 80 per cent alcohol. The chemical properties
are represented by the free acid content as acetic acid,
the ester content calculated as acetate of the alcohol
CjoHisO, and the alcohol content calculated as
CioHigO.
As regards the color, odor and taste of the oils dis-
tilled from the fresh herb at the three stages of growth
during the three seasons, some differences are noted.
The odor of the oils from the fruiting herb in each case
was decidedly more fragrant than that from the flow-
ering or budding herb. No apparent relationship
existed in the color of the various oils from the three
stages of plant growth during the three seasons. The
specific gravities and refraction of the oils from each
stage of growth differ among themselves as well as
from season to season. The rotations of the oils are
comparable during any one season, but differ from
season to season, while the solubilities vary likewise.
The solubility of the oils from the flowering and fruit-
ing stages of the fresh herb during the three years
Table IV — Comparis
Physical Properties, A
Tops ,
, Ester and Alcohol Content op Spearmint Oils Distilled from Leaves, Flowering
Entire Herb at Various Stages of Growth
Material Color, Odor and Taste
Budding Stage:
Herb Yellowish red color, faint
pleasant odor, bitter
pungent taste
Leaves Deep golden yellow, faint
characteristic odor, acid
bitter pungent aromatic
taste
Tops Pinkish, pleasant character-
istic odor, bitter pungent
aromatic taste
Flowering Stage:
Herb Dark green, agreeable flow-
ery odor, bitter aromatic
pungent taste
Leaves Yellowish green, pleasant
aromatic minty odor,
bitter pungent aromatic
taste
Tops Deep golden yellow, flow-
er)' aromatic minty odor,
slightly acid, bitter pun-
gent taste
Fruiting Stage:
Herb Straw, pleasant mild odor,
bitter pungent taste
Leaves Light straw, faint not pleas-
ant odor, acid, bitter
pungent taste
Tops Light straw, faint charac-
teristic odor, acid bitter
pungent taste
Budding Stage:
Herb Yellowish green, pleasant
characteristic odor, pun-
gent bitter aromatic taste
Leaves Dark yellowish green, faint
characteristic odor, ver>
bitter and pungent taste
Tops Light yellowish green, faint
flowery pleasant odor,
very bitter pungent taste
Flowering Stage:
Herb Dark golden yellow, strong
aromatic characteristic
odor, very pungent, bit-
ter taste
Leaves Pale golden yellow, pleas-
ant faint characteristic
odor, pungent bitter aro-
matic taste
Tops Dark golden yellow, faint
agreeable fatty odor,
slightly acid, bitter pun-
gent taste
Fruiting Stage:
Herb Pale brown with green tint,
fragrant flowery odor,
bitter, slightly pungent
taste
Leaves Pale brown with green tint,
mild, fragrant, charac-
teristic odor, very bitter
pungent taste
Tops Pale brown with green tint,
very flowery characteris-
tic odor, very bitter,
strongly pungent, aro-
matic taste
21° C. (6) At 23° C. (c)At24°C.
-Physicai
0.9316(a) —16.3
Solubility in
80 Per cent
Alcohol
Free Acid
(as acetic)
Per cent
Acid, Ester
Alcohol Content
Esters Calcd.
as Acetate Alcohol
of Alcohol Calcd. as
CioHuO CioHisO
Per cent Per cent
0.9776(a) —12.3 1.4923(a) 0.6 turbic
0.9351(a) —15.2 1.4906(a) 0.8turbi<
0.9289(a) —16.1 1.4864(a) 1 turbid
0.9383(a) —15.9 1.4887(a) 1 . 2 turhi.
0.9429(a) —13.8 1.4898(a)
0.9343(a) —17.4 1.4873(a)
1 4902(a)
1.4887(a)
1 slightly u
4 or more
0.8 turbid
0.9634(a) — 6.3
0.9421(a) — 10.2
0.9312(6) —22.8
0.9271(b) —22.4
0.9260(6)
0.9252(c) —20.3
0.9224(c) —19.2
0.9219(c) —19.8
1.4895(6)
1.4899(6)
1.4908(6)
0. 6 clear in excess
0.66 turbid in 1 . 5
0.66 turbid in 1 .5
1.4830(c) 0.5 turbid in 1.5 1.70
1.4800(0 0.6 turbid
1.4870(6) Faintly turbid
278
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 4
generally excels that of the budding herb, which would
perhaps indicate a higher content of esters and alco-
hols, and a lower content of terpenic compounds
in the oils during those stages of growth.
Discussing the physical properties of the oils from
the dry herb, the most conspicuous difference as com-
pared to the oils from the fresh herb was the odor
which was distinctly more aromatic in most cases,
although accompanied by a herb-like odor. The
specific gravities, rotation and refraction averaged
lower in case of the oils from dry plants than those
from the fresh herb. The oils from the dry herb
were, on the other hand, distinctly more soluble in
80 per cent alcohol than from the fresh herb.
The percentage of free acids as acetic acid varied
much among the oils from both fresh and dry herb
at the three stages of growth. The percentage of
esters, however, in the oils from both fresh and dry
plants was higher in most instances in the oils from
the flowering and fruiting herbs. The oils from the
dry plants showed noticeably higher ester content
than the fresh herb oils. The percentage of esters
varies during the several seasons from 3.0 to 10.8
per cent in the budding plant. 4.6 to 31.8 per cent
in the flowering plant, and 7.3 to 22.0 in the fruiting
plant. The percentage of free alcohols varies in about
the same ratio as the ester content, increasing in both
fresh and dry plants as the plant matures. The
percentage of alcohol in the oil from the fresh herb
varies from 9.1 to 16 per cent during the budding
stage, from 8.54 to 18.4 per cent during the flowering
stage, and from 10.9 to 21.4 per cent during the fruit-
ing stage. The oils from the dry herb vary in alcohol
content from 11. 7 to 15.7 per cent in budding herb,
from 12.7 to 28.2 per cent in flowering herb, and
from 15.6 to 30.5 per cent in fruiting herb.
While the percentage of free acids in the oils from
the dry herb shows no constant* increase or decrease
as compared with the oils from the fresh herb, the ester
and alcohol content of the oils from the dry herb at
the various stages of growth are considerably higher
than in the oils from the fresh herb at the same stages
of growth. The drying process has therefore tended
to cause chemical changes favoring esterification and
formation of alcohols.
In connection with the study of these oils, the oils
from the leaves and tops of the plants were examined
similarly and the results tabulated for comparison
with the oil from the fresh herb.
Table IV shows that in physical properties, the oils
from the leaves and tops do not differ greatly from the
oil from the whole fresh herb. The color of the oils
is distinctly variable. The odor of the oils from the
flowering tops seemed to excel that from the leaves
in fragrance and agreeableness in practically every
case. The specific gravity and refraction of the oils
from the leaves and tops are variable. The rotation
in all cases is lower than in that of the oil from the
whole fresh herb, while the solubility in 80 per cent
alcohol of the oils from leaves and tops also differs
from that of the oils from the fresh herb during the
three stages of growth. These differences in physical
properties apparently indicate a difference in general
composition of the oils from leaves and tops as com-
pared with that from the whole fresh herb in its three
stages of growth.
In acid value of the oils from leaves and tops much
variation exists during the two seasons and also dur-
ing the several stages of growth when compared with
one another, and also when compared with the oils
from the whole fresh herb at the three stages of growth.
In every case, the oils from the leaves and tops are
richer in esters than the fresh herb. As a general
rule these oils also proved to be richer in alcohols
than the fresh herb. The leaf oils in nearly every
instance contain somewhat lower percentages of alco-
hols than the oils from the flowering tops. Xo ap-
parent relationship seems to exist between the acid
content and the ester and alcohol content of the oils,
although it appears that the formation of esters and
alcohols is more pronounced in the flowering tops
than in the leaves. A general increase is noted in
most cases in the ester and alcohol content of the
oils from leaves and tops as the plants mature, the
fruiting stage producing oils in 1910 with a much
higher content of these constituents than the flower-
ing or budding stages.
effect OF frost action — In connection with the
above experiments it was thought desirable to study
the effect of frost upon the resulting volatile oil. On
account of the lateness of heavy frosts it was neces-
sary to utilize a second growth of spearmint. This
second crop had not even advanced to the budding
stage, the plants consisting mainly of leaves and stems.
The plants were distilled on November 18, after a
heavy frost, the action of which was very noticeable.
The oil obtained from the frozen plant was com-
pared with an oil obtained from unfrozen plants dis-
tilled at about the same stage of maturity. The
yield of oil, physical properties, and chemical composi-
tion of the oils from frozen and unfrozen plants are
compared in Table V.
Table V — Comparison of Yield. Physical Properties. Acid. Ester
and Alcohol Content op Spearmint Oils prom Frozen and
Unfrozen Plants
Items op Comparison Frozen Plants Unfrozen Plants
Physical Properties:
Yield (per cent) 0.11 0.13
Color Deep golden yellow Yellowish green
Odor Mild characteristic. Characteristic, very
very pleasant minty
Taste Bitter, slightly pun- Bitter, very pungent
gent, aromatic aromatic
Specific gravity 0.9180 at 24° C. 0.9252 at 23° C.
Rotation in 50 mm.
tube (degrees) — t.7 — 27.5
Refraction 14771 at 25° C. 1 .48:: at 23» C
Solubility in 80 per
cent alcohol (vol-
ume) 0.5. clear in excess 0.6 turbid in : or
more volumes
Chemical Composition:
Free acids ealc.l. as
acetic acid (percent) 0.79 0.85
Esters calcd. as acetate
of alcohol CitHuO
(percent 25.90 8.75
Alcohols icalcd. as
Ci.HuO) (per cent) . 19.26 12.22
The yield of oil from the frozen plants was only
slightly lower than from the unfrozen material. The
color of the oil from the frozen plants was lighter
and the odor and taste very decidedly milder and
more agreeable than that from the unfrozen plant.
Apr.. 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
The specific gravity and refraction were much lower
in the oil from the frozen plant. A most remarkable
difference between the oils is noted in the rotation,
the rotation of the oil from the frozen plants being
but one-sixth that of the unfrozen plants. The oil
from the latter doubtless contained much higher
content of laevogyrate compounds, possibly carvone.
The oil from the frozen plants was much more readily
soluble in 80 per cent alcohol, dissolving in one-half
volume of alcohol, showing no turbidity when alcohol
was added in excess, indicating a possible lower con-
tent of terpenes and a higher content of alcohol-solu-
ble compounds.
The ester and alcohol constituents of the oil from
the frozen plants differed greatly from the unfrozen
material. The much higher ester content is especially
significant, indicating increased activity in the es-
terification process in the frozen plants. The higher
alcohol content also points to the existence of favor-
able conditions, due to frost action, affecting the forma-
tion of alcohols in the oil.
CONCLUSIONS
The yield of oil in the spearmint plant is affected
by seasonal conditions, being distinctly higher in
some seasons than in others. The maximum con-
tent of oil appears to be present during the flowering
period, the tops containing the highest percentage of
oil. Drying of the plants or plant parts results in a
lower yield of oil and causes changes producing in-
creased ester and alcohol content. Esterification
and alcohol formation tend to increase as the plant
matures. Freezing of the plant produces a marked
increase in the formation of the odor-bearing esters
and alcohols.
Bureau op Plant Industry
Washington, D. C.
II
CARBONATION STUDIES
THE CARBONATION OF DISTILLED WATER
By Harrison E. Patten and Gerald H. Mains
Received September 25, 1917
Water is the principal solvent in carbonated beverages
such as wines, pops, malt liquors, etc., consequently
a knowledge of its solvent and holding power for carbon
dioxide gas is of basic importance. Data are extant
for the solubility of carbon dioxide in water up to mod-
' erate pressures.1 But very little work, if any, has been
done at higher pressures, especially upon the rate of
evolution of carbon dioxide from its aqueous solutions,
1 the so-called "holding power" of the solution. The
data here presented were secured on distilled water
in order to give fundamental characteristics which were
needed in connection with our further studies on car-
bonation.
METHOD AND APPARATUS
770 cc. of distilled water from our regular labora-
tory supply were placed in a quart champagne bottle,2
> Findlay and Crelghton, J. Chem. Soc, 97 (1910), 536; Findlay and
Shen, Ibid., 99 (1911), 1313; J01 (1912), 1459; Findlay and Williams,
Ibid., 109 (1913), 636; Findlay and King, Ibid., 103 (1913), 1170.
* This quantity of liquid used in a quart bottle gives a suitable gas
cushion, 18 to 25 cc. above the liquid, and approximates trade conditions of
bottling.
and iced until the liquid was at the freezing tempera-
ture. An impregnating apparatus, previously de-
scribed1 and consisting essentially of a rotating stirrer
fitting into the bottle, with means for admitting gas
while stirring, and of measuring the pressure of the gas,
was connected with a cylinder of carbon dioxide, and
the water impregnated under the conditions of pres-
sure and stirring given below. The finished product
was then examined as to its holding power for the gas.
Portions of the gas withdrawn from the bottle were
measured and analyzed in the apparatus shown in
Fig. I. This consists of a relatively large gas burette,
G, to hold the large quantity of gas which rushes out
of the carbonated water on opening the valve of the
stirring head; and a graduated gas burette, B, serving
to measure portions of the gas from G, before and after
absorption in sodium hydroxide solution in bulb A.
Levelling tubes C and D enable one to transfer gas
at will through the proper connections as shown in
Fig. I. The two-way stopcock E and exit tube per-
mit gas to be ejected from the system, after measure-
ment and analysis. The apparatus is filled with a
saturated brine solution which does not absorb enough
carbon dioxide during the short interval of contact
of gas and solution to affect the measurements of gas
volume.
Recovery of pressure in the bottle after the gas
cushion has been allowed to come to atmospheric
pressure2 is indicated on the pressure gauge when the
valve is again closed. The rate of pressure recovery
■ "Carbonation Studies — I. A Mechanical Stirrer for Impregnating
Liquids with Gases." Tins Journal, 9 (1917), 787.
« Accomplished by opening the stirring head valve for an instant and
allowing gas to escape into tube G, Fig. I.
2fo
THE JOURNAL OF INDUSTRIAL A X D ENGINEERING iHEMISTRY Vol. 10, No.
TadlE I—
-Pressure Recovery a>
d Asa
.ytical Data.
Distilled Water. Carbonati
1 Slow Speed Stirring
Op
BNXNG: First
Second
Third
POI KTH
Fipth
Sixth
Seventh
Eighth
Ninth
mperature
of Bottle: 0°
Opening
Pressure: 65 Lbs.
0'
0°
0°
0°
0
0
0°
0°
30.5 lbs.
31.1
lbs.
30.0 lbs.
30.1 lbs.
J7 0 lbs
27.5 lbs.
27.2 lbs.
PBRIOD(a) Pr.(6)
Period
Pr.
Period Pr.
Period
Pr.
Period Pr.
Period
Pr.
Period
Pr.
Period Pr.
Period
Pr.
M S. Lbs.
M S
Lbs.
M. s
Lbs.
M S
Lbs.
M. S. Lbs.
M S
Lba
M S
Lbs.
M. S Lbs.
M S
Lb..
0 0 0.0
0 0
0.0
0 0
0.0
0 II
0.0
0 0 0.0
0 0
0.0
0 0
0.0
0 0 0.0
0 0
0.0
>
0 5 1.0
0 1
5.0
0 1
2.0
0 1
4
0 1 3.0
0 1
3.0
0 1
6.0
0 1 3.0
0 1
2.0
1 10 2.0
0 10
8.0
0 2
i ii
0 4
6
0 2 5.0
0 2
4.0
0 3
7 0
0 2 6.0
1, 1
5.0
2 08 3.0
0 19
10.0
0 5
4 II
0 5
7
0 3 6.0
0 5
6.0
0 5
8.0
0 4 7.0
0 5
7.0
.1 20 5.0
0 24
11.0
0 7
5.0
0 8
8
0 5 7.0
0 7
7.0
0 8
•' 0
0 6 8.0
0 9
8.0
3 45 6.0
0 34
12.0
0 9
0 10
9
0 7 8.0
0 11
8.0
o 13
II. 0
0 10 9.0
0 11
9.0
a.
4 13 7.0
0 43
13.0
(i III
7.0
0 12
10
0 12 9.0
0 13
9.0
0 19
12.0
0 13 10.0
0 13
10.0
4 35 8.0
0 55
14.0
0 14
8.0
0 15
11
0 14 10.0
0 15
10.0
0 28
1.10
0 16 11.0
<i i;
II 0
4 55 9.0
1 15
15 0
0 17
9.0
0 21
12
0 17 11 .0
0 21
11.0
0 37
14.0
0 23 12.0
0 24
12.5
5 45 11.0
1 32
16.0
(1 24
10. 0
0 28
13
0 24 12.0
0 26
12.0
0 48
15.0
0 29 13.0
0 30
13.0
-
6 20 12.0
2 10
17.0
0 29
11 .0
0 38
14
0 32 13.0
0 36
13.0
1 2S
17.0
0 39 14.0
0 39
14.0
7 50 14.0
2 50
18.0
0 42
12.0
1 03
16
0 44 14.0
0 48
14 1)
1 55
18.0
0 50 15,0
0 53
15.0
i
8 45 15.0
4 00
19.0
0 52
13.0
1 18
17
0 55 15.0
1 05
15.0
2 35
19.0
1 07 16.0
1 09
16.0
10 00 16.0
5 35
20.0
1 09
14.0
1 45
18
1 11 16.0
1 23
16.0
3 30
20.0
1 29 17.0
1 27
17.0
0
11 30 17.0
7 45
21.0
2 15
16.5
2 15
19
2 19 18.5
3 08
19.0
8 55
22.5
2 05 18.0
2 02
18.0
19 20 18.5
12 30
23.0
3 05
18.0
3 07
20
3 24 20.0
5 48
21.0
15 25
24.0
3 07 19.0
2 47
19.0
H
26 30 19.0
16 25
24.0
4 05
19.0
4 20
21
8 39 23.0
9 58
.Mo
31 . .
25 =.
6 32 21.0
3 57
20.0
K
33 05 20.0
23 10
25.0
5 30
20.0
5 35
22
19 49 25.0
13 33
24.0
4* .
26.2
8 52 22.0
8 37
22.0
86 . . 21.0
34 00
26.0
7 15
21.0
7 45
23
30 . . 26.0
23 38
25.0
58 . .
27.0
17 02 24.0
17 42
24.0
1140 . . 30.5
46 . .
27.0
9 15
22.0
15 05
25
45 .. 27.0
50 ..
26.5
73 ..
27.5
37 .. 25.2
30 ..
25.3
76 ..
28.5
12 05
23.0
32 15
27.0
64 . .
27 0
61 .. 26.1 1
140 ..
129 ..
29.8
15 05
24.0
41 . .
27.5
1020 .
29.0
92 .. 27.2
253 ..
31.1
22 45
35 30
50 ..
1140 ..
25.0
26.0
27.0
30.0
68 ..
138 ..
175 ..
29.0
29.8
30.1
Cc
Gas:
Withdrawn(c) 166.0
57.0
55.4
58.2
55.1
33 -
56
49.5
43.2
Residual
I .5
2.6
1.1
0.6
0.5
1.
3
0.9
0.5
I
>er cent COj 96.5
97.4
95.3
98. 1
98.9
98.5
97.
7
98.2
98.8
(a) Period of Pressure Recovery is given in Minutes and Seconds, abbreviated M. and S.
(6) All gauge readings in this and the other tables are in lbs. persq. in. where zero on the gauge equals 14.7 lbs. per sq. in atmospheric pressure).
(c) All gas volumes given are for standard conditions (0° C. and 760 mm pressure) calculated from measurements at room temperature and pressure,
allowance being made for the vapor pressure of the saturated sodium chloride solution over which the gas was collected, as taken from the table in the foot-
note on page 281.
was secured by using a stop-watch started as soon as
the valve was closed, and taking simultaneous readings
of time and pressure as long as the pressure continued
to rise. After a sufficient number of pressure recovery
curves to give the characteristic rates for the bottle
had been taken, the remainder of the gas was with-
drawn in convenient portions into the analysis ap-
paratus, measured and analyzed. When practically
all of the gas that would come off at ice temperature
and atmospheric pressure was removed, the bottle
was raised to room temperature. Further portions
of gas were withdrawn, and the bottle was then placed
in a steam bath and the remainder of the gas removed
by boiling.
EXPERIMENTAL DATA AND DISCUSSION
Carbonation No. 1. Slow Speed Stirring
The conditions maintained during carbonation were as follows
Volume of distilled water used 7 To CC.
Volume of gas space ("gas cushion") over
free surface of water in bottle 18 cc.
Speed of stirrer 400 revolutions per minute
Temperature of liquid 0° C. (melting ice)
Carhonating pressure1 65 lbs. per sq. in.
1 All gas pressures are given in pounds per square inch above atmospheric
(14.7 lbs. per sq. in.) as read by a standardized pressure gauge.
time schedule — Stirred under 6j lbs pressure for 10 min.,
shut off carbon dioxide supply and stopped stirrer, and then
opened tin- exit valve for an instant, thus "blowing off" the
foreign gas accumulated in the gas cushion. Turned on gas,
stirred at 65 lbs. pressure for 23 min., and again removed surface
gas from bottle. Stirred again under tin same pressure for 2
hrs. 5 min., and placed bottle in cold Storage over night. Car-
bonation was resumed at 65 lbs pressure, and continued for 7
his 10 min. The bottle was then placed in cold storage over
two nights and a day. It then showed a pressure of 20 lbs.,
indicating that equilibrium corresponding to the carbonating
pressure had not been reached Carbonation VTOS Continued for
.; Ins, 50 min. When the stirrer was stopped, and the gas
supply shut off. the pressure in the bottle stood at 65 lbs. Total
time of stirring — 13 hrs 40 min. 1 round). Total period of
carbonation — 71 hrs.
The tests on the bottle of carbonated water were
commenced immediately after the completion of the
carbonation described above. The data for 1 7 re-
covery curves, together with the volume and composi-
tion of the gas evolved, are assembled in Table I,
whose headings are self-explanatory.
Typical rate of pressure recovery curves, plotted
from the data in Table I. using time intervals in minutes
as abscissas and pressure in pounds per square inch
above atmospheric as ordinates are shown in Fig. II.
pressure recovery curves — The curves plotted
for Carbonation No. 1 in Fig. II were selected from
the data with a view to securing uniformity in the
length of time during which the pressure was allowed
to rise, before the opening, and thus eliminating one
of the variable factors. This factor of length of time
between openings has a marked effect on the ensuing
rate of pressure recovery curve as will be shown in
subsequent data. In Carbonation Xo. 1. this effect
is obscured by other factors, e. g., the withdrawal of
an excessive portion of gas at the first opening.
In view of the impression which prevails in the trade,
that an artificially carbonated liquid loses its gas with
extreme rapidity as compared with a liquid naturally
carbonated (bottle fermented), the regularity of the
pressure recovery curves I which of course register
rate of gas evolution) is striking. One would rather
expect a sudden rise of the curve and then a rather
sharp cessation of pressure increase. With the ex-
ception of Curve 1, all of the curves given for Carbona-
tion No. 1 show this regularity, being in general of
logarithmic lypc.
Curve 1 shows a retardation in evolution of carbon
dioxide in the initial portion of the curve, due to the
Apr., 1018 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
281
Table I (C
included)
TEf
Eleventh
Twelfth
Thirteenth
Fourteenth
FlFTEE
NTH
Sixteenth
Seventeenth
0
0
C
°
0°
0°
0
0°
0°
0
0°
23°
100° C.
27.5 Lbs.
Lbs.
26.5 Lbs.
26.0 Lbs.
25.6 Lbs.
24.5 Lbs.
25.8 Lbs.
26.1
Lbs.
Period
Pr.
Period Pr.
Period
PR.
Period Pr.
Period
Pr.
Period
Pr.
Period Pr.
Period
Pr
M. S.
Lbs.
M. S
Lbs.
M. S.
Lbs.
M. S. Lbs.
M. S.
Lbs.
M. S.
Lbs.
M. S
Lbs.
M. S.
Lbs.
0 0
0.0
0 0
0.0
0 0
0.0
0 0 0.0
0 0
0.0
0 0
0.0
0 0
0.0
0 0
0.0
0 1
4.0
0 1
5.0
0 1
3.0
0 1 3.0
0 1
2.0
0 1
2.0
0 2
4.0
0 1
2.0
0 3
6.0
0 2
6.0
0 2
4.0
0 2 5.0
0 2
4.0
0 4
4.0
0 s
6.0
0 3
4.0
0 6
7.0
0 4
7.0
0 4
5.0
0 5 7 0
0 4
5.0
0 6
5.0
0 7
7.0
0 4
5.0
0 8
8.0
0 7
8.0
0 6
6.0
0 11 80
0 7
6.0
0 7
6.0
0 13
8.0
0 5
6.0
0 12
9.0
0 11
9.0
0 9
7.0
0 15 9.0
0 9
7.0
0 11
7.0
0 23
9.0
0 7
7.0
0 16
10.0
0 14
10.0
0 12
8.0
0 21 10.0
0 13
8.0
0 16
8.0
0 33
10.0
0 10
8.0
0 20
11.0
0 20
11 .0
0 16
9.0
0 27 11.0
0 17
9.0
0 21
9.0
0 49
12.0
0 13
9 0
0 27
12.0
0 28
12.0
0 22
10.0
0 38 12.0
0 24
10.0
' 0 28
10.0
1 04
13.0
0 18
10.0
0 39
13.0
0 39
13.0
0 30
11 .0
6 52 13.0
0 31
11 .0
0 36
11 .0
1 22
14 0
0 25
1 1 .0
0 49
14.0
0 53
14.0
0 39
12.0
1 07 14.0
0 40
12.0
0 51
12.0
1 59
15.0
0 36
12.0
1 06
15.0
1 11
15.0
0 51
13.0
1 37 15.0
0 55
13.0
1 07
13.0
2 44
16.0
0 50
13.0
1 26
16.0
1 41
16.0
1 08
14.0
2 12 16.0
1 14
14.0
1 29
14.0
3 59
17.0
1 05
14.0
1 56
17.0
2 19
17.0
1 33
15.0
3 14 17.0
1 41
15.0
2 04
15.0
5 29
18.0
1 32
15.0
2 36
18.0
4 14
19.0
2 08
16.0
4 34 18.0
2 21
16.0
2 54
16.0
8 24
19.0
2 OS
16.0
3 41
19.0
10 39
21.5
2 56
17.0
6 54 19.0
3 11
17.0
4 00
17.0
10 40
20.0
2 50
17.0
5 03
20.0
14 49
22.0
3 56
18.0
15 29 21.5
4 21
18.0
5 34
18.0
15 40
21.0
4 10
18.0
13 36
23.0
18 49
23.0
5 06
19.0
19 34 22.0
6 41
19.0
8 04
19.0
25 40
22.0
6 50
19.0
25 16
24.5
26 19
24.0
7 46
20.0
32 .. 23.0
9 31
20.0
11 54
20.0
47 . .
23.0
9 25
20.0
31 16
25.0
42 . .
24.5
12 16
21.0
49 . . 24.0
15 21
21.0
20 14
21.0
96 . .
24.0
25 10
22.0
54 . .
26.0
151 ..
26.5
16 46
22.0
90 . . 25.3
23 21
22.0
36 . .
22.2
126 . .
24.5
82 ..
26.8
23 06
23.0
164 . . 25.6
58 . .
23.5
2400 ..
25.8
202 . .
25.5
147 . .
27.2
40 . .
1140
24.0
26.0
94 . .
24.5
250 . .
26.1
55."
45.
8
41.0
51.3
45
7
44.3
53.
0
49
7
1 615! 5
766.5
983! 7
1.;
0.
8
0.7
1.2
0
4
0.5
1.
5
0
8
15.5
3.8
2.0
97. (
98.
3
98.3
97.7
99
1
98.9
97.
2
98
4
99.0
99.5
99.8
Gas Wi
fHDRAWN: At
0° C
2575.8 cc.
Total Residu
il Gas from NaOH Absorption .. .
43.2
cc
23° C
100" C
is in Bottle
766.5 cc.
. . 983. 7 cc.
Foreign Gase
Gas Cushion
Volume of Li
Preser
t
1 .0
18 cc
770 cc
per cent
4326.0 cc
Total G
removal of an excessive amount of gas in the first
opening and a consequent depletion of the gas con-
tent of the upper layers of the liquid; but the subse-
quent trend of this curve likewise becomes logarithmic.
In succeeding openings of the bottle the valve was
closed the instant that the gauge indicator stopped
falling, so that only the gas was withdrawn that had
been in excess of atmospheric pressure in the gas cushion
and any retardation of the recovery curve, due to ex-
cessive gas removal, was eliminated.
As portions of gas are withdrawn from the bottle
the amount of gas in the liquid, which is the driving
force behind the pressure recovery, is gradually de-
creased. Hence the normal recovery curves, taken
after like periods of standing, will naturally take the
same form and fall slightly below each other according
to their order of taking. Curve 1, due to the excessive
gas withdrawal, falls much below its normal position,
and as the upper layers have not yet regained their
full share of gas, this effect persists in Curve 2 to a
lesser extent, bringing it below its normal position.
The curves beyond No. 4 are for practically normal
conditions.
ACCORDANCE WITH HENRY'S LAW To One who has
not followed the carbonation industry, some of the
data presented and some of the considerations dis-
cussed would appear almost axiomatic; but in looking
over the field, it appears necessary to include these.
For example, the solubility of these gases can be very
closely calculated for various temperatures and pres-
sures from existing data according to Henry's law.
In the practical operation of carbonating machinery,
however, it would appear that saturation in respect
to carbon dioxide or other gas does not attain to the
value that would be expected.1
One of the contributory causes to this incomplete
saturation is the presence of foreign gases which lower
the partial pressure of the carbon dioxide gas. This
means that the effective pressure of the carbonation
is the partial pressure of carbon dioxide, and not the
total pressure of gases in the gas cushion as shown by
the gauge.
The total volume of gas forced into the system was
4326 cc. calculated to 0° C. and 760 mm. pressure,
allowing for the vapor tension1 of the brine solution
over which the gas was collected. Using the solu-
bility of carbon dioxide in water at o° C. and 760 mm.
as 1. 7 13 volumes2 carbon dioxide per unit volume of
water, at the indicated carbonating pressure, 65 lbs.
per sq. in., there would be according to Henry's law
7150 cc. of gas dissolved in the 770 cc. of water in the
bottle.
It might then be inferred that at this high pressure
Henry's law does not hold; but in this case we are not
dealing with equilibrium conditions. The initial pres-
sure, 65 lbs., simply represents the carbonation pres-
sure from the source of carbon dioxide gas plus the
partial pressures of any foreign gases3 left in the gas
cushion.
The partial pressure4 of carbon dioxide in the gas
1 From the data obtained by Emden, and given in Landolt-Bornstein,
"Physikalisch-Chemische Tabellen," 4th Ed., 1912, p. 410, Table 119,
the vapor tension of a solution of NaCl saturated at 20° C. was calculated
for various temperatures by graphical extrapolation. These calculated data
are given here for convenient reference in the following table:
of Sodium Chloride Solution
saturation point at 20° C.)
m. of Hg
9.6
10. 2
10.9
11.6
12.4
13.2
H I
Pressure
mm of Hg
15.0
15.9
16.8
17.7
18.7
19.8
20.9
Temp.
1 Henry's law is not expected, of
any gas such as carbon dioxide, which
undergoes polymerization when in solut
to hold absolutely rigid
bines with the solvent or w
Pressure
""" >:
22. 1
3.1 27.8
34 29 . 4
35 31.0
'Van Nostrand's "Chemical Annual," Olsen, 3rd Ed , 1913. p. 734,
Table XXV. Data by Hohr and Bock.
* The foreign gases present come from three sources: air originally
dissolved in the water used, air in gas cushion above the liquid, and (he small
amount of nitrogen in the carbon dioxide gas used. See paragraph on gas
analysis and composition for the quantities of foreign gas present.
* The value of the partial pressure of COl in the >::is cushion i* found
as follows: Since the opening pressure in the gas cushion was 65 lbs. above
atmosphcrii . r,t ". I ' ,i mm, phn , . ,.tm! the volume of foreign gas withdrawn
28 2
THE JOURNAL OF INDUS'! RIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 4
Fig. II — Pressure Recovery Curves
cushion of the bottle at this stage is 5.03 atmospheres
or 50. 2 lbs. above atmospheric pressure, and the volume
of COo in the liquid, if complete saturation had been
reached, would be 6635 cc. Actually there were
4190 cc. of carbon dioxide in the liquid. This simply
shows that saturation was not complete, and that
even after this extremely long period of stirring com-
plete equilibrium between the gas dissolved in the
liquid and the gas in the gas cushion under the carbon-
ating pressure was not reached.
When, however, the recovered pressure, 30.5 lbs.,
19 hrs. after the first opening of the bottle (Table I)
is reached, a comparison of the total carbon dioxide
contained in the liquid at that point, 4070 cc.,1 with the
theoretical volume calculated from solubility data and
at the first opening by reducing the pressure to atmospheric was 5.8 cc.
there must have been (5.8 X 5.42)-=-4.42 = 7.1 cc. of foreign gas in the gas
cushion before opening. With the volume of gas cushion 18 cc. the partial
pressure of foreign gas is 7.1 4- 18 = 0.39 atmospheres. The partial pres-
sure of carbon dioxide in the gas cushion is then 5.42 — 0.39 = 5.03 atmos-
pheres or 59.2 lbs. above atmospheric.
1 The total gas in the bottle at this point is 41t>0 ec. (4326 cc. — 166 cc.
withdrawn at the first opening). Of this volume, a portion (18 X 30.5 +
14.7/14.7 = 55.3 cc.) is in the gas cushion above the liquid, and the re-
mainder, 4105 cc. (reading to the nearest unit), is dissolved in the liquid. The
foreign gas withdrawn at the second opening is 1.5 cc; foreign gas in gas
cushion before withdrawal = (1.5 X 3.07)4-2.07-2.2 cc. This volume sub-
tracted from the total volume of foreign gas in the bottle, 37.4 cc, leaves
35.2 cc foreign gas in the liquid. The actual volume of COi in the liquid
then at the time of 2nd opening was 4105 — 35 « 4070 cc. The partial
pressure of foreign gas was 2.2/18 - 0.12 atmospheres or 1.8 lbs. The
partial pressure of carbon dioxide then equals 30.5 — ■ 1.8 «■ 28.7 lbs. above
atmospheric The calculated volume of COi in the liquid corresponding
to this pressure according to Henry's law is (28.7+14.7)4-14.7X0.770 X
1.713 - 3890 cc
Henry's law, 3890 cc, shows a slight degree of super-
saturation. Our observation has been that complete
equilibrium in the bottle between the gas in the liquid
and in the gas cushion is not quite reached at the end
of 19 hrs., but is approximately so after a 40-hr. period,
as will be shown by subsequent data. These results,
then, show that at high pressures of CO; we have a
close agreement with Henry's law.
Applying now these considerations to the case of
carbonated beverages as put out in the trade, it will
be seen how and why a poorly carbonated product
(with large percentage of foreign gas present or in-
sufficient period of carbonationl may have a high initial
pressure in the gas cushion, without having a corre-
spondingly great quantity of gas held in the liquid.
The result of this is that, when the pressure drops to
atmospheric upon opening of the bottle, the liquid may
remain almost non-efferveseent.
composition of the gas — The total residual gas
after absorption over sodium hydroxide was 43.2 cc.
or 1.0 per cent of the total gas.1 Analysis shows that
a large portion of the residual foreign gas in the gas
cushion is withdrawn at the first opening. Thus of the
total residual gas in the bottle 5.8 cc, or approxi-
mately 13 per eent. was withdrawn at the first opening.
In the next two openings also comparatively large
1 The carbon dioxide gas used in these carfaonattona showed an average
analysis of 99.7 per cent COs. The foreign sas contained no oxygen or
carbon monoxide, and consisted of nitrogen, with perhaps a trace of the
rare gases.
Apr., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
283
Table IIA — Carbonating Conditions: Carbona
Temperature of Water
during Carbonation
0° C.
jg • Pressure at
Interval End of Stirring
[rs. Min. I^bs. per sq. in.
Speed of
Stirrer
400 r. p. m
Carbonating
Pressure
70 lbs. per sq. ii
Subsequent Treatment
Closed valve.
Pressure
Recovered
Lbs. per sq. ii
Let bottle stand
Let bottle stand ovt
Gas supply shut off.
Gas supply turned <
Let bottle stand ov
nd began test (See Table IIB)
Pressure dropped to zero.
Pressure dropped to 34.5 lbs.
Sunday, pressure fell to 60 lbs. Connected to analysis apparatus
Total Stirring....
Table
10 55
IIB — Pressure
Recovery
Total Period op
2ARBONA
TION — 48 hrs.
>nation No.
40 min. (round).
2. Slow Speed
Stirring
and Analytical Data
Carb
First Opening
Second Opening
Third
Opening
Fourth Opening
Temperature of Bottle
0
0°
0
0"
0°
24°
100° C.
Opening Pressure
60.0 lbs.
43.5 lbs.
43.5 lbs.
39.0 lbs.
Period
Pressure
Pei
iod Pressure
Period
Pressure
Period
Pressure
Min
Sec
Lbs.
Min
Sec.
Lbs.
Min
Sec
Lbs.
Min
Sec.
Lbs.
0
0
0.0
0
0
0.0
0
0
0.0
0
0
0.0
0
2
3.0
0
1
5.0
0
1
4.0
0
3
8.0
0
5
6.0
0
8
10.0
0
3
8.0
0
6
10.0
0
11
10.0
0
10
11.0
0
5
10.0
0
9
12.0
0
15
12.0
0
19
14.0
0
12
14.0
0
14
14.0
0
23
14.0
0
28
16.0
0
18
16.0
0
20
16.0
0
31
16.0
0
42
18.0
0
28
18.0
0
30
18.0
0
45
18.0
1
05
20.0
0
37
19.0
0
44
20.0
1
01
20.0
1
23
21.0
0
48
20.0
0
56
21.0
0
15
21.0
1
43
22.0
1
02
21.0
1
11
22.0
1
31
22.0
2
10
23.0
1
23
22.0
1
32
23.0
s
1
56
23.0
2
41
24.0
1
44
23.0
1
52
24.0
2
22
24.0
3
25
25.0
2
12
24.0
2
28
25.0
3
02
25.0
4
11
26.0
2
53
25.0
3
10
26. Q
3
51
26.0
5
08
27.0
3
38
26.0
4
03
27.0
4
43
27.0
6
22
28.0
4
40
27.0
5
25
28.0
5
59
28.0
7
42
29.0
5
55
28.0
6
45
29.0
Hi
7
12
29.0
9
50
30.0
7
10
29.0
9
05
30.0
9
03
30.0
12
30
31.0
9
30
30.0
12
25
31.0
0
11
33
31.0
15
50
32.0
12
35
31.0
15
35
32.0
14
35
32.0
21
15
33.0
15
50
32.0
27
00
34.0
H
18
34
33.0
45
34.0
20
50
33.0
35
35.0
K
24
05
34.0
35
35.0
26
10
34.0
45
36.0
37
35.5
46
36.0
32
40
35.0
60
37.0
43
36.0
65
37.0
44
36.0
1000
40.3
59
37.0
91
38.0
61
37.0
70
38.0
107
38.5
100
38.0
96
39.0
2900
43.5
160
39.0
125
40.0
1140
43.5
Cc. Gas: Withdi
63.
6
89.0
91
1
72.0
2825.4
947
4
1041.0
Residual
10.
4
6.0
5
1
1.6
17.7
9
0
1.8
Per cent CO2
83.
6
93.3
94
4
97.8
99.4
99
1
99.8
Gas Withdrawn:
At
0°
C
3141
1 cc.
Total Residual Gas from NaOH Absorption
.. 51
6 cc.
24°
C
947
4cc.
Foreign
Case
1
0 pe
cent
] 1 in ,:
c
1041
0 cc.
Gas Cushion
25 cc.
770 cc.
Total Gas in Bottle
5129
5 cc.
portions of residual gas were found. After this period,
the volumes of residual gas in the portions withdrawn
at the various openings were much smaller and fairly
constant, except that upon standing for long periods
(over night) more of the foreign gas collected in the gas
cushion, giving a lower per cent of carbon dioxide in
the gas withdrawn at the succeeding opening.
effect of gas cushion — The volume of the gas
cushion was determined, as necessary to the determina-
tion of the partial pressures of the gases in it, and since
the rate of rise of pressure obviously is influenced
somewhat by the size of the space that the gas liberated
at the surface of the liquid has to fill.
CARBONATION NO. 2. SLOW SPEED STIRRING
A second bottle of distilled water was carbonated
with the stirrer rotating at the same rate and the data
of the first carbonation were practically duplicated.
The conditions of carbonation are given in Table IIA.
In Table IIB is presented the rate of pressure recovery
data for Carbonation No. 2, and the corresponding
curves are plotted in Fig. II.
discussion of data — The carbonating pressure from
the cylinder was a little higher in this case than in the
first carbonation (70 lbs. compared with 65 lbs.) and
consequently a somewhat greater volume of gas was
forced into the liquid in a slightly shorter time than in
the first carbonation. The data, however, coincide
with those of Carbonation No. 1 in general. It is
again shown that at this slow speed stirring (400 r.
p. m.) a very long period of stirring (11 to 13 hrs.)
is necessary to obtain a fair degree of carbonation,
and even after this long period the saturation point is
not reached. To illustrate, the partial pressure of
carbon dioxide gas at the first opening is 4.56 atmos-
pheres1 or 52.3 lbs. above atmospheric pressure, and
the corresponding volume of carbon dioxide that should
be dissolved in the liquid according to Henry's law,
is 6015 cc. The actual volume of CO2 in the liquid
at this point is only 4965 cc.
At the third opening, after the bottle had stood for
over 40 hrs. and equilibrium between the carbon di-
oxide in the gas cushion and in the liquid had prac-
tically been reached, we find a very close agreement
with Henry's law and solubility data. The actual
volume of carbon dioxide in the liquid at this point
is 4850 cc. The partial pressure of carbon dioxide
is 3.69 atmospheres or 39.6 lbs. per sq. in. above at-
mospheric pressure, and the corresponding volume of gas
in the liquid should be: 770 X r.713 X 3-69 = 4865 cc.
1 The partial pressure of CO2 is determined in a manner similar to that
in Carbonation No. 1, i. t., calculating the volume of foreign gas in the gas
cushion from the volume of foreign gas withdrawn at the first opening,
from that the partial pressure of foreign gas, and subtracting the latter
from the total initial pressure to obtain the partial pressure of COi. The
volume of CO) actually in the liquid is the total gas volume minus the volume
of gas in gas cushion, minus the volume of foreign gas in the liquid.
284
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 4
The agreement is as close as could possibly be
obtained within the limits of accuracy afforded by the
methods used.
rate of pressure recovery — By glancing at the
pressure recovery curves shown in Carbonation Xo.
2, Fig. II. it will be seen that the general form is of the
same logarithmic type as for the curves in Carbonation
No. 1. The curves lie very close together, over-
running one another, much as did the first four curves
in Carbonation Xo. 1. If a continued set of curves
had been taken in this case down to a low pressure re-
covery, the curves would have gradually fallen below
those preceding in a similar manner to the curves in
Carbonation No. 1.
There are three important factors that affect the
rate of pressure recovery from the same solution at
various stages. One which has been mentioned before
is the quantity of gas removed at the opening. The
removal of an excessively large amount of gas (by not
closing gauge as soon as indicator ceases to fall) strips
the gas from the top layers of solution, and retards
the rate of pressure recovery.
A second factor is the formation of bubbles on the
container surface. When gas escapes from the liquid
in a container, small bubbles form on the sides of the
container serving as nuclei for the liberation of gas
from solution. The pressure recovery curve taken after
the bottle has been standing over night shows a slow-
ing down due to the resolution of the bubbles that had
formed on the inner surface of the bottle. As soon as
the bottle is opened we again have the bubbles formed,
and if a second recovery curve is taken on the same day
the rate will be speeded up. The shorter the period
between openings the more will this speeding up be in
evidence.
A third factor affecting the rate of pressure recovery
is the relation between the concentrations of gas in the
various layers ofliquid and in the gas cushion at the
time of opening the bottle. When the bottle is opened
and the gas in excess of atmospheric pressure is with-
drawn from the gas cushion, the gas in the upper layers
of liquid rushes into the gas cushion while that in the
lower layers passes more gradually into both gas
cushion and stripped upper layers, until finally when
equilibrium is reached the concentration throughout
the liquid layers is practically uniform. However,
when the bottle is opened before equilibrium has been
the upper liquid layers are not at their full
concentration, and hence the rate of pressure recovery
is slowed down. The amount of this slowing down will
depend on the interval between the successive openings:
the shorter the interval the greater the tendency to
slow down the pressure recovery rate, due to this effect.
We have, then, two counterbalancing factors, forma-
tion of bubbles and relative gas concentrations in the
different liquid layers, both of which are dependent
upon the period between successive openings. The
shorter the period the more will the rate curve tend
to be speeded up, due to bubble formation, but at the
same time the more will it tend to slow down, due to
oncentration of gas in the upper layers. The
exact length of the period, the nature of the solution,
the total pressure in the bottle, the roughness of the
inner bottle surface (serving to accentuate bubble
formation) all go to determine which of these counter-
balancing factors will predominate. Often then the
curve will rise excessively during the first few minutes
owing to the presence of bubbles, and then recross
the preceding curve and fall below it, due to the low
concentration of the upper layers of solution at the
time of opening. The action of these factors may
be seen in the curves in Carbonation Xo. 2, Fig. II,
but are brought out more distinctly in Carbonations
Nos. 3 and 4.
composition of the gas — While the amount of
foreign gas in the bottle was slightly greater than in
Carbonation No. 1, the percentage of foreign gas
based on the total gas content was identical in the
two cases, being 1.0 per cent. Of the total foreign
gas present (51.6 cc.) 10.4 cc, or about 20 per cent, was
withdrawn at the first opening. It will be noticed
here again that the foreign gas does not come out of
the liquid as rapidly as the carbon dioxide does, so
that the volume of foreign gas in the portions with-
drawn is smaller than normal, except where the bottle
has been allowed to stand over night before opening.
effect of gas cushion" — The volume of gas cushion,
25 cc, is 7 cc. greater than that in Carbonation Xo. 1.
The smaller gas cushion would tend to favor a some-
what more rapid rise of pressure due to liberated gas,
but this is partly compensated, in case of the larger gas
cushion, by the increased area of the free surface of
liquid in the bottle, produced by the flaring of the neck.
This increased area permits the more rapid evolution of
gas. It was shown by measurement and graphical
calculations that, at the point on a standard champagne
bottle where the neck begins to flare, the increase in
volume of the gas cushion bears a linear relation to the
increase in free surface of the liquid in the bottle.
Bottles of such size as to furnish a 25 cc. gas cushion
were also used in Carbonations Xos. 3 and 4.
CARBONATION NO. 3. HIGH SPEED STIRRING
The remarkable slowness with which the carbon
dioxide was absorbed in Carbonation Xo. 1. sug-
gested that increased rate of stirring be tried. Conse-
quently the speed of the stirrer was increased from 400
revolutions per minute to 2500.
The conditions of carbonation for this bottle are
given in Table I II A.
The rate of pressure recovery data are presented in
Table 1 1 1 B. under appropriate headings, and the rate
curves plotted therefrom are shown in Carbonation
No. 3. Fig. II.
One is immediately struck by the tremendous in-
crease in efficiency of carbonation produced by a simple
increase in speed of stirring. The total gas forced
into the system was 6263 cc. stirring at 2500 r. p. m.
compared with 5130 cc. at 400 r. p. m. (Carbonation
Xo. :). the carbonation pressure, volume of liquid,
volume of gas cushion, and number of blow-offs being
me. The period of stirring was only 6 minutes
with the high speed stirring compared with approxi-
mately 11 hours for Carbonation Xo. 2. This means
that by increasing the rate of stirring about six times
Apr., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
285
Distilled Water
Used
770 cc.
Table IIIA — Carbonating
Temperature of Water
during Carbonation
Pressure at
End or Stirrin
Lbs. per sq. in.
ditions; Carbonation No.
3
Speed of
Stirrer
Carbonating
Pressure
Gas
Cushion
2500 r. p. m.
70 lbs. per sq. ic
25 cc.
Subsequent Treatment
Period of Pressure
of Rise Recovered
Sec. Lbs. per sq. ir
Total Stirring
6
Table
IIIB-
-Pressure R
First Opening
Second Openin
Temperature
of Bottle
0
0
Opening
Pre s
70.0 lbs
60.0 lbs
Period
Pressure
Period
I'KKSSC
Min
. Sec.
Lbs.
Min
. Sec.
Lbs.
0
0
0.0
0
0
0.0
0
1
10.0
0
1
5.0
0
2
15.0
0
10.0
0
3
20.0
0
6
25.0
0
5
25.0
0
14
28.0
0
15
30.0
0
30.0
0
19
31.0
0
28
31.0
0
22
32.0
0
33
32.0
>
0
25
33.0
0
40
33.0
0
31
34.0
0
47
34.0
0
37
35.0
0
52
35.0
0
0
45
36.0
1
03
36.0
0
55
37.0
1
19
37.0
X
1
03
38.0
1
34
38.0
£
1
14
39.0
1
54
39.0
1
25
40.0
10
40.0
O
1
42
41 .0
37
41.0
2
03
42.0
3
10
42.0
2
31
43.0
3
47
43.0
C
2
55
44.0
4
20
44.0
fc
3
25
45.0
5
01
45.0
O
4
02
46.0
5
52
46.0
4
50
47.0
7
05
47.0
as
6
00
48.0
8
52
48.0
7
05
49.0
10
35
49.0
8
15
50.0
12
15
50.0
9
35
51.0
15
52
51 .0
12
05
52.0
21
40
52.0
15
00
53.0
27
40
53.0
18
50
54.0
40
54.0
25
20
55.0
68
55.0
32
50
56.0
125
56.7
66
58.0
1
260
60.0
) Opened valve, letting off gas to zero
i noting pressure recovery in each case
Connected bottle to analysis apparatus
Total Period of Carbonation — 9 m
pressure. Closed valve, i
Recovery and Analytical
Third Opening
Data: Carbonation No. 3. High Speed Stirring
Fourth Opening Fifth Opening
56.7
bs.
54.0 lbs.
53.0 lbs.
Pei
IOD
Pressure
Period
Pressure
Period
Pressur
din
Sec
Lbs.
Min
. Sec
Lbs.
Min
. Sec.
Lbs.
0
0
0.0
0
0
0.0
0
0
0.0
0
1
5.0
0
1
15.0
0
1
10.0
0
2
10.0
0
2
20.0
0
15.0
0
3
15.0
0
5
25.0
0
3
20.0
0
4
20.0
0
9
27,0
0
5
22.0
0
7
25.0
0
13
28.0
0
8
24.0
0
14
28.0
0
16
29.0
0
1 1
25.0
0
23
30.0
0
22
30.0
0
13
26.0
0
29
31 .0
0
30
31 .0
0
17
27.0
0
34
32.0
0
38
32.0
0
22
28.0
0
41
33.0
0
47
33.0
0
27
29.0
0
50
34.0
0
58
34.0
0
34
30.0
0
58
35.0
1
10
35.0
0
43
31.0
1
10
36.0
1
26
36.0
0
52
32.0
1
27
37.0
1
46
37.0
1
03
33.0
1
44
38.0
2
08
38.0
1
18
34.0
2
04
39.0
2
30
39.0
1
32
35.0
2
27
40.0
3
01
40.0
1
49
36.0
2
53
41 .0
3
25
41.0
2
18
37.0
3
43
42.0
4
36
4.2.0
2
50
38.0
4
25
43.0
5
37
43.0
3
19
39.0
5
2.3
44.0
6
44
44.0
4
04
40.0
6
25
45.0
8
01
45.0
4
54
41.0
7
43
46.0
9
49
46.0
6
30
42.0
9
14
47.0
17
40
48.0
7
50
43.0
11
51
48.0
35
50.0
9
40
44.0
15
09
49.0
54
51.0
12
15
45.0
18
35
50.0
110
52.0
23
47.5
24
30
51.0
200
53.0
33
48.0
36
52.0
44
49.0
70
54.0
62
117
50.0
50.5
Withdrawn 133.0 114.7 111.2
Residual 10.9 5.9 2.7
Per cent COi 91.2 94.9 97.6
Gas Withdrawn: At 0° C 4548.5 cc.
26° C 856.4 cc.
100° C 858.2 cc.
Total Gas in Bottle 6263 . 1 cc.
we have increased the speed of carbonation over ioo
times.
We have a nearer approach to saturation of the
liquid at the end of this short period of high speed
stirring than with the extremely long period using slow
speed. The actual volume of carbon dioxide in the
liquid before the bottle is opened is 6090 cc, whereas
the volume corresponding to the partial pressure of
CO2 over th.e liquid (5.25 atmospheres) calculated from
solubility data and Henry's law is 6925 cc. After
withdrawing portions of gas, and letting the bottle
stand while the gas comes out of the liquid until
equilibrium is practically established, we have, as in
the two previous carbonations, a fairly close agree-
ment with Henry's law.
pressure recovery curves — In considering the
rate of pressure recovery curves for Carbonation No.
3, it will be noted that Curve 1, taken shortly after
carbonating, is somewhat high since the bubbles on
the container surface have not had time to be sup-
pressed. Curve 2, taken after standing over night,
gives the normal1 pressure recovery. Curve 3, taken
on the same day as No. 2, starts up fairly rapidly
1 We will consider as normal the pressure recovery from tin- quleacenl
state of the liquid, after equilibrium is practically reached.
121.0 103.0 3965.6 856.4 i
3.9 1.2 13.3 S.6
96.8 98.8 99.7 99.3
Total Residual Gas from NaOH Absorption.. . 44.4 cc.
Foreign Gases Present 0.7 per (
Gas Cushion 25 cc.
Volume of Liquid 770 cc.
because of bubble formation, but falls quite a bit be-
low it due to the subnormal concentration of the gas in
the upper layers. After standing over night Curve 4
again gives a normal pressure recovery, the difference
between the two normal curves, Nos. 2 and 4, being
due to the lowering of the total gas content of the liquid
by the volume of gas removed from the bottle between
the two openings. Curve 5 again shows a depression
due to low concentration of gas in the upper layers of
liquid. The regular logarithmic form of pressure
recovery curve is obtained here as in the other car-
bonations.
composition of the gas — The residual volume from
absorption over sodium hydroxide was 44.4 cc. or
0.7 per cent of the total gas. As in the previous car-
bonations a large portion of this foreign gas, 10.9 cc,
nearly 25 per cent, was withdrawn at the first opening.
Over 50 per cent of the foreign gas was withdrawn by
the fourth opening, whereas less than 8 per cent of the
total gas was withdrawn during the same time.
CARBONATION NO. 4
A second bottle of distilled water was carbonated
a1 the same high rate of stirring, ami in addition the
Of residual foreign gas in the gas cushion was
286
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. 4
Instilled Water
Used
770 cc.
-Period op Stirri:
Table IVA— Carb
mating Conditions:
Carbonation No. 4
Temperature of Wates
Speed of
Car bona ting
during Carbonation
Stirrer
Pressure
0° C.
2500 r. p. m.
70 lbs. per sq. i
Pressure at
End of Stikkin<
Lbs. per sq. in.
Subsequent Treatment
Period
of Rise
Sec.
Pressure
Recovered
Lbs. per sq. in.
64 J
opened valve, letting off gas to zero pressure. Closed
pressure recovery in each case
Connected bottle to analysis apparatus and began test ($« Table IVB)
1 10
Total St
run
I
Table IVB — Pressure Recovery
bonation No. 4 — High
Speed Stirring
and Analytical Data: Car
First Opening
Second Opening
Third Opening
Fourth Opening
Fifth Opening
Sixth Opening
Temperature
of Bottle
0°
0°
0"
0"
0°
0°
0°
20"
100° C.
Opening
Pressure
66.0 lbs.
48.5 lbs.
48.0 lbs.
46.0 lbs
47.5 lbs.
44.5 lbs.
Period Pressure
Period
Pressure
Period Pressure
Period Pressure
Period Pressure
Period Pressure
Min
Sec.
Lbs.
Min
Sec
Lbs.
Min
. Sec.
Lbs.
Min
Sec.
Lbs.
Min
Sec.
Lbs.
Min
Sec.
Lbs.
0
0
0.0
0
0
0.0
0
0
0.0
0
0
0.0
0
0
0.0
0
0
0.0
0
7
31.0
0
3
27.0
0
1
18.0
0
10.0
0
1
10.0
0
3
10.0
0
10
32.0
0
5
30.0
0
2
22.0
0
2
20.0
0
2
18.0
0
4
21.0
0
13
33.0
0
11
31.0
0
5
25.0
0
5
25.0
0
5
23.0
0
6
23 . 0
0
16
34.0
0
18
32.0
0
8
27.0
0
8
26.0
0
9
24.0
0
24.0
>
0
20
35.0
0
25
33.0
0
10
28.0
0
10
27.0
0
11
25.0
0
13
25.0
3
0
30
36.0
0
39
34.0
0
14
29.0
0
12
28.0
0
14
26.0
0
17
26.0
0
49
37.0
0
59
35.0
0
21
30.0
0
19
29.0
0
20
27.0
0
26
27.0
K
11
38.0
1
29
36.0
0
33
31.0
0
26
30.0
0
29
28.0
0
37
28.0
i
40
39.0
36
37.0
0
47
32.0
0
42
31.0
0
41
29.0
0
50
29.0
3
2
25
40.0
3
45
38.0
1
02
33.0
0
58
32.0
1
02
30.0
1
13
30.0
3
30
41.0
5
45
39.0
30
34.0
1
20
33.0
1
32
31.0
50
31.0
5
40
42.0
8
10
40.0
2
05
35.0
1
58
34.0
2
05
32.0
30
32.0
8
00
43.0
11
20
41.0
2
58
36.0
44
35.0
2
48
33.0
3
20
33.0
10
50
44.0
17
20
42.0
4
43
37.0
3
53
36.0
3
55
34.0
5
10
34.0
13
40
45.0
25
20
43.0
6
25
38.0
6
35
37.0
5
10
35.0
9
20
36.0
17
00
46.0
34
00
44.0
9
05
39.0
8
55
38.0
40
36.0
13
40
37.0
41
48.0
44
45.0
12
15
40.0
12
10
39.0
11
25
37.0
IS
40
38.0
< 1.120
48.5
70
46.0
17
00
41.0
16
30
40.0
14
40
38.0
25
30
39.0
X
1 20
165
47.5
48.0
25
41
58
73
100
00
42.0
43.0
44.0
45.0
46.0
23
37
56
76
1260
30
41.0
42.0
43.0
44.0
47.5
18
25
34
52
81
113
167
50
10
45
39.0
40.0
41.0
42.0
43.0
44.0
44.5
35
57
86
20
40.0
41.0
42.0
Cc. Gas:
Withdraw
J 120
.8
134
1
100.6
102.7
108.9
97.9
3761.4
657.7
1177.9
Residual
3
.9
3
0
0.J
0.4
0.9
0.4
7.7
1. 1
1. 1
Per cent COj 96
.8
97
8
99."
99.6
99.2
99.6
99.8
99.8
99.9
Gas Wi
AWN'
At 0°
C...
4426
4 cc.
Total Residual Gas from XaOH Absorption.. .
19.0
cc.
20°
100°
C...
C...
657
1177
7cc.
9cc.
Foreign G
Gas Cnshi
0.3
per cent
25 cc
Volu
me of Liquid.
770 cc
Total Gas in Bottle 6262 flee
19.0 cc. total residual gas from XaOH absorption
0.3 per cent — foreign gases.prcsent
more nearly eliminated by "blowing off" the surface
gas several times. The conditions of carbonating are
given in Table IVA.
Table IVB presents the data on rate of pressure re-
covery, and on the analysis of the gas. The rate of
pressure recovery curves are plotted in Carbonation
No. 4, Fig. II.
In Carbonation No. 4 the same volume of gas,
6262 cc, was forced into the system as in Carbonation
No. 3. No. 4 was stirred for seven minutes and
No. 3 for six minutes, but to offset this the carbonating
pressure in No. 3 was slightly greater. Also No. 4
had the surface gas "blown off" six times as com-
pared with twice in No. 3 and as this blowing off re-
moves quite a little gas from the system, it would
naturally take slightly longer to bring No. 4 to efficient
carbonation. The degree of saturation in Carbonation
No. 4 was almost exactly the same as in Carbonation
No. 3, and somewhat higher than in the carbonations
with slow speed stirring. The actual total carbon
dioxide in the liquid was 61 10 cc.,1 whereas the cal-
culated volume from the observed partial pressure
(5.30 atmospheres or 63.3 lbs. per sq. in. above atmos-
1 The method of determining the actual volume of COi
and the partial pressure of COi in the gas cushion is detailed i
col. 2 pat;e 281. and footnote 1, col. 1. page 282.
l the liquid
footnote 4,
pheric) was 6990 cc. Comparison of the observed
and calculated volumes of gas in the liquid at later
openings upon the attaining of equilibrium after the
bottle had stood overnight, showed a close agreement
with Henry's law and solubility data.
rate of pressure recovery — In considering the
rate of pressure recovery curves for Carbonation No.
4. it will be noticed that Curve 1, taken immediately
following the first opening of the bottle, shows a very
rapid rise due to presence of bubbles on the inner sur-
face of the container. TVhere the bottle stands over
night, pressure recovery Curve 2 shows a slowing
down due to re-solution of the bubbles. The curve
taken at this stage, when there is approximate equi-
librium between the gas in the various layers of liquid
and in the gas cushion, is in reality the normal form of
curve. Curves 3 and 4, taken the same day as Xo. 2,
are speeded up due to lack of time for re-solution of
the bubbles, formed at the opening of the bottle, and
lie fairly close to No. 2. Here the time elapsing be-
tween curves is such that the speeding-up effect due
to the bubbles predominates over the slowing-down
effect caused by low concentration of gas in the upper
layers. Curve 5. taken after standing over night, is
another normal curve. Xo. 6. taken on the same day,
again shows the speeding-up characteristic.
Apr., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
composition of the gas — The repeated "blow-offs"
during carbonation (six in number) have the effect of
giving a very pure carbon dioxide in the system.
After the first two openings of the bottle (Table
IVB), the gas portions withdrawn contained 99.5 per
cent of carbon dioxide, and the major portion of the
gas showed from 99.8 to 99.9 per cent carbon dioxide.
The total residual volume, or foreign gas, was only 19.0
cc, 0.3 per cent of the total, and about one-third as much
as in the other carbonations with only two blow-offs.
RELATION OF INITIAL PRESSURE TO GAS CONTENT
From the data and discussion that have preceded it
can readily be seen why the initial pressure (the pres-
sure of the gas cushion indicated on a gauge connected
to a bottle of carbonated liquid before opening the
bottle and removing any of the gas) of a bottle of car-
bonated liquid is no indication of the gas content of
indication of the amount of carbon dioxide in the
liquid. Fig. Ill shows graphically how far the initial
partial pressures of C02 in the four experimental
carbonations depart from the saturation curve be-
tween gas content and corresponding partial pressure
of carbon dioxide. This departure of the initial pres-
sure from the saturation curve is greater in the slow
speed stirring tests, Nos. 1 and 2, where the liquid was
not brought to as high a degree of saturation as in the
high speed carbonations, Nos. 3 and 4.
If the excess gas in the gas cushion of the bottle
is withdrawn, and the bottle is not kept at o° C.
but is allowed to warm up, an excess of gas passes into
the gas cushion, all of which will not go back into solu-
tion when the bottle is again brought to ice tempera-
ture. Hence the partial pressure of carbon dioxide at
that point will bear no direct relationship to the gas
500 soco /S00 ieea zsoo 3000 jseo +voo 4S00 s-aoo ssoo feoo 6Seo
Fig. Ill — Departure of Initial Partial Pressures of COa from the Saturation Curve
that liquid. If the bottle is taken directly from the car-
bonating machine and kept iced until the initial pressure
is read, that initial pressure will simply be the pressure
of carbon dioxide under which the liquid was carbonated
and the bottle was sealed, plus the partial pressure due
to any residual foreign gas in the gas cushion.
However, if the excess gas in the gas cushion is
drawn off and the bottle kept closed and iced until
the pressure recorded on the gauge has reached a maxi-
mum (point of equilibrium between gas in liquid and
in gas cushion), the partial pressure of the carbon di-
oxide1 in the gas cushion at' that time will be a true
' The method of determining the partial pressure of COi is to record
the total pressure, withdraw the excess gas in the gas cushion, measure
the volume of foreign gas withdrawn, from that calculate the volume of
foreign gas in the gas cushion before withdrawal, then from the volume
of the gas cushion and volume of foreign gas calculate the partial pres-
sure of foreign gas, subtract this from the total pressure to give the partial
pressure of COi.
content of the liquid. The reason that the gas after
once coming out from the liquid does not readily re-
enter is due to poor surface contact between the layers
of gas and liquid not in equilibrium. Even with a
stirrer rotating at 400 r. p. m., as has been shown in
the data, equilibrium is not complete after 1 1
or 12 hrs. of stirring. Such a condition of warm-
ing up and recooling with consequent increase in the
volume and pressure of gas in the gas cushion is the
natural result of the ordinary commercial methods of
handling artificial beverages.
SUMMARY
I — A method of study has been developed for sys-
tems under high pressure, which can be applied to the
statics and dynamics of gas-liquid and of gas—
liquid-solid systems.
II — Regular rate of pressure recovery curves nearly
288
THE JOIRXAL OF INDUSTRIAL AXD EXGIXEERI XG CHEMISTRY Vol. 10, No. 4
reproducible and evidently logarithmic in form have
been obtained.
Ill — A high degree of impregnation of water with
carbon dioxide gas has been obtained using a rotary
stirrer while maintaining the liquid under a steady
pressure of gas.
IV- The effect of an increase in speed of stirring is
to tremendously shorten the time of carbonation. and
at the same time increase the degree of impregnation.
V In an efficiently carbonated water the gas con-
tent, after the first opening of the bottle, closely ap-
proximates Henry's law-.
VI The degree of impregnation of a liquid with a
gas is not directly indicated by the "initial pressure,"
that is, the pressure of the gas over the free surface of
the liquid before the first opening of the bottle.
VI I — The length of time that the carbonated water
is allowed to stand before opening bears a marked re-
lation to the maintenance of the supersaturated con-
dition after the pressure in the gas cushion is released.
This effect is evidently due to the gradual solution of
fine gas bubbles retained on the inner surface of the
container.
VIII — By "blowing off" of the foreign gases in the
gas cushion, a higher degree of carbonation can be
secured. This principle has been used by the prac-
tical men in the trade.
IX — A high degree of carbonation may be obtained
using distilled water alone, as a solvent, and if this
product is allowed to stand for a period before opening.
the carbon dioxide gas is retained remarkably well.
Bureau of Chemistry
U. S Department of Agriculture
Washington. D. C.
EXAMINATION OF AMERICAN-MADE ACETYLSALICYLIC
ACID
By Paul Nicholas Leech
Received December 29, 1917
At the request of the Council on Pharmacy and
Chemistry, the A. M. A. Chemical Laboratory has
undertaken examinations of American-made synthetic
drugs. The most extensively used synthetic is acetyl-
salicylic acid and hence an investigation of this product
was deemed expedient.
For seventeen years acetylsalicylic acid was protected
by a United States Patent (the proprietors were not
given a patent in other countries) and sold under the
name "Aspirin." In February 191 7 the patent ex-
pired, and since then a number of firms have engaged
in the manufacture of acetylsalicylic acid, selling it
either as such or as aspirin, modified, of course, by a
distinctive firm designation. During this period the
former manufacturers (The Bayer Co.. New York,
in past years called Farbenfabriken of Elberfeld Co.,
New York) have been extensively advertising, both to
physicians and the public, the alleged superior qualities
of their product. The chemical examination, there-
fore, was concerned chiefly with tests of purity, and the
comparison of the American brands with the formerly
patented product.
In European countries, acetylsalicylic acid1 is de-
scribed in the various pharmacopoeias as a condensa-
tion product of acetic anhydride or acetyl chloride with
salicylic acid (o-hydroxybenzoic acid). Generally the
test of identification is hydrolysis of acetylsalicylic acid
and qualitative tests for acetic acid and salicylic acid.
For purposes of purity the requirements are essentially
that the specimen should have a certain melting point,
should show absence of salicylic acid by means of
ferric chloride (the manipulations for the tests are
variously described) and leave no appreciable ash.
The two tests of purity most generally employed,
however, are the melting point and the reaction with
ferric chloride.
MELTING POINT
The melting point of acetylsalicylic acid has been
given at various temperatures from 1180 to 1370 C.;'
the British Pharmacopoeia describes the melting point
at 1330 to 1350 C; the German Pharmacopoeia "about
l5S° C.;" the French Pharmacopoeia at 1350 C: Xeu<
and Xonofficial Remedies, 1917. 134-136° C. The
Bayer Company, in the patent trial at Chicago a
number of years ago, gave among the "four infallible
tests" a melting point of "about 135° C." Several
men have carefully determined the melting point in
recent years. Emery and Wright3 in 191 2 found that
•Aspirin. Bayer" melted at 130.5-1310 C. In France,
Francois4 has determined the melting point of pure
acetylsalicylic acid, which, according to his method,
is 132° C. When various samples of acetylsalicylic
acid were examined in this laboratory, it was found
that the melting point of none was as high as that de-
scribed in New and Nonofficial Remedies or the British,
French, or German pharmacopoeias when taken
according to the general method of the U. S. Pharma-
copoeia, Vol. 9, p. 596. On critical observation, it may be
seen that the melting point of acetylsalicylic acid is
preceded and accompanied by decomposition. If the
sample in the melting tube is heated from the original
room temperature of the bath to 120° C, the tem-
perature of melting will be lower than if the bath is
first heated to 120° C. and the melting-point tube
then placed in the bath.5 Thus the melting point of
acetylsalicylic acid, like so many organic compounds
which decompose and do not melt sharply, is un-
satisfactory and cannot be taken as an •'infallible
test" of purity, especially when determined by different
operators who do not give their method in detail.
After making a large number of melting-point de-
terminations of acetylsalicylic acid, alone and in
parallel with other operators, it was decided to use the
1 Unfortunately, the non-descriptive name "aspirin" has been used
extensively in European literature, and has even gotten into European
pharmacopoeias, instead of the scientific name 'acetylsalicylic acid."
' For reference to older literature see Beilstein. II. 1496 (889).
» "The Melting Temperature of Aspirin and Salicylic Acid Mixtures."
I'toc Assoc. Of. Agr. Chrm. 191S ; Bureau of Chemistry. Department
of Agriculture. Bull 162
• assay of Aspirin," J Mora Chim 15 1917), No 1 213.
* Similar observations were made t>y Emery and Wright, who state:
"An accurate determination of the melting temperature in this way (the
rate of heating was such as to give a rise in temperature of about 1° per
minute) is rendered difficult by the fact that "aspirin' decomposes on heat-
ing, as evidenced in the depression of the melting temperature of the pure
substance of about 1 ° for every five minutes' heating just below its melting
temperature."
Apr., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY 28g
method described in the U. S. Pharmacopoeia modified melting point and salicylic Acid determinations
, , „ _ , c , . Melting Point Free Salicylic Acid
by first heating the bath tO I20 C. betore attaching Brand Corrected Colorimetrically
the melting-point tube tO the thermometer. Acetylsalicylic acid, P. W. R.'. 130.O-UI.0- Colored, but Rowing less
„,, ,.. • , r -c j j. i r r -J Acetylsalicylic acid. Millikin-. . 130.0-1.11.0" No color
The melting point of purified acetylsalicylic acid Acetylsalicylic acid, Minikin?
was found to be 131.5-132.5° C. (car.).1 With the aJSS&SI?^ ' iimioi. 129™00° Noco,°r
exception of one specimen, which was obviously im- 5-gram capsules' 128.0-129.0(0) Colored but showing less
^ c 125.5-126.5 (0) than 0.1 per cent(a)
oure, the various specimens examined melted between Considerably more than
r '„,,,. , • 0.1 per cent(t>)
128 and nr C. as may be seen m the accompanying Acetylsalicylic add, Squibb=. . 131.0-132.0° No color
. . . j. . . Acetylsalicylic acid (Aspirin).1
table. It would appear that this range of melting Monsanto 131.0-132.0° No color
points would be more acceptable and reliable than the Acetylsalicylic acid, M. C. W.1 KlO.5-13. .5° Colored, but showing .ess
melting points described in various standards. Acetylsalicylic acid, m. c w.1 .3.. 5-132. 5° colored, but showing .ess
Acetylsalicylic acid, M. C. W.1 131.0-132.0° Colored, but showing less
PRESENCE OR ABSENCE OF FREE SALICYLIC ACID than 0.1 per cent
Aspirin, Bayer1 (before patent
It is generally conceded that the presence of salicylic As^dBayerV.< (after patent I31 -s-I32-5° No color
acid in amounts more than traces is deleterious. expired) 128.5-129.5° Colored but showing less
than 0. 1 per cent
Furthermore, the amount of Salicylic acid is a gOOd Aspirin, Bayer1.' (after patent ,„„„,„„,„ _ , J , , . ,
' . expired) 129.5-130.5° Colored, but showing less
index of the purity of the acetylsalicylic acid, because thano.i percent
, ,. , Vi-11 i-.l- Aspirin, Lehn and Fink' 130.5-131.5° 0.1 percent
the test IS SO delicate that, Under taVOrable Conditions, Aspirin, Lehn and Fink? 130.5-131.5° Colored, but showing less
mere traces may be determined and, as a rule, the Aspirin, Lehn and Fink1 131.0-112.0° Colored. butYho^Sng less
better the product, the less the amount of free salicylic , obtained on the open markct than ° l per cent
■j - Obtained from manufacturer.
<iLlu' 3 One-third of the capsules (a) contained a white powder; two-thirds of
The tests appearing in various pharmacopoeias for <-hc : capsules (6) contained a pink powder haying strong odor of acetic acid
, ... and not complying with the tests.
Salicylic acid as an impurity in acetylsalicylic acid do ' Not described in "New Nonofficial Remedies, 1917," the other prod-
not give concordant results, different workers inter-
• 1 ,, i-n- ,1 .. j ^ -1 j OTHER TESTS
pretmg the results differently, nor are they detailed
in such a manner as to yield maximum delicacy. New and Nonofficial Remedies, 19x7, requires that
., . , ,. ., , ., , . . ... , acetylsalicylic acid shall form a clear solution with
After experimentation, it was decided to establish J ,. , . .. .. . ,, . , , . ,
. • , , ^c i-i- warm sodium carbonate solution; that sulfates, chlorides
a limit test of approximately 0.1 per cent free salicylic , , , ' . , „
. , r , ,. ,. ... , and heavy metals shall be absent; that 0.5 g. shall
acid, when carried out according to the following • , ., , «n ^ u j * j
' leave no weighable ash. All the brands reported
in this paper complied with these requirements.
0.1 g. of the substance was placed in a dry colorimeter tube and 1 cc. , .
of alcohol.' previously distilled oyer NaOH. was added. After the acetyl- So far there has been no satisfactory quantitative
salicylic acid had dissolved. 48 cc. of water and 1 cc. of fresh 0. 1 per cent estimation of acetylsalicylic acid. True, various
ferric chloride (FeC1..6H80) solution were added. At the same time a methods have been proposed, but they are objection-
control was run by treating 1 cc. of a 'standard salicylate solution the , , i i i ■ r t i i- i-
same as above.'' If within two minutes the color given by the acetyl- able. It was thought that hydrolysis of acetylsalicylic
salicylic acid is not more intense than the color given by the "standard," acj,J an(i then titrating the Solution by Comparing the
the presence of not more than 0.1 per cent free salicylic acid* is proved. formed by ferric chloride with that of a Standard
The solutions used were prepared as follows: -«w _,
Redistilled alcohol was treated with a small amount of sodium hy- control might yield interesting results, providing that
droxide for 24 hours, then again distilled. t]le conditions were alike. For this purpose I g. of
The color standard was made bv dissolving 0.116 g. of dried sodium ,,.,. ., j- 1 j ■ tiui
salicylate in water, adding 1 minim of glacial acetic acid, and making up to acetylsahcyllC acid was dlSSolved in IO CC. of alcohol
looo cc. Each cc. represents o.i mg. of salicylic acid.' and diluted to iooo cc. The solution was then heated
The ferric chloride solution was made by diluting 1 cc. ferric chloride q8-IOO°C. for 2 hours, allowing the alcohol to
(FeCb.6HiO) test solution U. S. P. with 99 cc. of water. The diluted y b
solution must be freshly prepared each day. evaporate, then allowed to stand at room temperature
„..,, .. „ j. ., • , ■ (22° C.) for 22 hours. After adding water sufficient
With one exception, all of the commercial specimens v ' . , *", . . . „ ,
, , , .. e . ., . .. , . . to make iooo cc, it was compared colorimetrically lor
examined responded satisfactorily to the above test ,. . , , „,, c . . , .
. . . It. i- r -j • * salicylic acid strength. The amount of hydrolysis
showing less than i part salicylic acid in iooo parts ' . 6 , J J ,.
. , ,. .. ., %,, ■ j- • j t 14. • varied so with different samples under the same condi-
acetylsahcylic acid. The individual results are given . ,. , ,
. .. . ,, tions, that it was realized that an approximate assay
in the accompanying table. '. , ,. , , y >i
by this method was unreliable. If the assay were
■ Isolated crystals attached to the walls of the melting-point tube. Conditions, quantitative COm-
apart from the bulk of acetylsalicylic acid, melted at a lower temperature. j"«^ ""^^
i An excess of alcohol destroys or lessens the color when only a very parisons might be possible. In one experiment, after
minute amount of salicylic acid is present. 6o cjays trie hydrolysis 0f the acetylsalicylic acid was
» The control should be made each time as standing in the air changes "... , . _;j.i, <.!,„
iu tinctorial power. 6i per cent, which is in rough agreement with the
* The presence of pure acetylsalicylic acid does not seem to affect the w'Ork of TsaklatOS and Horsh.1
iron (Fe++ +) salicylic acid coloration. The small amount of acetic acid
was added to the sodium salicylate control solution (1) to simulate an acidity DISCUSSION
approximating the acidity of the acetylsalicylic acid, and (2) since acetyl- Apart from the proposed revision of the Standards
Salicylic acid gives by hydrolysis both acetic acid and salicylic acid, it was . i i- • r V ,.i:„ n„\A ■•.
thought advisable to and acetic acid to the standard. If there is any for the melting point and limit of Salicylic an,! Ill
Ijree acetic acid in a sample of acetylsalicylic acid containing salicylic acid acetylsalicylic acid, the examination shows that 1 here
(which I believe is generally the case when salicylic acid is present) then . appreciable 1 1 i 11 VlVtlrr l.clwccll tile ValMOUS brands
it would modify the color given by the same amount of salicylic acid ' '
alone. For this reason it was thought to be more comparable to have the ' A path Zlg., 1918, p. 247; Bull. soc. Mm.. IT (1915), 401. Studies
•tandard contain a slight amount of acetic acid. of the decomposition of aspirin del. i "„, ,v til ...,1s and
' This standard is somewhat similar to the one proposed by T. W. by conductivity measurements indicate that the reaction is exceedingly
Thoburn and Paul J. Hanzlik, J. Hiol. Chem., 23, 175. complex," T. and H. Chtm. .■Ids.. 10, 591.
290
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 4
of acetylsalicylic acid examined, all of them with one
exception (acetylsalicylic acid, Millikin, 5-grain
capsules, purchased on the open market) complying
with the tests described in this paper. The Journal
of the American Medical Association, in past years, has
protested repeatedly against the monopoly given to the
Bayer Company for their "Aspirin," contending that
acetylsalicylic acid (aspirin) was not new, and that
"Aspirin, Bayer" was simply a good brand of acetyl-
salicylic acid which could be bought in foreign countries
at much lower prices than here. Although the patent
in the United States has expired, "Aspirin, Bayer" is
still being retailed at higher prices than other products
which are now enjoying the privilege of American
manufacture.
Mr. Paul Bakewell,1 in an opinion answering the
warning circular of the Bayer Co. in reference to the
use of the word "aspirin" by firms other than Bayer,
argues very ably that acetylsalicylic acid, before the
patent was granted, meant the impure substance which
was not used therapeutically, while "aspirin" was
designated as the improved product (a new article of
manufacture, the particular acetylsalicylic acid made
under the Hoffman patent) and "is the substance
now known in pharmacy as aspirin" (statement made
by an officer of the Farbenfabriken of Elberfeld Co. in
U. S. Circuit Court, 1909). The products reported
in this paper are (with the one exception) the same as
described in the Hoffman patent, and, in the sense of
Mr. Bakewell's argument, are "aspirin " However,
it would seem better if the name acetylsalicylic acid,
instead of aspirin, were used, especially by physicians
in their prescriptions because (1) it is a generic,
scientific name; (2) "Aspirin, Bayer" is sold at higher
prices than other products, whereas chemically equiva-
lent products sold under the descriptive name may be
purchased at a lower price. Finally, the manufacture
of acetylsalicylic acid in this country is another ex-
ample of the fact that American chemists can produce
the drug synthetics, and at the same time make
products as good as, if not better than, those of German
origin.
I express my appreciation to Dr. W. A Puckner for
his kind interest.
Chemical Laboratory
American Mbdical Association
Chicago, Illinois
THE DETERMINATION OF ARSENIC IN INSECTICIDES1
BY POTASSIUM IODATE
By Gborgb S. Jamibson
Received January 8, 1918
The methods employed for the determination of
arsenic in insecticides are based upon the well-known
iodimetric processes. Arsenious compounds are
titrated with iodine in the presence of an excess of
sodium bicarbonate. Arsenic compounds in a strongly
acidified solution are treated with potassium iodide
and the iodine which is liberated by the reaction is
1 'In the Matter or Aspirin. Answer to the warning circular of the
Bayer Co. of June 1, 191 7," by Mr Paul Bakewell, Monsanto Chemical
Works.
* Published by permission of the Secretary of Agriculture.
titrated with sodium thiosulfate in the usual manner.
It is not proposed to discuss in detail the various
modifications of these methods that have been sug-
gested and investigated in connection with the analysis
of arsenical insecticides. The reader is referred to the
exhaustive reports published in the Journal of the
Association of Official Agricultural Chemists, 1915,
1916 and 191 7. The method adopted as official by
the A. 0. A. C. for the determination of total arsenic
is based upon the distillation of the arsenic as arsenious
chloride by means of cuprous chloride and concentrated
hydrochloric acid. The distillate obtained is diluted
to a definite volume and aliquot portions are titrated
with iodine in the presence of sodium bicarbonate.1
The object of this paper is to show that the iodate
titration as applied to the determination of arsenic
has many advantages over the iodimetric methods.
The iodate method, which is based upon titrating
arsenious compounds with a standard solution of
potassium iodate in the presence of 11 to 20 per cent
of hydrochloric acid, until the iodine liberated during
the first part of the reaction has disappeared from the
chloroform indicator, was first described by L. W.
Andrews.2 More recently the writer3 has shown that
arsenic can be accurately determined by this method,
and confirmed the results obtained by Andrews. It
may be well to enumerate again the advantages of the
iodate titration over the iodimetric for those who are
not familiar with the literature on this subject. One
great advantage is that the iodate solution is prepared
ready for use by simply weighing the calculated amount
of pure dry normal potassium iodate,4 dissolving it in
water, and diluting to the proper volume. No further
standardization of this solution is required at any
time so long as the evaporation of the water is pre-
vented (a solution kept for seven years showed no
measurable change). This is in marked contrast to
the work and time required to prepare the iodine solu-
tion as well as the sodium arsenite or sodium thio-
sulfate solutions used for its standardization and the
restandardizatioji necessary at frequent intervals.
Another marked advantage in favor of the iodate
titration is the exceedingly sharp and definite end-point
obtained with the chloroform indicator. Furthermore
cupric and ferric compounds as well as most kinds of
organic matter have no influence upon the accuracy
of the method. In the direct titration of insecticides,
cuprous and antimonious compounds react with
potassium iodate as is the case with the iodine titra-
tion, but fortunately these compounds occur only in
very small amounts.
In connection with the determination of total arsenic
in which the distillation process is employed in order
to obtain all the arsenic in the trivalent condition,
the iodate titration has the advantage over the iodine
method not only in regard to the time required but
also in that no sodium hydroxide or sodium bicarbonate
is used. The first potassium iodate solution employed
in the present investigation contained 3.567 g. of
1 Roark and McDonnell, Tins JoUKNAL, 8 (19W
• J. Am. Chcm. So. . 16 [90S), 756.
■ This Joukxal, S (1911), 250 44 -.150.
< Ibid.. 44 (1917), 151.
Apr., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY 291
KIO3 in 1000 cc. It had the value 1 cc. = 0.003300 g. percentage AsiOj Foond
of AS2O3. When this solution was exhausted, a more Gram kio> lodate Modifed
. j T, , . , Insecticide Taken Used Method Method
convenient one was prepared. It contained 3.244 g. Paris Green No. 1 2542 0.1237 222 5692 5705
of KIO3 in 1000 cc. and had the value 1 cc. = 0.003000 £S g£S & {§&":::: 8'i2o1 208 Self 56'93
g. of As203. For the preparation of these solutions, PgjOwngj.gsg....... 0.1325 22.85 56.90 £•
Kahlbaum's pure normal potassium iodate which Paris Green No. 12489 0.1533 28.95(c) 56^65 .'..
Ej l. J-J4. o/-. j ™_ j.- Paris Green No. 1 2489 0.H24 21.23(c) 56.67
had been dried at 140 C was used. The reaction Paris Green(a) 0.1649 31.22(c) 56. so 56.85
between the potassium iodate and arsenious com- ztoT Arsenica) 02088 2625 4168 4179
pounds is represented by the following equation: S&r^^tafoV." o.tlll 2o:toW tin ti.ll
Bordeaux Zinc Arsenite(&) 0.1788 18 50 34 14
As203 + KI03 + 2HC1 = As206 + IC1 + KC1 + H2O1 Bordeaux Zinc Arseniteti.) ... . 0.2000 20.72 34. 19 '.'.'.
Bordeaux Paris Green (a) 0.3179 30.60 31.76 31.70
For the determination of arsenious oxide in Paris %£*££ £™ g£$> ; ; ; ; ; g:f|» 21.90 31.71 31.61
green or other arsenite from 0.1 ? to 0.4 g. of the sample, W a. o. a. c. 1915 Referee Sample.
*? ,. .. . » . (6) A. O. A. C. 1916 Referee Sample.
depending upon the amount of arsenic present, was (0 kio« Sol. with 1 cc. = 0.003000 E. AsiO<.
weighed directly into a 250 cc. or 500 cc. glass-stoppered
bottle. 30 cc. of hydrochloric acid, sp. gr. 1.19, 20 The results obtained by the iodate method agree closely
cc. of water, and 6 cc. of chloroform were added. wlth those of the modified Hedge procedure. It was
The titration was made by adding the potassium iodate found preferable m the Hedge method to neutralize
solution, rapidly at first, while shaking the bottle so the larSer Part of the hydrochloric acid used to dissolve
as to give the contents a gyratory motion. When the the tnsecticide with 25 per cent sodium hydroxide
iodine which is liberated during the first part of the lnstead of neutralizing all the acid with sodium bi-
titration has largely disappeared from the solution, carb°*ate, as recommended, because this is liable to
the stopper is inserted and the contents of the bottle cause some loss of arsenic on account of the violent
are given a thorough shaking. From this point, the evolutton °f carbon dioxide.
titration is continued cautiously, shaking the stoppered In order to apply the iodate titration to the de-
bottle after each addition of iodate solution, until the termination of total arsenic in any arsenical insecticide
iodine color of the chloroform has disappeared which or fungicide, the official distillation process of the
marks the end-point. It is customary to allow the A- °- A- c- mentioned above was employed and the
titrated solution to stand 5 min., then if, after shaking distillation apparatus was arranged as follows: An
again, any color is observed in the chloroform, it is 8 oz- distilling bulb, provided with a long-stem 50 cc.
expelled with the smallest possible amount of iodate dropping funnel, was connected to a 24 in. Liebig
solution. It is very important to shake the solution condenser. The outlet of the condenser was con-
more thoroughly the nearer the end-point is approached, nected to a 500 cc. Erlenmeyer flask with a bent glass
otherwise the solution may be over-titrated. Further- tube which extended through a 3-hole rubber stopper
more, it has been found that the larger the volume I0r about 4 in. The middle hole carried a safety tube
of the solution being titrated, the more shaking is l8 in- lo"g which extended within half an inch of the
required to bring the chloroform carrying the iodine bottom of the flask. The third hole carried a bent tube
in contact with the potassium iodate. The entire which extended through a 2-hole stopper to within
determination, after a little practice with the iodate half an inch of the bottom of the second 500 cc. flask,
titration, can usually be completed in about 15 min. Another bent tube just passing through the second
It should be observed that as Andrews2 has shown, hole of this stopper was arranged so that it dipped
the strength of the hydrochloric acid in which the into the 50 cc. of water placed in a 250 cc. Erlenmeyer
titration is made, is of much importance. The acidity flask which served as a trap. During the distillation
of the solution at the end of the titration should not the first two Erlenmeyer flasks were surrounded by
be less than 11 per cent of actual hydrochloric acid cracked ice in a pan. The distillation flask rested in a
so as to prevent the hydrolysis of the iodine mono- circular hole cut through a heavy sheet of asbestos
chloride. On the other hand, the acidity should not board. A wire gauze was placed under the asbestos
be over 20 per cent, otherwise the reaction proceeds board. Before starting the distillation 50 cc. of
very slowly. It is a simple matter to keep the acid water were placed in the first receiver, 100 cc. in the
within the required limits. In order to facilitate second receiver, and 50 cc. in the third. The sample
calculations, and also if it is desired to weigh larger taken for analysis was weighed directly into the dried
amounts of the insecticide, a gram or factor weight distilling bulb and 5 g. of cuprous chloride were added,
may be employed. In such cases it would be recom- This was followed by 100 cc. of hydrochloric acid,
mended that the sample be dissolved in 200 cc. of sp.gr. 1. 19, which washed any material sticking to the
hydrochloric acid, sp. gr. 1.19, and made to 500 cc. neck into the bulb. Care must be taken that none
volume; then to each 100 cc. aliquot, 10 cc. of hydro- of the sample or cuprous chloride enters the outlet
chloric acid should be added to maintain the proper tube of the distilling bulb. When the volume in the
acidity. Using a potassium iodate solution of which distillation bulb is reduced to about 40 cc, 50 cc.
1 cc. = 0.003300 g. As203l the following results were more of the acid are added through the dropping funnel
obtained: and the distillation is continued until the volume
,,,„.,,,, is again reduced to about 40 cc. Then 25 cc. more
1 Am. J. Set.. 44 (1910. 151. . , . , , , , _, ,. ..,, ,. . „ . , ,
*Loc.cit. of the acid are added. The distillation is finished
292 TEE JOURNAL OF INDUSTRIAL AND ENGINEERING I HEMISTRY Vol. 10, No. 4
when the contents of the bulb are reduced to not more Total arsenic as
Cc of KIOj ASjOj P« cent
than 20 cc. This procedure ensured the distillation . Gram tscd for iodate official
, ,. ,, . ,, ., ,. .... .. Insecticide Taken 100 cc. Aliquot Method Method
or all the arsenic. Alter the distillation was com- Pans Green No 1^542 0478'' 18 20 57 06 57 is
pleted, the condenser and connecting tubes were gffigSSSt iUS:!:: "1o \%\l 11%
thoroughly rinsed into the receivers. The contents Fgjgj-jg............. ... 0.5m 23.33 56.88 56.92
of the first two Erlenmeycr flasks were transferred to a Bordeaux Paris Green(a) 0.5865 12.55 32.09 32. 06
500 cc. graduated flask. These flasks were rinsed Bordeaux Paris Greent,.) ° 652°{b n'ls 32:09 32.'2
1 ,. . ,. f ., ., . , Lead Arsenate-Arscnite(d) 0.4052 7.20 26.65
several times, using the entire contents of the th.rd Lead Arsenatc-Arsenitcij.) 0.4945 8.80 2670 26 71
flask which served as a trap. Then each flask was SSrf£S!^taS*i(i).V.V.: 0M.06 uiS &JS till
rinsed again with a small quantity of water. All of Bordeaux zinc Arsenite(fc) 0.6193 14. 18 34.34 34.38
,, . . .. , . ./ , . j„ , t, r (0) A. O. A. C. 1915 Referee Sample.
the rinsings were added to the graduated flask. Before (6) a. o. a. c. 1916 Referee Sample.
diluting to the mark, the solution in the c,oo cc. flask .. . . r ,.~ ., . - , .
. ' , , J their transference difficult, it was found preferable to
was warmed to 20 C An aliquot of 100 cc. was . , , . . ,.„
, , . .. ... .. , , , , . , , ... weigh portions of the samples by difference from
placed in the titration bottle along with 6 cc. of chloro- . . ., .. . . ,
; . . , ... ., . . . , . specimen tubes rather than attempt to weigh, for
form and titrated with the potassium iodate solution , T, u , ,
, .. , , „ r., , . example, an exact 0.5 g. The results of the test
as described above. It more than 2s or 26 cc. of the , . .. . . 7 ., , ,
. , , .. . , . analyses by the iodate method given above show
iodate solution were required, 10 to 15 cc. of con- „ ... .. , . . , , ., „ . ,
, , , , . . , , , , , , o . , excellent agreement with those obtained by the official
centrated hydrochloric acid were added before finish- .. , ° . lt . . , . ,
,,,.,. . , . . , method. I his accurate method is not only quicker,
ing the titration in order to maintain the proper , . . . , . .... . _^
?,. _ . ,. . f . , but is simpler than the iodine titration. The very
acidity, .bor comparison, aliquots were titrated with . ^ . , , , , , . . A,
, , . ,. . ,. , _ . , definite and remarkablv sharp end-point, the great
standard iodine solution according to the official , ... . ." , , , .
.,■,,., . ,-. . „ stability of the potassium iodate solution, and the
method of the A. 0. A. C. ,. ....:,.. , , „
TT . . . , . , .. , , . . readiness with which it can be prepared all recommend
Using a potassium iodate solution ot which 1 cc. = . . , ,. . ■
. „ .. , ,, , , . . its use in place of the lodimetnc procedure.
0.003000 g. AS2U3, the following results were obtained:
On account of the physical property of the powdered v s d.p«tkwiC« w-i.t»«
insecticides which made them adhere to glass, making Washington, d. c.
LABORATORY AND PLANT
NOTES ON SODIUM CYANIDE
By W. J. Sharwood
Received January 15, 1917
The contradictory evidence given by certain "ex-
perts" in a recent sensational murder trial indicates
an imperfect realization, even by some chemists, of the
fad that commercial potassium cyanide can scarcely
be said to exist at the present time, its place having
been usurped by the sodium compound. Sodium
cyanide is now widely used as a solvent of the precious
metals in ore treatment, in electroplating, and also
as a source of hydrocyanic acid for fumigation,
especially in western orchards where gaseous hydro-
cyanic acid is applied as an insecticide to individual
trees which are covered with tents during the process.
The sodium cyanide of commerce is one of the purest
technical salts now available, containing 96 to 98
:t NaCN, with less impurity than is found in
most samples of potassium cyanide sold as chemically
I wish to suggest here that chemists might with
advantage make a point of recognizing the use of
sodium cyanide, and call it by that name in their
laboratories. As with so many other alkali-metal
.salts, we can now use the sodium instead of the potas-
sium compound as a reagent, except in the very few
cases where the potassium ion is essential to the re-
action, or where there is some marked difference in
solubility. Sodium cyanide not only contains less
carbonate and sulfide, but is cheaper, reacts identically
with the salts of silver, copper, zinc, etc., c.v
concentrated solutions, and is more permanent in
solution than ordinary potassium cyanide, showing
less decomposition and no discoloration on keeping.
It has an additional advantage in not being del-
iquescent.
It seems desirable for the medical and pharmaceuti-
cal professions to revise their standards for cyanides — -
presumably this has been done in preparing the new
Pharmacopoeia. The alkaline cyanide now sold must
be much more poisonous than the old material, which
was no doubt the basis of most of the familiar state-
ments as to its lethal effects. It has long been stated
that s grains of cyanide have repeatedly proved fatal —
at which rate a pound would suffice to kill some 1400
people. This statement no doubt refers to cyanide
of ill old type, containing probably 30 to 35 per cent
assium cyanide or. say. 12 to 14 per cent of
cyanogen. Modern sodium cyanide — commercial as
well as "C. P. " — contains 50 to 52 per cent cyanogen,
or practically four times as much as the material
formerly sold, and is presumably four times as lethal
in its action, so that a pound would suffice for over
5000 fatal doses.
Nearly thirty y< hen potassium cyanide
was suggested as a practical solvent for extracting
gold from ore. various objections, mainly based on
limited experience, were raised: It would not dissolve
gold in practical quantities; its solution was extremely
unstable; it was highly dangerous on account of its
poisonous qualities; the world's sources of supply were
altogether insufficient. All these objections have
proved groundless. Both gold and silver are success-
fully and economically extracted; the dilute solution
"keeps'* admirably when handled on a large scale;
Apr., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
2 93
the only recorded deaths attributable to its use have
been due to gross carelessness; the supply has been
enormously augmented with increased demand and the
quality improved, while the price per unit of cyanogen
has been reduced to a fraction of the former cost.
At that time, in addition to its use for electroplating,
potassium cyanide was employed widely, but in com-
paratively small quantities, in western gold mills for
the purpose of removing stains from the amalgamated
copper plates and facilitating the amalgamation of the
gold. Samples of the commercial salt which I have
tested usually contained from 10 to about 35 per cent
of potassium cyanide, with a large proportion of
potassium carbonate; it was a highly deliquescent
mixture, sold in tin cans holding from 1 to 20 lbs.
This material was derived from hoofs, horns, and the
like, by first preparing and crystallizing potassium
ferrocyanide, which was then heated, alone or with
addition of potassium carbonate or carbon, the re-
duced iron, etc., being allowed to settle through the
fused mass. Sodium was present only in small quanti-
ties, and the deliquescence was due to the potassium
carbonate remaining or resulting from the decom-
position of the cyanide. Sometimes sodium carbonate
was used in fusing the ferrocyanide.
With increasing demand other sources of nitrogen
were drawn on. Ferrocyanide was obtained from
coke and gas works; thiocyanates from the same
source were desulfurized. Ferrocyanide was made to
give a larger yield by reducing it with metallic sodium,
or with a lead-sodium alloy, yielding a mixed cyanide,
NaCX + 2KCN. Beet-sugar waste (schlempe) was
made to yield a certain amount of cyanide. Synthetic
methods have also been introduced; ammonia and
metallic sodium forming sodamide (NaNH2) which,
on heating with carbon, finally yields nearly pure
sodium cyanide, etc.
Formerly it was possible to purchase fairly pure
potassium cyanide for special purposes, prepared by
passing hydrocyanic acid into an alcoholic solution of
potash; but pure sodium cyanide was very difficult
to get. Some years ago I obtained some sodium
cyanide of German manufacture, labeled "C. P."
and "very highest purity," but when trying to prepare
pure sodium zinc cyanide the first crystals to separate
proved to be those of the potassium compound, the
sample of guaranteed sodium cyanide containing
nearly 1 per cent of potash and a considerable amount
of carbonate. Commercial fused sodium cyanide of
domestic origin, now obtainable for something like
28 cents per pound1 in lots of 100 lbs. or more, contains
a mere trace of potash, and only 2 to 4 per cent of all
impurities combined.
Originally, as just mentioned, commercial cyanide
contained potassium as the positive radical with
various impurities, such as carbonate, but little or no
sodium or other base was usually to be found. It was
tested by titrating the cyanogen with standard silver
nitrate, Liebig's method, and analysts were accus-
tomed, quite correctly, to report it in terms of KCN;
40 parts of CN found being reported as 100 of KCN*.
1 Since 1916, when this was written, war conditions have increased the
price of cyanide materially.
It may be recalled that pure KCN contains, by
calculation, 39-97 per cent of CN; pure NaCN con-
tains a much higher proportion, 53.07 per cent CN.
For most purposes these are taken as 40 per cent and
53 per cent, respectively.
As the potassium in commercial cyanide was
gradually replaced by the lighter atom of sodium,
other things remaining the same, the percentage of
cyanogen was correspondingly increased. This allowed
manufacturers to make a salt containing a large pro-
portion of impurity, which would still titrate 38 or
39 per cent cyanogen and would be reported on the
old basis as 97 or 98 per cent KCN. Pur,e sodium
cyanide, by the same system, would have been re-
ported as 5300/40 or 132.8 per cent KCN. In fact,
sodium cyanide was sometimes deliberately diluted
with inert material (carbonate, etc.) to supply the
demand for 98 per cent KCN. At first there was a
prejudice against the use of sodium cyanide in gold
extraction, some early experiences indicating that it
was less efficient, but laboratory tests indicate that
equivalent amounts of the cyanides of potassium,
sodium, and calcium are equal in effect, and sodium
cyanide is now almost exclusively used in the industry.
In fact, with the present shortage of potassium, owing
to war and other conditions, it would be impossible to
supply the potassium compound in anything like the
required quantity.
Until recently, however, cyanide has continued to
be sold and used on the basis of its KCN equivalent,
even if no trace of potassium was present; thus com-
mercial NaCN was commonly sold as "128 per cent
KCN," and most works using cyanide also continued
to make up their solutions on the basis of KCN. For
the past year cyanide has for the first time been
generally sold on the more rational basis of its cyanogen,
or its actual NaCN, content; thus the highest grade
is now offered as either "sodium cyanide 96 to 98
per cent" or "cyanogen 51 to 52 per cent," while the
old, so-called "98 per cent KCN" used to carry about
39 per cent cyanogen. Four pounds of this sodium
cyanide are therefore chemically equivalent, and
actually equal in effect as a solvent, etc., to about
5 lbs. of the old "potassium cyanide," and there is a
corresponding saving of about one-fifth in freight and
storage. There is no reason why all users of cyanide
should not accept the rational method of reporting the
concentration of their solutions in terms of the sodium
cyanide which they actually are using, and discard the
absurd fiction of calling it — or translating it into —
potassium cyanide, which causes unnecessary trouble
in making up solutions, etc.
At various times commercial cyanide has been cast
in thin slabs, and in large bricks weighing up to 50
lbs. or even more. Some produced in the wet way
has been sold in granular form, and some briquetted.
The most recent and convenient system is to cast it
mechanically into uniform egg-shaped cakes weighing
an ounce each, so that for many purposes, such as
fumigation, no further weighing is necessary. It was
formerly shipped in boxes with an air-tight lining
of sheet zinc, of 112 or 224 lbs. each; tin-plate is
294
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 4
now used for lining and 200 lbs. is the usual net
weight.
ANALYSIS
For titrating potassium cyanide it has been the uni~
versal custom to make up a solution containing 1.303
per cent silver nitrate, so that 1 cc. was equivalent to
10 mg. KCN. This was roughly 0.0767 N. For
titrating commercial sodium cyanide it is possible,
by a convenient coincidence, to use N/10 or N/20
silver solution without necessitating any calculation.
One cc. of N/10 silver solution is equivalent (by
Liebig's titration, or using the preferable modification
with potassium iodide indicator) to 5.202 mg. of
CN, or to^exactly 9.802 mg. of NaCN. Now 98 is
almost the exact percentage of actual NaCN in the
high-grade commercial material now in use. Therefore
we can titrate solutions with N/ 10 silver nitrate and
call 1 cc. equivalent to 10 mg. of the actual 98 per cent
salt which has to be weighed out in making up the
solutions. For technical purposes it is perhaps prefer-
able to use N/20 solution (1 cc. = 5 mg. commercial
NaCN) as the end-point with iodide indicator is very
delicate and the burette readings then also indicate
"pounds per ton of solution" directly. For instance,
taking a 10 cc. sample: suppose 2 cc. of N/20 silver
nitrate are consumed; this indicates 10 mg. or 0.10
per cent of commercial sodium cyanide in solution,
or 2 lbs. per ton of solution — the "ton" or "fluid ton"
used in hydro-metallurgy being about 32 cu. ft., or the
volume of 2000 lbs. of water.
When determining sodium and potassium in a
mixed cyanide, chlorides and carbonates being the
usual impurities, it is often possible to work by directly
evaporating with hydrochloric acid, gently igniting
and weighing the mixed chlorides remaining, and
titrating chlorine in part of the residue. The follow-
ing formula, based on 1914 Atomic Weights, gives the
results in the most direct manner possible:
If A = grams mixed chlorides, and
B = total grams chlorine in mixed chlorides;
then K in grams = 2.4286 A — 4.004 B, and
Na in grams = 3.004 B — 1.4286 A = A — B — K.
Not infrequently the class of cyanide can be de-
termined simply by titrating cyanogen and alkalinity
in a freshly prepared solution, using methyl orange as
indicator.
The determinations in the following table may be
taken as typical.
It may not be out of place to call attention to the
importance, when testing cyanides for the presence of
alkaline sulfide, of preparing the solution at the
moment of making the test, or, what is better, of dis-
solving the solid cyanide in the reagent to be applied.
If the cyanide is dissolved in water and allowed to
stand even a few minutes, the sulfide content may be
seriously diminished, and traces of sulfide may be
easily overlooked. Three simple methods are avail-
able: Shaking with fine lead carbonate suspended in
water; dissolving the solid cyanide in a solution of
silver nitrate containing slightly less than 1 mol.
AgNOa for 2 equiv. CN; or dissolving the solid cyanide
in a little mercuric chloride solution; each of these
reagents yielding a black precipitate or dark coloration.
The sulfide may be quantitatively determined by the
silver or mercury method.
Cc. normal acid
neutralized by one
gram of sample
iv ,1 _& tJ.
1 Z !S3 n°- £° "HZ
<n O o ft. S S u
Per cent Per cent Cc Cc. Ce.
1 "Straight" Potassium
Cyanide Strong
test 38.2 95.5 13.0 14.9 14.7
2 Mixed Salt, high in f Fairly
potassium J strong 39.0 97.5 13.5 15.5 15.0
I test
3 Similar to No. 2 I in each 39.3 98.25 14.0 16.0 15.1
4 Sodium Cyanide, diluted Strong
with carbonate test 38.4 96.0 19.3 14.75
5 Similar to No. 4 Strong
test 40.4 101.0 19.5 15.5
6 Sodium Cyanide (com-
mercial) Trace 51.5 128.75 18.0 20.4 19.8
7 Pure KCN (calcd.) 39.95 100.00 .. 15.34 15.34
8 Pure NaCN (calcd..) 53.07 132.8 .. 20.37 20.37
9 NaCN (73.5%) diluted
with NaiCO. (calcd) 39.0 97.5 .. 20.0 15.0
10 NaCN (73.5%) diluted
with NaCl (calcd.) 39.0 97.5 .. 15.0 15.0
Incidentally, while sodium cyanide is not deliques-
cent, it is decidedly more soluble in water than potas-
sium cyanide. The following determinations were
made with the commercial salt, using a sample titra-
ting about 98 per cent NaCN.
Actual Commercial
NaCN NaCN (98%) Actual
Sp. Gr. per 100 Cc. per 100 Cc NaCN
18-20" C Grains Grams Percent
1.205 44.75 45.65 37.9(a)
1.122 25.65 26.16 22.86
1.087 18.3 18.67 16.84
1.0475 9.65 9.84 9.22
(a) Nearly saturated.
A fair approximation to the concentration of a not
too dilute solution of such material may be obtained
from the formula:
(Specific Gravity — i) X 200 =
Grams NaCN per 100 cc.
STABILITY OF SOLUTIONS
In dilute solutions there is no apparent difference
in the stability of sodium as compared with potassium
cyanide; in each case decomposition is greatly in-
creased by access of air and retarded by presence of
free alkali.
Two strong solutions were prepared, one containing
approximately 10 per cent of commercial sodium
cyanide, the other 13 per cent of "straight" potassium
cyanide. They were kept in stoppered 200 cc. bottles,
which were at first completely filled, but from which
small samples were taken at intervals and titrated for
cyanogen and for alkalinity toward methyl orange.
NaCN KCN
CN per A'/IO H1SO1 CN per 2V/10 HiSO,
100 cc. per cc. 100 cc. per cc.
Grams Cc. Grams Cc.
Original solution 5.12 19.2 4.59 17.8
After 20 days 5.09 19.3 4.40 18.1
After 40 days 4.93 19.4 4.24 18.3
After 38 months 3.05 22.4 2.32 20.0
Condition after 3 years. . . . Colorless and clear Clear yellow solution.
Strong odor of Very slight brown
ammonia deposit on glass
Strong odor of
ammonia
This indicates that in strong solutions there is com-
paratively little difference in stability, the advantage,
if any, lying on the side of the sodium compound,
which lost about 40 per cent of its cyanogen in 38
Apr., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
29S
months against nearly 50 per cent lost by commercial
potassium cyanide.
HoMESTAKB MlNB
Lead, South Dakota
A COMPARISON OF THE PROXIMATE AND MINERAL
ANALYSIS OF DESICCATED SKIM MILK WITH
NORMAL COWS' MILK
By Everhart P. Harding and Hugo Rinostrom
Received August 30, 1917
The purpose of this paper was to compare the prox-
imate and mineral analysis of desiccated skim milk
with normal cows' milk and to determine, if possible,
whether foreign substances had been added before
or during desiccation.
METHOD OF DESICCATION
There are two general methods used in making
desiccated milk. One is drying the milk on steam-
heated drums and the other is spraying the milk into
a chamber through which a current of hot air is pass-
ing. All drum processes of drying the milk are really
the moisture content which varies from 2 to 9 per cent
or even more.
The fat content, of course, depends upon the ex-
tent to which the fat is removed before the milk is
desiccated. The amount present is very small, rarely
exceeding 2 per cent.
A number of proximate analyses have been made
from time to time, but the majority have been made
within the last 10 years. Of the eight analyses given
in Table I, all except the first have been reported
since 1905.
EXPERIMENTAL PART
Four different samples of desiccated skimmed milk
were purchased on the market or obtained from users
of milk powders. Sample I was made by the Inter-
national Milk Products Company, Detroit, Michigan;
Sample II by the Minnesota Dry Milk Company,
Anoka, Minnesota; Sample III by the International
Milk Company, Plymouth, Michigan; and Sample
IV by the California Central Creameries, San Fran-
cisco, California.
Table I — Percentage Composition
TeichertW)
8.54
1.31
32.71
50.24
7.20
(a) Mitchindust, 1889, 90; VNa., 4, 419; Chem. Zentr., 61 (1890), 72. (6) Che
des allgem. osier. Apolheker Vereins, 1905-6, 8; Z Nahr. Genussm., 13 (1907), 285.
Cenussm., 20 (1910), 476. (<■) This Journal, 4 (1912), 543. (J) Allgauer Monatschr.f. Milchwirlsch
109. (j) Ibid., 26 (1913), 445. (h) J. Soc. Chem. Ind., 34 (1915), 109
Milchindust(a)
Water 4.17
Fat 1.65
Protein 35 . 56
Lactose 52 . 37
Ash 7.51
Max Popp(6)
Mansfield (c)
4.54
8.96
1.25
0.57
35.01
30.59
51.22
48.62
7.98
8.10
Skim Mas Powders
) Fleming(e)
TeichertC/)
Goy(«)
2.53
7.40
2.81
1.81
1.56
2.10
38.16
32.50
33.51
49.32
52.57
53.43
8.21
6.27
8.04
-Zlg., 33 CI 909), 647. (c) XVIII Jahresberichl der
(d) Jahr. Milch. Unter. Allgau zu Memming.e<i. 1909,
Vieh., 1 (1913), 31; Z. Nahr. Genuss
Mohan(A)
8.3
1.7
33.8
49.3
6.9
unter.-anstalt
11; Z. Nahr.
71., 26 (1913),
Table II — Percentage Composition op Skim Milk Powders as Givbn in Tablb I Computed
Moisture-Free Basis
Milchindust Max Popp
Protein 37.09
Lactose 54 . 65
Ash 7.83
36.77
53.66
8.36
Mansfield
0.62
33.60
53.40
8.89
Teichert
1.43
35.76
54.90
7.87
Fleming
1.85
39.03
50.44
8.39
Teichert
1.62
35.07
56.44
6.77
34.48
54.97
8.27
36.86
53.76
7.52
modifications of the Just-Hatmaker1 process, in which
the milk is spread in thin films on to drums by a dis-
tributing pipe.
In the spraying process, the milk is pumped through
a nozzle and delivered in a fine spray into a chamber
through which a current of heated air is passing.
The extent to which the proteins are coagulated de-
pends largely upon the method used in desiccating
the milk. To increase the emulsifying power of the
casein different substances may be used.
odor and color — The color of the powders was
yellowish white, except Sample III, which had a brown-
ish tinge and an unpleasant odor. The other three
samples had a milk-like odor.
emulsifying quality — The emulsifying power of
the powders was tried with water at room tempera-
ture and at 400 C. Approximately 2 g. of milk pow-
der were stirred up with a little water to a uniform
paste. Water was then added slowly with vigorous
stirring until about 20 cc. had been added, giving an
Table III— Percentage Minbral Composition op Mh.k Ash and Whole Milk
Potassiu
Caldu"
Marchand
1000 Parts
of Milk
oxide 1.071
ude 0.636
1 oxide 1 . 864
ium oxide 0.299
Ferric oxide 0. 127
Chlorine 0.751
Phosphoric anhydride 2. 102
Sulfuric anhydride 0.323
Carbon dioxide 0.277
Silica 0.006
Moisture
Carbon and impurities
Loss
Total ash 7.456
Oxygen corresponding to chlorine 0. 176
Corrected ash 7.28
(a) Z. Biol., 10, 295. (b) Bet., Raden, 1886-6, 64.
PROXIMATE ANALYSIS
The composition of the different desiccated skim
milks is surprisingly uniform with the exception of
1 J. A. Just, U. S. Patent 712,545, Nov. 4. 1912; J. Soe. Chem. Ind.,
«1 (1902), 1548; J. R. Hatmakcr, English Patent 21,617, Oct. 4, 1902;
J. Soc. Chem. Ind., 22 (1903), 1 145.
Schrodt
Richmond
Bat
cock
Per cent
Per cent
Per cent
Per 1000
of Milk
in Ash
Fleischmann(6)
in Ash
in Ash
in Ash
Parts Milk
22.14
21.539
25.42
28.71
25.02
1.75
13.91
11.817
10.94
6.67
10.01
0.70
1.599
20.05
20.383
21.45
20.27
20.01
1.40
0.210
2.63
3.120
2.54
2.80
2.42
0. 17
0.0035
0.04
0.300
0.11
0.40
0.13
0.01
21.27
12.813
14.60
14.00
14.28
1.00
24. 7S
29.000
25.11
29.33
24.29
1.70
2.378
4. 11
trace
3.84
0.27
0.533
0.97
0.300
0.250
0.353
8.360
104.79
102.886
103.28
0.383
4.79
2.886
3.28
7.977
100.00
100.000
100.00
100.00
'■
emulsion of approximately the same consistency and
composition as normal skim milk. Samples I and II
emulsified well with water at room temperature,
giving a milk-like emulsion, without any settling of
protein in 4 hours. Sample III gave a very poor
emulsion, yellowish brown in color. A flocculent
296
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 4
precipitate collected immediately on top of the emul-
sion, and a precipitate settled to the bottom in a
short time. After 4 hours the emulsion was strati-
fied, the middle stratum having a serum-like, but turbid,
appearance. Sample IV gave a fair emulsion from
which some protein settled in 4 hours. With water
at 400 C, Samples I, II and IV gave good emulsions
without any settling of protein in 4 hours. Sample
III gave the same kind of an emulsion as with water
at room temperature, except that stratification pro-
ceeded more slowly.
proximate analysis — The powders were analyzed
for moisture, ash, fat, protein, lactose and acid con-
tent and the acidity recorded as free lactic acid. The
following results were obtained:
Table IV — Proximate Analysis
Sample I Sample II Sample III Sample IV
Per cent Per cent Per cent Per cent
Ash 7.89 7.98 7.45 7.49
Fat 1.42 1.82 1.01 0.85
Protein 32.86 33.72 37.01 33.41
Moisture 5.60 4 71 7.09 6.60
Lactose 48.49 47.67 41.38 47.13
Acidity 1.58 1.57 1.43 1.69
97.84 97.47 95.37 97.17
Hydration of lactose... 2.43 2.38 2.07 2.37
Total 100.27 99.85 97.44 99.54
Table V — Averages op the Proximate Analysis on Moisture-Free
Basis
Sample I Sample II Sample III Sample IV
Per cent Per cent Per cent Per cent
Ash 8.36 8.37 8.02 7.02
Fat 1.50 1.91 1 08 0.91
Protein(a) 34.81 35.38 39.83 35.77
Lactose 53.94 52.52 46.76 53.00
Acidity 1.67 1.64 1.54 1.81
100.28 99.82 97.23 99.42
(a) With one molecule of water of crystallization.
Taiu.k VI — Proximate Analysis Computed on Milk Containing Nine
Per cent "Solids-not-Fat"
Sample I Sample II Sample III Sample IV
Per cent Per cent Per cent Per cent
Ash 0.75 0.75 0.72 0.72
Fat 0.135 0.179 1.097 0.082
Protein 3.13 3.18 3.58 3.22
Lactose 4.85 4.73 4.20 4.78
Acidity 0.16 0.15 0.14 0.16
Table VII — Ash. Protein, and Lactose Content Compared with the
Amount Found in Normal Milk
Ash Protein Lactose
Per cent Per cent Per cent
Richmond 0 73 3.41 4.70
Leach 0.71 3.55 488
Babeock 0 . 70 3 . 80 4 . 50
Sample 1 0.75 3.12 3.45
Sample II 0.75 3.18 4.73
Sample III 0.72 3.58 4.20
Sample IV 0.72 3.22 4.78
With the exception of Sample III, the proximate
analyses of the powders compared favorably with
the analyses made by others on skim milk powders
In Sample III the lactose is extremely low and the
protein extremely high and these results were confirmed
by repeated determinations. The use of some other
number than 9 for "total solids-not-fat'' would either
Table VIII — 'I'm: MlNBRAX Constituents in tiii-: Aah
Sample I Sample II Sample III Sample IV
Per cent Per cent Per cent Per cent
Potassium oxide 24.05 25.49 22.44 25.81
Sodium oxide 8.35 9.37 9.60 8.02
Calcium oxide 23.57 21.99 25.86 23.32
Magnesium oxide 3.18 2.92 3.07 3.08
Ferric oxide(a) 0.035 .0.035 0.034 0.049
Sulfuric anhydride(t) 0.38 12.14 13.69 12. IS
Phosphoric anhydride(t>) . . . 32.69 31.44 32.78 34.25
Chlorinc(c) 12.46 14. :8 14.04 12.37
U) The iron was determined volumctrically by Lacks and Frieden-
thal's modification of the potassium sulfocvnnidc method.
(6) The sulfur and phosphorus were determined on the milk powders.
The organic matter was completely oxidized in a closed cartridge with
sodium peroxide and the phosphorus determined by the titration method.
(«) The chlorine was determined by the method of Paul Poetschke,
This Journal, 1 (1910). 210.
Table IX — Mineral Constituents in the Commercial Powders
Computed on the Moisture-Free Powder, Ash and Normal
Milk Basis
Sample I
Commercial Normal Milk
Sample Dry Powder Ash 9% Solid*
Percent Percent Percent Parts per 1000
Potassium oxide 1.90 2.01 24.05 1.809
Sodium oxide 0.66 0.700 8.35 0.630
Calcium oxide 1.86 1.97 23.57 1.773
Magnesium oxide 0 251 0.266 3.18 0.239
Ferric oxide 0 00273 0.0029 0.035 0.026
Sulfuric anhvdride 0.897 0 951 11.38 0.856
Phosphoric anhydride 2.58 2.73 32.69 2 457
Chlorine 0.981 1.04 12.46 0.936
Sample II
Potassium oxide 2.03 2.13 25.49 1.917
Sodiumoxide 0.746 0.783 9.37 0.705
Calcium oxide 1.75 1.84 21.99 1 656
Magnesium oxide 0.232 0.244 2.92 0.220
Ferric oxide 0.0027 0.0029 0.035 0.0026
Sulfuric anhydride 0.971 1 02 12.14 0.918
Phosphoric anhydride 2.51 2 63 31.44
Chlorine 1.14 1.20 14.28 1.080
Sample III
Potassium oxide 1.68 1.80 22.44 1.620
Sodiumoxide 0.715 0.77 9.60 0.693
Calcium oxide 1.92 2.07 25.86 1.863
Magnesium oxide 0.228 0.246 3.07 0.221
Ferric oxide 0.0025 0.0027 0.034 0.0024
Sulfuric anhydride 1.02 1.10 13.69 0.990
Phosphoric anhydride 2.45 2.63 32.78 2.367
Chlorine 1.05 1.13 14.04 1.017
Sample IV
Potassium oxide 1.93 2.07 25.81 1.863
Sodiumoxide 0 600 0.643 8.02 5.787
Calcium oxide 1.75 1.87 23.32 1.683
Magnesium oxide 0.230 0.247 3.08 0.222
Ferric oxide 0.0036 0.0039 0.049 0.0035
Sulfuric anhydride 0.909 0.974 12.15 0.876
Phosphoric anhydride 2.57 2.75 34.25 2.475
Chlorine 0.926 0.992 12.37 0.893
increase the protein still more or decrease the lactose
still more. This ratio of protein to lactose is ab-
normally high for herd milk.
The mineral constituents are found in Tables VIII
and IX.
Tables IX and III give a comparison of the per-
centages of mineral constituents found in the milk
powders and their ash and that found in normal
cows' milk and its ash. In reducing the percentages
of the mineral constituents as found in the milk pow-
der to corresponding percentages in normal cows'
milk, 9 per cent was assumed as representing the total
solids-not-fat in normal cows' milk.
CONCLUSION
The percentages of the mineral constituents in the
four samples agree quite closely, but do not agree
very well with those found by other analyses. The
potassium oxide and chloride agree well. The sulfuric
anhydride is much higher than that found by others;
this is due to the method used in its determination.
The calcium oxide, magnesium oxide and phosphoric
anhydride are all higher than the values found by
others. The higher phosphorus content may be due
entirely to the method used in its determination or
also in part due to the addition of some phosphate
used as an emulsifier. The calcium is also much
higher and may have been added in some form as an
emulsifier. The ferric oxide content is lower and this
is probably due to the method used in its determina-
tion. A low percentage of ferric oxide in milk has
been found by the "cupferon" method.1 This method
was tried but did not give consistent results.
The color, odor, emulsifying power, high protein,
low laetosc. high calcium and phosphorus content,
and low total approximate analysis would indicate
i Z. \ahr. Gexussm., 23 11912), 514.
Apr., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
297
that Sample III was not genuine desiccated skimmed
milk powder.
Chemical Laboratory
University of Minnesota
Minneapolis, Minnesota
AN IMPROVED AUTOMATIC PIPETTE- WASHING
DEVICE
By Aubrey Vail Fuller
Received November 17, 1917
Since his publication of an article in This Journal,
Vol. 9. p. 1046, entitled "A Convenient Automatic
Device for Rapidly Washing Pipettes," the author
has designed a modified form of the apparatus referred
to, which embodies several improvements.
In the accompanying illustration A is a cylindrical
metal tank, provided with a siphon, B, and an inlet
pipe, C. D is a brass rod which carries at its lower
extremity a disk of rather heavy brass gauze, to which
is fastened three legs of such length that when placed
in the cylinder the gauze is supported at a level slightly
above the tops of the two lower orifices. There should
be about l/i6 in. clearance all around between disk
and tank.
The operation of the device is as follows: Water
is admitted through the inlet C which is connected
to the supply tap, at such a rate that the speed at which
the siphon empties the tank is somewhat greater than
the speed at which the tank is filled. The pipettes
to be washed are then placed, tip up, in the tank, the
lower ends resting on the gauze. As the tank is alter-
nately filled and emptied the pipettes are rinsed. To
remove the pipettes they are raised to within easy
reach by means of the "lifter" D.
With an apparatus of the dimensions of that pic-
tured, the period of a complete cycle is approximately
e
Biochem. Division
Bureau of Animal I
S. Department of Agri
Washington, D. C.
45 sec. Inasmuch as two cycles are required for the
average pipette, only about one and one-half minutes
are necessary for thorough rinsing. Its capacity
terms of 25 cc. transfer
pipettes is 13, and in terms
of 1 cc. measuring pipettes
about 100, when loosely
packed. The time economy
of such a device over hand
washing is thus apparent.
The points in superiority
of this device over the one
previously described are:
(1) greater capacity, (2)
smaller table space occu-
pied, (3) lower first cost,
(4) cleansing of both out-
side and inside of pipette.
It might be mentioned
that an apparatus of this
type would find particular
application in laboratories
conducting serological work,
where large numbers of
pipettes must be rinsed
before sterilization. Its
field of usefulness is, how-
ever, entirely general and
the details of its construc-
tion admit of wide varia-
tions to suit peculiar con-
ditions.
C
' — B,
ADDRL55L5
METHODS OF GAS WARFARE'
By S. J. M. Auld, British Military Mission
All I can do in the short time available is to give you, if I can,
a general idea of what gas warfare really means on the Western
Front at the present time. Some of you may have gotten the
idea that gas is just an incident, and that there is not as much
attention being paid to it as there was two years ago. That idea
is entirely wrong. Gas is used to a tremendous extent, and the
amount that has been and is being hurled back and forth in shells
and clouds is almost unbelievable. I will try' to give you a general
idea of what is occurring and make the lecture rather a popular
than a technical description. I shall also, for obvious reasons,
have to confine myself to describing what the Germans have
been doing, and will say nothing about what we are doing.
Possibly the best plan would be to state more or less chron-
ologically what occurred. I happened to be present at the
first gas attack and saw the whole gas business from the begin-
ning. The first attack was made in April 191 5. A deserter had
come into the Ypres salient a week before the attack was made,
and had told us the whole story. They were preparing to poison
us with gas, and had cylinders installed in their trenches. No one
believed him at all, and no notice was taken of it.
1 Report of a lecture delivered before the Washington Academy of
Science* on January 17, 1918. Reprinted from the Journal of Iht Waih-
intlon Academy of Sciincts, 8, No. 3, February 4, 1918.
Then came the first gas attack, and the whole course of the
war changed. That first attack, of course, was made against
men who were entirely unprepared — absolutely unprotected.
You have read quite as much about the actual attack and the
battle as I could tell you, but the accounts are still remarkably
meager. The fellows who could have told most about it didn't
come back. The Germans have claimed that we had 6ooo killed
and as many taken prisoners. They left a battlefield such as
had never been seen before in warfare, ancient or modern, and
one that has no compeer in the whole war except on the Russian
front.
What the Germans expected to accomplish by it I am not sure.
Presumably they intended to win the war, and they might con-
ceivably have won it then and there if they had foreseen the
tremendous efTect of the attack. It is certain that they expected
no immediate retaliation, as they had provided no protection for
their own men. They made a clear and unobstructed gap in
tin lines, which was only closed by the Canadians, who rallied
on the left and advanced, in part through tin: gas cloud itself
The method first used by the German . and retained ever
since, is fairly simple, but requires great preparation beforehand.
A hole is dug in the bottom of the trench close underneath the
parapet, and a gas cylinder is buried in the hole It is an ordi-
nary cylinder, like that used for oxygen or hydrogen. It is then
covered first with a quilt of moss, containing potassium car-
298
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 4
bonate solution, and then with sand bags. When the attack is
to be made the sand bags and protecting cover are taken off the
cylinder, and each cylinder is connected with a lead pipe which is
bent over the top of the parapet. A sand bag is laid on the
nozzle to prevent the back "kick" of the outrushing gas from
throwing the pipe back into the trench. Our own methods are
practically identical with those first used by the Germans.
The success of a cloud gas attack depends on thorough prepara-
tion beforehand. The attackers must know the country, the
layout of the trenches, and the direction and velocity of the wind
with certainty. Favorable conditions are limited practically to
wind velocities between 12 and 4 miles an hour. A wind of
more than 12 miles an hour disperses the gas cloud very' rapidly.
An upward current of air is the worst foe of gas. The weight
of the gas is not an important factor in carrying it along, for it
mixes rapidly with air to form the moving "cloud." The time
occupied by a gas attack is too short to permit of much diffusion
of the gas out of the original mixture.
The gas attack must be planned very carefully. If the trench
line is very irregular it is likely that the gas will flow into a portion
of one's own trenches. The limits of safety in wind direction
are thus determined by the direction of the lines of the trenches.
The Germans use a 400 angle of safety; that means that on a
given straight portion of the front the wind direction must lie
between the two directions which make angles of 40 ° with the
neighboring sections of the front. The most suitable type of
country is where the ground slopes gently away from where the
gas is being discharged. The Germans made one mistake in
believing that hilly or wooded country would not do. This
was refuted by the French, who made a successful gas attack
in hilly and wooded country in the Vosges, as admitted in a
captured German report. If the country is flat like that about
Ypres, and the wind direction is right, there is very little diffi-
culty about making an attack, especially if the enemy does not
know anything about it. The element of surprise is important.
German gas attacks are made by two Regiments of Pioneers,
with highly technical officers, including engineers, meteorolo-
gists, and chemists. They brought their first cylinders into the
line without our knowing anything about it, except from the
deserter's report which was not believed The element of sur-
prise was greatly lessened when we began to know what to look
for and to recognize the sounds incident to the preparation of a
fas attack.
The first attack was made with chlorine. If a gas attack is
to be made with gas clouds, the number of gases available is
limited. The gas must be easily compressible, easily made in
large quantities, and should be considerably heavier than air.
If to this is added the necessity of its being very toxic and of
low chemical reactivity, the choice is practically reduced to two
gases: chlorine and phosgene. Chlorine is to gas warfare
what nitric acid is to high explosives. Pure chlorine did not
satisfy quite all the requirements, as it is very active chemically
and therefore easily absorbed. Many men in the first attack
who had sufficient presence of mind saved themselves by burying
their faces in the earth, or by stuffing their mufflers in their
mouths and wrapping them around their faces.
There were several gas attacks of almost exactly the same
kind early in 1915. There was no gas between the end of May
1915 and December 1915, and by that time adequate protec-
tion had been provided.
The first protection was primitive. It consisted largely of
respirators made by women in England in response to an appeal
by Kitchener. They were pads of cotton wool wrapped in
muslin and soaked in solutions of sodium carbonate and thio-
sulfate; sometimes they were soaked only in water. A new
type appeared almost every' week. One simple type consisted
of a pad of cotton waste wrapped up in muslin together with a
separate wad of cotton waste. These were kept in boxes in the
trenches, and on the word "gas" six or eight men would make
a dive for the box, stuff some waste into their mouths, then
fasten on the pad and stuff the waste into the space around the
nose and mouth. But this got unpopular after a bit, when it
was discovered that the same bits of waste were not always used
by the same men. During the early part of 191 5 this was the
only protection used.
Then came the helmet made of a flannel bag soaked in thic-
sulfate and carbonate, with a mica window in it. A modified
form of this device with different chemicals is still used in the
British army as a reserve protection. It is put over the head
and tucked into the jacket, and is fool-proof as long as well
tucked down. This stood up very well against chlorine.
In 1915 we got word from our Intelligence Department of a
striking kind. It consisted of notes of some very secret lectures
given in Germany to a number of the senior officers. These
lectures detailed materials to be used, and one of them was
phosgene, a gas which is very insidious and difficult to protect
against. We had to hurry up to find protection against it.
The outcome was a helmet saturated with sodium phenate. The
concentration of gases when used in a cloud is small, and 1 to
1000 by volume is relatively very strong. The helmet easily
gave protection against phosgene at a normal concentration of
1 part in 10,000. That helmet was used when the next attack
came in Flanders, on the 19th of December. This attack was
in many ways an entirely new departure and marked a new era
in gas warfare.
There are three things that really matter in gas warfare, and
these were all emphasized in the attack of December. They
are: (1) increased concentration; (2) surprise in tactics; (3) the
use of unexpected new materials.
Continued efforts have been made on both sides to increase
the concentration. The first gas attack, in April 1915, lasted
about one and a half hours. The attack in May lasted three
hours. The attack in December was over in thirty minutes.
Thus, assuming the number of cylinders to be the same (one
cylinder for every meter of front in which they were operating),
the last attack realized just three times the concentration of
the first, and six times the concentration obtained in May.
Other cloud gas attacks followed, and the time was steadily
reduced; the last attacks gave only ten to fifteen minutes for
each discharge. We believe that the cylinders are now put in
at the rate of three for every two meters of front, and may even
be double banked.
The element of surprise came in an attack by night. The
meteorological conditions are much better at night than during
the day. The best two hours out of the twenty-four, when
steady and downward currents exist, are the hour between
sunset and dark and the hour between dawn and sunrise. Gas
attacks have therefore been frequently made just in the gloam-
ing or early morning, between lights. This took away one of
the easy methods of spotting gas, that of seeing it, and we had
to depend upon the hissing noises made by the escaping gas, and
upon the sense of smell.
Another element of surprise was the sending out of more
than one cloud in an attack. After the first cloud the men
would think it was all over, but ten minutes or half an hour
later there would come another cloud on exactly the same front.
These tactics were very successful in at least one case, namely,
the attack near Hulluch in 1916. Some of the troops discarded
their helmets after the first wave and were caught on the second,
which was very much stronger than the first.
Efforts were also made to effect surprise by silencing the gas.
But silencers reduced the rate of escape so greatly that the
loss of efficiency from low concentration more than made up for
the gain in suddenness Another method was to mix the gas
up with smoke, or to alternate gas and smoke, so that it would
be difficult to tell where the gas began and the smoke ended.
Apr., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
299
The last attack made on the British by this means was in
August 1 916. Since that time the Germans have used gas
three times on the West Front against the French, and have also
used it against the Italians and the Russians. It has been
practically given up against the British, although the method is
by no means dead.
The last attack was a slight set-back in the progress of gas
defense. The casualties had been brought down to a minimum,
and, as shown by the fact that the percentage of deaths was
high, protection was complete in all cases where used, casualties
being due to unpreparedness in some form. The attack in
question was brought on under difficult conditions for the de-
fenders, as it was made on new troops during a relief when twice
as many men were in the trenches as normally. Furthermore,
they had to wear helmets while carrying their complete outfit
for the relief. This was the second time the Germans caught us
in a relief, whether through information or luck we cannot say.
The protection that had been devised against phosgene proved
effective at the time, but provision was made to meet increased
concentration of phosgene. We never had any actual evidence
during the attack that phosgene was being used, as no samples
were actually taken from the cloud, but cylinders of phosgene
were captured later. Glass vacuum tubes, about 10 by 30 cm.,
with a tip that could be broken off and then closed by a plasti-
cine-lined glass cap, were distributed, but the only one that
came back was an unopened tube found in a hedge, and marked
by the finder "Dangerous; may contain cholera germs." In
a gas attack everybody keeps quiet or else has a job on hand,
and conditions are not conducive to the taking of gas samples.
The original types of vacuum tube were smaller than those now
used.
There was a long search for materials that would absorb
phosgene, as there are few substances that react readily with it.
The successful suggestion came from Russia. The substance
now used very extensively by all is hexamethylenetetramine
(urotropine), (CH2)6N<, which reacts very rapidly with phosgene.
Used in conjunction with sodium phenate, it will protect against
phosgene at a concentration of 1 : 1000 for a considerable period.
An excess of sodium hydroxide is used with the sodium phenate,
and a valve is provided in the helmet for the escape of exhaled
air. The valve was originally devised so that the hydroxide
would not be too rapidly carbonated, but it was found in addi-
tion that there is a great difference in ease of breathing and
comfort if a valve is placed in the mask. The helmet is put
on over the head, grasped with left hand around the neck and
tucked into the jacket. This form is still used in reserve.
By this, time gas shells were beginning to be used in large num-
bers, and it became evident that protection by a fabric could not
be depended on with certainty. The box type of respirator was
the next development. Respirators have to fulfil two require-
ments which are quite opposed to one another. In the first place
they should be sufficiently large and elaborate to give full pro-
tection against any concentration of any gas, whereas military
exigency requires that they be light and comfortable. It is
necessary to strike a balance between these two. Upon a proper
balance depends the usefulness of the respirator. Oxygen ap-
paratus will not do on account of its weight and its limited life.
Two hours' life is excessive for that type. The side that can first
force the other to use oxygen respirators for protection has
probably won the war.
The concentrations of gas usually met with are really very
low. As has been said, a high concentration for a gas cloud is
1 part in 1000, whereas concentrations of 2 or 3 per cent can be
met by respirators depending on chemical reactivity. One such
respirator is a box of chemicals connected by a flexible tube with
a face-piece fitting around the contours of the face, and provided
with a mouthpiece and nosepiece.
As regards the chemicals used there is no secret, for the Ger-
mans have many of the same things. Active absorbent char-
coal is one of the main reliances, and is another suggestion that
we owe to the Russians. Wood charcoal was used in one of
their devices and was effective, but most of the Russian soldiers
had no protection at all.
We wanted to protect against chlorine, acids and acid -forming
gases, phosgene, etc., and at one time were fearful of meeting
large quantities of hydrocyanic (prussic) acid (HCN). At one
period every prisoner taken talked about the use of prussic acid,
saying that the Kaiser had decided to end the war and had given
permission to use prussic acid. Protection was evidently needed
against it. The three things that then seemed most important
were: (1) chlorine and phosgene; (2) prussic acid; (3) Iachrymators.
Charcoal and alkaline permanganate will protect against nearly
everything used, even up to concentrations of 10 per cent for
short periods.
The German apparatus, developed about the same time, is of
different pattern, and is still employed. It consists of a small
drum, attached directly to the front of the face-piece, and
weighs less than the British respirator but must be changed more
frequently. It has no mouthpiece. The chemicals are in three
layers: first, an inside layer of pumice with hexamethylene-
tetramine; in the middle, a layer of charcoal (sometimes blood
charcoal); and outside, baked earth soaked in potassium car-
bonate solution and coated with fine powdered charcoal.
As regards the future of the gas cloud, it may be looked upon
as almost finished. There are so many conditions that have to
be fulfilled in connection with it that its use is limited. It is
very unlikely that the enemy will be able to spring another com-
plete surprise with a gas cloud.
The case is different with gas shells. The gas shells are the
most important of all methods of using gas on the Western
Front, and are still in course of development. The enemy
started using them soon after the first cloud attack. He began
with the celebrated "tear" shells. A concentration of one part
in a million of some of these Iachrymators makes the eyes water
severely. The original tear shells contained almost pure xylyl
bromide or benzyl bromide, made by brominating the higher
fractions of coal-tar distillates.
The German did his bromination rather badly. As you know,
it should be done very carefully or much dibromide is produced,
which is solid and inactive. Some of the shells contained as
much as 20 per cent dibromide, enough to make the liquid pasty
and inactive. The shells used contain a lead lining, and have a
partition across the shoulder, above which comes the T. N. T.
and the fuse. These shells had little effect on the British, but
one attack on the French, accompanied by a very heavy bombard-
ment with tear shells, put them out badly. The eyes of the men
were affected, and many of the men were even anesthetized by
the gas, and were taken prisoner.
Our first big experience was an attack at Vermelles. The
Germans put down a heavy barrage of these shells and made an
infantry attack. The concentration was great, the gas went
through the helmets, and the men even vomited inside their
helmets. But it is difficult to put down a gas barrage, and there
is danger that it will not be a technical success. In the instance
cited certain roads were not cut off sufficiently, so that reinforce-
ments got up. This attack, however, opened our eyes to the
fact that, as in the case of gas clouds, concentration would be
developed so as to make it high enough to produce the required
effect under any circumstances.
When the Germans started using highly poisonous shells,
which was at the Somme in 1916, they did not attend to this
sufficiently, although enormous numbers of shell were used.
The substance used was trichloromethyl-chloroformate, but not
in great strength. It had no decided reaction on the eyes, hence
the men were often caught.
300
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 4
The quantity of gas that can be sent over in shells is small.
The average weight in a shell is not more than 6 pounds, where-
as the German gas cylinders contain 40 pounds of gas. To put
over the- same amount of gas as with gas clouds, say in five
minutes per thousand yards of front, would recjuire a prohibitive
number of guns and shells. It becomes necessary to put the
shells on definite targets, and this, fortunately, the Germans did
not realize at the Somme, although they have found it out since.
The use of gas out of a projectile has a number of advantages
over its use in a gas cloud. First, it is not so dependent on the
wind. Again, the gunners have their ordinary job of shelling,
and there is no such elaborate and unwelcome organization to
put into the front trenches as is necessary for the cloud. Third,
the targets are picked with all the accuracy of artillery fire.
Fourth, the gas shells succeed with targets that are not accessible
to high explosives or to gas clouds. Take, for instance, a field
howitzer dug into a pit with a certain amount of overhead cover
for the men, who come in from behind the gun. The men are
safe from splinters, and only a direct hit will put the gun out
of action. But the gas will go in where the shell would not.
It is certain to gas some of the men inside the emplacement.
The crew of the gun must go on firing with gas masks on, and
with depleted numbers. Thus it nearly puts the gun out of
commission, reducing the number of shots say from two rounds
a minute to a round in two minutes, and may even silence it
entirely. Another example is a position on a hillside with
dugouts at the back, just over the crest, or with a sunken road
behind the slope. Almost absolute protection is afforded by
the dugouts. The French tried three times to take such a posi-
tion after preparation with high explosives, and each assault
failed. Then they tried gas shells, and succeeded. The gas
flows rapidly into such a dugout, especially if it has two or more
doors.
Among the effective materials used by the Germans for gas
shells were mono- and trichloromethyl-chloroformate. Prussic
acid never appeared; the Germans rate it lower than phosgene
in toxicity, and the reports concerning it were obviously meant
merely to produce fear and distract the provisions for protection.
During the last five months the actual materials and the
tactics used by the Germans have undergone a complete change.
The lachrymator shells are less depended upon than formerly
for "neutralization," but are still a source of annoyance. Mere
annoyance, however, may be an effective method of neutralizing
infantry. For instance, where large amounts of supplies and
ammunition are being brought up there are always cross-roads
where there is confusion and interference of traffic. A few gas
shells placed there make every man put on his mask, and if it is
a dark night and the roads are muddy the resulting confusion
can be only faintly imagined. It may thus be possible to neu-
tralize a part of the infantry by cutting down their supplies and
ammunition
The use of a gas shell to force a man to put on his mask is
practicalh neutral] ation. If at the same time you can hurt
him, so much the better. Hence the change in gas-shell tactics,
which consists in replacing the purely lachrymatory substance
l>\ "iii ili it is also poisonous.
One substance used foi this method of simultaneously harrass-
ing and seriously injuring was dichloro-diethylsulfide (mustard
gas). Its use was begun in July of last year at Vpres, and it
was largelj used again at Nieuport ami Armentieres \ heavy
bombardment of mustard gas shells of all calibers was put on
these towns, as many as 50,000 shells being Bred in one night,
The effects of mustard gas ire those of a "supei lachrymator."
It has a distinctive smell, rathei like garlic than mustard It
has no immediate effect on the eyes, beyond a slight irritation,
After several hours tin - swell and inflame and prac
tieally blister, causing intense pain, the nose discharges freely,
and severe coughing and even vomiting ensue. Direct contact
with the spray causes severe blistering of the skin, and the
concentrated vapor penetrates through the clothing. The
respirators of course do not protect against this blistering.
The cases that went to the hospitals, however, were generally
eye or lung cases, and blistering alone took back very few men.
Many casualties were caused by the habit that some of the men
had fallen into of letting the upper part of the mask hang down
so as not to interfere with seeing. The Germans scored heavily
in the use of this gas at first. It was another example of the
element of surprise in using a new substance that produces new
and unusual symptoms in the victims.
Up to the present time there has been no material brought
out or either side that can be depended on to go through the
other fellow's respirator. The casualties are due to surprise
or to lack of training in the use of masks. The mask must be
put on and adjusted within six seconds, which requires a con-
siderable amount of preliminary training, if it is to be done
under field conditions.
Among other surprises on the part of the Germans were
phenylcarbylamine chloride, a lachrymator, and diphenyl-
chloroarsine, or "sneezing gas." The latter is mixed in with
high explosive shells or with other gas shells, or with shrapnel.
It was intended to make a man sneeze so badly that when he
puts on his mask he is not able to keep it on. The sneezing
gas has, however, not been a very great success.
All bombardments now are of this mixed character. The
shells used are marked with differently colored crosses, and defi-
nite programs are laid down for the use of the artillerymen.
As regards the future of gas shells, it should be emphasized
that the "gas shell" is not necessarily a gas shell at all, but a
liquid or solid shell, and it opens up the whole sphere of organic
chemistry to be drawn upon for materials. The material placed
inside the shell is transformed into vapor or fine droplets by
the explosion and a proper adjustment between the bursting
charge and the poisonous substance is necessary. Both sides
are busy trying to find something that the others have not used,
and both are trying to find a "colorless, odorless, and invisible"
gas that is highly poisonous. It is within the realm of possibili-
ties that the war will be finished, literally, in the chemical labora-
tory.
The Germans have not altered their type of respirator for
some time, and it is not now equal in efficiency to the British or
American respirator. The German respirator, even in its latest
form, will break down at a concentration of 0.3 per cent of
certain substances. The German design has given more weight
to military exigency, as against perfect protection, than has the
British. Another tiling that weighs against changes in design
is the fact that the German, already handicapped by the lack
of certain materials, must manufacture 40,000,000 respirators a
year in order to supply his Austrian. Bulgarian, and Turkish
allies, as well as his own army.
In the British and American armies the respirator must
always be carried with the equipment when within 12 miles of
the front. Between 12 and 5 miles a man may remove the
respirator box in order to sleep, but within 5 miles he must wear
it constantly. Within 2 miles it must be wont constantly in
the "alert" position (slung and tied in front). When the alarm
is given he must get the respirator on within six seconds. The
American respirator is identical with the British. The French
have a fabric mask made in several layers, the inner provided
with a nickel salt to stop HCN, then a layer with In -x.imethylene-
tcti amine: it has no valve and is hot to wear. The French also
use a box respirator, consisting of a metal box slung on the back,
with a tube connecting tn the face mask; the latter is of good
Para rubber and is provided with a valve. One disadvantage
of this form is the danger of tearing the single rubber sheet. The
German mask now contains no rubber except one washer; the
elastics consist of springs inside a fabric, and the mask itself
Apr.. 19 1 8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
301
is of leather. It hardens and cracks after being wet, and is too
dependent upon being well fitted to the face when made.
(The lecturer exhibited various types of gas shells, helmets,
masks, and respirators.)
The following compounds have been used by the Germans in
gas clouds or in shells:
1— Allyl-iso-thiocyanate (allyl mustard oil), C1H1NCS (shell).
2 — Benzyl bromide, CeHsCHjBr (shell).
3 — Bromo-acetone, CH-Br.CO.CHj (hand grenades).
4 — Bromated methyl-ethyl-ketone (bromo-ketone) , CHjBr.CO.CjHs
or CHj.CO.CHBr.CHj (sheU). Dibromo-ketone, CHj.CO.CHBr.CH!Br
(sheU) .
5 — Bromine, Br2 (hand grenades).
6 — Chloro-acetone. CHjCl.CO.CH3 (hand grenades).
7— Chlorine, Ck (cloud).
8— Chloromethyl-chloroformate (palite), CICOOCHjCl (sheU).
9 — Nitro-trichloro-methane (chloropicrin or nitroehloroform), CCla-
NO2 (shell).
10 — Chlorosulfonic acid, SOj.H.Cl (hand grenades and "smoke pots").
1 1— Dichloro-diethylsulfide (mustard gas). (CHzClCHihS (shell).
12 — Dimethyl sulfate, (CHslaSO. (hand grenades).
13— Diphenyl-chloro-arsine, (C.Hj)iAsCI (shell).
14 — Dichloromethyl ether, (CH;C1).0 (shell).
15 — Methyl-chlorosulfonate, CHsClSOj (hand grenades).
16— Phenyl-carbylamine chloride. CsHsNCCl; (shell).
1 7 — Phosgene (carbonyl chloride), COCb (cloud and shell).
18 — Sulfur trioxide, SOs (hand grenades and shell 1.
19 — Trichloromethyl-chloroformate (diphosgene, superpalite), Cl-
COOCCb (shell).
20— Xylyl bromide (tolyl bromide), CHjCsHjCHiBr (shell).
THE CONSUMPTION AND COST OF ECONOMIC
POISONS IN CALIFORNIA IN 1916'
By George P. Gray
Intimately associated with the production and storage of both
animal and vegetable foods is the problem of the control of
insects, plant diseases, and rodents, the importance of which is
scarcely realized except by those directly concerned. A recent
proclamation of the President, however, has given the matter
definite recognition by placing the distribution of arsenical
insecticides under authority of the Food Administrator. The
quantity and kinds of chemicals used in this way as well as in the
control of flies, mosquitoes, etc., in the interest of the public
health, is of especial interest at the present time to an audience
of chemists.
In view of the prevailing high prices of all economic poisons2
and the acute shortage of others, it seemed of the highest im-
portance to know as fully as possible the normal consumption in
California and to make an estimate of probable increased de-
mands in the future. Steps were therefore taken to collect
statistics on consumption, and to ascertain, if possible, whether
or not serious shortage of important materials were to be
anticipated, and whether conditions could be relieved by the
substitution of cheaper materials for more expensive. It also
appeared that if the facts were known concerning the normal
consumption, the prospective producer of raw materials would
have valuable information concerning the advisability of de-
veloping new sources of supply.
In the collection of statistics the writer is indebted to Mr.
G. H. Hecke, State Commissioner of Horticulture. Through his
office, reports were received from 28 county horticultural com-
missioners, representing 71.67 per cent of the total acreage of
fruits in the state, exclusive of grapes. These reports have been
compiled and are shown in Table I. It seems reasonable to
1 Address before the California Section of the American Chemical
Society, San Francisco, January 12, 1918.
' The term "economic poisons" was suggested by the writer's associate,
Mr. M. K. Miller, as being appropriate in referring to the diversified and
yet closely related group of materials used for the control of weeds, in-
sects, fungi, and rodents. The qualifying word "economic" serves to
distinguish between poisons which are made to serve useful purposes in the
control of pests, and the more popular conception of poisons as being harm-
ful to man, and often used with criminal intent. Science. N. S., 44. >To.
1185. 264.
assume that the consumption of economic poisons is roughly
proportional to the acreage of fruits. The figures shown in the
last column of Table I are estimated on that basis.
While it is known that there are inaccuracies in the reports
submitted, it is believed that the information received from them
is of sufficient value to warrant its publication. It will be
noticed that many of the materials listed have important uses
other than as economic poisons, but so far as possible the amounts
represent only that consumed in the control of pests. The
commissioners went to unusual pains in segregating the amounts
used in that way.
In order that these data may be more intelligible to producers
of raw materials, some of the more important items have been
reduced to tons of raw materials required for their production,
or of the better-known commodities which are quoted in the
New York market, and are given in Table II.
COMMENTS
Extended comment will not be made at this time on the
situation as a whole, but only such observations as seem justified
by the information at hand.
arsEnicals — It is interesting to note that of the 6000 odd tons
of white arsenic normally consumed in the United States, about
one-sixtieth was used in California alone in the control of in-
sects. Aside from the use of arsenic in the control of insects,
some little interest is now being taken in the possible utility- of
arsenicals in the control of weeds. During the past year there
were used in California about three tons of white arsenic in
weed control experiments.
The unusual fluctuation in the price of arsenic during the
period of the war has caused no little apprehension concerning the
adequacy of the supply of this material. The New York price
of white arsenic at one time was five hundred per cent above
normal. In January 19 18 it was still quoted four hundred per
cent above normal. The reason commonly assigned for the high
prices of arsenic is that the importations, which usually amount
to about 3000 tons annually, have been stopped, thus depleting
the stocks on hand and severely taxing the output of domestic
producers, which is normally about equal to the imports. It
is believed, however, that many times more than the normal
consumption of arsenic in the United States can be produced
as a by-product from smelter smoke and that the high price of
arsenic is artificial. It is sincerely to be hoped that the govern-
ment control will relieve the situation in respect to this very
important economic poison.
copper sulfate — The price of this raw material for the
preparation of copper fungicides was for a short time nearly four
times normal, but during the past year, it has been slightly less
than double. The great demand for copper during the war will
hold the price high, although not as high as many other chemicals.
Much of it is a by-product in the production of other materials
and uses up copper which is not salable in other forms. Sulfur
fungicides have been substituted for copper compounds to a
large extent, where possible.
sulfur — Sulfur prices held practically normal until after
declaration of war by tin United States, but are now about one
hundred per cent above normal. Reliable information indicates
that this country may face an actual shortage of sulfur.
Enormous quantities of pyrites are used in the manufacture of
sulfuric acid, much of this being imported from Spain. Im-
portations have now ceased, so that the sulfuric acid plants are
obliged to use sulfur or obtain local pyrites. The American
producers of sulfur are developing new deposits and it is re-
ported that promising deposits of pyrites are being investigated
by the Government so that production may meet consumption.
SODIUM CYANIDE A shortage of sodium cyanide for Fumigating
citrus trees, and Other purposes, occurred during the fumigating
302 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. 4
Table I— Consumption and Cost op Economic Poisons in California in 1916
Average price Cost in 28 Totals in 28 Estimated totals
Consumption in 28 to consumer counties reporting counties reporting for entire state
Material counties reporting Dollars Dollars Dollars Dollars
While Arsenic 14,686 lbs. 0.183 2,688
Paris Green 13 616 lbs. 0.435 5,923
LeS^nate.Pas'te: ::..: 6"'^8{bs. 0.110 69,677
Lead Arsenate. Dry 'S?1?^^ rHoO 9 772
7inc Arsenite 32,575 lbs. 0.300 V, //^
Z,in^ Arserau. 110:575 154 784
Copper Sulfate. .".... .'.' .' . .' .' ' ' .' .'.".'"" 729,' 850 lbs. 0. 142 103,639
Bordeaux Pastes 103,754 bs. 0.24 12,865
Bordeaux Powders 37,6251bs. 0.12* 4,515 &
Copper Compounds
iScES*16 : I:JB:3SiK: S:S?f ^lU
SulfuncAcid . . 664,553 927,240
Cyanide and Acid
s„lf,.r 4,514,103 lbs. 0.037 167,022
Sxim^u^:::::::::::: «£»«* g.gg .? ,
£&^S&::::::::::::::::: i*:«.i*.
Sulfur and Compounds
lT-roiene .... 58,448 gals. 0.106 6,254
SwrA*:::::::::::::::::.::::: ili'SAH8- Swi lo'iio
Crude Petroleum 254'6™gaS- °>'?nA »'?»
Coml. Emulsions 286, 400 gas. 0.106 30,358
MiscibleOUs f?'2??BaS- ?'200 3964
Coal tar "DiDs" 11,637 gals. 1.200 IJ.VOI
Coal-tar Dips «. 81,020 113,046
Oils and Emulsions
Fish-Oil Soap, Hard 22o'2io£9- n067 3'998
Fish-Oil Soap! Liquid 5?'5nn'b^ o'SoO 1*480
&„5S2,fiOT :::::::::::::::: eoS: SSKlr S:S28 ii:S?5
boap rowoers 29,081 40,576
Soaps and Lmulsipiers •■
gSSBars-^::::::::::::::::::: S:Sfc
Limb and Caustics ••'* " '
« . ss 17S lbs 0.036 1,986
Tobacco Leaves 2„,i;,iJ!:* i rm 62 211
Tnhar™ Kitrarts 60,224 lbs. 1.033 o-,^il
Tobacco Extracts 64,197 89,573
Tobacco and Extracts ' ' .. ,n ->c m-r
. ■ I6 979nzs 1.102 18,711 18, /ll 26,107
Strychnine 9 065 gals 2 091 18 955 18,955 26,448
Formaldehyde 56 741 gal 1603 90 956 90,956 126,909
Carbon Bisulfide 5^ 724 fbs 0 971 6 400 6,400 8,930
Pyrethrum 103 lbs' 0.220 23 23 32
Quassia ififi h!' 0 404 269 269 375
Hellebore «6bs. 0 404
Iron Sulfate. ... 19M bs' 1824 3 559 3,559 4,966
Corrosive Sublimate 1 , « i ids.
1,635,437 2,281,899
Cost of Standard Remedies 133,856 186,767
Cost of Proprietary Preparations *
„ $1,769,293 $2,468,666
Total
season of .9.6. There was an ample supply during the past give an estimate of any probable increase or decrease in the
season owing to the output of new plants which started opera- demand for economic poisons in the future. Not enough of the
commissioners, however, were willing to venture an estimate
^Ta'rbon BISULFIDE-Carbon bisulfide is rather a novelty in the for one to foresee the future in this respect. The agriculturist
chemical line, as its price has been scarcely affected by the war. has so many problems starmg him in the face for solution-
It was quoted in New York at 6>A cents in January 1914 and at labor, high price of suppl.es, marketing, etc.-that he. himself
7»A cents in January 1918, this being scarcely more than the is scarcely able to predict whether or not his efforts at pest control
normal fluctuation. This fact is especially gratifying in view will have to be relaxed, as we go deeper and deeper mto the war.
of the fact that this is the most important fumigant for use in the or whether this vital factor in the production of most foodstuffs
control of insects infesting stored grain, beans, and many other can be given even greater attention than in the past,
products It is also the most approved material for the winter It is quite certain that the consumption of rodent poisons,
control of ground squirrels. strychnine, saccharine, and carbon bisulfide, will be enormously
increased in California during 101S. In the interest of the
Table II — Raw Materials Required for the Preparath >n op Some of ......... .. ... • ,. ,
the More Important Economic Poisons Consumed in Cal.pornia public health and in the conservation of the agricultural resources
Durinc the year 1916 of the state, all federal, state, and county organizations con-
White Arsenic '05 tons cerned are making a united and special effort in a state-wide
nine Vitriol 358 tons . . .
Litharge '87 «°ns campaign against the ground squirrel.
Zinc :■•■■•■ 'j [™ It seems quite unlikely that the consumption of the other
Sodium Cyanide l ,479 tons economic poisons will be less in the future than in the past. In
Sulfur10. .Acld.(.55°. Ba,"nC) '.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'. 4*988 tons fact, there are many reasons for anticipating a greater demand:
Crude Petroieum and Distillates 9,S'2S! the coming into bearing of new acreages of fruit; more extensive
Coal-tor Creosote 12, 000 gals. e. .... r , ...
Soaps (chiefly fish-oil and soap powders).... 7<7 tons inter-cropping; higher prices for farm products, especially,
Cr wheat, beans, etc., which heretofore had been so low as to dis-
rodent poisons — Strychnine is now selling about two hundred courage, in a large measure, the control of pests. Contra!
per cent above normal. Saccharine, used as a "camouflage" in measures will now in many cases be profitable which ordinarily
strychnine-coated barley to mask the intensely bitter taste of the are unprofitable. Let us hope that the prices of the economic
strychnine, is now being quoted at over !\v> per lb. and at times poisons will not be artificially inflated, and that the agriculturist
is very difficult to obtain at any price. Some other equally wni not be unduly exploited by the "profiteer."
effective, but cheaper "camouflage" is much needed for use in lNSECTIClnB AND ftjnoic.de Laboratory
preparing squirrel and gopher poisons. Agricultural Experiment Station
INCREASED CONSUMPTION — The commissioners were asked to University op California, Berkeley
Apr., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
3°3
THE DEBT OF PREVENTIVE MEDICINE TO
CHEMISTRY'
By George W. Goler
In attempting to discuss this subject, I feel very much in the
position of the college president who, when addressing his students
on the difficulty of acquiring knowledge and the ease of forgetting
facts, said, "I once studied chemistry and I perhaps had a fair
student's knowledge of that useful branch of science, but while
my course in chemistry enabled me better to understand some of
the commoner things in the world about me, the only chemical
fact that I now recall is, that the chemical formula for water is
H02."
Chemistry has done so much for preventive medicine, that
just to indicate the debt that the latter science, preventive medi-
cine, owes to the former, chemistry, would take all the time you
ought to spare for the purpose, and the facts presented would be
more clearly and succinctly stated in various articles to be found
both in books of reference and in the technical journals. I have
therefore thought that it might be useful briefly to review the
part chemistry has played in the promotion of health and the
prevention of some of the commoner diseases. And when I
speak upon this subject, it is as one whose early acquaintance
with chemistry dates from the lectures of Chandler of New York,
more than 30 years ago, and a few years later those of Witthaus,
whose talks of two hours with five minutes intermission served,
with small laboratory training, to make of me all the chemist
that I am. So, with this training, permit me to tell you of part
of the debt which medicine owes to chemistry.
Out of the mystery which the Greek alchemists sought for in
the four elements and out of their failure to find the "philosopher's
stone" and to transmute the baser metals into gold, came the
rise of a new group of men, the iatro chemists, chief among them
the 15th century chemists, Basil Valentine, and his later proto-
type, Paracelsus, half charlatan, half scientist. These and their
followers, unfortunately, agreed that the true use of chemistry
is not to make gold but to prepare medicine. This step led men
insensibly away from the early teaching of the Greek physicians
concerning baths, diet, regimen, and all the things that really
obtain for the promotion of health and the prevention of disease.
The simple rules of the Greeks whereby, in pneumonia for in-
stance, they bathed and annointed the patient, washed out his
mouth and cared for his teeth, laid him on a soft bed under the
trees and prayed to the gods, were displaced by the unfortunate
teaching of Valentine, Paracelsus and others, who rather sought
for a mysterious something in chemistry that should cure disease.
We have, therefore, to thank the chemists for the drug instead of
the hygienic treatment of disease. Of course the chemists of
the iatro-chemical school, as they were called, failed in their
treatment; first, because no drug or drugs then known could
materially affect disease, and second, because the causes of dis-
ease were unknown. The early chemist, having failed in this
respect, even tried to devise methods of disinfection that he might
fight the foul smells of disease with a substance that smelled as
bad as or worse than some of the horrid diseases that prevailed
in the period we are considering.
But we owe so much to the chemist for what he has done, that
we ought not to blame him because his chemicals failed. The
doctor without the chemists has been responsible for quite as
many failures; for is it not the doctor who evolved the humoral
theory of disease for which the four humors, bile, black bile,
blood and phlegm gave rise to the bilious, sanguine, choleric and
melancholic temperaments? And these humors rose, clouded
the brain, became crossed in 80,000 different ways; and if you
wanted to prescribe for the patient, the only thing you had to
do, beside finding the remedy, was to find in which of the 80,000
■ humors were crossed. Of course, if the doctor didn't
'Address before the Rochester Section of the American I I I
Society, December 19, 1917.
find out, he either gave a small handful of calomel, or better still,
and much more dramatic, he bled the patient. Half a pint, a
pint or a quart was not an uncommon bleeding. And if he didn't
get enough blood out by opening a vein, he opened an artery.
And if the humor still persisted, he inserted a pump, that is, if
the patient still lived. Tradition and authority descended from
Valentine, Paracelsus and Galen are largely responsible for the
introduction of drug methods of treating disease.
While these are interesting examples of speculation and con-
jecture in medicine and chemistry, there was no less of guesswork
in much of the chemistry and medicine of even 50 years ago.
From the early workers in both branches of science, we have the
development of the miasmatic theory of disease, formulated by
Pettinkofer, who was the first real health officer of Berlin 50
years ago. While Pettinkofer is to be credited with much good
chemical work, it was he who devised the theory that ground
water and ground air were the causes of such disorders as typhoid
fever. He and his workers did much to keep alive the sewer gas
theory in its relation to infections, and it was his work which
probably prevented the earlier recognition of malaria as a mos-
quito-borne disease and not a malaria, and typhoid as a water
and food rather than a sewer-gas-borne disease.
Now while the early laboratory workers were obsessed by the
teachings of the fathers of chemistry and medicine, there were
a few brave men of independent thought who applied themselves
to new and original methods of research in an endeavor to dis-
cover the elusive things of the air which they believed caused
disease. They, like Spallanzani (1776), successfully overthrew
the general accepted theory of spontaneous generation of micro-
organisms, by showing that if putrescible fluids were heated to a
sufficiently high temperature they remained unchanged for in-
definite periods. And, while discussing the manner in which air
was admitted to the flasks in which the fluids were kept, occupied
various chemical observers for years, it was not until three-
quarters of a century later that Schroeder (1854) showed that a
loose plug of cotton wool in the mouth of a flask containing boiled
putrescible fluid excluded the organisms of the air and prevented
fermentation in the fluid. But not all fluids kept in such pro-
tected flasks remained unfermented, for occasionally the contents
of such a flask would spoil. It was the genius of Pasteur that
explained the phenomena, as he made clear other similar, inex-
plicable things.
Pasteur, in 1865, showed that certain organisms and dormant
stages or spores that resisted one or more boilings, and that the
repeated application of heat was required to destroy these bodies
and prevent the fluids containing them from fermenting. Here,
by chemists, were two great contributions, not only to preventive
medicine but to all medicine and surgery, the cotton air-filter
and sterilization by heat.
The next great discovery by a chemist, probably the one great
discovery that has made it possible for medicine to make the
advances it has made in the last quarter of a century, was the
discovery of aniline by the German chemist Runge in 1854, and
five years later (185 9), the discovery of the first aniline dye, mauve,
by the English chemist, Perkin. Then in rapid succession came
a number of other aniline colors.
For many years all the scientific workers in cellular physiology
and pathology had sought new methods for bringing more clearly
into view the secrets believed to lie held within and around the
cell. For this purpose various chemicals and dyestuffs, both
those derived from logwood, iodine, cochineal and Other substances
have been used, but it was not until the coal tars yielded their
dyes that the m many bacterial cells wen- revealed.
Between 1850 and 1863, Davaine, a distinguished French
physician, had been working on the cause of anthrax, a virulent
and fatal disease of wool sorters. As eai
seen the anthrax organism, but it was not until 1863, 13 years later,
that he was able to prove the exact relationship betwei D
3° 4
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING ( HEMISTRY Vol. 10, No. 4
thnix bacillus and anthrax. Then, in 187.5, Obermeier discovered
in the blood of patients suffering from a relapsing fever an or-
ganism which proved to be the cause of the fever. Tin be two
■ 11 1 ■ . then laid the foundation for the germ theory of disease,
the first stone of which had been cut by that "skeptical chemist,"
Boyle, mon than 200 years before, when he said, "The problem
of infectious disease will be solved by him who discovers the
nature of putrefaction."
Then, in 1S77, came Weigert. who showed that many organisms
otherwise translucent might be stained by aniline dyes. So,
following closely upon the heels of the discovery of these dyes
by the chemists, came their application to the revelation of new
forms of bacteria by staining them
About this time Koch showed, by the use of solid culture media
and the plate method, a way of obtaining bacteria in pure cultures.
Still further advances in the domain of preventive medicine were
thus made possible and the demonstration of the bacterial cause
of infectious disease further extended. Thus, by methods of
staining and plate culture, and pure culture work, and the de-
velopment of other modes of bacterial research numerous dis-
coveries in preventive medicine were made possible, among them
the following:
Neisser in 1879 showed the gonococcus within the cells of
gonorrheal pus. In 1880 Kberth and Koch, and in 1884 Gaffky,
discovered the bacillus of typhoid fever, first by seeing them as
unstained organisms and later by viewing them as stained bodies
under the microscope. While in 1865 Villemin, and later Con-
heim in 1877, showed that tuberculosis might be transmitted to
healthy animals by the inoculation of tuberculous material, it
remained for Koch, in March 1882, to demonstrate by stained
specimens of the tubercle bacillus its presence in the sputum
and tissues of tuberculous animals and man. While the glanders
bacillus discovered by Loeffler and Stats (1882) and the spirillum
of Asiatic cholera discovered by Koch in 1884 were first viewed
without stains, their further study and the development of
methods of diagnosis and immunization were the results of the
combined methods of chemical and bacteriological research.
In 1884 Pasteur discovered the present known method of
treatment for rabies, a disease that had previously caused a
mortality of 100 per cent, and reduced the mortality to a fraction
of 1 per cent in those bitten by dogs known to be rabid.
Of world wide interest was and is the discovery of the bacillus
of diphtheria by Klcbsaud Loeffler in [884. From 1659, when in
New England there was first described an epidemic of diphtheria,
known as "bladders in the windpipe," diphtheria had exacted an
annual toll of thousands of deaths and hundreds of heart, kidney
and blood vessel diseases as its late, remote consequences. So
when Loeffler announced that by using staining methods he had
discovered the bacillus which is the cause of diphtheria, the
scientific world almost paused for breath, and then resumed its
labors with renewed hope for the conquest of this most dread
disease of childhood.
The writei remembers attending a reception at Washington,
given in the splendid Hall of The American Republics, to the
foreign and American delegates at the international Congress of
Hygiene and Demography in [912. In the receiving line, next
to the venerable Di Samuel P. Wolcott, stood the commanding
figure of Koch and next beyond him the slight, boyish Loeffler.
As I went down tin- receiving line accompanied by Dr. McKay
of Saskatoon. B ( . and shook the distinguished guests by the
hand. McKay, a highly patriotic Canadian, turned at the end
of the line and said, speaking oJ Loeffler, "I'd rather shaki hands
with him than with my Sovereign."
Shortly after Loeffler found the diphtheria bacillus, two
French investigators, Koux and Versin. discovered bj chemical
methods the diphtheria toxin. They and others having paved
the way, You Hchring in 1 So.; succeeded in preparing diphtheiia
antitoxin. Time does not permit me to relate what has been
accomplished in preventive medicine by the methods of I
for intubation, combined with the administration of diphtheria
antitoxin in laryngeal diphtheria. Suffice it to relate that in
our city of Rochester the deaths from diphtheria have fallen
from 189 per thousand in the year before diphtheria antitoxin
was introduced, to less than 9 per thousand in 1915. In 1884
Nicola, a German, and Kitasato. a Japanese, simultaneously
discovered the bacillus of tetanus or lockjaw. This disease had
been known since man began to record his observations in writing.
It accompanied wounds in war as noted by Larrey. Napoleon's
chief surgeon. It is to-day one of the most feared complications
of wounds, not only in the army and navy, but m civil life as well.
Its dangers have been very greatly diminished by the preparation
and introduction of tetanus antitoxin, both for immunization
and treatment. The bacillus of epidemic influenza was discov-
ered by Pfeiffer of Berlin in 1892, the bacillus of plague by Yersin
in 1893. By various complex physiochemical procedures, first
Neisser and later others, including Bordet and Gengou, succeeded
in showing that when an antigen, 1. <•., bacteria, blood cells and
body cells, meets in the body of a treated animal a receptor with
which it unites certain reactions are produced, known as fixation
of the complement. With this work as a basis of procedure , the
long search for ultramicroscopic or faintly staining organisms
was prosecuted with vigor. Then, too, the developing science of
serology, founded upon physiochemical reactions of great delicacy,
helped to advance the new work in preventive medicine. The
field of research in syphilis offered wide opportunity. In 1903
MetchnikofT and Koux demonstrated the inoculability of syphilis
from man to apes, and in 1905 Schaudin showed by biochemical
methods the presence in the sera of inoculated animals of a faintly-
staining spiral, the cause of syphilis, the spirochita palladia.
In 1906, Wasserman, applying the serum complement reaction
of Bordet-Gengou, discovered the test for syphilis known as the
Wasserman test. Four years later, in 191 1, Noguchi, a Japanese
at the Rockefeller Institute, succeeded in cultivating the spirillum
of syphilis in pure culture, demonstrating it both by staining
methods and by powerfully transmitted light; he also discovered
a valuable test the I.uetiu test for obscure cases of syphilis.
Almost simultaneously Erlich in Germany by a masterly series
of chemical experiments, using the work of Elenhuth, succeeded
in introducing arsenic within the benzol ring and gave to us a
compound, salvarsan or 606, for the treatment of syphilis.
Little more than a \ ear later Bordet and Gengou made another
remarkable discovery. While ten years before they had an-
nounced the discovery of the bacillus of whooping-cough, it was
not until 1912 that their work was confirmed by other observers.
To them we owe not only the discovery of the bacillus of whooping-
cough, but the ability to produce a vaccine for the successful
prevention of that most dangerous disease of childhood.
In this resume I must not neglect to mention the discovery of
the organism of epidemic cerebrospinal meningitis and the de-
velopment of a serum for its successful treatment; also the discov-
ery oi the organism of infantile paralysis: all done at the Rocke-
feller Institute by I'lexuer Nor must we forget that most re-
markable discovery of Henry Plot/, a young physician in Mt.
Sinai Hospital, of the bacillus of typhus Though much remains
to be accomplished by the combined methods of work of the
chemist and biologist, we ma} readilx see that much has already
been done The secrets of measles and scarlet fever and cancer
still n main secrets They are as hidden as the cause of the com-
mon cold.
The length of this paper forbids me to speak of many other
debts which medicine owes to chemistry, but 1 must refer to the
work of Can ell and I 'akin, who have devised methods for both
the prevention and the treatment of disease by disinfecting the
nose, nasopharynx and mouth so that those who are carriers of
such diseases as infectious meningitis may be rendered less dan-
gerous as contacts; and the same workers have succeeded in
Apr., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
3°5
perfecting a method which promises much for the antiseptic
treatment of deep, contused and dirty wounds.
Chemical methods are responsible for the clearing up of much
that is obscure in that class of diseases of the kidney usually
known as Bright's disease. In the treatment of that super-devil
of nutritional disturbances, diabetes, the chemistry of nutrition
has taught us practically all we know. To chemistry we are
indebted for chloroform, quinine, ether and cocaine, and for the
methods of water, milk and food analysis, and to the chemist
we largely owe the newer methods of sewage purification. For all
these we thank you, and we trust that the professions united
may labor still further for the betterment of the race.
Health Bureau
Rochester, New York
WILLIAM H. NICHOLS MLDAL AWARD
INTRODUCTORY ADDRESS
By Charles H. Herty
It is a striking fact that in the midst of feverish war prepara-
tions, while our minds are filled with death-dealing chemical
reactions, we are met together this evening to pay tribute to
a quiet worker in the university laboratory, who with infinite
patience and consummate skill has accomplished brilliant re-
sults in an extremely complex and difficult field of chemical
research, that dealing with the fundamental processes of life.
I take it as a healthy sign and one presaging great good to chem-
istry in America that in these days of intense application of
science to industrial processes the worker in pure chemistry has
been chosen as the recipient of the Nichols Medal.
Under the terms stipulated by its donor, Dr. William H. Nichols,
whom happily we have with us to-night in the capacity of leader
of the organized chemists of this country, this medal is awarded
annually by our Section to the author of the best original
article published during the preceding year in the journals of
the American Chemical Society. In reaching its decision the
Committee has construed broadly the conditions of award,
realizing fully that in certain lines of research results cannot be
withheld indefinitely in order to present in one contribution a
comprehensive report of an entire investigation. Such action
might lead to loss of priority, and would undoubtedly diminish
that stimulative effect which follows the publication of definite
chapters in the progress of investigation which in its very nature
must require years for completion. On the basis of such broader
interpretation of the terms of award, the Committee has this
year unanimously awarded the medal to Dr. Treat B. Johnson,
Professor of Organic Chemistry in the Sheffield Scientific School
of Yale University. During the past year Dr. Johnson con-
tributed four articles to the Journal of the American Chemical
Society. A fair measure of his activity can be gained from the
fact that these four constitute the continuation of a series of
one hundred and fifty-four contributions on which his name
has appeared as author.
Through this multitudinous array of original communica-
tions Dr. Johnson has shown his courage and ability in bring-
ing light into one of the darkest and yet most important fields
of chemistry. In reading the advanced copy of his address,
and noting the brilliant progress he has made through calling
the element sulfur to his aid, I am almost forced to describe his
activity as devilish. Beginning in 1898, the output of papers
from his laboratory has been continuous — two decades of ac-
complishment to which we all join in paying heartiest tribute.
While his name is almost intimately associated with the chemis-
try of pyrimidine compounds, he has included within the scope
of his fertile investigative spirit the subjects of the hydantoins.
furfurans, the thiocyanatcs, hippuric acid, the phthalimidcs,
acetamide, pyrrole compounds, thiopolypeptides, thioamides,
the higher phenols, the purines, sarcosine, divicine, vitiatine,
etc.
We are interested to-nigfat, however, not only in the scien-
tific achievements but in the personality of the man whom it
Is "in privilege to honor. Like so many other gnat Ameri-
cans, he was born "down on the farm," near Bethany, Conn.,
on March 29, 1875. In 1898 he graduated from the Sheffield
Scientific School with the degree of Ph.B., and three years later
received his doctorate from Yale University, having specialized
in organic chemistry. A laboratory assistant during his post-
graduate course, Dr. Johnson was in 1902 appointed instructor
in chemistry in the Sheffield Scientific School. In 1909 he was
promoted to an assistant professorship, and in 1914 was ad-
vanced to professor of organic chemistry.
In addition to his work as an investigator, his sterling traits
as a teacher have impressed themselves upon many of the
younger men now active in chemical work. Through his force
of character he has proved himself an excellent organizer and
executive. His interests have not been confined solely within
university walls. He has taken frequent opportunity to visit
chemical plants, and in many has cooperated with their staffs.
In one particular case his suggestions proved so valuable that
he was urged to leave university work at a decided increase in
salary, but declined.
Upon inquiry I learned that his principal recreation is work,
that between the writing of his papers he finds time to drive
his auto, which in itself sometimes means work, takes delight in
"canned" music, as any other human being would, and gets
constant inspiration and refreshment from trips back to the
farm. To those of us who have had the pleasure of associating
with him at the meetings of the American Chemical Society
it is needless to emphasize his genial temperament and charming
personality.
In this incomplete manner I have tried to picture to you
something of the personality and activities of Dr. Johnson,
and it now becomes my pleasant duty to present to you Dr.
William H. Nichols, president of the American Chemical
Society, who in his life has taken part in many presentations,
and who I am sure will sanction the statement that in no similar
occasion has he taken greater pleasure than in this.
New Yore City
PRESENTATION ADDRESS
By William H. Nichols
It is true, as the Chairman remarked, that I have taken part
in many presentations, but it is interesting to me that on such
occasions I have never acted as the recipient. My situation on
such occasions is best described by paraphrasing a familiar
expression and saying, "It is easier to give than to receive."
As to the Nichols Medal, I must say that this was in no wise
an original idea with 111c, but was suggested by a group of friends
interested in the New York Section of the American Chemical
Society. Fortunately I was able to dissuade them from carry-
ing out their original intention of placing my features upon
the medal, but they insisted on giving it its present name,
though I feel, and always have felt, that it should be called
the New York Section Medal.
Before presenting the medal to Dr. Johnson may I be par-
doned a few words concerning the work to which I have been
called by the members of the American Chemical Society?
This is the first time since my election to office as president that
I have had opportunity to meet witli any large group of its
members, and I desire to express here the feeling of astonish
ment at the great growth of this organization. When 1 think
3°6
THE JOURNAL OF INDUSTRIAL A SO ENGINEERING ( BEMISTRY Vol. 10, Xo. 4
of its earliest days, and of the association at that time with
my friend Dr. Charles F. Chandler, we two being the only sur-
viving charter members, it seems like a romance that its mem-
bership now should exceed 11,000; and I have been informed to-
night by the secretary of the New York Section that within
the past two years this Section, at that time the largest Section
of the Society, had increased in membership fifty per cent.
What a striking commentary is furnished by these figures on the
increased appreciation of chemistry in this country!
In looking around for the duties I might have to perform I
have been amazed at the remarkable piece of organization
machinery which my predecessors have constructed. So ad-
mirably has this work been done that there seems little left
for me to do. While I cannot hope to do much to better the
fine record they have al-
ready made, nevertheless
I pledge myself to every
effort to prevent any ret-
rogression.
As to the subject of the
evening, I must be frank
in saying that I know
nothing of pyrimidine
chemistry, but am expect-
ing to learn much from
Dr. Johnson's address to-
night. I have been
deeply interested, how-
ever, in the account of his
career, and in looking over
the list of his numerous
publications, that which
has impressed me most of
all has been the fact that
in the great majority of
his papers his name ap-
pears in joirt authorship
with those of his students.
This fact is a clear indi-
cation of his magnanimity,
of his willingness to share
high honor, to give every
credit to those associated
with him, and to encour-
age his younger co-
workers. I desire to con-
gratulate Professor John-
son on the fine influence
he is exerting through
this evident close and
congenial association
with the young men who
come under the influence
of this great teacher, and
it gives me the utmost pleasure to present to him herewith
this medal which has been unanimously awarded to him by the
Committee
ACCEPTANCE OF MEDAL
By Treat B. Johnson
Mr. Chairman, Ladies and Gentlemen:
I thank you heartily for this honor the New York Section has
conferred upon me.
The reward of a scientific man is not in the money he gets
for his services, but more than anything else, in the feeling of
satisfaction that comes from the knowledge that he has accom-
plished something which his colleagues recognize as a valuable
contribution to science.
By conferring this honor on me to-night I see such a recogni-
tion of the value of my work, and I assure you tfiat I deeply
appreciate the honorable distinction. I also desire to express
my heartfelt thanks for the kind words the representatives of
your Section have spoken.
The credit for the work upon which you have made this
award to-night does not belong to me alone. The investiga-
tions are the result of the energy of several men who have studied
under my direction. I take pleasure at this opportune time in
expressing my appreciation of their support and spirit of co-
operation.
Treat B. Johnson William H. Nichols Medalist. 1918
THE DEVELOPMENT
OF PYRIMIDLNE
CHEMISTRY
MEDAL ADDRESS
By Treat B. Johnson
We are celebrating to-
night the one-hundredth
anniversary of the discov-
ery of the first pyrimidine
compound to be described
in the chemical literature.
One hundred and forty-
two years ago, in 1776,
Scheele made the interest-
ing observation that, if
uric acid is treated on a
porcelain dish with a few
drops of nitric acid, the
uric acid dissolves and
after drying leaves behind
a characteristic, red,
amorphous residue. In
18 1 7, or forty-one years
after this historical ob-
servation, the behavior of
uric acid on oxidation was
investigated by Brugna-
telli.1 He showed that
this naturally occurring
substance is destroyed by
oxidation with nitric acid
and chlorine water and
actual 1 y succeeded in
isolating from the prod-
ucts of reaction a definite
oxidation product, which
was afterwards proved to
be the pyrimidine — al-
loxan.
The following year, in 1818, Brugnatelli's publication was
followed by that of the English chemist, Prout,5 also dealing with
the chemistry of uric acid. Prout had repeated the work of
Scheele ami observed that the product obtained by interaction
of uric acid and nitric acid reacts with ammonia, giving an intense
red color which is destroyed by acids. This observation led to
the development of the well known murexide lest for uric acid
and related purines Prout believed that he was dealing here
with the ammonium salt of a complex acid and found that his
d< i pi] eolored product interacted with mineral acids with forma-
tion of a colorless, crystalline substance. It was afterwards
shown that Prout was not dealing with the true nucleus of murex-
1 Phil. Mag.. 68. 30, Ann. chim. phys., 8, 201.
> Phil. Trans.. 1818, 420.
Apr., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
3° 7
ide, but actually had in hand the cyclic compound uramil or
the second pyrimidine compound to be described in the chemical
literature.
Later in 1820, Prout1 showed that the pyrimidine alloxan is
also formed by the oxidation of murexide. In other words, the
first pyrimidine combinations to be recorded in the chemical
literature were hexahydro derivatives of pyrimidine, and were
revealed to us by the study of reactions which were applied to
■determine the constitution of the naturally occurring purine—
uric acid.
Ever since the discovery of these two pyrimidine compounds,
purine and pyrimidine chemistry have closely interlocked. The
development has been reciprocative and a revelation of chemical
facts has been made, which constitutes one of the most interesting
and important chapters of organic chemistry. We now know
that representatives of both series of compounds function in
vital changes taking place in both the plant and animal kingdom,
and it is on account of this biochemical connection that the study
of the chemistry of cyclic compounds of these two series has re-
ceived and deserves so much attention.
A careful review of the pyrimidine literature will reveal the
fact that, while the development of this field of chemistry has
been progressive and the investigations very productive both
from a chemical and a biochemical standpoint, there were, how-
ever, certain periods of activity which were characterized by the
number of original contributions to the literature that were funda-
mental in character, and which had a directing influence on the
later lines of pyrimidine investigation. The number of investi-
gators who made such contributions to chemical literature was
not large, but the results of their labors were like sign posts by
the roadside. Not only have their deductions proven to be
sound, but the way was opened up by their work for later dis-
coveries, which progressively revealed to us our present knowledge
of the physiological importance of certain representatives of this
interesting series of compounds.
In order to bring to your attention, in the time at my disposal,
the most important developments in pyrimidine chemistry, I
have subdivided our one hundred years of research activity into
the following six periods:
1817-1838 1863-1883 1893-1903
1 838-1 863 1 883-1 893 1 903-1918
No attempt will be made to review completely the pyrimidine
chemistry of any one period, but it is my purpose to present
briefly a periodical succession of experimental discoveries, which
I believe to be the most important, and to lay emphasis on those
that were the most ingenious and original, and consequently
contributed the most to the development of our subject.
1817-1838
For a period of twenty years after Prout's pioneer work dealing
with the action of nitric acid on uric acid, one can search chemical
literature in vain for any work that may be considered as an
important contribution to pyrimidine chemistry. The state of
chemistry' at that time was one of transition, and it was not until
the beginning of our second period of development, or ten years
after Wohler had given to chemistry his synthesis of urea from
ammonium cyanate, that important and successful investigations
were carried out, which directed the attention of organic investi-
gators to the chemistry of pyrimidine compounds.
1 838-1 863
The great achievement of our second period of pyrimidine
history was the discovery of chemical reactions, which gave us
the first conception of the possible transformations of uric acid.
These facts were revealed to us by the joint investigations of
Liebig and Wohler on the nature of this physiologically important
acid. Their first paper was published in the Annalen in 1838,*
1 Annals of Philosophy (London), 14, 363.
• Ann., 26, 241.
and was followed by a series of pubUcations on the chemistry of
uric acid which have since become classic. When one considers
that they were working at a time when organic chemistry — or
what now is called organic chemistry — had no existence, it seems
marvelous that their experimental work was so well done and
that it has survived the test of careful experimental investigation.
Liebig and Wohler established by their experimental work the
important transition changes effected by the oxidation of uric
acid under different conditions, and revealed to us the existence
of several pyrimidine combinations of biochemical interest,
which have since been the subject of very extensive research.
Of these compounds may be mentioned, for example, alloxan,
uramil, alloxantine, thionuric acid and dialuric acid.
NH — CO NH — CO NH — CO CO — NH
CO CO
CO CHNH2 CO CH — O — COH CO
NH — CO NH — CO
Alloxan Uramil
NH — CO
! I
CO CHSH
I I
NH — CO
Thionuric acid
NH — CO CO — NH
Alloxantine
NH — CO
I I
CO CHOH
I I
NH — CO
Dialuric acid
While the structure of these compounds was not established until
several years after the activity of Liebig and Wohler, neverthe-
less, so clear a picture of the chemical relationship existing be-
tween these compounds was revealed by their work that it ex-
cited the chief attention of several investigators for many years
afterwards.
Schlieper and Gregory, pupils of Liebig and Wohler, also con-
tributed to the development of this period, and published im-
portant papers dealing with the chemistry of alloxantine, hydurilic
acid, nitrohydurilic, allituric and dilituric acids.
1 863-1 883
The work which stands out most prominently in our third
period of pyrimidine development is that of four investigators,
namely :
1. Baeyer 3. Mulder
2. Medicus 4. Grimaux
It was Baeyer,1 a pupil of Schlieper, who continued the work
of Liebig and Wohler on the structure of uric acid, and who first
gave us a correct idea of the chemical relationship existing be-
tween dialuric acid, alloxan, hydurilic acid, pseudouric acid,
alloxantine and uramil. He established the fact that all of these
compounds are derivatives of a cyclic amide of malonic acid to
which he assigned the name — barbituric acid, and showed that
they can be made synthetically from this cyclic ureide. The
correct constitution was assigned to barbituric acid by Mulder'
in 1873.
Baeyer prepared his pyrimidine (barbituric acid) by the re-
duction of its dibrom derivative, which was prepared from Schlie-
per's violuric acid, and showed that it is easily decomposed by
fusion with alkali giving carbon dioxide, ammonia and malonic
acid. In other words, Baeyer unraveled by his investigations
the whole chemistry of this interesting series of uric acid deriva-
tives, and, by revealing their generic relationship to malonic
acid of the aliphatic scries, opened the way for new developments
which finally led to the preparation of these same combinations
by synthetical methods.
Bacyer's work was followed, in 1878, by that of Grimaux,1
who accomplished the first synthesis of barbituric acid by allow-
ing malonic acid to internet with una in the presence of phos-
' Ann., 127 (1863), I, 199; 130, 129.
■ Ber., 6 (1873), 1235.
• Compl. rend., 87, 752.
3o8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 4
phorus oxychloride. The contribution to literature of this im-
portant synthesis, together with the results of Baeyer's investiga-
tions, and the appearance of the classic paper by Medicus' in
1875, in which he proposed structural formulas for uric acid,
xanthine, guanine, theobromine and caffeine, that were after-
wards proven to be correct, were the crowning features of a period
of activity which will always be conspicuous for its productive-
ness and originality.
1 883- 1 893
A new chemistry of pyrimidine and its derivatives began to
undergo development in the year 1883. The work of Grimaux
on barbituric acid, to which I have just referred, and that of
Kmil Fischer in the field of purine chemistry from 1881 to 1883
not only completely established the importance of the chemistry
of cyclic ureides, but also was the beginning of developments in
a field of research which gave to us a new chapter of pyrimidine
chemistry.
Three investigators, whose interest was excited by the activities
of these pioneers in synthetic chemistry, and who foresaw the
possibilities of opening up new lines of research by the applica-
tion of synthetical methods, were Robert Behrend, Adolph Pinner
and Ernst von Meyer. Their work stands out as the crowning
achievements of our fourth period of pyrimidine history.
Behrend's preliminary paper on the behavior of urea towards
ethyl acetoacetate was published in the Berichle der Deutsche
Chetnische Gesellschaft1 in 1883. An interpretation of the reac-
tion between these reagents was given the following year, and
this was then followed by a series of important publications on
pyrimidine compounds. Behrend presented in these papers
original chemical data which led to a clear recognition of the
structure of 4-methyl-uracil and its important derivatives.
Amidouracil, hydroxy-xanthine and isobarbituric acid were
described in 1885.
In [889 Behrend and his student Roosen3 were able to enrich
science with their original synthesis of uric acid, which has since
become classic and is recorded in every textbook of organic
chemistry.
NH — CO NH — CO XH — CO
CO CH
NH — C.CH3
4-Methyluraci]
CO CNH2
NH — CH
Amidouracil
CO CNH.CONH,
XH— CH
Hydroxy xanthine
CO COH
I II
NH — CH
Isobarbituric Acid
Behrend confined his attention in his researches to the study
of pyrimidine condensations produced by the interaction of ureas
and thioureas with fl-kctone esters. Immediately after he had
announced his synthesis of 4-methyluracil, Pinner entered this
field of investigation and extended the application of Behrend's
reaction by showing that amidines also condense with fi-ketone
esters, in a manner similar to urea, giving pyrimidines. This
new reaction was applied successfully by Pinner' and his co-
workers with a ^rcat variety of amidiue combinations, thereby
: 1 s of pyrimidine compounds which were
characterized by their basic properties. Much attention has
been paid to this series since the investigation of Pinner but. so
far as the writer is aware, no representative of this class of
pyrimidines has been shown to occur in nature, or has found any
commercial application.
I Ann., 76 (1875), 230.
« Ber., 16, 3027.
• Ann.. 861, 235.
• Ber., 17 (1884). 2519; 18, 759. 2845.1a0. 2361.
It was Pinner who first proposed and used the name — pyrimi-
dine— to designate the mother substance of this group of cyclic
ureides.
E. von Meyer,' the third member of our group, enriched science
with a new method of entering the pyrimidine series, by applying
and correctly interpreting an old reaction which was discovered
by Frankland and Kolbe, in Bunsen's laboratory at Marburg
in 1848. These earlier investigators had shown that an aliphatic
nitrile like ethylcyanide is changed by heating with sodium or
potassium into a crystalline substance having basic properties.
Baeyer later showed that a similar change can be brought about
with methylcyanide.
unique transformations were thoroughly investigated by
von Meyer and shown to be processes of polymerization, whereby
the aliphatic nitrile enters first a dimolecular condition. In
some cases these simpler polymerized forms were isolated. If,
however, the process of heating with sodium is continued a further
polymerization can be brought about and the dimolecular nitrile
transformed into a pyrimidine compound. This type of change
is of special significance because it is the only nucleus-synthetic
or polymerization reaction connecting the aliphatic with the
pyrimidine series.
Besides the work of the three investigators — Behrend, Pinner
and von Meyer — there is one other important contribution that
was made in this period, to which I must call attention. I refer
to the work of Arthur Michael, the first American investigator to-
contribute to pyrimidine chemistry. It was Michael who recom-
mended, in 1887, the use of sodium ethylate as a condensing agent,.
and who was the first one to show that the sodium salts of diethyl-
malonatc and ethylai ndense with urea, thiourea,
and guanidine compounds, in the presence of this reagent, to-
fonn pyrimidines.5 The introduction of this reagent opened
up an almost unlimited field of investigation which has led to-
discoveries having far-reaching consequences.
1893-1903
During these earlier periods of activity, which I have hastily
reviewed, physiological chemistry had not been concerned with
any special pyrimidine compounds, although derivatives of this,
class of compounds had been given special prominence by the
investigations of Behrend who began his synthesis of uric acid
with a substance of this class. This condition of affairs prevailed
until about the year 1S9; when important researches were
executed which opened up new paths and founded lines of pyrimi-
dine research which have since proved very fruitful.
The leading spirit in this progress, and the one who was in-
strumental in promoting this change, was Kossel, whose im-
portant investigations dealing with the constitution of nucleic
acids were at this time attracting the attention of physiologists -
and organic chemists throughout the scientific world.
Nucleic acids had been known to chemistry since 1874 when
they were discovered by Miescher. but practically nothing was •
revealed regarding their constitution until Kossel undertook their
chemical investigation. Through his brilliant work the chemistry
of these acids was advanced to .1 point where they were dis-
entangled from proteins and were recognized by physiologists
as one of the normal constituents of the animal cell.
kos-cl had already enriched science with his important dts-
coverj of tin- "alloxuric bases" among the products of hydrolysis
of these acids. Three of these purine compounds — namely,
guanine, xanthine and hypoxanthine — were known to chemistry,
while the fourth, adenine, was a new combination. Notwith-
standing the advance which was made by these discoveries the
chemistry of nucleic acids was -till in a state of chaos at the be-
ginning of out sixth |H-riod 1893 The nucleic acids of different
origin differed in regard to the relative quantities of the purine ■
' /. prakt Chrm., 31. 261 . 36. 337; 39, 156.
: Am Chrm. J., 9, 219: .'. prakt i ■-.. ».• . [2] 36, 456.
Apr., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
3°9
bases formed on hydrolysis and it was questionable whether
previous investigations had been conducted with impure or
partly decomposed acids. In order to obtain further data which
would give character to these acids as a class and furnish a
definition which would sharply distinguish them from other
constituents of the animal body, Kossel and Neuman subjected
thymus nucleic acid, in 1893, to a very careful chemical examina-
tion. As a result of that investigation chemistry was enriched
with the discovery of two new pyrimidine compounds, namely:
thymine and cytosine. Thymine was discovered in 1893' and
in the following year cytosine was isolated as a cleavage product
of thymus nucleic acid. Eight years later appeared the publica-
tion of Ascoli- announcing the discovery of uracil among the
cleavage products of yeast nucleic acid.
These three pyrimidines are now recognized as normal con-
stituents of nucleic acids. Cytosine and uracil are produced by
the hydrolysis of both animal and plant nucleic acids, while
thymine results only from animal nucleic acids.
The first structural investigation of the pyrimidine compounds
formed by hydrolysis of nucleic acid was made with thymine.
The researches of Kossel, Steudel and Jones3 were especially
fruitful and showed the similarity of this substance in chemical
properties to Behrend's 4-methyluracil, but they completely
excluded their identity. Cytosine was next examined by Kossel
and Steudel4 and shown to be an amino combination, and its
relation to uracil was established by the action of nitrous acid.
By oxidation with barium permanganate thymine and cytosine
were converted into urea and biuret, respectively, thereby com-
pleting the evidence upon which Kossel constructed the formulas
of these three combinations. Whether this evidence was suf-
ficient to constitute proof of their structure or not is now a mat-
ter of little importance. Kossel concluded that all three com-
binations were pyrimidines and represented them by structural
formulas which were later proven to be correct by the synthetical
work of Emil Fischer and that of Wheeler and Johnson.
It is impossible for me to take up at this time the later physi-
ological development in this interesting field and I shall refer
hereafter to this phase of pyrimidine chemistry only in so far
as the development has been associated with my own individual
work.
Such was the state of affairs at the end of our period 1893-
1903. Again biochemistry and organic chemistry had been
brought closer together, and a prominence given to the chemistry
of pyrimidines which it had never had before.
1903-1918
If we disregard the important work of the two German in-
vestigators, Gabriel and Traube, the more important develop-
ments in pyrimidine chemistry during our last period of pyrimi-
dine history can be traced to the activities of investigators in
this country, namely: my colleague, Levene, and the organic
chemists of the Sheffield Laboratory. It was in 1903, or the be-
ginning of our last period, that attention was first directed to the
study of pyrimidines in our laboratory. The work of Kossel
and his coworkers on nucleic acids was then beginning to excite
the attention of leading biochemists in this country, and his de-
ductions regarding the constitution of uracil and thymine had
been proven to be correct by Fischer and Roeder5 who had pre-
pared these two pyrimidines by means of an interesting synthesis.
It was during this period of activity that my predecessor,
Professor Henry L. Wheeler, started his investigations in pyrimi-
dine chemistry and opened up a field of research for our labora-
tory, which has been very productive both from a synthetical
and a biochemical standpoint. Since that time we have con-
1 Ber., 26, 2751.
>Z. phyticl. Chem., 31, 161.
'Ibid., »9, 20, 303; 30, 539.
« Z. Physiol. Chem., 87 (1902), 245; 37, 527, 377; 38, 49.
' Ber., 34, 3751, 4129.
tribu,ted to chemical literature about eighty-five publications
dealing with various phases of pyrimidine chemistry.
Our first work on pyrimidines was really an extension of Pin-
ner's researches on amidines, in which we made use of a new
type of amidine combinations, namely: pseudothioureas in con-
densation reactions. Previous to our work amidines of this
type had never been utilized in synthetical processes. Their
salts were well known, but the free bases had previously been
considered as unstable combinations, which were incapable of
existing in a free condition. We found by investigation that this
conclusion was based on incomplete evidence. We not only were
able to show that these bases are quite stable in aqueous solution
at low temperature, but also found them to be far more reactive
towards various reagents than urea. The simple combinations
interacted smoothly with /3-ketone-esters in alkaline solution
giving representatives of a new class of pyrimidines, which have
since proven very valuable to us for developing new synthetical
processes. It was the discovery of this reaction that gave us
an entrance to a new field for research and led to the develop-
ment of new syntheses of uracil, thymine and cytosine.
The importance of our method of pyrimidine synthesis is illus-
trated by the reaction between pseudomethylthiourea and the
sodium salt of ethyl formylacetate or the first step in the process
leading to the formation of uracil. As is well known the sodium
salt of this ester and also those of the higher ester homologues
fail to react with urea in alkaline solution with production of
pyrimidine compounds. Behrend prepared his 4-methyluracil
by allowing ethyl acetoacetate to interact with urea in the pres-
ence of hydrochloric acid. A similar reaction cannot be applied
with esters of the simplest 0-ketonic acids because such combina-
tions show a great tendency to undergo molecular condensations
in the presence of acids giving derivations of benzene. On the
other hand, their sodium salts condense smoothly with the
simple pseudothioureas in aqueous solution giving 2-mercapto-
pyrimidines.
Ethyl formylacetate and ethyl formylpropionate, for example,
condense with pseudomethylthiourea giving 2-methylmercapto-6-
oxypyrimidine and 2-methylmercapto-5-methyl-6-oxypyrimidine,
respectively. These compounds are characterized by the ease
with which they undergo hydrolysis. When digested with hydro-
chloric acid the mercapto group is removed almost quantitatively
with formation of uracil and thymine, respectively. The com-
plete synthesis of these two naturally occurring pyrimidines1 is
represented as follows:
COOC2H6 NH, COOC2H6
CCH3
II
NaO.CH
CH3SC
II
N-
( + )
CCH,
II
-CH
CH3SC
II
NH
( + )
II
NaO.CI-
[
[
NH — CO
1 1
1 1
CO CCH,
il
NH — CH
(Thymine)
'
'
NH — CO
1 !
NH
1
— CO
1
1 1
CO CH
«_
1
CH»SC
CH
N
-CH
Nil CH
(Uracil)
Fischer and Roeder's method of synthesizing these two pyrimi-
dines consists in heating urea with acrylic- and a methylacrylie
acids, respectively, and brominating the hydrouracils thus formed.
1 Am. Chem. J., 89 (1903), 478
3i°
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 4
Nft COOH
l 1
NH -
1
-CO
1
1 !
CO + CH
1 II
NH2 CH2
1
— > CO
1
NH-
1
CH2 -
1
-CH2
NH-
|
-CO
1
•
1
CO
1
CHBr
The bromine derivatives are then converted into uracil and thy-
mine by treatment with alkali or pyridine. Fischer's method
has the disadvantage that the unsaturated acids are not easily
accessible combinations and the yields are much below those
obtained by our method. Fischer's synthesis of uracil is repre-
sented by the following expression:
NH — CO
CO CH
I I II
NH — CH2 NH — CH
(Uracil)
Having succeeded in perfecting new and practical syntheses of
uracil and thymine we naturally turned our attention next to
the problem of preparing cytosine from nucleic acids synthetically.
Our 2-methylmercapto-6-oxypyrimidine resulting from the con-
densation of pseudomethylthiourea and the sodium salt of ethyl
formylacetate proved to be an excellent starting point for a
synthesis of this base. It interacted smoothly with phosphorus
halides with destruction of the acidamide grouping giving a 2-
mercapto-6-chlorpyrimidine. This combination proved to be
an oil which could be distilled without decomposition. When
heated with alcoholic ammonia under pressure it was transformed
smoothly into the corresponding aminopyrimidine. The latter
compound is stable in cold acid solution, but when such solutions
are heated mercaptan is evolved and the pyrimidine is transformed
quantitatively into cytosine. The compound formed by this
reaction agrees in all its properties with cytosine1 obtained by
hydrolysis of nucleic acids. The complete synthesis is repre-
sented as follows:
NH — CO N = CC1
CH,SC
II
N-
CH
II
CH
■ CH,SC CH
II II
N — CH
N = CNH2
I I
CH3SC CH
N == CNH2
I I
CO CH.H.O.
N — CH NH — CH
This is the only practical method for the preparation of cytosine,
which has so far been developed. The method is one of general
application and has been utilized by us for the preparation of
several derivatives of this interesting pyrimidine base.
The identity of our synthetical cytosine with the natural pro-
duct was established by direct comparison with a sample of the
base from the nucleic acid of the spleen, which was kindly sent
to us at that time by Dr. Levcnc, and also by comparison with
a natural specimen which we succeeded in isolating from the
uracil fraction after hydrolysis of tritico-nucleic acid of the wheat
embryo.2 This was the first time that cytosine was shown to
be a constituent of a plant nucleic acid.
Following our work on the synthesis of uracil, thymine and
cytosine the problem of pyrimidine formation by condensation
of pscudothioureas with /3-ketone esters received much attention.
It was found by experimentation with a great variety of esters
that our method of operating, while original, had, however, its
limitations. Thiourea gave better yields of pyrimidines when
condensed in aqueous solution with some ketone esU-is than
when pseudothioureas were employed, and it also reacted better
> Am. Chem. J.. J9, 492.
• Ibid., 29, 505.
in alcohol solution in the presence of sodium ethylate than under
any other condition. We also found that while practically every
/3-ketone ester, which we carefully examined, interacted with a
pseudothiourea with formation of a pyrimidine, on the other
hand, it was impossible to obtain a satisfactory condensation of
a malonic ester or cyanacetic ester or any of their derivatives
with a pseudothiourea with formation of a barbituric acid com-
pound. Urea and thiourea, as is well known, interact smoothly
with these esters in the presence of sodium ethylate.
The one objectionable feature of our method of synthesizing
uracil and thymine from a pseudothiourea is the disagreeable
odor produced by hydrolysis of the mercaptopyrimidine due to
the formation of mercaptan. The study of thiourea condensa-
tions led to important results in that we were able to develop
a synthesis of uracil and thymine that is an improvement over
the pseudothiourea method.
When this reagent is condensed with the sodium salt of ethyl
formylacetate a much larger yield of pyrimidine is obtained than
when a pseudothiourea is employed. The condensation takes
place with formation of 2-thiouracil as follows:
COOCjHs NH — CO
NH,
CS + CH
NH. NaOCH
= CS
CH + CHsOH + NaOH
NH — CH
The thiouracil is many times less soluble than any corresponding
2 -mercaptopyrimidine which we have examined.
Having obtained this sulfur derivative it remained to discover
a simple method of replacing the sulfur with oxygen and con-
verting it into uracil. This was accomplished by applying a
new method of desulfurization, which depends on the action of
chloroacetic acid on a cyclic thiourea grouping of this character.
The change is brought about by digesting the pyrimidine in
aqueous solution with the halogen acid when the sulfur is re-
moved in the form of thioglycollic acid and uracil is formed.
The process involves, first, an addition of the halogen acid to
sulfur and, secondly, a hydrolysis of the addition-product with
formation of uracil.1 Thymine is easily prepared by application
of similar reactions with thiourea and ethyl formylpropionate.
NH — CO
I I
CS CH
I I
NH — CH
NH — CO
CI
s = c
CH
HOOCCH/
NH— CH
NH — CO
I I
CO CH + HC1 +HSCH.COOH
NH — CH
This method of dcsulfurizing has been widely applied in our
laboratory and is applicable not only for desulfurizing pyrimi-
dines, but also thiohydantoins and thiopurines.
In the time at my disposal it is impossible to give you a com-
prehensive view of all our earlier work on mercaptopyrimidines.
As is the case in the early development of every new field of
research, a large amount of information was acquired, which
now appears unessential, and it is not my desire to discuss to-
night phases of our work which have a purely abstract interest
only.
The most important developments of our earlier activities,
from a biochemical standpoint, were the discovery of a color
test for uracil and cytosine1 which is extremely delicate and
should prove of great value for the detection of these pyrimidines,
and, secondly, the development of a method of separating uracil
■ .4 m. Chem. J., 40, 54".
•/. Biol. Chem., 1907, 1SJ.
Apr., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
3"
from thymine and determining them quantitatively in mixtures of
these substances.1
Another line of investigation which led to important con-
clusions was that dealing with the question of substitution in
pyrimidine compounds when such combinations are subjected
to the process of alkylation. While many of the derivatives
synthesized and studied had in themselves only a purely chemical
interest, nevertheless by the systematic application of certain
color tests to various representatives of this class, we were able
to reveal some very interesting structural relationships.
The reagents productive of color reactions, which have been
found to be very useful in these developments are diazobenzene-
sulfuric acid, which was introduced into biochemistry by Pauly and
Burian, and the uric acid and phenol reagents of Folin and Denis.'
These are prepared from sodium tungstate, phosphomolybdic acid
and phosphoric acid. In our work on alkylation we were enabled
by use of the diazo reagent to determine, with a considerable
degree of certainty, the position of substitution, namely, 1 or 3,
in a uracil combination.' Our work with Folin's reagents re-
Tealed the interesting fact that these were specific for amino
groups, and could be employed to determine whether such a
radicle is substituted in the 5-position of a uracil compound.
The further application of these reagents is still under investiga-
tion.
While these investigations to which I have been referring
were in progress, we constantly had in mind the importance of
obtaining experimental data, which would aid in elucidating the
nature of the linking of the pyrimidines — uracil, thymine and
cytosine — in the nucleic acids. These natural products were
known to be composed of phosphoric acid, purines, pyrimidines
and sugars, but ten years ago, we had practically no knowledge
of the way in which these four constituents were linked together
in these complicated molecules. Furthermore, there was much
doubt at that time whether the pyrimidines actually existed as
such in these combinations.
Burian* made the assumption that the pyrimidines result
from purines by degradation of the purine constituents of nucleic
acids through hydrolysis and supported his deductions in-
directly by showing that such cyclic combinations can be trans-
formed into pyrimidines by digestion with acids in the presence
of carbohydrates. Osborne,6 Levene and Steudel produced
evidence showing that Burian's conclusions were incorrect, and
that pyrimidines do not result from purine bases. They postu-
lated, furthermore, that uracil and thymine are primary products
•f hydrolysis, and do not result from any process involving the
removal of an amino group from any aminopyrimidine of the
nature of cytosine or isocytosine, but are present in the nucleic
acids in their simple forms.
It was Levene and his coworkers who cleared up this con-
troversy on constitution, and whose investigations advanced
our knowledge to such a degree that we were finally able to obtain
a picture of the molecular structure of these acids. Levene suc-
ceeded in showing that these combinations are composed of
characteristic complexes to which he assigned the name —
nucleotides. The latter are compounds consisting of phosphoric
acid conjugated with a complex composed of a carbohydrate and
• purine or pyrimidine. In other words, according to Levene, a
nucleic acid may be a single nucleotide or composed of several
nucleotides. Regarding the nature of the union of the individual
nucleotides in a nucleic acid we have no very definite knowledge.
The constitution of nucleotides has been partly elucidated by
the work of Levene.6 He has been able to prove the order of
the groups in these combinations by showing that they may be
'/. Biol. Chem., 1908, 407.
• J. Am. Chem. Soc. 86 (1914), 970.
• J. Biol. Chem.. 1908, 163.
' Z. physiol. Chem.. 61, 438.
• Am. J. Physiol.. 81, 157.
•J. Am. Chem. Soc., 86 (1913). 586.
transformed by hydrolysis into two types of complexes depending
upon the experimental conditions employed.
For example, it is possible to detach from a nucleotide phos-
phoric acid giving a simpler complex containing sugar in combina-
tion with a purine or pyrimidine. To such combinations Levene
assigned the name nucleosides. The second decomposition in-
volves a removal of the nitrogenous nucleus leaving the phos-
phoric acid in combination with the carbohydrate.
Phosphoric Acid - ■ Carbohydrate
Purine
Pyrimidine
Direct proof of the presence of the nucleoside combinations has
been presented by the isolation of the pentose nucleosides, namely,
guanosine, adenosine, uridine and cytidine from yeast nucleic
acid and of guanine hexoside from thymus nucleic acid.
Of these various nucleosides the only ones in which we are
interested to-night are uridine and cytidine. These are combina-
tions of uracil and cytosine, respectively, with the pentose sugar-
ribose. Regarding the nature of this nucleoside union and the
position substituted by the sugar in the pyrimidine ring, sufficient
data have not been presented to enable us to express structurally
the exact constitution of these compounds. Levene and LaForge'
have concluded, however, from very good evidence, which
we have not time to discuss to-night, that this linking is probably
of a glucosidic nature, and that the carbohydrate may be joined
to the pyrimidine in one of two positions, viz., the 3- or 4-position
of the ring. If these assumptions be correct then the con-
stitution of uridine, for example, may be expressed by one of the
two following formulas:
NH — CO
t I
CO CH
HOCH,.CH.HOHC.HOHC.CH.NH
NH — CO
I I
CO CH
CH
I II I o ,
NH — C.CH.CHOH.CHOH.CH.CH,OH
In order to throw further light on the question of constitu-
tion of these pyrimidine nucleosides, we have been making a
study, during the past three years, of pyrimidine combinations
containing as side chains groups having the structure of alcohols.
This work has been developed from the assumption that the
pyrimidines — uracil, thymine and cytosine — are linked to car-
bohydrates at position 4 in nucleosides, and that this linkage is
between two carbon atoms as represented in Levene's formula
for uridine.
The simplest representatives of this class of compounds are
the monatomic primary and secondary alcohol derivatives of
uracil, thymine and cytosine. Such combinations may be con-
sidered as the prototypes of their respective series, and therefore
would be expected to exhibit a chemical behavior similar to that
of the natural nucleosides.
We have synthesized, in the course of our work, four repre-
sentatives of this class of compounds, namely, the two primary
nuclepsides of uracil and thymine represented by Formulas I
and II, and their corresponding secondary nucleosides III and IV.
NH - CO NH — CO
CO
CH
NH — C.CHjOH
(I)
Ber., 46, 608.
CO CCH,
NH — C.CH2OH
(ID
312
THE JOURNAL OF INDUSTRIAL AND ENGINEERING < HEMISTRY Vol. 10, Xo. 4
Previous to our investigations we had absolutely no knowledge
of hydroxvpyrimidine combinations of this type.
NH — CO NH — CO
II II
CO CII CO CCH,
I II /CHa /CH2
NH — CCH^ NH — CCH S
V)H \)H
(III) (IV)
Our investigations have revealed to us the facts that these
simple nucleosides behave in an entirely different manner from
the natural nucleosides when subjected to intense hydrolysis.
hi no case have we been utile to break down such a combination
into uracil or thymine and an aldehyde. This would involve a
cleavage of the side chain from the pyrimidine ring.
The primary nucleosides obtained by synthesis are character-
ized by their great stability. They exhibit the normal behavior
of primary alcohols and, when subjected to the action of acids,
interact with these reagents to form esters. In other words,
they react as might be predicted, and do not conform in chemical
behavior to that of a natural nucleoside like uridine.
In the light of these interesting developments it became of the
greatest interest for us to extend our investigations to a study of
the behavior of secondary nucleosides on hydrolysis. Such com-
binations (Formulas III and IV) approach in constitution still
closer to that which has been assigned to natural nucleosides.
We found to our surprise that these pyrimidines are far less
resistant to the action of acids than the primary nucleosides.
They did not respond, however, to a chemical change on hydrol-
ysis that was productive of either uracil or thymine with cleavage
of the secondary alcoholic side chain. On the other hand, they
underwent a transformation which is unique and sharply dif-
ferentiates them from primary nucleosides.
The two nucleosides III and IV undergo a profound molecular
change on prolonged heating with acids and are transformed,
with evolution of carbon dioxide, into derivatives of glyoxaline.
In other words, the introduction of a secondary alcohol group
into the 4-position of uracil and thymine tends to decrease the
stability of the pyrimidine nucleus to such an extent that it can
easily be ruptured by hydrolytic agents.
In the case of the uracil nucleoside the product of hydrolysis
is identical with 2-oxy 4.5,-dimethylimidazol which has previously
been described by Kunue' and Biltz.2 The identity of the two
products was established by the fact that both substances interact
with acetic anhydride with formation of the same acetyl deriva-
tive.
The thymine nucleoside undergoes hydrolysis with evolution
of carbon dioxide, and formation of 2-oxy-4,5-ethylmethylimid-
azol which has already been described by Gabriel and Posner.'
In other words, the two nucleosides react in a perfectly analogous
manner. The transformation is one which has the greatest
biochemical interest, and, when time permits, will receive more
attention in our laborat'u .
NH — CO NH — CCH
CO CH
CO
/CH3
NH — CCH< NH — CCH,
\)H
NH — CO XH — C.C5HS
CO CCHS
NH — C.CH<
CO
I
NH — C.CHj
sOH
This reaction, which we have discovered, suggests again a
genetic relationship between naturally occurring pyrimidines and
imidazoles. As far as the writer is aware, this is the first time
that it has been shown that a pyrimidine can be transformed into
a glyoxaline combination by hydrolysis. Liebig and Wohler
made the interesting discovery that uric acid can be transformed
smoothly into allantoin with destruction of the pyrimidine nucleus
of the purine. Behrend later showed that 4-methyl uracil also
can be transformed under certain conditions into parabanic
acid, but in both cases the transformations were brought about
by the combined effect of oxidation and hydrolysis.
Our rearrangements are unique in that they can be effected
by hydrolysis alone and without first destroying the unsaturated
condition of the uracil and thymine molecule. Whether a
lengthening of the carbon side chain and the introduction of
more hydroxy] groups will weaken the attraction between the
carbon atom in position 4 and permit of hydrolysis to take place
without destruction of the pyrimidine ring remains to be de-
termined.
Sheffield Scientific School of Yale Univbrsity
New Haven, Connbcticct
MESSAGE FROM PROF. BOGERT
Professor M. T. Bogert, who was to have been present to
address the meeting on "Organic Chemistry in Modern War-
fare," sent the following message:
"Urgent war business will prevent my attending the meeting
Friday,night for which I am very sorry. Permit me to congratu-
late Dr. Johnson upon the honor he has received and the Amer-
ican Chemical Society upon the recipient selected. Few men
in our country have done so much for the cause of synthetic
organic chemistry as Dr. Johnson. He has been a wonderfully
prolific worker and is a recogruzed leader of not only national,
but international, reputation Greetings to Johnson, Nichols,
and all fellow members "
CURREJMT INDUSTRIAL NLW5
THE EKENBERG PEAT PROCESS
Experiments "" the treatment of peat l>v a modified Ekenberg
process an- being conducted at Chateauneuf, Bretagne, Prance.
According to a paper in Comples RendlU of September 3.
the peat is first compressed in presses of the Mabille «>r Aurep
types to reduce the water in it from about 90 to 60 per cent
'flu prat is then treated with superheated steam at 1600 C.
for 23 min. and then either compressed again or at once dried,
which is lust done in special chambers, though air drying may
be applied. The product which i^ called turbon still contains
' Ber., 28, 2040.
'Ibid., «0, 4801.
• Ibid., »7, 1037.
20 to 25 per cent of moisture but does not absorb moisture as
it would do if the cellulose in the peat had not been destroyed
by tlu steam heat The calorific value is stated to be raised
by 10 per cent over that of dried peat; the turbon yields 61 per
cent volatile matter. 36 per cent fixed carbon. .? per cent ash.
With suitable arrangement of the batteries of autoclaves and
utilization of exhaust steam, a heat efficiency of from 85 to
91 per cent is claimed to be realized 111 this process, which can
be worked throughout the year. The turbon is fired directly
or sent to gas works (with ammonia recovery) or converted
into power gas for internal-combustion engines. This last
mentioned utilization has so far proved the most satisfac-
tory.— A. McMillan
Apr., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
3i3
NORWEGIAN IRON INDUSTRY
The present situation has taught Norway how dangerous it
is to be dependent on foreign supplies of pig iron, steel and steel
plates, says the Anglo-Norway Trade Journal. The problem
has been under consideration for some time and one of the chief
points to be settled was the geographical position of the new
works. A number of Stravanger people working in connection
with a large English company have formulated plans for works
at Straumpol in Tysfjorden near Narvik for the production of
250,000 tons of pig iron annually and for the provision of a large
rolling mill. The close proximity of Narvik, which is the ship-
ping port for Swedish ore, and also of Kirkenaes, the shipping
port for the best Norwegian ore, is, of course, an obvious ad-
vantage but, in addition to this, Straumpol is reported to be
a natural harbor with good industrial sites having easy access
to water power. The transportation of coal from England
would be cheap but, beyond this, the geographical position in
relation to Spitzbergen should not be overlooked, seeing that
a Norwegian group is now working energetically to develop the
Spitzbergen coal field. The total capital required is estimated
at $5,500,000. — M.
MAGNETIC SEPARATIONS AND THE RARER METALS
The use of magnetic separators in treating minerals in a fine
state of division has reached a high point of efficiency, says a
contemporary. Thus in treating monazite sand, magnetite
is removed by the weakest magnet, ilmenite by the intermediate
and monazite by the strongest magnet. The use of a series of
magnets of different strengths enables discrimination to be made
between substances of varying magnetic susceptibility. Mag-
netic separators of the multipolar type have proved of great
utility in purifying some classes of zinc ores, while the magnetic
tungsten materials, wolframite and ferberite, appear to lend
themselves particularly well to magnetic treatment. — M.
NEW SOURCE OF ALCOHOL
As a commercial possibility, says a contemporary, the nipa
palm, abounding in the swamps of the Philippine Islands, seems
to be unusually attractive, both as a producer of sugar and of
alcohol. Already a quantity of the sap is used by Manila
distillers in making what is regarded by many persons as the
best alcohol manufactured. It is claimed that nipa furnishes
the cheapest raw material in the world for the manufacture of
alcohol and that denatured alcohol made in this way is a fuel
for gasoline motors which is cheaper than gasoline and fully as
efficient. It is further stated that with a motor built for the use
of alcohol this fuel would be twenty to thirty per cent better
than gasoline. There are over one hundred thousand acres of
nipa swamp now available in the Archipelago, of which about
90 per cent have never been touched, and it is estimated that
the untapped swamp area of the island would yield fifty million
gallons of alcohol fuel every season. — M.
NEW RUST PREVENTION
According to Metal Industry, 11 (1917), 527, a new rust
prevention process recommended for small machine parts is
an application to the surface of the iron or steel of iron phosphates.
After thorough (leaning, the articles are immersed in a bath
containing ferric and ferrous phosphates with a little manganese
dioxide and, at boiling water temperature, they are left until
hydrogen is no longer given off. The articles are then ail
dried when they may he treated with mineral oil or painted,
japanned or otherwise finished. As the phosphate surface is
attached chemically to the metal no rust forms even in cracks
in the paint. — M.
TRANSVAAL DEPOSITS OF CHROME ORE AND
MAGNESITE
The British Trade Commissioner in South Africa reports the
discovery of deposits of chrome ore and magnesite on a farm
situated on the Oliphants River, Lydenberg District, Northern
Transvaal. Reliable authorities report the existence of both
minerals in large bodies and of high quality. This is understood
to be the first important discovery of chrome ore in South
Africa outside of Rhodesia. The ore yields 44.6 per cent Cr203,
besides iron and magnesium oxide. The magnesite shows the
following analysis: MgO = 45.75 per cent, CO2 = 49.17 per
cent, with silica, lime, iron oxide and alumina. It is said to be
almost equal to the best Greek magnesite. The area of the
reefs in question extends to more than 3,000 acres. — M.
NEW OIL NUTS
"Tucan" or "large Panama" kernels are harder and tougher
than palm kernels or copra, and, according to the Times Trade
Supplement, yield 37 to 48 per cent of a cream-colored and fairly
hard fat resembling palm kernel oil, but having a slightly higher
melting point. The residual meal is inferior to coconut or palm
kernel meal and is likely to be indigestible judging by the tough-
ness of the kernels. The kernels are said to be sold at a cheaper
rate than fine palm kernels. "Paraguay" kernels are small and
round and weigh about 28 to the oz. The skin of the kernels is
almost as black and the flesh is softer than that of the palm
kernels. They contain 65 per cent of fat which is softer than
coconut or palm oil and is only semi-solid at ordinary tempera-
tures. The residual meal is richer in proteins than coconut cake
and should have a high feeding value. The market value of the
kernels would be a little above that of palm kernels and below
that of copra. There does not seem to be any particular diffi-
culty in the way of exploiting either of these nuts. The shells
can be cracked by machinery such as is used for palm nuts in
West Africa. — M.
CATALYTICAL BLEACHING OF OILS
The use of catalytic agents, such as finely divided nickel in
the hydrogenation of oils, says the Oil and Color Trade Journal,
53 (1918), 123, having proved so successful, it is probable that
the employment of them in other directions may follow as a
matter of course. In the bleaching of oils, for instance, catalytic
agents such as finely divided lead and animal charcoal have
been of service, as well as oleate of manganese, etc. In a paper
recently published in a contemporary, experiments were de-
scribed showing the influence of several catalytic agents upon
tallow, palm oil and beeswax when a current of air is blown
through the melted material. The catalysts employed were
air-bleached palm oil, oleates of manganese, copper, cobalt,
lead, iron and nickel, the silkstone soap of A. Finlay and Company,
Belfast, and the cobalt soap preparation from the latter. In
the case of the palm oil, bleaching occurred both with and with-
out the catalysts, but with the latter the time requisite for
bleaching was shortened, especially with cobalt and manganese
salts. The experiments with beeswax and tallow were not so
successful. — M.
GAS-HEATED ISOTHERMAL ROOM
In the Physical Institute of Konigsberg, a constant tempera
ture room had been made by providing double walls with insu-
lating layers. The room, however, proved damp in summer,
dry in winter, but never comfortable. It was heated by hot
water pipes. A gas heater with automatic control has been
added and a pleasant temperature is maintained within 0.040 C.
The electrically controlled gas valve, which is described by
(, Hoffmann in the Physikalische Zeitschrifl of July 15. '9>7.
has the shape of a U. The limbs are wound with coils like an
3U
THE JOURNAL OF INDUSTRIAL AND ENGINEERING I HEMISTRY Vol. 10, Xo.
electro-magnet and the passage connecting the two limbs at the
bottom is closed when the magnet is energized and a plate raised.
A small pilot jet is always left burning and the control is effected
by a spiral built up of strips of zinc and iron like a compensating
pendulum. The spiral ends in a contact arm, bearing against
an adjustable screw. The device is inserted in a shunt of the
lighting circuit and the gas when the temperature sinks below
the normal. The device thus operates intermittently and keeps
the temperature within the limits 18.10 and 18.2 ° C. [Com-
pare This Journal, 10 (1918), 38.] — M.
MAGNETO IGNITION
According to the Gas World, 68 (1918), 11, it is true that con-
tinued use tends to strengthen the permanent magnetism in
a magneto machine and not to weaken it, as is generally supposed
to be the case. It is, therefore, very rarely necessary to re-
magnetize the steel pole pieces and usually only when the instru-
ment has been exposed to undue heat. Apart from defects due
to over-lubrication or lack of lubrication or wear of incorrectly
designed bearings or dirty contacts of the brush-gear, experience
has shown that very little trouble indeed arises so far as magneto
construction is concerned. Ignition difficulties far more fre-
quently result from broken wires, dirty contacts, incorrect
timing due to wear of pins and catch points, or worn make-or-
break sparking points, if low tension machines are employed, or
too large a spark gap or defective insulation of the plug, if of
high tension type. Cases are occasionally met with, where,
in a gas engine room, two or more displaced magnetos are to be
seen and it would surprise the owners of such engines if they
were made to realize how these could be set to work equal to
new with a very slight amount of overhauling. — M.
DETACHABLE ENGINES FOR SHIPS
The idea of an "economic ship" proposed by Mr. H. de M. Snell,
says the Times Engineering Supplement, is to have the propelling
machinery detachable, so that it may be moved from hull to
hull, his estimate being that one set would serve for three hulls,
or even for five or six in the case of coastwise or cross-channel
traffic. For propulsion he would employ electric drive, the cur-
rent being derived from alternators worked by oil engines or
steam turbines. The motors and reduction gearing would re-
main permanently in the ship but the generating plant would
be held in place by mechanical attachments which would be
secured or released in a few seconds, and would collectively be
able to resist a working stress of over 1000 tons. A pamphlet
dealing with the proposal shows designs for four ships rang-
ing in carrying capacity from 1,200 to over 10,000 tons.
In some cases, the "electromobile," as the power unit is termed,
contains accommodation for officers and engineers in addition
to the machinery, and is sometimes placed amidships and some-
times on the poop. Its transference from one hull to another
will be effected at the terminal ports by means of pontoons.
Among the advantages Mr. Snell claims for his scheme are that
it would mean a large saving in capital outlay for a given carrying
capacity, with a reduction in the interest charges and in the cost
of wages of officers and crews; that it would effect a great saving
in the time and labor required for construction, particularly in
the case of the machinery; and that the area of the machinery
exposed to damage by submarine or mine would be reduced to a
minimum. — -M.
SYNTHETIC MATERIALS
Numerous synthetic perfumes, says the Oil and Color Trade
Journal, 53 (1918), 209, are getting very scarce and are hardly
obtainable on the spot. Forward orders for aubepine are being
declined owing to the scarcity of the raw materials necessary.
As much as $19 has been paid for small parcels. Coumarin.
of which supplies are very short, is offered without engagement
to come forward at $39 and, on the spot, as much as $40 has
been asked and paid. Heliotropine has further advanced and
at $8 is regarded as cheap. Bromo-styrol and vanillin are scarce
and very dear, but methyl salicylate and benzaldehyde are
rather easier and more plentiful. Phenylmethyl alcohol is
$31.50 to $37.50 according to quality, there being several grades
of this article to be found at present on the market. — M.
INSULATING MATERIAL
An insulating material lately patented is composed of 52 per
cent pulverized asbestos, 14 per cent sifted mica, 20 per cent
mineral caoutchouc, 10 per cent rubber solution, 3 per cent
sulfur and 1 per cent resin. The proportions can be varied as
required. The mixture is hard, claimed to be almost incombusti-
ble, can be molded and wrought and, for insulation and other
purposes, it is proposed as a substitute for porcelain, marble,
slate, and vulcanized substances. — M.
LAMINATED BELTING
The introduction of high-speed steel, says the Times Engineering
Supplement, has demonstrated the necessity of increasing
the power of machine tools and has emphasized the need for
the highest efficiency possible in the transmission of the power
required to drive them. The Tullis protection edge laminated
belt, which has been designed to suit the new conditions, with
certain machine tool drives, is claimed to be efficient, because
it transmits the full power without slip, and economical be-
cause it gives a longer life and increases the output of the tool.
With the usual laminated belting the constant contact with
the belt forks cuts up the outside strands and, though the center
strands may still be in excellent condition, before the belt can
again be put into order, it has to be completely taken down
and reassembled with new outer strands. In the Tullis belt
the patent edge is designed to resist the action of the forks,
with increase in the life of the belt. The edge also binds the
threads which hold the strands together in such a manner
that even if one of the stitches becomes cut or broken the others
are not affected. The ends of the strands are drawn together
by pins which are removed as the cross sewing progresses.
When this is complete the edges are sewn down. As an alterna-
tive to sewing the edges, they may be held together by ordinary
metal clasps, which is a quicker method and makes a simple
joint. — M.
BRITISH BOARD OF TRADE
During the month of January the British Board of Trade re-
ceived inquiries from firms in the United Kingdom and abroad
regarding sources of supply for the following articles. Firms
which may be able to supply information regarding the things
are requested to communicate with the Director of the Com-
mercial Intelligence Branch, Board of Trade, 73 Basinghall St,
London, E. C.
FOR:
Machinery and Pl
Tarring fcit
Making oilskin
Splitting ostrich quills for making
Charcoal, nut, lump and flake
Copper tubes, made by electrolytic
process
brushes^-scrubbing brushesand Die-casting machines
dandy brushes Dies for die-casting machines
AUbrn"iofp°rotrahce,or"he1,cnUm- ^ectxo-deposition of copper for
Coloring typewriter ribbon. vinous purposes as a substj-
Covering copper wire for magnets ,u,c for castings
with insulating material, the Electro-tinning plant
wire to be drawn through a Hollow stMl w- suitabie for
liquid mature with rubber as a production of hypodermic needle.
Manufacturing macaroni, vermi- Light mineral oil (182.600 gal.)
celli Paraffin oil lamps, cheap; glass or
Manufacturing surgical needles china
Pin-making (safety and ordinary) R photographic paper
Appliances for removing the _. v ' v * "^
husks of almonds or nuts Tinder lighters
when being blanched Ultramarine blue
— M.
Apr., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
3i5
5CILNTIFIC SOCIETIES
TENTATIVE STANDARD METHODS FOR THE SAMPLING
AND ANALYSIS OF COMMERCIAL FATS AND OILS
Adopted September 22, 1916, and January 13, 19181
The following methods have been adopted by the Committee
on the Analysis of Commercial Fats and Oils of the Division of
Industrial Chemists and Chemical Engineers of the American
Chemical Society as tentative standards for the use of the
trade, pending their official adoption by the American Chemical
Society.
They are the result of three years of continuous and conscien-
tious effort on the part of the Committee and they have given
excellent satisfaction in the hands of the members of the Com-
mittee and others who have used them, and have been found
to answer the commercial needs of the fat and oil industry in a
satisfactory manner.
They are published for the purpose of adoption by any con-
tracting parties so desiring and for the purpose of eliciting
suggestions and criticisms from fat and oil chemists. Com-
munications on the subject of the methods should be addressed
to W. D. Richardson, c/o Swift and Company, Chicago,
and will be presented to the Committee at their regular monthly
meeting next following.
The Committee is now work ing on methods for cold and flow
tests, melting point, and moisture in oils of the coconut group
in the presence of free acids.
SAMPLING
TANK CARS
i. sampling WHn-E loading — Sample shall be taken at dis-
charge of pipe where it enters tank car dome. The total sample
taken shall be not less than 50 lbs. and shall be a composite of
small samples of about 1 pound each, taken at regular intervals
during the entire period of loading.
The sample thus obtained is thoroughly mixed and uniform
3-lb. portions placed in air-tight 3-lb. metal containers. At
least three such samples shall be put up, one for the buyer,
one for the seller, and the third to be sent to a referee chemist
in case of dispute. All samples are to be promptly and correctly
labeled and sealed.
2. sampling from car on track2 — (a) When contents are
solid.' In this case the sample is taken by means of a large
tryer measuring about 2 in. across and about 1 l/i times the depth
of the car in length. Several tryerfuls are taken vertically
and obliquely toward the ends of the car until 50 lbs. are accumu-
lated, when the sample is softened, mixed and handled as under
(1). In case the contents of the tank car have assumed
a very hard condition, as in winter weather, so that it is impos-
sible to insert the tryer and it becomes necessary to soften the
contents of the car by means of the closed steam coil (in nearly
all tank cars the closed steam coil leaks) or by means of open
steam in order to draw a proper sample, suitable arrangements
must be made between buyer and seller for the sampling of the
Car after it is sufficiently softened, due consideration being
given to the possible presence of water in the material in the car
as received and also to the possible addition of water during the
steaming. The Committee knows of no direct method for
sampling a hard-frozen tank car of tallow in a satisfactory
manner.
(6) When contents are liquid. The sample taken is to be
a 50-lb. composite made up of numerous small samples taken
from the top, bottom and intermediate points by means of a
bottle or metal container with removable stopper or top. This
1 Published by the Committee February 1918. Superseding and can-
celling previous i-sues.
1 Live steam must not be turned into tank cars or coils before samples
are drawn, since there is no certain way of telling when coils are free from
leaks.
1 If there is water present under the solid material this must be noted
and estimated separately.
device attached to a suitable pole is lowered to the various de-
sired depths when the stopper or top is removed and the container
allowed to fill. The 50-lb. sample thus obtained is handled as
under ( 1 ) .
(c) When contents are in semi-solid condition, or when stearins
has separated from liquid portions. In this case a combination
of (a) and (b) may be used or by agreement of the parties the
whole may be melted and procedure (b) followed.
BARRELS, TIERCES, CASKS, DRUMS, AND OTHER PACKAGES
All packages shall be sampled, unless by special agreement
the parties arrange to sample a lesser number; but in any case
not less than 10 per cent of the total number shall be sampled.
The total sample taken shall be at least 20 lbs. in weight for each
100 barrels, or equivalent.
1. barrels, tierces and casks — (a) When contents are
solid. The small samples shall be taken by a tryer through
the bunghole or through a special hole bored in the head or side
for the purpose, with a i-in. or larger auger. Care should be
taken to avoid and eliminate all borings and chips from the sam-
ple. The tryer is inserted in such a way as to reach the head
of the barrel, tierce, or cask. The large sample is softened,
mixed and handled according to tank cars (1).
(b) When contents are liquid. In this case use is made of a
glass tube with constricted lower end. This is inserted slowly
and allowed to fill with the liquid, when the upper end is closed
and the tube withdrawn, the contents being allowed to drain
into the sample container. After the entire sample is taken
it is thoroughly mixed and handled according to tank cars (i).
(c) When contents are semi-solid. In this case the tryer
or a glass tube with larger outlet is used, depending on the de-
gree of fluidity.
(d) Very hard materials, such as natural and artificial stea-
rines. By preference the barrels are stripped and samples ob-
tained by breaking up contents of at least 10 per cent of the pack-
ages. This procedure is to be followed also in the case of cakes
shipped in sacks. When shipped in the form of small pieces
in sacks they can be sampled by grab sampling and quartering.
In all cases the final procedure is as outlined under tank cars
(1).
2. drums — Samples are to be taken as under (i)» use being
made of the bunghole. The tryer or tube should be sufficiently
long to reach to the ends of the drum.
3. OTHER packages — Tubs, pails and other small packages
not mentioned above are to be sampled by tryer or tube (depend-
ing on fluidity) as outlined above, the tryer or tube being in-
serted diagonally whenever possible.
4. mixed lots and packages — When lots of tallow or other
fats are received in packages of various shapes and sizes, and
especially wherein the fat itself is of variable composition, such
must be left to the judgment of the sampler. If variable, the
contents of each package should be mixed as thoroughly as pos-
sible and the amount of the individual samples taken made pro-
portional to the sizes of the packages.
ANALYSIS
SAMPLE
The sample must be representative and at least three pounds
in weight and taken in accordance with the standard methods
FOR THE SAMPLING OF COMMERCIAL FATS AND OILS. It must
be kept in an air-tight container in a dark, cool place.
Soften the sample if necessary by means of a gentle heat,
taking care not to melt it. When sufficiently softened, mix
the sample thoroughly by means of a mechanical egg beater
or other equally effective mechanical mixer.
moisture and volatile matter
apparatus: Vacuum Oven— The committee Standard Oven.
description— The Standard P. A. C. Vacuum Oven has been
designed with the idea of affording a simple and compact vacuum
3i6
THE JOURNAL OF INDl SI KIM. AND ENGINEERING < HEMISTRY Vol. 10, No. 4
oven which will give as uniform temperatures as possible on the
shelf. As the figure shows, it consists of an iron casting of rec-
tangular sections with hinged front door made tight by means
of a gasket and which can be lowered on opening the oven so
as to form a shelf on which samples may be rested. The oven
contains but one shelf which is heated from above as well as
below by means of resistance coils. Several thermometer
holes are provided in order to ascertain definitely the tempera-
ture at different points on the shelf. In a vacuum oven where
the heating is done almost entirely by radiation it is difficult
to maintain uniform temperatures at all points, but the F. A. C.
oven accomplishes this rather better than most vacuum ovens.
Larger ovens containing more than one shelf have been tried
by the Committee, but have been found to be lacking in tempera-
ture uniformity and means of control. The entire oven is sup-
ported by means of a 4-in. standard pipe which screws into the
base of the oven and which in turn is supported by being screwed
into a blind flange of suitable diameter which rests on the floor
or work table.
Moisture Dish — A shallow, glass dish, lipped, beaker form,
approximately 6 to 7 cm. diameter and 4 cm. deep shall be stand-
ard.
determination — Weigh out 5 grams (±0.2 g.) of the pre-
pared sample into a moisture dish. Dry to constant weight
in vacuo at a uniform temperature, not less than 15' C, not
more than 20 ° C. above the boiling point of water at the working
pressure, which must not exceed 100 mm. of mercury.1 Con-
stant weight is attained when successive dryings for i-hr. periods
show an additional loss of not more than 0.05 per cent. Re-
port loss in weight as MOISTURE and volatile matter.2
The vacuum oven method cannot be considered accurate in
the case of fats of the coconut oil group containing free acid and
the Committee recommends that it be used only for oils of this
group when they contain less than 1 per cent free acid. In
1 Boiling point of Water at reduced pr.
Pressure
mm. Hg
100
4(1
Boiling point Boiling point
+ 15*0. + 20°C.
34
4''
54
2 Results comparable to those of the Standard Method may be ob-
tained on most fats and oils by drying 5-gram portions of the sample, pre-
pared and weighed as above, to constant weight in a well-constructed and
well-ventilated air oven held uniformly at a temperature of 105-110° C.
The thermometer bulb should be close to the sample. The definition of
constant weight is the same as for the Standard Method.
JBrvcket on Hinges
Standard Fat ANALYSIS Co
OVKN FOR DKTKKMIMN.. MoiSTlKK
Volatile Matter in Fats and Oils
Apr., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
317
the case of oils of this group containing more than 1 per cent
free acid, recourse should be had temporarily to the routine
control method for moisture and volatile matter1 until the Com-
mittee develops a more satisfactory method.
The air-oven method cannot be considered even approximately
accurate in the case of the drying and semi-drying oils and those
of the coconut oil group. Therefore, in the case of such oils as
cottonseed oil, maize oil (corn oil), soy bean oil, linseed oil,
coconut oil, palm kernel oil, etc., the vacuum-oven method
should always be used, except in the case of fats of the coconut
group containing more than 1 per cent free acid, as noted above.
INSOLUBLE IMPURITIES
Dissolve the residue from the moisture and volatile matter
determination by heating it on a steam bath with 50 cc. of kero-
sene. Filter the solution through a Gooch crucible properly
prepared with asbestos,2 wash the insoluble matter five times
with 10-cc. portions of hot kerosene, and finally wash the residual
kerosene out thoroughly with petroleum ether. Dry the cruci-
ble and contents to constant weight as in the determination of
moisture and volatile matter and report results as insoluble
impurities.
soluble mineral matter
Place the combined kerosene filtrate and kerosene washings
from the insoluble impurities determination in a platinum dish.
Place in this an ashless filter paper folded in the form of a cone,
apex up. Light the apex of the cone, whereupon the bulk of the
kerosene burns quietly. Ash the residue in a muffle, to constant
weight, taking care that the decomposition of carbonates is
complete, and report the result as soluble mineral matter.3
When the percentage of soluble mineral matter amounts to more
than 0. 1 per cent, multiply the percentage by 10 and add this
amount to the percentage of free fatty acids as determined.
free fatty acids
The alcohol* used shall be approximately 95 per cent ethyl
alcohol, freshly distilled from sodium hydroxide, which with
phenolphthalein gives a definite and distinct end-point.
determination — Weigh 1 to 15 g. of the prepared sample
into an Erlenmeyer flask, using the smaller quantity in the case
of dark-colored, high acid fats. Add 50 to 100 cc. hot, neutral
alcohol, and titrate with N/2, N/4, or N/10 sodium hydroxide,
depending on the fatty acid content, using phenolphthalein
as indicator. Calculate to oleic acid, except that in the case
of palm oil the results may also be expressed in terms of palmitic
acid, clearly indicating the two methods of calculation in the
report. In the case of coconut and palm kernel oils, calculate
to and report in terms of lauric acid in addition to oleic acid,
clearly indicating the two methods of calculation in the report.
In the case of fats or greases containing more than o. 1 per cent
1 The following method is suggested by the Committee for routine
control work: Weigh out 5- to 25-gram portions of prepared sample into
a glass or aluminum (Caution: Aluminum soap may be formed) beaker or
casserole and heat on a heavy asbestos board over burner or hot plate,
taking care that the temperature of the sample does not go above 130° C.
at any time. During the heating rotate the vessel gently on the board
by hand to avoid sputtering or too rapid evolution of moisture. The proper
length of time of heating is judged by absence of rising bubbles of steam,
by the absence of foam or by other signs known to the operator. Avoid
overheating of sample as indicated by smoking or darkening. Cool in
desiccator and weigh.
' For routine control work, filter paper is sometimes more convenient
than a prepared Gooch crucible. It must be very carefully washed to re-
move the last traces of fat. especially the rim.
* For routine work, an ash may be run on the original fat, and the solu-
ble mineral matter obtained by deducting the ash on the insoluble impuri-
ties from this. In this case the Gooch crucible should be prepared with an
ignited asbestos mat so that the impurities may be ashed directly after being
weighed. In all cases ignition should be to constant weight so as to insure
complete decomposition of carbonates.
• For routine work methyl or denatured ethyl alcohol of approximately
9S per cent strength may be used. With these reagents the end-point is
not sharp.
of soluble mineral matter, add to the percentage of free fatty
acids as determined 10 times the percentage of soluble mineral
matter as determined. This addition gives the equivalent of
fatty acids combined with the soluble mineral matter.
titer
standard thermometer — The thermometer is graduated
at zero and in tenth degrees from io° C. to 65 ° C, with one auxil-
iary reservoir at the upper end and another between the zero
mark and the 10° mark. The cavity in the capillary tube be-
tween the zero mark and the 10° mark is at least 1 cm. below
the io° mark, the io° mark is about 3 or 4 cm. above the bulb,
the length of the thermometer being about 37 cm. over all.
The thermometer has been annealed for 75 hrs. at 450 ° C. and
the bulb is of Jena normal 16'" glass, or its equivalent, moder-
ately thin, so that the thermometer will be quick-acting. The
bulb is about 3 cm. long and 6 mm. in diameter. The stem of
the thermometer is 6 mm. in diameter and made of the best
thermometer tubing, with scale etched on the stem, the gradua-
tion is clear-cut and distinct, but quite fine. The thermometer
must be certified by the U. S. Bureau of Standards.
glycerol caustic solution — Dissolve 250 g. potassium
hydroxide in 1000 cc. dynamite glycerin with the aid of heat.
determination — Heat 75 cc. of the glycerol-caustic solution
to 150° C. and add 50 g. of the melted fat. Stir the mixture
well and continue heating until the melt is homogeneous, at no
time allowing the temperature to exceed 1500 C. Allow to cool
somewhat and carefully add 50 cc. 30 per cent sulfuric acid.
Now add hot water and heat until the fatty acids separate out
perfectly clear. Draw off the acid water and wash the fatty
acids with hot water until free from mineral acid, then filter
and heat to 1300 C. as rapidly as possible with stirring. Trans-
fer the fatty acids, when cooled somewhat, to a i-in. by 4-in.
titer tube, placed in a 16-oz. salt-mouth bottle of clear glass,
fitted with a cork that is perforated so as to hold the tube
rigidly when in position. Suspend the titer thermometer so
that it can be used as a stirrer and stir the fatty acids slowly
(about 100 revolutions per minute) until the mercury remains
stationary for 30 seconds. Allow the thermometer to hang
quietly with the bulb in the center of the tube and report the
highest point to which the mercury rises as the titer of the fatty
acids. The titer should be made at about 20° C. for all fats
having a titer above 300 C. and at 10° C. below the titer for all
other fats.
unsaponifiable matter
Extraction cylinder — The cylinder shall be glass-stoppered,
graduated at 40 cc, 80 cc. and 130 cc, and of the following
dimensions: diameter about i'/i rn., height about 12 in.
petroleum ETHER — Redistilled petroleum ether, boiling under
750 C, shall be used. A blank must be made by evaporating
250 cc. with about 0.25 g. of stearine or other hard fat (pre-
viously brought to constant weight by heating) and drying as
in the actual determination. The blank must not exceed a few
milligrams.
determination— Weigh 5 g. (±0.20 g.) of the prepared
sample into a 200-cc. Erlenmeyer flask, add 30 cc. of redistilled
95 per cent (approximately) ethyl alcohol and 5 cc of 50 per
hi aqueous potassium hydroxide, and boil the mixture for one
hour under a reflux condenser. Transfer to the extraction
cylinder and wash to the 40-CC. mark with redistilled 95 per cent
ethyl alcohol. Complete the transfer, first with warm, then
with cold water, till the total volume amounts to 80 cc. Cool
the cylinder and contents to room temperature and add 50 cc.
of |» troleum ether. Shake vigorously for one minute and allow
to wale until both layers are clear, when the volume of the
upper layer should be about 40 cc. Draw off the petroleum
ether layer as closely as possible by means of a slender glass
siphon into a separatory funnel of 500 cc. capacity. Repeat
3 i !
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 4
extraction four more times, using 50 cc. of petroleum ether each
time. Wash the combined extracts in a separatory funnel three
times with 25-cc. portions of 10 per cent alcohol, shaking vigor-
ously each time. Transfer the petroleum ether extract to a
wide-mouth tared flask or beaker, and evaporate the petroleum
ether on a steam bath in an air current. Dry as in the method
for moisture and volatile MATTER. Any blank must be
deducted from the weight before calculating unsaponifiable
matter. Test the final residue for solubility in 50 cc. petroleum
ether at room temperature. Filter and wash free from the in-
soluble residue, if any, evaporate and dry in the same manner
as before. The Committee wishes to emphasize the necessity
of thorough and vigorous shaking in order to secure accurate
results. The two phases must be brought into the most inti-
mate contact possible, otherwise low and disagreeing results
may be obtained. When the unsaponifiable matter runs over
5 per cent, more extractions are recommended.
WITS METHOD FOR THE DETERMINATION OF IODINE VALUE
preparation OF reagents — Wijs Iodine Solution — (1) Dis-
solve separately 7.9 g. of iodine trichloride and 8.7 g. of iodine
in glacial acetic acid on the water bath, taking care that the solu-
tions do not absorb moisture. The two solutions are then
poured into a iooo-cc. flask and the flask is filled up to the mark
with glacial acetic acid.
Or (2) dissolve 6.5 g. of resublimed iodine in one liter of C. P.
glacial acetic acid and pass in washed and dried chlorine gas
until the original thiosulfate titration of the solution is just
doubled. This is then preserved in amber glass-stoppered
bottles, sealed with paraffin until ready for use.
N/10 Sodium Thiosulfate Solution — Dissolve 24.8 g. of C. P.
sodium thiosulfate and dilute with water to one liter at the
temperature at which the titrations are to be made.
Starch Paste — Boil 1 g. of starch in 200 cc. of distilled water
for 10 min. and cool to room temperature.
Potassium Iodide Solution — -Dissolve 150 g. of potassium iodide
in water and make up to one liter.
N/10 Potassium Bichromate — Dissolve 4.903 g. of C. P.
potassium bichromate in water and make the volume up to
one liter at the temperature at which titrations are to be made.
Standardization of the Sodium Thiosulfate Solution — Place
20 cc. of the potassium bichromate solution, to which has been
added 10 cc. of the solution of potassium iodide, in a glass-stop-
pered flask. Add to this 5 cc. of strong hydrochloric acid.
Dilute with 100 cc. of water, and allow the N/10 sodium thio-
sulfate to flow slowly into the flask until the yellow color of the
liquid has almost disappeared. Add a few drops of the starch
paste, and with constant shaking continue to add the N/10
sodium thiosulfate solution until the blue color just disappears.
determination — Weigh accurately from 0.10 to 0.50 g.
(depending on the iodine number) of the melted and filtered
sample into a clean, dry, 16-oz. glass-stoppered bottle containing
15-20 cc. of carbon tetrachloride or chloroform. Add 25 cc.
of iodine solution from a pipette, allowing to drain for a definite
time. The excess of iodine should be from 50 per cent to 60
per cent of the amount added, that is, from 100 per cent to 150
per cent of the amount absorbed. Moisten the stopper with a
10 per cent potassium iodide solution to prevent loss of iodine
or chlorine but guard against an amount sufficient to run down
inside the bottle. Let the bottle stand in a dark place for '/«
hr. at a uniform temperature. At the end of that time add 20
cc. of 10 per cent potassium iodide solution and 100 cc. of dis-
tflled water. Titrate the iodine with 7V/io sodium thiosulfate
solution which is added gradually, with constant shaking, un-
til the yellow color of the solution has almost disappeared
Add a few drops of starch paste and continue titration until
the blue color has entirely disappeared. Toward the end of
the reaction stopper the bottle and shake violently so that any
iodine remaining in solution in the tetrachloride or chloroform
may be taken up by the potassium iodide solution. Conduct
two determinations on blanks which must be run in the same
manner as the sample except that no fat is used in the blanks.
Slight variations in temperature quite appreciably affect the
titer of the iodine solution, as acetic acid has a high coefficient
of expansion. It is, therefore, essential that the blanks and
determinations on the sample be made at the same time. The
number of cc. of standard thiosulfate solution required by the
blank, less the amount used in the determination, gives the thio-
sulfate equivalent of the iodine absorbed by the amount of sam-
ple used in the determination. Calculate to centrigrams of
iodine absorbed by 1 g. of sample (= per cent iodine absorbed).
saponification number (koettstorfer number)
preparation of reagents— A" 2 Hydrochloric Acid — Care-
fully standardized.
Alcoholic Potassium Hydroxide Solution — Dissolve 40 g. of
pure potassium hydroxide in one liter of 95 per cent redistilled
alcohol (by volume). The alcohol should be redistilled from
potassium hydroxide over which it has been standing for some
time, or with which it has been boiled for some time, using a
reflux condenser. The solution must be clear and the potas-
sium hydroxide free from carbonates.
determination — Weigh accurately about 5 g. of the filtered
sample into a 250 to 300 cc. Erlenmeyer flask. Pipette 50 cc.
of the alcoholic potassium hydroxide solution into the flask,
allowing the pipette to drain for a definite time. Connect the
flask with an air condenser and boil until the fat is completely
saponified (about 30 minutes). Cool and titrate with the N/2
hydrochloric acid, using phenolphthalein as an indicator. Cal-
culate the Koettstorfer number (mg. of potassium hydroxide
required to saponify 1 g. of fat). Conduct 2 or 3 blank deter-
minations, using the same pipette and draining for the same
length of time as above.
NOTES ON THE ABOVE METHODS
SAMPLING
The standard size of sample adopted by the Committee is
at least 3 lbs. in weight. The Committee realizes that this
amount is larger than any samples usually furnished even when
representing shipments of from 20,000 to 60,000 lbs., but it be-
lieves that the requirement of a larger sample is desirable and
will work toward uniform and more concordant results in anal-
ysis. It will probably continue to be the custom of the trade
to submit smaller buyers' samples than required by the Com-
mittee, but these are to be considered only as samples for in-
spection and not for analysis. The standard analytical sample
must consist of 3 lbs. or more.
The reasons for keeping samples in adark, cool place are obvious.
This is to prevent any increase in rancidity and any undue in-
crease in fatty acids. In the case of many fats the Committee
has found in its cooperative analytical work that free acid tends
to increase very rapidly. This tendency is minimized by low
temperatures.
MOISTURE AND VOLATILE MATTER
After careful consideration the Committee has decided that
moisture is best determined in a vacuum oven of the design
which accompanies the above report. Numerous results on
check samples have confirmed the Committee's conclusions.
The oven recommended by the Committee is constructed on
the basis of well-known principles and it is hoped that this type
will be adopted generally by chemists who are called upon to
analyze fats and oils. The experiments of the Committee in-
dicate that it is a most difficult matter to design a vacuum oven
which will produce uniform temperatures throughout; and one
of the principal ideas in the design adopted is uniformity of tem-
perature over the entire single shelf. This idea has not quite
been realized in practice but, nevertheless, the present design
approaches much closer to the ideal than other vacuum ovens
Apr., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
3i9
•commonly used. In the drawing the essential dimensions
are those between the heating units and the shelf and the
length and breadth of the outer easting. The standard Fat
Analysis Committee oven (F. A. C. oven) can be furnished by
Messrs. E. H. Sargent & Company, 125 West Lake Street,
Chicago.
The Committee realizes that for routine work a quicker method
is desirable and has added one such method and has also stated
the conditions under which comparable results can be obtained
by means of the ordinary well-ventilated air oven held at 105
to no" C. However, in accordance with a fundamental prin-
ciple adopted by the Committee at its first meeting, only one
standard method is adopted and declared official for each de-
termination.
The Committee realizes that in the case of all methods for
determining moisture by means of loss on heating there
may be a loss due to volatile matter (especially fatty acids)
other than water. The title of the determination moisture
and volatile matter indicates this idea, but any considera-
ble error from this source may occur only in the case of high
acid fats and oils and particularly those containing lower fatty
acids such as coconut and palm kernel oil. work on which is now
in progress to be reported at a later date. In the case of ex-
tracted greases which have not been properly purified, some
of the solvent may also be included in the moisture and volatile
matter determination, but inasmuch as the solvent, usually a
petroleum product, can only be considered as foreign matter,
for commercial purposes, it is entirely proper to include it with
the moisture. The Committee has also considered the various
distillation methods for the determination of moisture in fats
and oils, but since according to the fundamental principles
which it was endeavoring to follow it could only standardize
one method, it was decided that the most desirable one on the
whole was the vacuum-oven method as given. There are cases
wherein a chemist may find it desirable to check a moisture de-
termination or investigate the moisture content of a fat or oil
further by means of one of the distillation methods.
INSOLUBLE IMPURITIES
This determination, the title for which was adopted after
■careful consideration, determines the impurities which have
generally been known as dirt, suspended matter, suspended solids,
foreign solids, foreign matter, etc., in the past. The first sol-
vent recommended by the Committee is hot kerosene to be fol-
lowed by petroleum ether kept at ordinary room temperature.
Petroleum ether, cold or only slightly warm, is not a good fat
and metallic soap solvent, whereas hot kerosene dissolves these
substances readily, and for this reason the Committee has recom-
mended the double solvent method so as to exclude metallic
soaps which are determined below as soluble mineral matter.
SOLUBLE MINERAL MATTER
Soluble mineral matter represents mineral matter combined
with fatty acids in the form of soaps in solution in the fat or
oil. Formerly, this mineral matter was often determined in
combination by weighing the separated metallic soap or by
weighing it in conjunction with the insoluble impurities. Since
the soaps present consist mostly of lime soap, it has been cus-
tomary to calculate the lime present therein by taking 0.1 the
Weight of the total metallic soaps. The standard method as
given above is direct and involves no calculation. The routine
method given in the note has been placed among the methods,
although not adopted as a standard method for the reason that
it is in use in some laboratories regularly. It should be pointed
Out, however, that the method cannot be considered accurate
for the reason that insoluble impurities may vary from sample
to sample to a considerable extent and the error due to the pres-
ence of large particles of insoluble impurities is thus trans-
ferred to the soluble mineral matter.
FREE FATTY ACID
The fatty acid method adopted is sufficiently accurate for com-
mercial purposes. In many routine laboratories the fat or oil
is measured and not weighed, but the Committee recommends
weighing the sample in all cases. For scientific purposes the
result is often expressed as "acid number," meaning the number
of milligrams of KOH required to neutralize the free acids in
one gram of fat, but the commercial practice has been, and is,
to express the fatty acids as oleic acid or in the case of palm oil,
as palmitic acid, in some instances. The Committee sees no
objection to the continuation of this custom so long as the ana-
lytical report clearly indicates how the free acid is expressed.
For a more exact expression of the free acid in a given fat, the
Committee recommends that the ratio of acid number to saponi-
fication number be used. This method of expressing results is
subject to error when unsaponifiable fatty matter is present,
since the result expresses the ratio of free fatty acid to total
saponifiable fatty matter present.
TITER
At the present time the prices of glycerol and caustic potash
are abnormally high but the Committee has considered that
the methods adopted are for normal times and normal prices.
For routine work during the period of high prices the following
method may be used for preparing the fatty acids and is recom-
mended by the Committee:
50 grams of fat are saponified with 60 cc. of a solution of 2
parts of methyl alcohol to 1 of 50 per cent NaOH. The soap
is dried, pulverized and dissolved in 1000 cc. of water in a porce-
lain dish and then decomposed with 25 cc. of 75 per cent sulfuric
acid. The fatty acids are boiled until clear oil is formed and
then collected and settled in aiso-cc. beaker and filtered into a
50-cc. beaker. They are then heated to 130 ° C. as rapidly as
possible with stirring, and transferred, after they have cooled
somewhat, to the usual i-in. by 4-in. titer tube.
The method of taking the titer, including handling the ther-
mometer, to be followed is the same as that described in the
standard method. Even at present high prices many labora-
tories are using the glycerol-caustic potash method for preparing
the fatty acids, figuring that the saving of time more than com-
pensates for the extra cost of the reagents. Caustic soda can-
not be substituted for caustic potash in the glycerol method.
UNSAPONIFIABLE MATTER
The Committee has considered unsaponifiable matter to in-
clude those substances frequently found d.ssolved in fats and
oils which are not saponifierl by the caustic alkalies and which
at the same time are solubl in the ordinary fat solvents. The
term includes such substances as the higher alcohols, such as
cholesterol which is found in animal fats, phytosterol found in
some vegetable fats, paraffin and petroleum oils, etc. Unsapon-
IFIABLE MATTER should not be confused in the lay mind with
INSOLUBLE IMPURITIES OF SOLUBLE MINERAL MATTER.
The method adopted by the Committee has been selected
only after the most careful consideration of other methods,
such as the dry extraction method and the wet method making
use of the separatory funnel. At first consideration the dry ex-
traction process would seem to offer the best basis for an un-
saponifiable matter method, but in practice it has been found
absolutely impossible for different analysts to obtain agreeing
results when using any of the dry extraction methods proposed.
Therefore, this method had to be abandoned after numerous
trials, although several members of the Committee strongly
favored it in the beginning.
iodine number — The iodine number adopted by the Com-
mittee is that determined by the well-known Wijs method.
This method was adopted after careful comparison with the
Hanus and Hubl methods. The Hiibl method was eliminated
from consideration almost at the beginning of the Committee's
320
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. Xo. 4
work for the reason that the time required for complete absorp-
tion of the iodine is unnecessarily long and, in fact, even after
absorption has gone on over night, it is apparently not com-
plete. In the case of the Hanus and Wijs methods complete
absorption takes place in from 15 minutes to an hour, depend-
ing on conditions. Formerly, many chemists thought the
Hanus solution rather easier to prepare than the Wijs solution,
but the experience of the Committee was that the Wijs solu-
tion was no more difficult to prepare than the Hanus. Further-
more, absorption of iodine from the Wijs solution appeared to
take place with greater promptness and certainty than from the
Hanus and was complete in a shorter time. Results by the
Wijs method were also in better agreement in the case of oils
showing high iodine absorption than with the Hanus solution and
showed a slightly higher iodine absorption for the same length
of time. However, the difference was not great. The Com-
mittee investigated the question of substitution since it has
been suggested that in case of the Wijs solution substitution
of iodine in the organic molecule might occur, and found no
evidence of this in the time required for the determination,
namely, '/» nr . or even for a somewhat longer period. One
member of the Committee felt that it was not desirable to in-
troduce the Wijs method into these standard methods since
the Hanus method was already standardized by the Associa-
tion of Official Agricultural Chemists, but the Committee felt
that it must follow the principle established at the commence-
ment of its work, namely, that of adopting the method which
appeared to be the best from all standpoints, taking into con-
sideration accuracy, convenience, simplicity, time, espense,
etc., without allowing precedent to have the deciding vote.
SAVING FATS FROM GARBAGE
On February 23rd Secretary' Parsons offered the assistance of
the American Chemical Society to the United States Food
Administration in a campaign for the recovery of fats from
garbage. The following reply was received:
Washington-, D. C,
March 5, 1918
Mr. Charles L. Parsons,
American Chemical Society,
Washington, D. C.
Dear Sir: Beg to acknowledge receipt of your letter of
February 23rd and am to-day sending the enclosed letter to
the following nun. with reference to cities named:
A. D. Camp, Cleveland, Ohio
Cleveland, East Cleveland, El-
yria. I.oraine, Akron, Canton.
Youngstown
// /. OK*, Columbus. 1
Columbus. Dayton
A'. J. Quinn, Chicago, III.
Chicago, in
A'. /'. Calvert, Wilmington. Del.
Wilmington, Del.
L. B. Case, Dlrott
Detroit, Mich,
A. J. Salalhe. Schenectady. -V. 1'.
Schenectady, 1 tica
H. W.Rhodemamel.lndianapolis.lnd.
Indianapolis. Fort Wayne
£. C. Stone. Barlford, Conn.
Bridgeport. Conn
Sheppard 7". Powell. Baltimore, lid.
Baltimore, Md.
J. II Graham, Philadelphia, Pa.
Philadelphia. York. Ta Atlantic
City. X. J
Charles F. Rolh, Ntw York City
Neil York City
D.r.ul II Childs, Buffalo. X . V.
Buffalo. N\ Y
i ( itcKthey, Washington, D. C.
Washington, D. C.
E. Schragenheim, Toledo, Ohio
Toledo. Ohio
J. XI. Johltn. Jr., Syracuse, N 1
Syracuse, N. Y.
I. F. Sickell. St. Louis. ito.
St. Louis. M"
R, .;,.:',. ,\ 1
Rochester, N Y
R. it. ilenve, Pittsburgh. Pa.
Pittsburgh, Braddock. YVilkii
burg
S. T. Arnold. Providence. R. I.
Boston. New Bedford. Mass.
Henry L.Payne. Los Angeles. Cal.
Los Angeles, Cal.
it. C. Sneed. Cincinnati, Ohio
Cincinnati. Ohio
Trusting that the procedure outlined meets with your approval
and that you, too, will assist in any way possible to carry out the
policy indicated, we are
Very truly yours,
; Food Administration
(Signed) F. C Bamman
Garbage Utilization Division
Dear Slr:
The Secretary of the American Chemical Society, Mr.
Charles L. Parsons, has kindly offered the assistance of your
Society in a campaign for saving fats from garbage.
We have recently called the attention of certain of our State
Administrators to the fact that garbage reduction plants within
their respective states were adding to our valuable resources by
the recovery of grease and fertilizer tankage; that on an average
there was being recovered per annum from the garbage produced
by a family of four, sufficient glycerine to furnish, as nitro-
glycerine, the powder charge of three 75 mm. shells, enough fatty
acids for about fifty cakes of soap, and ample fertilizing ele-
ments to replace the soil depletion of about three bushels of
wheat. We also furnished them with a data sheet of the present
extent of this industry, copy of which is attached hereto.
We suggested to the Food Administrators that an active
campaign be inaugurated to see that all garbage in cities
where such plants were available be utilized in such plants and
that private incinerators or the practice of burning garbage in
furnaces, etc., be eliminated.
Your city has a reduction plant available and anything you
can do to decrease the destruction of garbage will be deeply ap-
preciated.
We are also interested in securing the utilization of garbage in
cities not now utilizing their garbage but, with the prevalent
shortage of labor and material, the erection of new reduction
plants is extremely difficult and our main effort therefore in
such cities is to secure utilization by feeding. We understand,
however, that some cities are investigating disposal by reduction
and anything you can do to secure the introduction of this sys-
tem in such cities will likewise be of great assistance.
Very truly yours.
1 S. Food Administration
(Signed) F. C. Bamman
Garbage Utilization Division
The above list of cities includes all that are disposing of their
garbage by the reduction process at the present time.
2*> Cities Are Disposing of Garbage by Reduction
Total Population About 1 3. 200.000
Estimated present grease production 72.000.000 lbs.
This amount of grease will produce 10.000.000
lbs. of nitroglycerine, enough for the powder
charge of about 16.000,000 of our 3-in. shells
or the famous French 7^ mm, shells
The fatty acids it contains are sufficient for the
manufacture of about JOO.OOO.OOO twclve-
Bstimated present fertilizer tankage production 150.000 tons
This amount of tankage contains about 9,000,-
000 lbs. of nitrogen. J2.000.000 lbs. of phos-
phate of lime and 2.000.000 lbs of potash,
enough to replace the nitrogen and other ele-
ments taken from the soil by 3,000,000 bu. of
a heal
Estimated present value of the above amounts of
grease and fertilizer tanka ?1 1.100. 000
Estimated amount of garbage turn,; destroyed an-
nually in the above 29 cities 1^0,000 tons
Estimated amount of grease in the above 150,000
tons of garbage . ... 9.000.000 lbs.
This amoiyit of grease will produce about
hi lbs of nitroglycerine, immgh for the
powder charge of about 2,000.000 of our 3-in.
shells or the French 75 mm ■
The tatty acids it contains are sufficient for the
manufacture of about 25.000000 twelve-
ounce cakes of soap.
Estimated amount of fertilizer tankage in the above
1230,000 cons of 1 22,500 tons
This amount of fertilizer tankage contains
about 1,230,000 lbs of nitrogen 3 mki.ooo lbs.
of phosphate of lime and 350 000 lbs of potash,
enough for the replacement of the elements re-
moved from the soil by 1.000.000 bu of wheat.
Apr., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
321
AMERICAN INSTITUTE OF MINING ENGINEERS
The 1 16th Meeting of the American Institute of Mining En-
gineers was held in New York City, February 18 to 21, 1918.
PROGRAM OF PAPERS
NON-FERROUS METALLURGY
The Disadvantages of Chrome Brick in Copper Reverberatory Furnaces.
F. R. Pynb.
Fine-Grinding and Porous-Briquetting of the Zinc Charge. W. McA.
Johnson.
High-Temperature Resistance Furnaces with Ductile Tungsten or Molyb-
denum Resistors. W. E. Ruder.
Zinc Refining. I, E. Wemple
Bone-Ash Cupels. F. P. Dewey.
An Automatic Filter at Dupue, Illinois. G. S. Brooks and L. G.
Duncan.
mining and milling
Hints on Bucket-Elevator Operation. A. M. Nicholas.
Recent Test on Ball-Mill Crushing. C. T. VanWinkle.
Theory and Practice of Ball-Milling with Peripheral Discharge Mills.
P R. Hikes.
New Method of Separating Materials of Different Specific Gravities.
T. M. Chance.
iron and steel
The Erosion of Guns. H. M. Howe
Transverse Fissures in Steel Rails. J. E. Howard,
metallography
Grain-Size Inheritance in Iron and Carbon Steel. Z. Jeffries.
The Time-Effect in Tempering Steel. A E. Bellis.
Some Structures in Steel Fusion Welds. S. W. Miller.
Effect of Copper in Steel. C. R. Hayward and A. B. Johnston.
Two sessions were also devoted to the consideration of em-
ployment problems, some of the topics considered being the
necessity of a thoroughly capable employment manager, care
of workmen while on duty, suitable living conditions for labor,
the training of workmen for better positions, and the crippled
soldier in industry.
AMERICAN ELECTROCHEMICAL SOCIETY
, The board of directors of the American Electrochemical
Society, at a meeting held in Philadelphia on February 22, 1918,
decided to hold the Spring Meeting in the South during the
week of April 28. The meeting will take the form of a trip
through the chemical, electrochemical and metallurgical cen-
ters of the South, the plan being to leave Washington, D. C,
on the evening of Sunday, April 28, and spend April 29 in
Kingsport, Tenn., April 30 in Knoxville, May 1 in Chattanooga.
May 2 at Muscle Shoals, and May 3 in Birmingham, Ala. Re-
turning, the party will arrive in Washington on Sunday, May 5.
Mr. C. F. Roth is chairman of the Committee on Arrangements
and may be addressed at Grand Central Palace, New York
City.
CALENDAR OF MEETINGS
American Electrochemical Society — Spring Meeting, South-
ern trip, week of April 28, 1918.
American Society of Mechanical Engineers — Worcester,
Mass., June 4 to 7, 1918.
American Institute o'f Chemical Engineers — Summer Meeting,
Berlin, N. H., June 22, 1918.
American Society for Testing Materials — Atlantic City,
June 25 to 28, 1918.
NOTL5 AND CORRESPONDENCE
REVISED STATEMENT FROM THE CHEMICAL SERVICE industry or that his services are essential to the prosecution
SECTION of the war, and that his place cannot be filled by a man or woman
Soon after the March issue had gone to press a revised form not in the Army. Except in the cases of members of the Re-
of the announcement from the Chemical Service Section was serve CorPs. the action taken wi" cons,st of a recommendation
received. It is herewith printed in full, that which is in addition to the Adjutant General of the Army, that the man concerned
to the statement in the March number being printed black. be discharged from the National Army, National Guard or Reg-
_ „ „ ular Army, as the case may be, reenlisted or recommissioned
Office of the Chief of the Chemical Service Section, . , , ... _ „ , . , ..
„ in the proper branch of the Reserve Corps, and placed on the
1 106 New Interior Building . ,. _ ., „ , , ., „ „
^ _ inactive list. In the cases of members of the Reserve Corps,
Washington, D. C. , . . . . .. .. . ..
the action will consist of a recommendation that the man con-
By an order of the Secretary of War the Adjutant General cemed be p,aced on ihe inactive list.
of the Army has authorized the Chief of the Chemical Service The Secretary of War further directs that upon the transfer
Section of the National Army to initiate such measures as are to the Enlisted Reserve Corps for this purpose the enlisted
necessary to secure deferred classification for chemists whose man so transferred will be directed to report to the employer
services are essential to war industries. Under the Selective who requires his services. The employer in each case will
Service Regulations such action is limited to a letter of advice be advjsed Dy the man's transfer for the specific purpose in-
to the Local and District Exemption Boards transmitted through tende(i anti wm be requested to report to the Department
the Adjutant General's office, substantially as follows: Commander at the end of each month the status of the soldier,
•The chemical Service Section of the War Department has Investi- anci should at any time the soldier separate himself from such
gated the status of your company in connection with the production of war ^ g , wiU immediately notify the Adju-
material and considers it important that the elnciencv of vour organisation r J - . ... * •* ±s n
be maintained, in this connection the services of tant General of the Army of such separation and, if practicable,
as a technical expert in have been in- the latest address of the man.
vestigatcd and it is believed that his continued employment in war indus- ^he enclosed forms (printed in March issue) indicate the proper
tries would be to the best interests of the Government. You are therefore requesting action-a separate application must be made
advised to apply to the local exemption board for deferred classification in _, .
■his case on the ground that he is a necessary highly specialized technical for each man. Wirt. H. WALKER, Lieut. Col.
Opcrt of a necessary industrial enterprise. Such action, of course, should ( /'«•/, Chemical Service Section, N. A.
ht taken only with Mr 's consent. If
he prefers to enter the military service, please advise this office of that DPITPAnPTlNFW rFNSTTS
fact in order that his services may be utilized where most needed." PREPARfcDINxibb L,*.INbUS>
Under the same order of the Secretary of War the Chief of The Bureau of Mines has published OS Technical Paper 179
the Chemical Service Section will initiate action for the re- a classification of thi return! oi the census ol mining engineers,
turn to civil industries of any expert chemist whose service metallurgists, and chemists made at the request of the Council
in the industry from which he was taken is of more importance of National Defense. The paper can I" obtained from the
to the Government than are his services in a military capacity. Bureau of Mines until the limited fir, edition is exhausted;
He must certify that the man is considered indispensable in after that, for 5 cents from tin Superintendent of Documents,
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 4
Government Printing Office, Washington, D. C. The following
excerpt will be of special interest to chemists:
The accompanying table shows the 15,000 chemists classified
according to the various industrial groups. The miscellaneous
group of 1,130 includes 240 men not actually engaged in labora-
tory work, but holding administrative positions such as presi-
dents, treasurers and secretaries of chemical companies. It also
includes 157 leather chemists, 116 research chemists, a number
of dentists, editors, physicians, chemical engineers, and consulting
chemists.
Chemists Classified by Chieh Industrial Groups
1 Acids, alkalies, and salts 1 ,405
2 Alcohol and acetone 339
3 Ammonia oxidation 81
4 Analytical chemistry 3,808
5 Barium compounds 208
f Cement and lime 584
7 Coal, gas, tar, and coke 1 ,294
8 Dyes and textiles 775
9 Electrochemistry 769
10 Explosives (high) 962
11 Explosives (black powder) 150
1 2 Fats and soaps 834
13 Fertilizers 844
14 Foods 1,619
15 Glass and ceramics 262
16 Inorganic chemicals 532
1 7 Nitrogen (synthetic) 1 28
18 Organic chemicals (other than 2) 888
19 Paints and varnish 577
20 Petroleum and asphalt 769
21 Pharmaceuticals 983
22 Pyrotechnics 42
23 Rubber and allied substances 494
24 Sugar, starch, and gums 592
25 Water, sewage, and sanitation f 1,035
26 Wood products 368
27 Metallurgical chemistry 494
27a Alloys, ferrous 323
276 Alloys, non-ferrous 360
27c Aluminum and magnesium 127
27d Antimony, bismuth, and cadmium 54
27* Chromium and manganese 82
27/ Copper 379
27« Gold and silver 337
27* Iron and steel 1,415
27« Lead 209
27/ Mercury 25
27* Nickel and cobalt 68
27/ Platinum metals 75
27m Radium and uranium 99
27n Silicon and titanium 89
27o Zinc 255
27* Other metallurgy 126
28 Professors and instructors 1,285
29 Miscellaneous 1.130
The following table shows the number of chemists who re-
ported experience in foreign countries:
Country Chemists
Africa 13
Australasia 10
Austria-Hungary 24
Canada 203
Central America 15
Cuba 60
Europe: •
Belgium 6
Denmark 10
France 38
Great Britain 117
1 'i many 231
Holland 10
Italy II
Norway-Sweden 2\
Russia 30
Spain 5
.Switzerland 18
Others 10
Not specified 171
Far East (including Philippines) 80
Greenland
India
Mexico 117
Newfoundland
South America 14
West Indies 32
GOVERNMENT CONTROL OF PLATINUM
On Friday, March i, 1918, the Council of National Pcfense
issued the following statement:
Through Ordnance Requisition No. 510 from the Secretary
of War, the Government has taken over control of the produc-
tion, refining, distribution, and use of crude and refined platinum
for the period of the war. The control will be exercised through
the Chemical Division of the War Industries Board. The Chem-
ical Division sent out to-day to the industry requests for inven-
tories of the existing stock of crude and refined platinum and
platinum-iridium alloys as of March 1, 1918.
The letter stated that it was not the intention of the Govern-
ment to take over and handle directly the present stock of plat-
inum but to permit its shipment by the producers or dealers
subject to certain conditions. Upon the fixing by the Secre-
tary of War of a reasonable price for crude, refined, and alloyed
platinum, notice will be given ard blanks issued governing de-
livery and distribution.
DIRECTIONS TO PRODUCERS
The letter sent out by the Chemical Division includes the fol-
lowing directions to producers:
1 — That producers, refiners and dealers in platinum continue to dis-
pose of their product for Government purposes, and for that only, as di-
rected by the Chemical Division.
2 — That producers, refiners and dealers in platinum who are also
consumers use platinum for Government purposes, and for that only, as
directed by the Chemical Division.
3 — That all obligations arising out of transactions in the production
or delivery of crude, alloyed, or refined platinum released as above, includ-
ing all claims for shortage, poor quality, damage, or loss in transit, be borne
by the producer or seller, as the case may be, in accordance with existing
trade practices.
Distribution may be made by consent of this board through agencies
under existing arrangements, provided that there results no increase over
the existing price to the user.
The undersigned, on separate application in each case, will consider
permitting the delivery of a limited amount of platinum for essential com-
mercial purposes not for Government account.
Proper blanks upon which application for release of shipment should
be made will be furnished on application.
The following list indicates, in general, the order of preference which
will be followed in releasing platinum for shipment: first, military needs
of the United States Government; second, military needs of allied Govern-
ments; third, essential commercial purposes.
SUPPLEMENTARY STATEMENT
On March 4 the following statement was published as a sup-
plement to that of March 1 :
The Council wishes to state that in issuing Ordnance Requisi-
tion No. 510, commandeering crude or raw platinum now in
the hands of importers or refiners of this precious metal, it is to
be understood that this commandeering order does not apply
to or interfere with the purchase by the consumer of any manu-
factured articles containing platinum.
This explanation is made so that the public may clearly un-
derstand the purpose of this action by the Government.
This action of the Government will be welcomed by those who
have been concerned lest the available supplies should be insuf-
ficient to meet our war needs, especially since affairs have taken
such a turn in Russia as to make it very improbable that we may
hope to draw further from that source, "where the mines are
mostly shut down and a commercial market does not exist."
Even so, it is doubtful if the unmanufactured stocks in the hands
of dealers and refiners will begin to be enough. If not, the sole
resource is to take possession of manufactured articles at s
valuation.
It is regrettable that our Government did not clearly cover in
its order all the metals of the platinum group. It does not appear
from the statement of the Council of National Defense above
quoted that there is any restriction on dealings in the other metals
of the group that arc 1'roc from platinum. Yet there seems to
be an even greater relative scarcity of much needed iridium than
of platinum. A supplementary order should be issued without
delay so worded as to include all the metals of the group.
How far the present action of our Government follows what
has been done by the British Government is made evident by
the official documents and a letter from the Ministry of Munitions
of War on January 31, 1 9 1 8, to the American Embassy in London,
copies of which have been placed at my service by the Bureau of
Apr., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
3*3
Foreign and Domestic Commerce. The official documents are
six in number : Letter sent to all persons likely to hold platinum ;
Order placing platinum under the Defense of the Realm Act;
Copy of the Regulation; Requisition Notice; Form of Permit
authorizing dealers and dental manufacturers to dispose of their
stocks which were fully manufactured prior to the date of the
order.
From the letter referred to, it appears that the use of platinum
for jewelry and other non-essential purposes has been absolutely
prohibited. Dental manufacturers were rationed but were
allowed to reconvert their old stocks which contained large
quantities of platinum so that they could make them into new
stock containing less platinum. The Controller of Non-Ferrous
Materials Supply became the only purchaser of platinum outside
the country and the only seller of platinum inside the country.
No platinum can be sold without a permit from the Department
and no permits are granted unless the platinum is required for an
approved purpose. Persons authorized to buy scrap platinum
must sell it to one of four designated firms, who in turn have to
sell all that they have obtained to the Government. So success-
ful has this method of collecting scrap been that more than 75
per cent of the platinum sold by the Department per month is
covered by scrap purchased for more than two years. At present
the amount purchased represents only 50 per cent of the sales,
which it should be understood do not include the very large quan-
tities of platinum supplied for certain war purposes.
It may be added that the fixed price in England for platinum
was increased in December 1916 from 210 shillings to 290 shillings
per ounce and that in February 1918 the price for scrap was
further increased to £18 and for new platinum to £20 per ounce.
Washington, D. C. W. F. HrLLEBRAND
March 14, 1918
PLATINUM RESOLUTION BY THE ARGENTINE
CHEMICAL SOCIETY1
To the President of Die American Chemical Society:
I have the honor to address you as President of the Argentine
Chemical Society in view of the resolution of our Directors in
one of its last meetings.
The Argentine Chemical Society is advised as to the vote cast
by the American Chemical Society recommending to all
persons in the United States a restriction in the use of platinum
in view of the high price it has reached, and the recommendation
that all this metal be employed for the scientific and technical
uses for which it must be employed.
The Board of Directors of the Argentine Chemical Society,
over which I have the honor to preside, deems that this proposi-
tion of the American Chemical Society is extremely favorable
and essential to science, and in this view has voted to make com-
mon cause with it in the hope that it will be considered by all
the countries which it will benefit.
1 greet you with the greatest consideration, and remain
(Signed) G. F. Schaefer
Socikdad Quimica Argkntina President
Callb Lavalle 1790 [Signature illegible ]
Buenos Aires, January 15, 1918 Secretary
Senor G. F. Schaefer, Presidenle,
L Sociedad Quimica Argentina,
Calle Lavalle 1790,
Buenos Aires, Argentina, S. A.
Dear Sir:
I was much gratified to receive your esteemed favor of January
15th in which you announce that the Sociedad Quimica Argentina
has taken action similar to that taken by the American Chem-
ical Society on the subject of the use of platinum. This gives
nie double pleasure; first, that the action of our Society should
1 Ttie first letter ii a translation.
meet with favorable consideration by yourself, and, second, that
it should have been the means of bringing from you a communica-
tion which I sincerely trust will be followed by many others.
We are much interested in progress of all kinds in Argentina,
and will be delighted to be kept in touch particularly with its
progress in chemistry. I trust, therefore, that you will from
time to time honor us with further communications.
With cordial greetings from this Society to yourself and the
great Society over which you preside, I have the honor to remain,
Yours very truly,
(Signed) William H. Nichols
President
New York City
February 26, 1918
LICENSING OF FERTILIZER INDUSTRY ORDERED
By the President of the United States of America
a proclamation
Whereas under and by virtue of an act of Congress entitled
"An act to provide further for the national security and defense
by encouraging the production, conserving the supply, and con-
trolling the distribution of food products and fuel," approved
by the President on the 10th day of August 1917, it is provided,
among other things, as follows:
That by reason of the existence of a state of war it is essential
to the national security and defense, for the successful prose-
cution of the war, and for the support and maintenance of the
Army and Navy, to assure an adequate supply and equitable
distribution, and to facilitate the movement of foods, feeds, fuel,
including fuel oil and natural gas, and fertilizer and fertilizer
ingredients, tools, utensils, implements, machinery, and equip-
ment required for the actual production of foods, feeds, and fuel,
hereafter in this act called necessaries; to prevent, locally or
generally, scarcity, monopolization, hoarding, injurious specula-
tion, manipulations, and private controls, affecting such supply,
distribution, and movement; and to establish and maintain
governmental control of such necessaries during the war. For
such purposes the instrumentalities, means, methods, powers,
authorities, duties, obligations, and prohibitions hereinafter
set forth are created, established, conferred, and prescribed. The
President is authorized to make such regulations and to issue such
orders as are essential effectively to carry out the provisions of
this act.
And Whereas it is further provided in said act as follows:
That from time to time, whenever the President shall find it
essential to license the importation, manufacture, storage,
mining, or distribution of any necessaries, in order to carry into
effect any of the purposes of this act, and shall publicly so an-
nounce, no person shall, after a date fixed in the announcement,
engage in or carry on any such business specified in the announce-
ment of importation, manufacture, storage, mining, or distribu-
tion of any necessaries as set forth in such announcement, unless
he shall secure and hold a license issued pursuant to this section.
The President is authorized to issue such licenses and to prescribe
regulations for the issuance of licenses and requirements for sys-
tems of accounts and auditing of accounts to be kept by licensees,
submission of reports by them, with or without oath or affirma-
tion, and the entry and inspection by the President's duly author-
ized agents of the places of business of licensees.
And Whereas it is essential, in order to carry into effect the
purposes of said act and in order to secure an adequate supply
and equitable distribution and to facilitate the movement of
certain necessaries hereafter in this proclamation specified, that
the license powers conferred upon the President by said act be
at this time exercised to the extent hereinafter set forth.
Now, therefore, I, Woodrow Wilson, President of the United
States of America, by virtue of the powers conferred on me by
324
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 4
said act of Congress, hereby find and determine and by this
proclamation do announce that it is essential, in order to carry
into effect the purposes of said act, to license the importation,
manufacture, storage, and distribution of the following neces-
saries: Fertilizers and fertilizer ingredients, including sulfuric
acid, phosphate rock, acid phosphate, bones (raw, ground, or
steamed), bone-black, basic slag, sodium nitrate, ammonia sulfate,
cottonseed meal, slaughterhouse tankage, garbage tankage, castor
pomace, fish scrap, base goods, cyanamid, calcium nitrate, dried
blood, acidulated leather, hair, hoof meal, horn dust, ground
leather, other unacidulated ammoniates, potash salts, cement
dust, blast-furnace dust, kelp ash, kelp char, dried kelp, wood
ashes, cottonseed hull ashes, potassium nitrate, tobacco waste,
mixed fertilizers, sulfur, and all other fertilizers and fertilizer
ingredients.
All individuals, partnerships, associations, and corporations
engaged in the business of importing, manufacturing, storing, or
distributing fertilizers or fertilizer ingredients (except those
specifically exempted by said act of Congress, and except to the
extent to which licenses have been issued under the proclamation
of the President of January 3, 1918, relating to ammonia, am-
moniacal liquors, aud ammonium sulfates) are hereby required
to secure licenses on or before March 20, 1918, which will be issued
under such rules and regulations governing the conduct of the
business as may be prescribed.
The Secretary of Agriculture shall carry into effect the pro-
visions of said act, and shall supervise and direct the exercise of
the powers and authority thereby given to the President, as far
as the same apply to fertilizers and fertilizer ingredients, and to
any and all practices, procedure, and regulations applicable
thereto, authorized or required under the provisions of said act,
and in this behalf he shall do and perform such acts and things
as may be authorized or required of him from time to time by
direction of the President and under such rules and regulations
as may be prescribed by the President from time to time. All
departments and agencies of the Government are hereby directed
to cooperate with the Secretary of Agriculture in the performance
of the duties hereinbefore set forth.
Applications for licenses must be made to the Law Department,
License Division, United States Food Administration, Wash-
ington, D. C, upon forms prepared for that purpose.
Any individual, partnership, association or corporation, other
than as hereinbefore excepted, who shall engage in or carry on
the business of importing, manufacturing, storing, or distributing
fertilizers or fertilizer ingredients, after the date aforesaid, with-
out first securing such license, will be liable to the penalties pre-
scribed by said act of Congress.
In witness whereof I have hereunto set my hand and caused
the seal of the United States to be affixed.
Done in the District of Columbia this 25th day of February,
in the year of our Lord 191 8 and of the independence of the
United States of America the one hundred and forty-second.
Woodrow Wilson
By the President :
Robert Lansing
Secretary of Slate
In the enforcement of the regulations prescribed in the Presi
dent's proclamation, the Secretary of Agriculture has announced
thai he will be assisted bj the following committee:
Charles \V Merrill, chairman; C L. Alsberg, Karl F. Keller
man, A 1; Taylor, !•'. \\ Brown, I. 1. Summers.
RESEARCH INFORMATION COMMITTEE
The following statement is authorized by the Council of
National Defense
I — By joint action the Secretaries of War and Navy, with
the approval of the Council of National Defense, have au-
thorized and approved the organization, through the National
Research Council, of a Research Information Committee in
Washington with branch committees in Paris and London,
which are intended to work in close cooperation with the officers
of the Military and Naval Intelligence, and whose function
shall be the securing, classifying, and disseminating of scientific,
technical, and industrial research information, especially relating
to war problems, and the interchange of such information
between the allies in Europe and the United States.
ORGANIZATION OF COMMITTEES
2 — The Washington committee consists of:
(a) A civilian member, representing the National Research Council,
Dr. S. W. Stratton, chairman.
(6) The chief. Military Intelligence Section.
(c) The Director of Naval Intelligence.
3 — The initial organization of the committee in London is:
(a) The scientific attache representing the Research Information
Committee: Dr. H. A. Bumstead, attache.
(b) The military attache, or an officer deputed to act for him.
(c) The naval attache, or an officer deputed to act for him.
4 — The initial organization of the committee in Paris is:
(a) The scientific attache representing the Research Information
Committee: Dr. W. F. Durand. attache.
(6) The military attache, or an officer deputed to act for him.
(c) The naval attache, or an officer deputed to act for him.
FUNCTIONS OF FOREIGN COMMITTEES
5 — -The chief functions of the foreign committees thus
organized are intended to be as follows:
(a) The development of contact with all important research laboratories
or agencies, governmental or private; the compilation of problems and sub-
jects under investigation: and the collection and compilation of the results
attained.
(6) The classification, organization, and preparation of such informa-
tion for transmission to the Research Information Committee in Wash-
ington.
U) The maintenance of continuous contact with the work of the offices
of military and naval attaches in order that all duplication of work or
crossing of effort may be avoided, with the consequent waste of time and
energy and the confusion resulting from crossed or duplicated effort.
id) To serve as an immediate auxiliary to the offices of the military and
naval attaches in the collection, analysis, and compilation of scientific,
technical, and industrial research information.
(e) To serve as an agency at the immediate service of the commander-
in-chief of the military or naval forces in Europe for the collection and
analysis of scientific and technical research information, and as an auxiliary
to such direct military and naval agencies as may be in use for the purpose.
(/) To serve as centers of distribution to the American Expeditionary
Forces in France and to the American Naval Forces in European waters of
scientific and technical research information, originating in the United
States and transmitted through the Research Information Committee in
Washington.
(g) To serve as centers of distribution to our allies in Europe of scientific,
technical, and industrial research information originating in the United
States and transmitted through the Research Information Committee in
Washington.
(h) The maintenance of the necessary contact between the offices in
Paris and London in order that provision may be made for the direct and
prompt interchange of important scientific and technical information.
(0 To aid research workers or collectors of scientific, technical, and
industrial information from the United States, when properly accredited
from the Research Information Committee in Washington, in best achiev-
ing their several and particular purposes.
6 — -The headquarters of the Research Information Committee
in Washington are in the offices of the National Research Council.
1023 Sixteenth Street; the branch committees are located at the
American Embassies in London and Paris.
DYESTUFFS ASSOCIATION
At the meeting of manufacturers of and dealers in dyestufffl
held in Rumford Hall. Chemists' Club, New York City, on March
6, 1918, to hear the report of the < >t. ionization Committee and
to form a permanent organization, it was decided by a vote of
27 to 5 to confine the association strictly to manufacturers
of ilyes aud intermediates.
The resolution presented to the meeting by the committee
mi/ation read as follows
Apr., 191J
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
325
Inasmuch as the interests of the American dyestuffs industry
will be better served by having one association consisting of
manufacturers only, and a separate association for dealers,
now therefore be it
Resolved, That the organization committee recommend to
the meeting on March 6, that there be formed an association
of manufacturers of intermediates and dyes under the name
of "Dyestuff Manufacturers' Association of America," or some
similar name; and that there be formed a separate association
consisting of dealers in dyestuffs and bearing an appropriate
name.
The following were elected to the board of governors:
George H. Whayley John Campbell Co. New York
M. R. Poucher E. I. du Pont de Nemours & Co. Wilmington, Del.
Albert Blum United Piece Dye Makers Lodi, N. J.
August Merz Heller & Merz Co. Newark, N. J.
M. S. Orth Marden, Orth & Hastings Cor. New York
R. G. Jeffcott Calco Chemical Co.
Frank Hemingway Frank Hemingway, Inc.
L. A. Ault Ault & Wiborg
J. Merritt Matthews Grasselli Chemical Co.
W. H. Cottingham Sherwin-Williams Co.
Robert W. Kemp Holliday, Kemp & Co.
Robert P. Dicks Dicks, Davis & Co.
Elvin H. Killheffer Newport Chemical Co.
Samuel Isermann Chemical Co. of America
I. Stanley Stanislaus Stanley Aniline Chem. Co.
Several of these will be selected as incorporators. Adjourn-
ment was taken subject to the call of the board of governors.
New York
April
New York
April,
Cincinnati
April,
Cleveland
April,
Cleveland
April
New York
May
New York
Carroliton,
Wis.
New York
Lock Have
a. Pa.
Series
FOOD IN WAR TIME
A special emergency war course on Food in War Time is being
given at the College of the City of New York under the chemistry
department as Chemistry 29. One unit of college credit will be
given those who have the necessary prerequisites and who com-
plete all the required work, but those who wish to take the course
without credit may enter as auditors. There is no tuition fee.
A registration fee of one dollar for the entire course is charged.
The lectures will be given in Doremus Lecture Theatre at 4
p. M. Dates, lectures, and lecture topics are as follows :
Series of Lectures by miss laura caublE, Consultant in House-
hold Economy
March 1. The Problem of^Human Feeding. Food Requirements.
(Exhibit.)
March 5. Relative Food Values. The Choice of Foods. (Exhibit.)
March 8. Making the Food Budget. Cost of Maintenance. (Exhibit.)
March 12. The City's Markets. The Question of Distribution.
March 15. The City's Source of Food Supply. New Foods. A Problem
of Cooperation.
Series of Lectures by mr. Robert mcdowell ALLEN, Formerly
Food and Drug Commissioner of Kentucky, Expert
of the Ward Baking Company
March 19. Cereals, World Production and Distribution.
March 22. Bread Making in the Home and Bakery.
March 26. Applied Science in Bread Making.
April 9. Governmental Regulation — Sanitation and Conservation.
A phi. 12. Cereals in the Diet.
Series of Lectures by dr. lucius p. brown, Department of
Health, N. Y. City; Director of Bureau of
Foods and Drugs
16. Food Wastes After the Crop has Matured.
19. Non-Essential Food Industries.
23. Dehydration of Foods.
26. The Work of the U. S. Department of Agriculture in War Time.
30. Food Conservation for War Aid Purposes.
3. The U. S. Food Administration and Its Contacts with the
Citizen.
7. Food Adulterations and Sanitation in War Time.
Series of Lectures by dr. h. c. Sherman, Professor of Food Chem-
istry, and miss mary G. Mccormick, Instructor in
Nutrition, Columbia University
May 10. The Food Situation from the Standpoint of Nutrition.
May 14. Food as the Source of Human Energy.
May 17. Food as Material for Body Building.
May 21. Nutritional Characteristics of the Different Types of Food.
May 24. Relative Economy of the Different Types of Food.
May 28. The Importance of the Milk Supply.
May 31. The Opportunity of the Food Consumer.
MEETING WAR CONDITIONS AT RENSSELAER POLY-
TECHNIC INSTITUTE
The class of 191 8 is to be graduated May first instead of the
middle of June, and the class of 1919 on January 1, 1919. This
plan necessitates the running of instructional work all summer,
keeping the Institute going under full pressure for the upper
classes without vacation mterm'ssions. Unless modified by
future changes, the work of the Freshman and Sophomore classes
will continue as usual.
WASHINGTON LETTER
By Paul Wooton. Metropolitan Bank Building. Washington. D. C.
Success finally has crowned the prolonged efforts of representa-
tives of the chemical industry to obtain a deferred classification
for those chemists whose services are essential to the war indus-
tries. Prof. M. T. Bogert, chairman of the Committee on Chem-
istry for the National Research Council, and Dr. C. L. Parsons,
Secretary of the American Chemical Society, with the efficient
aid of other prominent chemists, were most active in securing
this concession from the Secretary of War.
While the details of the reorganization of the War Industries
Board have not been announced at this writing, it is stated
authoritatively that it will have no bearing on the Chemical
Section. The reorganization, however, is certain to have the
important effect of defining the authority of the Chemical Section
! much more clearly than was the case previously. It is under-
stood that L. L. Summers will continue as the administrative
head of this section. He is being assisted in his administrative
work by C. H. MacDowell. Mr. MacDowell also has direct
charge of nitrates, alkalies, and chlorine. Dr. Samuel A. Tucker,
of Columbia University, Dr. H. R. Moody, of the College of the
City of New York, and J. M. Moorehead. of Chicago, have been
added to the personnel of the section. Drs. Tucker and Moody
are well known instructors in chemical subjects. Mr. Moorehead
l» a consulting chemical engineer. He will look after toluol and
gas production for the War Industries Board.
patent had been issued led to inquiry at the Patent Office. In
reply J. T. Newton, the commissioner of patents, writes as follows:
"The Patent Office has not issued a patent to Garabed on his supposed
invention. We have numerous applications for such things. In fact we
get them almost daily, but as they are against demonstrated scientific prin-
ciples, we refuse to grant patents thereon on the same ground, for example,
that we refuse to grant patents for perpetual motion.
"I am sorry so much publicity has been given to this case, becajse it has
a tendency to give a wrong impression of inventors as a class. They have
done more for progress in America than has any other class and Garabed
Giragossian is the exception and is not characteristic."
No patent has been issued to Garabed Giragossian for his
"free energy generator." A report to the effect that such a
Exports of chemicals in January had a total value of $15,500,-
637. I" January of 191 7, the value of chemical exports was
$17,102,702. Imports of chemicals in January of 191 8 totalled
54,925, 744. This compares with $4,046,080 in the corresponding
month of 1917. Marked increases were shown in the amounts
of chemicals sent to Japan, Brazil, British India and Prance.
The principal decreases were shown in forwardings to the 1 faited
Kingdom and to Mexico.
Some confusion having arisen as to the definition of the terms
"ammonia, ammemiacal liquors or ammonium sulfate, from what-
ever source produced" as used in the proclamation of January
.}, the Pood Administration has interpreted it as meaning only
the prime products of ammonia as produced in by-prodm t a >ke
oven plants, coal gas plants and nitrogen fixation plants. This
3*6
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, Xo. 4
excludes druggists, wholesalers and dealers handling only second-
ary products. It also excludes persons using the prime products
solely as ingredients in the manufacture of products not subject
to license.
If it should become necessary, as seems quite probable, to re-
strict the use of ammonia, the Food Administration is making
it very clear that plants with a low degree of efficiency will be
the first to suffer. A great deal of waste has taken place, espe-
cially in the artificial ice industry, it is said, and many plants are
reporting increased efficiency in the use of ammonia which is
making possible the same output as in previous years with savings
of ammonia running as high as 60 per cent.
Paint manufacturers and dealers at a meeting with officials
of the Council of National Defense entered into a voluntary
agreement to reduce house paints to 32 shades, after July 1.
At present, more than 100 shades of house paint are being manu-
factured. To conserve tin, several sizes of containers are to be
eliminated. The reduction in the number of shades has been
carried even further. Enamels, for instance, will be restricted
to eight shades; floor paint to eight; roof and barn paint to two;
shingle stains to twelve; carriage paint to eight; marine varnishes
to four.
Certain manufacturers of fertilizers have been charged by the
Federal Trade Commission with using unfair methods of competi-
tion. Two large companies are said to have purchased raw ma-
terials at prices higher than were justified by conditions. This
had the effect it is alleged of pushing prices to a point where
they were prohibitive to small competitors. This and other
charges will be the subject of a hearing in Washington on April 10.
To expedite traffic and to keep close account of the car supply,
the Committee on Fertilizers of the Chemical Alliance has named
transportation sub-committees in the railroad centers of the
fertilizer- producing territory. The Committee on Fertilizers is
one of the most active organizations doing war work in Washing-
ton and is rendering a very efficient service to the industry, all
fertilizer manufacturers who come to Washington agree.
To meet very general objection to the sulfuric acid question-
naire prepared by the War Industries Board, new blanks are being
sent out to the industry. The War Industries Board question-
naire called for so much clerical work each week that it is being
replaced by the simpler questionnaire. The new inquiry asks
only for production for the previous month, stocks on hand at
the beginning and the end of each month, shipments, and total
delivery on all contracts for the United States and the allied
governments. In addition, manufacturers who are receiving
raw materials from the government are asked to. state their re-
quirements for the ensuing three months.
Horace Bowker, Henry Howard, E. R. Grasselli, Charles H.
McDowell, A. G. Rosengarten, D. W. Jayne, Charles G. Wilson,
W. D. Huntington, F. A. Lidbury. J- D- Cameron Bradley and
E. T. Connolly attended the meeting of the Board of Directors
of the Chemical Alliance which was held in Washington on Feb-
ruary 20.
C. H. Conner, of New York, is in charge of the wood chemical
division of the Raw Materials Committee of the War Industries
Board.
Weekly reports showing the production of by-product coke
and the factors which prevent this industry from operating at
maximum capacity have just been started by the Geological
Survey. During the limited time covered by the new reports
the industry has been operated at about 75 per cent of capacity.
The chief limiting factor is inability to secure coal, which is
chargeable almost entirely to car shortage.
UNVEILING OF THE, PORTRAIT OF HLRMAN FRA5CH
On Sunday, the 3rd of March, it was the pleasure of the
trustees of the Chemists' Club of New York to entertain Mrs.
Herman Frasch and a party of her friends at luncheon. The
occasion was the presentation by the guest of honor of a re-
markably life-like and well-painted portrait of the late Herman
Frasch. His daughter, Mrs. Whiton, and Mr. Hubert Vos, who
painted the portrait, were among the company. In the absence
of President Whitaker in Washington, Vice President Gustave
W. Thompson presided. When coffee was served the following
address was made by Mr. Ellwood Hendrick, of the committee
appointed by the trustees to arrange for the ceremony:
There are two attitudes of mind in which to meet in memory
of one who has gone ahead of us upon the long journey : we may
congregate in dolor and address ourselves to regret at our loss
in his passing, or we may, and I think with greater loyalty,
rejoice in our good fortune and be glad that ours was the privilege
to enjoy the benediction of his friendship. Let us to-day follow
the path of the Greater Loyalty.
This is a large club and our members are of various rank and
circumstance; indeed we are of many sorts and conditions of
men Some of us live out our little lives and hardly cast a
ripple upon the surface of our days. A few do big things.
"The moving finger writes, and having writ " there stands
emblazoned a message for all mankind to see. Of such was
Herman Frasch.
The emblazoned messages soon become so familiar that we
take them as matters of course. The men who write them are
usually modest. The feature of great men that is most often
observed is that they are not peculiar at all but are. rather,
remarkably like other men. They have the gift of vision, the
art to do and the energy to persevere; and these are not showy
qualities. As they complete their tasks, the world mechanically
takes a step forward. Very frequently this happens so quietly
that we need an historical perspective to find the origins of
progress.
As a member of the club Mr. Frasch was especially interested
in the efforts to make things run smoothly. In the council of
good fellowship he would offer very sane and human views of
such situations as arose, with which others were certain to
agree and, as likely as not, re-propose his own ideas to him.
He didn't mind; his main interest was to get things done.
In the course of time he grew rich, and this is a burden which
few of us can bear without deterioration. It did not injure
him. To members of the club, most of whom are in modest
circumstances, he never showed a trace of rich man's vanity.
Now very successful men are often difficult and wayward and
even childish in their demands, and although we are happily
free from them in the club, they abound in profusion throughout
the land. The best answer as to the cause of their offenses
is that they are short a generation of habits of grace in living and
thinking. No one ever suggested that Herman Frasch lacked
any needful generation of this sort. Wherever his forebears
lived they must have been richly endowed with sympathy.
This will explain the quality of his friendship for the club and
his relations to it. They were never ostentatious, but they
could always be counted on in time of need and when the clouds
hung low.
One of his most distinctive qualities offers no side for any
consideration save that of deep regret that he is not living to-
day. That was his clean-cut, straightforward attitude toward
affairs. He believed in this country. He was one hundred
per cent American, despite his foreign birth. He was one of us.
When the scientific history of the great war is written, many
instances that are now but slightly considered will loom large
in the records. Let us note one of them. After the Germans
had been turned at the Marne they entrenched themselves and
proceeded with their repeated efforts to break through the allied
lines in the West. The British had hardly any high explosives
and the French barely enough for their own use. The United
States undertook to supply them but a difficulty arose: Spanish
Apr., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
32;
pyrites could not be brought over in adequate quantity to provide
sulfuric acid to make them. The greatest pyrites mine in the
country had been flooded — as likely as not by one of von Bern-
storff's agents. Without high explosives the allied line would
surely have weakened, and owing to the machinations of German
agents the manufacture of munitions in this country almost
came to a stop. At this point the results of the genius of the
American, Herman Frasch, and the altruistic attitude of the great
company which he founded came into play. By releasing their
vast store of sulfur at a nomijal price for the making of muni-
tions the march of Prussian madness was stopped and the awful
1 fate of Belgium and Picardy and Champagne was averted for
I Brittany and Normandy and even England itself. When we
think of the countless thousands of men and women and little
children thus saved from the atrocities of the German hordes, we
may well be proud that one of our number was of such potent
influence as an instrument of mercy!
Every one of us has his world within himself. What we
touch and smell and see and hear will often make it or mar it for
us. A kindly glance, the pressure of a hand, a word of en-
couragement: these things have their moments of fate. We
shall now have, thanks to the abundant generosity of Mrs.
Frasch, the likeness of our friend and fellow member for com-
panionship. Thanks to the subtle art of Mr. Vos, it speaks.
And thanks to his own good fellowship, his integrity of purpose
and his resolution for the right, the voice is kindly, full of
pleasant memories to those of us who knew him, and full of
encouragement to those of us who are young.
The party then entered the Social Room where the portrait
was unveiled by Mrs. Frasch and formally accepted for the club
by Vice President Thompson.
PERSONALS
Lieut. A. W. Davison has been transferred from Washington
to Niagara Falls, New York, where he is supervising chemical
plant construction and experimental operation at the Oldbury
Electrochemical Company.
Mr. W. S. Allen, for many years chief chemist of the Laurel
Hill plant of the General Chemical Company, has been trans-
ferred to New York. Mr. J. B. Barnett is the new chemist in
charge at the Laboratory.
Dr. Paul H. M.-P. Brinton, professor of analytical chemistry
in the University of Arizona, has been commissioned Captain
in the Ordnance Reserve.
Mr. Pope Yeatman, consulting engineer of New York, has been
placed in charge of the non-ferrous metals department of the
War Industries Board, succeeding Eugene Meyer, Jr.
Mr. Nicholas Kozeloff has been appointed bacteriologist of
the Louisiana Sugar Station to succeed Mr. W. L. Owen.
The U. S. Bureau of Mines has broadened the scope of its
station at Urbana, 111., to include work in coal and metal mining
and the metallurgical industries of the Middle West. The present
safety work will be continued and all work will be conducted
under a cooperative agreement with the mining department of
the University of Illinois. The bureau staff is under the superin-
tendence of E. A. Holbrook, supervising mining engineer and
metallurgist. Other members are W. B. Plank, in charge of
safety, and F. K. Ovitz, chemist.
M. Henri Jequier, metallurgist of the Societe Meniere et
Metallurgique de Penarroya, and Dr. Auguste Hollard, consulting
engineer, are on a visit to this country. The Penarroya Com-
pany, which has its headquarters in Paris, and mines and works
in Spain, is the largest smelter and refiner of lead in Europe.
Dr. Yogoro Kato, professor at the Tokyo College of Tech-
nology and Director of the Nakamura Chemical Research Insti-
tute in Tokyo, who is on a professional visit to this country,
attended the recent annual meeting of the American Institute of
Mining Engineers in New York.
The Patent Office Society announces that a composite com-
mittee has been created by the National Research Council to
make a preliminary study of the problems of the U. S. Patent
Office. This committee is understood to comprise the following
members: Leo H. Baekeland, Wm. F. Durand, Thos. Ewing,
1 Frederick P. Fish, Robert A. Millikan, E. J. Prindle, Michael
I. Pupin and S. W. Stratton. The action of the National Re-
pjearch Council in forming such a committee is understood to be
in conformity with the wishes of the Commissioner of Patents
J. T. Newton and Secretary of the Interior F. K. Lane. The
special committee of the Patent Office Society urges all interested to
forward any patent reform suggestions to Dr. Wm. F. Durand,
National Research Council, Washington, D. C. It is not ex-
pected that patent reform can claim primary consideration during
the continuance of the war, but it is felt that the time is ripe for
at least a study of conditions.
Dr. B. Johnsen, formerly of the Forest Laboratories, Montreal,
Canada, as chemical engineer in pulp and paper, is now research
chemist for the Hammermill Paper Company, Erie, Pa.
Colonel W. R. Lang, professor of chemistry and director of
chemical laboratories, University of Toronto, has left for Halifax
to take up staff duties in his new appointment in the Halifax
Military District, under General F. L. Lessard.
The March meeting of the Delaware Section was held on
March 8 in Wilmington. Following an informal dinner, Prof.
Edward Hart spoke on "The Manufacture of Nitric Acid."
The following officers have been elected: Chairman, Lammot
du Pont; Vice Chairman, J. G. Melendy; Secretary, R. P.
Calvert; Treasurer, D. S. Ashbrook; Councillors, C. M. Stine
and Firman Thompson.
Mr. Henry C. Howard, Jr., treasurer and chief chemist of the
Charles A. Newhall Company, Seattle, Washington, has joined
the 30th Engineers and is now stationed at Ft. Myer, Va. Mr.
Howard has specialized in electrochemistry and has recently
developed a process for the manufacturing of potassium per-
chlorate, the potassium salts being derived from kelp. The
process is now being operated on a commercial scale in Seattle.
Dr. E. H. Leslie has resigned from his position as chief chemist
of the Petroleum Corporation of Los Angeles and has assumed
new duties as technical adviser to the Sales Department of the
U. S. Industrial Alcohol Company and the U. S. Industrial
Chemical Company. He will be located in their main offices
at 27 William Street, New York City.
Mr. John Clifford English, well known in Philadelphia and
New York as a chemist, physicist and expert in acoustics, died
suddenly at San Antonio, Texas, where he had gone to regain
his health.
Dr. S. A. Mahood, formerly instructor in organic chemistry
at Cornell University, is now research chemist in the U. S. Forest
Products Laboratory, Madison, Wisconsin.
Mr. W. H. Whitcomb, formerly professor of chemistry at
Miami University, Oxford, Ohio, is now with the United States
Rubber Company engaged in laboratory development work.
Mr. T. F. Chin, of Pekin, China, principal technical expert of
the Chinese Ministry of War, is in this country with the Chinese
mission to make purchases for the outfitting of an extensive chem-
ical laboratory at Pekin for his government.
Mr. V. T. Stewart has been given charge of the new laboratory
at Silver Lake, N. J., which will serve all the plants of Thos. A.
Edison located at that point. He was previously engaged in
research work on primary batteries for one of these plants.
Mr. Frank L. McCartney, formerly with Sharp and Dohme,
but during the past two years manager of the Albodon Company,
lias been appointed Captain, Sanitary Corps, National Army,
and will be stationed at the Medical Supply Depot, New York
City. He is ex-chairman of the New York Board of Trade and
Transportation, Drug Trade Section, and is president of the
New York Branch of the American Pharmaceutical Association.
He has been granted leave of absence by the Albodon Company
for the duration of the war.
Dr. W. F. Faragher has resigned his position as research chemist
for the Alden Speare's Sons Co. to become senior fellow at the
Mellon Institute of Pittsburgh.
3 -'8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. Xo. 4
Dr. Fred W. Upson, for the past four years professor of agri-
cultural chemistry in the Nebraska College of Agriculture, will
on June i become head of the department of chemistry in the
University of Nebraska. A chemical laboratory which is modern
in every respect will be ready for occupancy at that time. The
work of the departments of chemistry will be combined under the
direction of Dr. Upson.
Dr. George L. Clark, who left a professorship at the University
of Arizona to take the Ph.D. at the University of Chicago in
January 191 8, is engaged in research at the American University
Experiment Station, Washington, D. C.
Prof. DM. Folsom, of the department of mineralogy of Stan-
ford University, has been appointed Fuel Administrator of the
Western States. His jurisdiction will cover Idaho, Montana,
Utah, Arizona, New Mexico, Nevada, Oregon, Washington,
California and Alaska.
Mr. Sydney J. Jennings, vice president of the U. S. Smelting,
Refining and Mining Company, has been elected president of the
American Institute of Mining Engineers to succeed Philip M.
Moore, of St. Louis.
Prof. G. H. Clevenger has resigned as research professor of
metallurgy at Stanford University and is now engaged in directing
cooperative experimental work which is being done by the United
States Bureau of Mines, Netherlands East Indies Government,
Research Corporation of New York, and others.
Mr. Arthur F. Brown, formerly with Swan-Meyers Company,
is now located with the Griswold Worsted Company, Darby, Pa.
Dr. John Johnston has been appointed Secretary* of the National
Research Council. Dr. Johnston will devote his activities
largely to the development of an industrial research section,
the purpose of which is to assist in the organization of research
by industries, a work similar to that now being carried out
under government auspices in Great Britain and some of the
British Dominions by the committee of the Privy Council for
scientific and industrial research.
Word was received late in February' announcing the death
of Thomas Tyrer, one of England's most prominent pharmaceuti-
cal chemists, at the age of seventy-six. He %vas one of the patri-
archs of the Society of Chemical Industry, at one time its presi-
dent, and at the time of his death was Hon. Treasurer of that
organization. He was a fellow of the Institute of Chemistry,
of the Chemical Society and of the Statistical Society. He
served as president of the British Pharmaceutical Conference,
with which body he was closely identified throughout his life.
Mr. Tvrer was well known in the United States and was a mem-
ber of the American Chemical Society. His last visit to this
country' was in 1895. It was as a result of his unremitting
labors that alcohol for use in the arts became tax-free in the
British linipire.
Major Samuel C. Prescott, of the Sanitary Corps, National
Army, who is professor of biology at the Massachusetts Insti-
tute of Technology, is about to make an extended tour through
the cantonments of the South and West.
Professor Elmer P. Kohler, of the chemistry' department of
Harvard University, has been called to Washington, D. C. He
will be stationed at the American University Experiment Sta-
tion of the Bureau of Mines as assistant to the Director in
charge of research problems. Professor Kohler's work at Cam-
bridge will be carried on by Professor Forris J Moore, of the
Massachusetts Institute of Technology, and by I >r. G. Albert
Hill, of the Harvard chemical department As a consequence
^sor Kohler's call the Harvard University detachment
of the Chemical Service Corps has inn transferred to Wash-
ington. Included in the detachment are the following mem-
bers of tlie Northeastern Section: Lieut. Lee I. Smith, Sergeant
Roy I. ('.inter and Private Alexander D. MacDonald.
Dr. William M. Burton has been awarded the 1018 Willard
Gibbs gold medal by the Chicago Section of the A. C. S. Dr.
Burton was born in Cleveland. Ohio, November 17. 1865, and
received his early education in the public schools of that city.
In 1886 he was graduated from Western Reserve University with
the degree of A.B. He then went to Johns Hopkins where he-
took his Ph.D. in chemistry 111 1889. Dr. Burton then entered
tlie employ of the Standard Oil Company of Ohio as chemist.
he went to the Standard ( >il Company of Indiana, where
he has been successively chemist, assistant superintendent and
general superintendent of the company's refinery at Whiting,
Ind., and now is vice president of the company, in charge of all
manufacturing activities. In 1913 Dr. Burton brought out a
practical pressure still process for converting high boiling point
products of petroleum into products of low boiling point, thereby
largely increasing the supply of gasoline and other naphtha
products.
Lieut. Ellery R Files of the Gas Defense Service has been
transferred from Washington to be instructor of the National
Army camp at Yaphank, L. I.
Mr James Brown, formerly professor of chemistry at Butler
College, has entered the commercial field and is now located in
New York City.
Mr Grover B. Purkey. assistant foreman in the chemical
department of Eli Lilly & Company, died February 2. Mr.
Purkey was born at Morocco, Indiana, and was a graduate of
Purdue University
Dr. Martha Tracy, of the Philadelphia Section, has been ap-
pointed Dean of the Woman's Medical College of Pennsylvania.
The Bureau of Standards has announced the appointment
of Mr. Samuel S. Wyer, a consulting engineer of Columbus,
Ohio, and Mr. Willard F. Hine, chief gas engineer of the Public
Service Commission of the First District, New York State, as
consulting engineers on the staff of the Bureau of Standards.
These engineers will assist the Bureau in conferences and special
investigations from time to time in order that the Bureau's
regular staff may be augmented for particular and important
work. These two appointments are the first which have been
made by the Bureau under its new program of appointing
permanent specialists in different fields to assist it as advisers
and consultants in its investigations.
Dr. Francis G. Benedict, director of the nutrition laboratory
of the Carnegie Institute, Brookline, Mass., has received a gold
medal from the National Institute of Social Sciences, in recogni-
tion of his "notable service to mankind." The medal was
presented at the recent fifth annual dinner of the National
Institute in New York City.
Dr. Arthur H. Elliott, emeritus chief chemist of the New
York Consolidated Gas Company and emeritus professor of
chemistry and physics in the College of Pharmacy, died on
March 2, at the age of seventy years.
Mr. H. E. Ives, of the United Gas Improvement Company of
Philadelphia, Pa., has entered the Science and Research Division
of the Signal Corps, and may be reached at 1023 Sixteenth
Street, Washington, D. C.
Lieut. Col. Allerton S. Cushman, U. S. A., now connected
with the Frankford Arsenal, will speak before the Philadelphia
Section of the A. C. S. on "Chemistry and Its Applications to the
Manufacture of Military Primers " on April 18, 1918.
Dr. Charles L. Reese, of E.I. du Pont de Nemours and Co.,
will deliver an illustrated lecture on "Explosives" before the
Franklin Institute, Philadelphia, on April 4.
Mr. Samuel Batterman has entered the government service.
He is in the Division of Forestry.
Mr. A. P. Peterson, formerly with the Western Electric
Co., is now Second Lieutenant, U. S. R., 26th infantry, A. E. F.
Dr. Julius Stieglitz, Mr. A V. H. Mory and Mr. William
Hoskins were the delegates of the A. C. S. to the Congress of
National Service, which was held in Chicago, February 21, 22
and 23. The Congress was under the auspices of the National
Security League.
Lieut. Harold J. Brownlee. Company C, 110th Regular
Engineers, has been promoted to Acting Captain. He is located
at Camp Doniphan, Fort Sill, Okla.
Tlie National Aniline and Chemical Company held its annual
meeting on February iS. Stockholders voted to increase the
number of directors and the following names were added to the
Board: L. C. Jones. Clinton S. Lutkins, R. C. Taggesell and
Orlando F. Weber. The other directors re-elected are J F Schoell-
kopf, J. F. Schocllkopf, Jr., C. P. Hugo Schoellkopf of the
Schoellkopf Aniline and Chemical Works, Inc.; W. Beckers,
Eugene Meyer. Jr., Charles J Thurnauer, of the W. Beckers
Auiline and Chemical Works. Inc.; I F. Stone of the National
Aniline and Chemical Company; Henrv Wigglesworth, J. M.
Goetchius of the General Chemical Company, T. M. Rianhard,
W. II Mclllravy of the Barrett Company; H. H. S. Handy and
E. L. Pierce of the Semet-Solvav Company.
At the adjourned meeting of the board of directors held on
March 12, the following officers were elected for the ensuing
year: President and Chairman of the Board, William J. Mathe-
son; Vice Presidents, William Beckers, Robert Alfred Shaw,
I. P. Stone and C. L. Jones; Treasurer. Henry I. Moody;
Assistant Treasurers, G. W Yates and T. S. Baines; Secretary,
William T. Miller. Assistant Secretary, W. E. Rowley: Chairman
of the Executive Committee, Henry Wigglesworth.
Apr., 191S
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
329
INDUSTRIAL NOTL5
List of Applications Made to the Federal Trade Commission for Licenses Under
the Enemy Act"
Year Pat. No. Patentee Assignee1
1906 837,017 Carl Auer von Welsbach
Vienna, Austria-Hun-
gary
1910 976,760 Carl Auer von Welsbach, Treibaeher Chemische
Vienna, Austria-Hun- Werke Gesellschaft, M.
gary B. H. of Treibach. Aus-
tria-Hungary
1915 1,123,843 Philipp Burger, Berlin
Germany
1903 724,789 Rene Bonn, Mannheim, Badische Anilin & Soda
Germany Fabrik, Ludwigsbafen-
on-the-Rhine. Germany
1904 753,659 Reni Bohn, Mannheim, Badische Anilin & Soda
Germany Fabrik, Ludwigschafen-
on-the-Rhine, Germany
1903 739,145 Rene Bohn, Mannheim, Badische Anilin & Soda
Germany Fabrik, Ludwigschafen-
on-the-Rhine, Germany
1914 1,104,943 Rudolf Uhlenhuth, Farbwerke vorm. Meister
Hochst - on - the - Main, Lucius & Briining,
Germany Hochst - on - the - Main,
Germany
1915 1,145,934 Adolf Steindorff and Rob- Farbwerke vorm. Meister
ert Welde, H6chst-on- Lucius & Briining,
the- Main, Germany Hochst - on - the - Main,
Germany
1907 844,914 Rene Bohn, Mannheim, Badische Anilin & Soda
Germany Fabrik, Ludwigschafen-
on-the-Rhine, Germany
1901 682,523 Ren£ Bohn, Mannheim, Badische Anilin & Soda
Germany Fabrik, Ludwigschafen,
Germany
1903 739,579 Rene Bohn, Mannheim, Badische Anilin & Soda
Germany Fabrik, Ludwigschafen-
on-the-Rhine. Germany
1914 13,848 Georg Korndorfer and Farbwerke vorm. Meister
Reissue Baptist Reuter, Hochst- Lucius & Briining,
on-the-Main, Germany Hochst - on - the- Main,
Germany
1913 1,075,171 Albrecht Thiele & George Chemische Fabrik auf
Wichmann, Berlin, Actien (vorm. E. Scher-
Germany ing), Berlin, Germany
1914 1,101,111 Arthur Zitscher
1912 1,034,853 Adolf Winther, August
Leopold Laska and
Arthur Zitscher
1912 1,042,356 August Leopold Laska
Arthur Zitscher, and
Felix Kunert
1916 1 ,206,232 August Leopold Laska
1915 1,150,863 Richard Just and Fritz
Eckard
1916 1,193.566 Felix Kunert, Offenbach- Chemische Fabrik. Gries-
on-the-Main, Germanv heim-Elektron, Frank-
fort-on-the-Main, Ger-
many
1910 976,760 Carl Auer von Welsbach, Treibaeher Chemische
Vienna, Austria-Hun- Werke Gesellschaft, M.
gary B. H., Treibach, Aus-
tria-Hungary
1915 1,127,027 Felix Kunert & Edwin Chemische Fabrik Gries-
Acker, Offenbach-on- heim-Elektron, Frank
the-Main, Germany fort-on-the-Main, Ger
1 This column in the March issue was incorrectly headed "Assignor."
Enemy Controlled Patents Pursuant to the "Trading with
Patent
Pyrophoric alloy
Depolarizer for galvanic cells
Blue dye and process of mak-
Anthracene derivative and
process of making same
Anthracene dye
Process of producing amino-
anthraquinones
Finely divided vat dyestuffs
and process of making
Process of making £
cene dye
thra-
Blue dye and process of mak-
ing same
Blue coloring-matter
Derivatives of diaminodioxy-
arsenobenzene and process
of making same
Process for the manufacture
of 2-phenylquinolin-4-car-
boxylic acid
ompounds for use in th
production of dyestuffs
Process of producing dye-
stuffs on the fiber by means
of the one-bath method
Applicants
New Process Metals Co ,
New York
French Battery & Carbon
Co., Madison, Wis.
National Aniline & Chemical
Co., 244 Madison Ave.,
New York
National Aniline & Chemical
Co., 244 Madison Ave.,
New York
National Aniline & Chemical
Co., 244 Madison Ave.,
New York
National Aniline & Chemical
Co., 244 Madison Ave.,
New York
National Aniline & Chemical
Co., 244 Madison Ave.,
New York
National Aniline & Chemical
Co., 244 Madison Ave.
New York
National Aniline & Chemical
Co., 244 Madison Ave.,
New York
National Aniline & Chemical
Co, 244 Madison Ave
New York
Farbwerke-Hoechst Co., New
York, N. Y.
E. I. du Pont de Nemours &
Co., Wilmington, Del.
E. I. du Pont de Nemours &
Co., Wilmington, Del.
E. I. du PontdeNe
Co., Wilmington, Del
E. I. du Pont de Nemours &
Co., Wilmington, Del.
E. I. du Pont de Nemours &
Co., Wilmington, Del.
Welsbach Company, Glo
cester City, N. J.
The Aetna Explosives and Chemical Company is to build a
plant at Huntington, Pa., which will be adapted for the manu-
facture of dyes and chemicals after the close of the war, when the
orders for smokeless powder are expected to decrease. The
buildings will cost about $500,000.
Mr. Alexander T. Vogelsang, First Assistant Secretary of the
Interior, recently called a conference of all government officials
in the department interested in oil development. Many mem-
bers of Congress were invited. The purpose of the assemblage
was to discuss the plans for the development of the oil shale lands
of Colorado, Wyoming and adjacent states, and to outline a
iprogram of legislation.
I Acting for the United States Government the Atlas Powder
iCompany has started the construction of a $6,000,000 ammonium
nitrate plant in Maryland.
The Board of Directors of the Chemical Alliance, Inc., have
appointed a Philadelphia subcommittee, as follows: J. S. Coale
of I. P. Thomas and Sons Co., Raymond W. Tunnel of P. W
Tunnel & Co., Inc., Theodore J. Taylor of the American Agricul-
tural and Chemical Company. Mr. Frank Groves of the Groves
Fertilizer Works has been added to the Cincinnati committee.
Local committees for other points are now under Consideration.
Manufacturers at points when- local subcommittees havi been
appointed are urgently requested to confer with SUCfa Committee
on all local transportation matters
Another medical discovery ranking with phenolsulfonephthal-
ein has been announced by Johns Hopkins University. It is
the application of a product called benzyl acetate or benzyl
benzoate as a local anti-spasmodic and a substitute for opium,
or any one of its derivatives, or cocaine, heroin, and other narcotic
alkaloids. The substance itself is not new, but it is the dis-
covery of its peculiar properties in causing a relaxation of the
muscles and producing the same effect as any of the narcotics
mentioned, but without their ill results, that constitutes its
importance. The discovery was made by Dr. David I. Macht,
lecturer on pharmacology and instructor in medicine at the
Medical School.
According to a statement made by Secretary Lane, develop-
ment of American mines would supply 2,000,000 tons of mine nils
now imported and allow vessels now engaged in this work to
carry additional food and supplies to the overseas forces. He
believes that American mines can supple all these essential wai
minerals if given proper assistance by the Federal Government
He has asked Congress to make a special appropriation so that a
large force of metallurgists can set to work immediately on
necessary changes in practice to permit the use of lower grade
manganese ores. He says new mines will be Opened .is permanent
industries and new operators will be informed as to the best
practices. Secretary Lane cites the urgent need for nitrates,
sulfuric acid from pyrites and sulfur, manganese, Hake graphite,
tin, mercury, potash, tungsten, chromite, magnesite and mica.
3$°
THE JOURNAL OF INDUSTRIAL AND ENGINEERING I BEMISTRY Vol. 10, No.
The United States Government will finance the erection and
operation in Canada of a plant, which will cost in the neighbor-
hood of $2,000,000, for the manufacture of acetic acid on a large
scale. Announcement to this effect was made at the annual
meeting of the Shawinigan Water and Power Company, held in
Montreal recently. It is understood that work will be started
immediately on the new plant, which will be a duplicate of the
plant owned and operated by the Shawinigan Water and Power
Company through its subsidiary, the Canadian Electro Products
Company. As the new plant will be financed by the United
States Government, and its affairs will be separate from those
of the Canadian Electro Products Company, it is probable that
a new subsidiary company will be incorporated immediately.
The Bureau of Standards has purchased eight acres of land
west of Connecticut Avenue, Washington, D. C, and has let
contracts for a new engineering laboratory, 175 by 350 feet, and
four stories in height. The new building and its equipment will
cost in the neighborhood of Si, 000,000 and will increase the ca-
pacity of the Bureau by 50 per cent. The Pittsburgh laboratory
of the Bureau, including the work on glass and ceramics, will be
transferred to Washington. It is expected that the new building
will be ready for occupancy during the coming summer.
An announcement by the U. S. Food Administration states
that during 1918 the Government should have for munitions
alone many million pounds of ammonia more than it is possible
to make by working all existing plants producing ammonia in this
country to their maximum capacity. In view of this, a request
for cooperation in the saving of ammonia was sent to 15,000 ice-
making and cold storage firms.
The Ironton Portland Cement Company is erecting a potash
recovery plant. The dust from 2000 barrels of cement will be
handled daily. When it was ascertained that the dust escaping
from Portland cement plants carried a fair percentage of potash,
experiments were undertaken by the Western Precipitation Com-
pany. A year's trial has resulted in a greater income from potash
than from cement.
According to the Textile World Journal paper is being used
extensively in Germany in the manufacture of various articles of
wearing apparel, and recently at Chemnitz an exhibition of such
goods and paper yarns was held. The German weavers, on
account of the lack of yarns of other material, are making in-
creasing use of paper. It is expected that the paper yarns will
soon be requisitioned by the Government for the needs of the
army. The consumption is so great that the mills cannot satisfy
the demands.
The stock of the Schutte and Koerting Company has been
transferred to the Alien Property Custodian of the United States
and on February 23, at his instance, the Board of Directors
was reconstructed as follows: E. Pusey Passmore, governor
of the Federal Reserve Bank, Philadelphia; Ralph J. Baker,
assistant general counsel of the Alien Property Custodian; D. W.
Hildreth, treasurer of Schutte and Koerting Co.; T. H. John-
ston of Schutte and Koerting Co.; Chas. S. Calwell, president
of the Corn Exchange National Bank, Philadelphia. The new
board elected the following officers: President, Chas. S. Cal-
well; Treasurer, I). W. Hildreth; Secretary, Ralph J. Baker.
According to information received from K. P. McElroy who
handled the patent and case, Judge Geiger in the federal court
at Milwaukee has rendered decision holding that the patent
824,906 granted H. O. Chute for process of making wood alcohol
is valid and infringed by the Wisconsin Chemical Co. at Hackley,
Wis. The patent claims the process of making wood alcohol
from pyroligneous liquor by distilling the crude acid through a
continuous column or "beer" still to produce a distillate of about
24 per cent alcohol from which the oils separate readily and this
alcohol is treated with excess of alkali and redistilled in con-
tinuous column stills, producing perfectly miscible alcohol of
greater than 82 per cent strength. The process and apparatus
was introduced by the patentee at Ashland, Wis., in 1905, and
later in the year the Cleveland Cliffs Co. bought apparatus and
license for their plants at Marquette and Gladstone. Later
it was used at Manistique, Newberry and Antrim, Mich. In
1907 the Lake Superior Iron and Chemical Co. bought license
for its use at Ashland, Newberry, Manistique, and Elk Rapids.
Suit was brought against the Antrim Chemical Co. and com-
promised by their purchasing a license. About 1200 cords of
wood were worked daily under this patent process. The Wis-
consin Chemical Co. at Hackley put in a plant and used the
process, and suit was begun against them in 19m) with the final
determination of the validity of the patent as indicated by the
above decision.
The New Jersey State Board of Public Utility Commissions
has extended for thirty days the order of January 26 last, allowing
the Public Service Gas Company to lower its gas standard. This
action was brought about by the urgent request from the produc-
tion division of the Army Ordnance Department of the United
States Government to recover as much toluol as possible for the
manufacture of explosives.
Considerable interest has been aroused in the non-combusti-
ble substitute for celluloid which has been invented by a pro-
fessor in a Japanese university, and for the manufacture of
which a company has been organized in Japan. The factory
buildings are now in course of construction and it is planned
to begin in April of this year, or soon after, the manufacture of
waterproof cloth, composition tiles and insulators. As soon
as the machinery, which has been oidered in the United States,
arrives, the manufacture of imitation leather, linoleum, stained
glass, marble, lacquers and varnishes will be started. Patent
rights have been obtained for the process in Japan and have
been applied for in Great Britain, France and the United States.
Of the twenty-one patents applied for in this country, eleven
have actually been granted under date of November 6, 1917,
and bear serial numbers 1,245,818 and 1,245,975 to 1,245,984,
inclusive. Copies of these patents may be obtained from the
U. S. Patent Office, Washington, D. C.
One molybdenum mill is completed and two are about to start
operations in Summit County, Colorado. The mill at Climax,
Colorado, is turning out a high-grade molybdenite concentrate,
said to be solely for Government use. One mill at Camp Urad,
near Empire, Colorado, will have a daily output of 250 tons of
the ore.
A company has been organized in Sweden for the utilization
of the enormous peat deposits by the Wielandt process of dis-
tillation, by which a coke is produced. By-products include
ammonium sulfate, wood alcohol, acetic acid, tar, motor fuels,
lubricating oils, creosote, hard and soft paraffin, and pitch.
According to the Journal of Commerce, scarcity of phosphate
rock has become so acute that several sulfuric acid plants will
be forced to close, owing to their inability to store acid which
ordinarily is mixed immediately on manufacture with the phos-
phate. Another serious side to the phosphate rock situation is
the fact that fertilizer shipments are being delayed.
The Newago Portland Cement Company, Newago, Mich.,
has contracted with the Western Precipitation Company of
Los Angeles for the necessary equipment to recover potash by
the Cottrell process from the fumes of its cement plant. The
Newago plant uses limestone and shale from quarries in northern
Michigan, and has an output of about 70,000 barrels of cement
per month. The mill uses what is known as the wet process of
manufacturing cement. The best feature of this new industry
is that it is certain to be permanent! The initial cost of in-
stallation of equipment is high, but the operating cost is
trifling.
The Government will shortly take over the Dow Chemical
Company's plants at Midland and Mount Pleasant, Michigan,
and will advance ?j ,000,000 for enlargement and new equipment
in order to adequately supply the chemicals needed in the
manufacture of munitions. Mr. Dow will continue in the
management, but otherwise the plants will be conducted as
Government industries.
One of the first American owned and controlled companies
to receive a license for the manufacture of drugs formerly made
in Germany was the Rector Chemical Company, 2 Rector Street,
New York, which holds license No. 5 for the manufacture of
"Procaine," the drug introduced by the Germans as "Novocain."
The German patent is set forth in the license. The manufac-
turing process has been approved by the Federal Trade Com-
mission, which will have supervision of samples, tests and the
price charged. The Farbwerke-Hoechst Company also holds a
license for making "Procaine," but neither that company nor
H. A. Metz has any interest in the Rector Chemical Company.
A published statement that Mr Met/ owned the stock of the
Rector Company was an error, it being the Farbwerke-Hoechst
Company, only, in which Mr. Metz is interested. The two com-
panies are competitors in the manufacture of "Procaine." The
name is a contraction of pro-cocaine, the drug being a substitute
for cocaine, as explained by Dr. Julius Stieglitz in an article in
the Journal of the An. ■ Association of February 23,
who announces that the Rector Chemical Company has had the
assistance of Professor Bailey of the University of Texas in per-
fecting their manufacturing processes.
Apr., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
33i
GOVERNMENT PUBLICATIONS
By R. S. McBridb, Bureau of Standards, Washingto
NOTICE — Publications for which price is indicated can be
purchased from the Superintendent of Documents, Government
Printing Office, Washington, D. C. Other publications can
usually be supplied from the Bureau or Department from which
they originate. Commerce Reports are received by all large
libraries and may be consulted there, or single numbers can be
secured by application to the Bureau of Foreign and Domestic
Commerce, Department of Commerce, Washington. The regu-
lar subscription rate for these Commerce Reports mailed daily is
$2.50 per year, payable in advance, to the Superintendent of
Documents.
GEOLOGICAL SURVEY
Geologic Structure in the Cushing Oil and Gas Field, Okla-
homa, and Its Relation to the Oil, Gas, and Water. C. H.
Beal. Bulletin 658. 61 pp. The geologic work done in the
field has disclosed the following principal facts: (1) The fold-
ing of the formations in the Cushing field usually becomes
greater with increase of depth, and there are many marked differ-
ences in structure among the Layton, Wheeler, and Bartles-
ville sands and the surface beds. (2) The interval between the
Layton and Bartlesville sands is generally greater around the
edges of the anticlines than on their crests. (3) The distribution
of the bodies of oil, gas, and water indicates that the source of
the oil lies west of the Cushing field. (4) In general, the oil area
in an elongated dome, where folding is simple, extends farther
down on the long axes of the anticline or dome than on the steeper
sides. (5) The water surfaces on which the oil and gas rest in
the different sands are not level but are inclined away from the
centers of the anticlinal folds.
Tin Resources of the Kings Mountain District, North Carolina
and South Carolina. A. Keith and D. B. SterrETT. Bulletin
660-D, from Contributions to Economic Geology, 1917, Part 1.
24 pp. Published December 10, 1917. "The presence of cas-
' siterite, oxide of tin, at many places in the Kings Mountain and
Lincolnton quadrangles, at one place near Gaffney, in the
Gaffney quadrangle, and at one locality in the Gastonia quad-
rangle, has led to much prospecting and to attempts at mining.
In at least one place — the Ross mine, near Gaffney — placer
mining was temporarily done at considerable profit. Several
prospects have also been opened in the Lincolnton and Gastonia
quadrangles north and northeast of the Kings Mountain quad-
rangle. Practically all the work on cassiterite-bearing veins
has been done at a loss, but this work has not been sufficiently
conclusive to prove or disprove the value of some of the deposits."
Louisiana Clays Including Results of Tests Made in the
Laboratory of the Bureau of Standards at Pittsburgh. G. C.
Matson. Bulletin 660-E, from Contributions to Economic
Geology, 1917, Part 1. 12 pp. Published November 26, 1917.
The Antimonial Silver-Lead Veins of the Arabia District,
Nevada. A. Knopf. Bulletin 660-H, from Contributions to
Economic Geology, 191 7, Part 1. 7 pp. Published January
I7, 1918. "The Arabia district, in Humboldt County, Nev.,
I is an old mining camp which, long idle after its first period of
^activity in the late sixties, has again become active under the
itimulus of the present high prices of lead, antimony, and silver."
Mining Developments and Water-Power Investigations in
Southeastern Alaska. T. Chapin, H. M. Eakin and G. H.
Canfiei.d. Bulletin 662-B, from Mineral Resources of Alaska,
1916-B. 92 pp.
The Gold Placers of the Tolovana District, Alaska. J. B.
Mertib, Jr. Bulletin 662-D, from Mineral Resources of
Alaska, 1916-D. 57 pp.
Gold Placers of the Anvik-Andreafski Region, Alaska. G. L.
Harrington. Bulletin 662-F, from Mineral Resources of
Alaska, 1916-F. 17 pp.
Lode Deposits and Gold Placers near the Nenana Coal
Field, Alaska. R. M. Overbeck and A. G. Maddren. Bulle-
tin 662-G, from Mineral Resources of Alaska, 1916-G. 52 pp.
Lode Mining in the Fairbanks District, Alaska. J. B. Mertie,
Jr. Bulletin 662-H, from Mineral Resources of Alaska, 1916-H.
22 pp.
K Bibliography of North American Geology for 1916, with Sub-
ject Index. J. M. Nickles. Bulletin 665. 100 pp. The
bibliography of North American geology, including paleontology,
petrology, and mineralogy, for the year 1916 follows the plan
and arrangement of its immediate predecessors. It includes
publications bearing on the geology of the continent of North
America and adjoining islands; also Panama and the Hawaiian
Islands. Papers by American writers on the geology of other
parts of the world are not included. Textbooks and papers,
general in character, by American authors are included ; those by
foreign authors are excluded unless they appear in American
publications.
Zinc Carbonate and Related Copper Carbonate Ores at
Ophir, Utah. G. F. Loughlin. Bulletin 690-A, from Contri-
butions to Economic Geology, 1918, Part 1. 14 pp. Published
December 24, 191 7. From the processes of deposition here
described it is to be expected that bodies of lamellar zinc car-
bonate like those at Ophir will prove to be of high grade, owing
to the complete removal of limestone, but of small dimensions
and confined to the immediate vicinity of fractures and open
bedding planes. Such small bodies are not likely to lead to
larger bodies of massive ore, unless they lie near to ground-
water level, or to some impervious stratum or fault that im-
pounded the waters containing the oxidized compounds of zinc.
In districts where mixed sulfide deposits in limestone contain
both copper and zinc in considerable quantity the resulting
carbonate ores of both metals are to be expected in the oxidized
zone, the copper carbonate immediately below the position of
the original sulfide body or its siliceous casing, and the zinc
carbonate below the copper carbonate. The details of these
relations, as well as the richness and size of the carbonate bodies,
depend on such local factors as the purity and permeability of
the limestone replaced and the relative openness of bedding planes
and fractures, which must be determined for each deposit or
group of deposits.
The Helderberg Limestone of Central Pennsylvania. J. B.
REESIDE, Jr. Professional Paper 108-K, from Shorter Con-
tributions to General Geology, 1917. 41 pp. Published
December 13, 191 7.
Chemical Analyses of Igneous Rocks. H. S. Washington.
Professional Paper 99. 1182 pp. Paper, $1.75. This is a
revision and expansion of Professional Paper 14. It contains
more than a thousand large pages of tabulations of rock analyses.
These are arranged according to the character of the rock and
form probably the most complete summary of analyses ever
prepared. The report can be obtained from the Superintendent
of Documents at $1.75 per copy.
BUREAU Or CENSUS
Cast-iron Pipe. Census of Manufactures 1914. Separate.
7 pp. This and the following separates are each one of a series
of bulletins being issued by the Bureau, presenting statistics
of industries concerning which inquiries were made at the quin-
332
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No.
quennial census of manufactures in \>>\\. Statistics arc pre-
sented in three sections: Suiiiniar- , giving general
data compiled fur industry; special statistics relating to materials,
products, and methods of manufacture; and Slate tallies, giving
comparative summary, by States, for 1904, 1909 and 1914.
and detailed statistics [or industry, by States, [914
Iron and Steel. Census of Manufactures, 1 9 1 4 . Separate.
68 pp.
Brass, Bronze and Copper Products. Census of Manufactures,
1914. Separate. 11 pp.
Canning and Preserving. Census of Manufactures, 1914.
Separate. 31 pp.
Manufacture of Buttons. Census of Manufactures, 1914.
Separate. 9 pp.
Miscellaneous Textiles. Census of Manufactures, 1914.
Separate. 27 pp.
Silk Industry. Census of Manufactures, 1914. Separate.
24 pp.
BUREAU OF MINES
Seventh Annual Report of the Director. For the fiscal year
ended June 30, 1917. 106 pp. Paper, 15 cents.
Directions for Sampling Coal for Shipment or Delivery.
G. S. 1'ope. Technical Paper 133. 15 pp. Paper, 5 cents.
"In the field work of the Bureau of Mines need has arisen for a
circular giving brief directions for sampling coal at points in the
field where the conditions for sampling are not fixed, and usually
no such facilities are at hand for methodically collecting and pre-
paring samples as are available at power plants that regularly
receive and sample coal. Frequently there is need of sampling
a special shipment of coal as it is loaded into railroad cars at
lb. nunc or as it is unloaded from railroad cars into bins or ships,
and at such times there is need of printed instructions regarding
hand methods of sampling. This paper has been prepared to
meet the need stated and is issued in the hope that it will be of
service in the collection and preparation by hand of samples of
coal in the field."
Gypsum Products: Their Preparation and Uses. R. W.
Stone. Technical Paper 155. 64 pp. Paper, 20 cents.
This paper has been prepared by R. W. Stone, of the U. S.
Geological Survey, from information collected by him in the
course of a comprehensive investigation of the gypsum deposits
in the United States for the Geological Survey. The distribu-
tion of the deposits, their extent, their stratigraphic relations,
and the conditions under which they formed will be described
in a Survey bulletin. This report discusses the methods of
mining or quarrying gypsum, the equipment and operation of
plants for reducing the crude rock to commercial plaster, and
the various forms in which gypsum products are marketed.
Although a minor industry, the manufacture of gypsum
possesses decided importance. In 1915 the total amount of
calcined plaster produced in this country amounted to 1,613,720
short ton ,.946,018, and the total value of all gypsum
products was approximately $7,000,000. Sixty-eight plants
ed in the production of gypsum and the manufacture
"I gypsum products, and these plants represented a capital
investment oi pmii.ii.lv not less than $20,000,000.
In vuw ..1 ih, greatei attention being given to fire resistance
and othet desirable features of construction, the use of gypsum
products in buildings 1-; 1 •., \lso, as manu-
industries become more varied and refined, the use
tm product i"i othei purposes than in building- will
Pol these reasons this papet is printed bj the
Bureau ol Mines in th( hope that it will aid the development
and utili itio ountry's mini 1 and h ill
thereby promote tin advancementfof the general welfan
Compressibility of Natural Gas and Its Constituents, with
Analyses of Natural Gas from 31 Cities in the United States.
G. A. BfKREi.i, and I. W. Robertson. Technical Paj
1'' pp. Paper, 5 cents. "As a continuation of the work de-
scribed in a previous publication of the Bureau of Mines, which
1 the compressibility of the natural gas used in Pitts-
burgh, Pa., at pressures ranging from atmospheric up to 35.5
atmospheres, this paper shows the compressibility of three of
the hydrocarbon gases (methane, ethane, and propane) that
comprise natural gas, of carbon dioxide f another constituent
of natural gas), and of natural gas from nine different cities.
In addition, it contains analyses of natural gas from 31 cities
and presents a formula by which the compressibility of any
natural gas can be determined from the analysis. Data regard-
ing other analyses and the composition and characteristics of
natural gas, are given in previous publications of the Bureau
of Mines."
Methods for Increasing the Recovery from Oil Sands. J O.
Lewis. Bulletin 148. 120 pp. Paper, 15 cents. "In the
face of a demand that is increasing faster than the production
and that, in the consensus of opinions of well-informed authorities,
is soon likely to outstrip the productive capacity, it is well
to consider whether it is not possible to extract more oil from
1 the known sources of supply. It is universally acknowledged
that by the usual production methods much oil is left under-
ground, the general opinion being that at least 50 per cent of
the oil in a field remains unrecovered when the field is abandoned
as exhausted. From the writer's own investigations he believes
the average recovery is even less, and if any considerable por-
tion of this oil being left underground could be made available
it would have a tremendously favorable influence on the petroleum
industry and all the industries dependent on it.
"In this publication are considered the principles involved
in increasing recovery and methods of extracting more oil from
the oil-bearing formations than by the usual ways of producing.
These methods are: The use of gas or vacuum pumps, forcing
compressed air or gas through the oil-bearing formations, dis-
placing the oil by water, and better utilization of the natural
pressures in the oil-bearing formations. Especial attention is
being given to a process commonly known as the Smith-Dunn
for forcing compressed air through oil-bearing formations be-
cause it is believed to hold most promise for the future."
DEPARTMENT OF AGRICULTURE
The Expansion and Contraction of Concrete and Concrete
Roads. A. T. Goldbeck and F. H. Jackson, Jr. Contri-
bution from the Office of Public Roads and Rural Engineering.
Bulletin 532. 31 pp. Paper. 10 cents. Issued October 13.
Increased Yield of Turpentine and Rosin from Double Chipping.
A \V. SCHORGBR AND R. I. PbttigrBW. Bulletin 567. Con-
tribution from the Forest Service. 9 pp. Paper. 5 cents.
Issued October 2. Describes a method of securing more nav
stores from the same tree, and is of interest to all naval-sto
operators.
The Recovery of Potash as a By-Product in the Cement
Industry. \Y. H. Ross. A R. Mkrz and C. R. Wac-.ner.
Bulletin 572. Contributions from the Bureau of Soils. 23 pp.
cents. Issued October 5. A discussion of the possi-
bility of recovering potash from waste in cement-producing
plants and .1 description of the various processes used.
A Guide for Formulating a Milk Ordinance. Prepared in
the Dairy Division of the Bureau of Animal Industry' and the
Bureau of Chemistry. Bulletin 585. Contribution from the
Bureau of Animal Industry and the Bureau of Chemistry. 4 PP-
Paper, 5 cents Issued October 18. Of interest to town. city.
and other officials interested in the improvement of the milk
supply.
* Apr., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
333
NEW PUBLICATIONS
By Irene DeMatty, Librarian. Mellon Institute of Industrial Research, Pittsburgh
Agricultural Bacteriology. H. W. Conn. 8vo. 357 pp. Price, $2 00.
P. Blakiston's Son & Co., Philadelphia.
Analysis: Essentials of Volumetric Analysis. H. W. Schimpf. 3rd Ed.
8vo. 366 pp. Price, $1 60 John Wiley & Sons, Inc., New York.
Analysis: Qualitative Analysis Section of Chemistry by Experimentation.
W. F. Hoyt. 12mo. 160 pp. Price, $0.25. D. Van Nostrand & Co.,
New York.
Analysis: Quantitative Chemical Analysis. F. Clowes and J. B. Cole-
man. 11th Ed. 8vo. 604 pp. Price, 12s. 6d. J. & A. Churchill,
London.
Analysis: Standard Methods of Chemical Analysis. W. W. Scott. 2nd
Ed. 8vo. 898 pp. Price. $6.00. D. Van Nostrand Co., New York.
British Grasses and Their Employment in Agriculture. S. F. Armstrong.
8vo. 199 pp. Price, $2.00. G. P. Putnam's Sons, New York.
Chemistry: Travaux pratiques de chimie general. G. Lepercq. 8vo.
83 pp. M. Girard et E. Briere, Paris.
Coking: Modern Coking Practice. J. E. Christopher. 8vo. 124 pp.
Price, 7s. 6d. Crosby Lockwood 8c Son, London.
Dyes and Dyeing. C. E. Pellew. 12mo. 274 pp. Price, $2.00. Robert
M. McBride, New York.
Earthenware: Notes on the Manufacture of Earthenware. E. A. Sande-
man. I2mo. 375 pp. Price, $3.00. D. Van Nostrand Co. New
York.
Electrochemistry: L'Electrochimie et l'Electrometallurgie. A. Le
sbur. 8vo. 267 pp. Price, 9 fr. H. Dunod et E. Pinat, Paris.
Fans, Heaters and Air Washers. B. F. Sturtevant Co. 4to. 959 pp
Price, $7.50. The Author, Boston.
Food: Its Composition, Preparation and Effects. J. H. Tilden. 12mo
306 pp. Price, $3.50. The Author, Denver, Col.
Forging: A Manual of Practical Instruction. J. Jernberg. 8vo. 131 pp
Price, $1.00. American Technical Society, Chicago.
Fresh Water Biology. H. B. Ward and G. C. Whipple. 8vo. 1111 pp
Price, $6.00. John Wiley & Sons, Inc., New York.
Fuels: The Calorific Power of Fuels. Herman Poole. 3rd Ed. 8vo
267 pp. Price, $3.00. John Wiley & Sons, Inc., New York.
Gas Chemists' Handbook. 8vo 354 pp. Price, $3.50. American Gas
Institute, New York.
Gas-Engine Handbook. E. W. Roberts. 12mo. 315 pp. Price, $2.00.
Gas Engine Pub. Co., Cincinnati.
Gas, Gasoline and Oil Engines. G. D. Hiscox. 22nd Ed. 8vo. 640
pp. Price, $2.50. Norman W. Henley Pub. Co., New York.
History of Commerce and Industry. C. Herrick. 8vo. Price, $2.00.
The Macmillan Co., New York.
Industrial Chemistry: L'Enseignement de la chimie industrielle en France.
E. Grandmouoin. 16mo. 185 pp. Price, 3fr.50. H. Dunod et E.
Pinat, Paris.
Internal Combustion Engine Manual. F. W. Sterling. 4th Ed. 8vo.
168 pp. Price, $2.00. D. C. R. Beresford, Washington, D. C.
Iron Prices: Complete List of Base Prices, Differentials, and Extras on
Iron, Steel and Non-Ferrous Products. Penton Publishing Co. 8vo.
42 pp. Price, $2.00. Penton Pub. Co., Cleveland.
Metals: A la recherche de deux metaux inconnus. Max Gerber. 8vo.
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Microscopic Analysis of Cattle Foods. T. N. Morris. 12mo. 74 pp.
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Oils and Fats: Aids to the Commercial Analysis of Oils, Fats and Their
Commercial Products. G. F. Pickering. 8vo. 141 pp. Price,
7s. 6d. Charles Griffin 8; Co., London.
Oils and Fats: Technical Handbook of Oils, Fats and Waxes. P. J. Fryer,
and F. E. Weston. 8vo. 279 pp Price, $3.00. G. P. Putnam's Sons,
New York
Organic Chemistry Including Certain Portions of Physical Chemistry.
H. D Haskins. 12mo. 472 pp. Price, $2.00. John Wiley & Sons
Inc., New York.
Sands: A Supplementary Memoir on British Resources of Sands and
Rocks Used in Glass Manufacture. P. G. H. Boswell. 8vo. 92 pp.
i on. Longmans. Green & Co., New York.
Staining and Polishing. Including Varnishing and Other Methods of Fin-
ishing Wood. 8vo. 218 pp Price. 3s. 6d, Evans Bros., London.
Steam Engines: Les Machines & vapeur. P. Cordier. 18mo. 402 pp.
Octave Doirj et fils. Paris.
Steel and Its Heat Treatment. D. K Bi-i.lkns. 2nd Ed. 8vo. 483 pp.
Price, $4.00 John Wiley 8: Sons. Inc., New York
Technical Mechanics, Statics and Dynamics. I-;. K. Mai klk 8vo. 381
pp. Price, $2.75. John Wiley & Sons, Inc., New York.
Thermodynamics: Notes on Thermodynamics. II W SPAHOLBR. 12mo.
77 pp. Price, $1.00. John Wiley & Son-;. Inc., New York.
Transmission Gears. V. I 164 pp. Price, 8s. 6d. Charles
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Wood: Seasoning of Wood. J. B. Wagner. 8vo. 274 pp. Price, $3.00.
D. Van Nostrand Co.. New York.
RECENT JOURNAL ARTICLES
Absorption Refrigerating Machines. F. C. Spangler. Power, Vol. 47
(1918), No. 8, pp. 274-277.
Acetylene: Characteristics and Properties of Acetylene. G. G. Pond.
Journal of Acetylene Lighting, Vol. 19 (1918), No. 9, pp. 295-297.
Acid Making: Theory and Practice of Acid Making. E. R. Barker.
Paper, Vol. 21 (1918), No. 23, pp. 24-28.
Bauxite Products. J. M. Hill. Mining and Scientific Press, Vol. 116
(1918), No. 8, pp. 267-268.
Blast Furnace: Description of Manchurian Blast Furnace. C. F. Wang.
Blast Furnace and Steel Plant, Vol. 6 (1918), No. 3, pp. 109-111.
Bleaching: Notes on Bleaching Cotton. J M. Matthews. Color Trade
Journal, Vol. 2 (1918), No. 2. pp. 53-58.
Burner-Gas Cooling. A. S. CoscER. Paper, Vol. 21 (1918), No. 23,
pp. 19-24.
By-Product Coke Oven and Its Products. W. H. Blauvelt. Transac-
tions of the American Institute of Mining Engineers (1918), No. 135, pp.
597-614.
Canvas Tubing for Mine Ventilation. L. D. Frink. Mining and Scien-
tific Press, Vol 116 (1918), No. 7, pp. 223-227
Cellulose: The Estimation of Cellulose in Wood. B. Johnsen and R. W.
Hovey. Paper, Vol 21 (1918), No. 23, pp. 36-52.
Colors: The Action of Carbonate of Lead, Sulfate of Lead and Zinc Oxide
on Tinting Colors. G. B. Heckel. Paint and Varnish Record, Vol. 14
(1918), No. 3. pp. 10-16.
Dextrine: The Development of the American Dextrine Industry. Joseph
Morningstar. Color Trade Journal, Vol. 2 (1918). No. 2, pp. 67-69.
Dyestuffs of the Ancients. C. E. Pellew. Color Trade Journal, Vol. 2
(1918), No. 2, pp. 50-52.
Engineering and Cooperation. I. N. Hollis. Journal of the Cleveland
Engineering Society, Vol 10 (1918), No. 4, pp. 225-250.
Filtration: Plate- and Frame-Filtration. D. R. Sperry. Metallurgical
and Chemical Engineering, Vol. 18 (1918), No. 5, pp. 258-260.
Furnaces: High-Temperature Resistance Furnaces. W. E. Ruder.
Mining and Scientific Press, Vol. 116 (1918), No. 9, pp. 301-303.
Glass: Some Common Problems in Melting and Working Glass. W. E.
S. Turner. Journal of the Society of Glass Technology, Vol. 1 (1917),
No. 4, pp. 210-213.
Glass: The Use of Semi-Automatic Glass Making Machinery in America.
R. E McCaulEy. Journal of the Society of Glass Technology, Vol.1
(1917), No. 4, pp. 203-209.
Inorganic Chemical Synonyms. E R Darling. The Chemical Engineer,
Vol. 26 (1918), No. 3, pp. 107-112.
Leather: The Making of Artificial Leather. DuPonl Magazine, Vol. 8
(1918), No. 2, pp. 8-10.
Lubrication: Notes on the Theory of Lubrication. Lord Raleigh Philo-
sophical Magazine, Vol. 35 (1918). No. 205, pp. 1-12.
Manchuria Coal and Iron Deposits. C F Wang. The Iron Trade Re-
view, Vol. 62 (1918), No. 7, pp. 433-435.
Manganese: Estimation of Manganese in Aluminum Alloys and Dust.
J. E. Clennell. Engineering and Mining Journal, Vol. 105 (1918),
No. 9, pp. 407-410.
Metallography of Aluminum. R. J. Anderson Metallurgical and Chem-
ical Engineering, Vol. 18 (1918). No. 4, pp. 172-178.
Mineral Blues. C S Weiirly Color Trade Journal, Vol. 2 (1918), No. 2,
pp. 71-73.
Nickel and Brass Plating of Die Castings. R. J. Hazucha. The Metal
Industry, Vol. 16 (191X1. No 2, l> 83
Nickel Silver: Some Uses and Properties of Nickel Silver as Applied to
the Optical Trade. ('. C Holder. The Metal Industry, Vol. 16
(1918), No. 2, pp. 69
Nitrocellulose from Wood Pulps. \Y E B Maker. Paper, Vol. 21 (1918),
No. 23, pp 78-82.
Occluded Gases in Ferrous Alloys. (".. Alleman and C. J. Darlington.
Journal of the Franklin Institute, Vol. 185 (1918), No. 2, pp. 161-198.
Paper: Practical Paper Making. J J Sullivan Pulp and Paper
ine, Vol. 16 (1918), No. 8, pp. 173 1/6.
Paper: A Review of Pulp and Paper Manufacturing in Canada. A 1.
DAWB. Pull, an.l Papi I 16 (1918), No. 9, pp. 207-209.
Porcelain: Experimental Investigation of Porcelain Mixes. ('. r
\ Klinefelter. I fa not, Vol. IS (1918), No. 3,
Potash Recovery from Blast Furnace Dust, k A BERRY and I' " M'
Arthur. Blast Furnace 'n,,l Steel riant. Vol, 6 (1918), No 3, pp. 130-
134.
334
MARKET REPORT— MARCH, 1918
WHOLESALE PRICES PREVAILING IN THE NEW YORK MARKET ON MARCH 20, 1918
INORGANIC CHEMICALS
Acetate of Lime 100 Lbs.
Alum, ammonia, lump 100 Lbs.
Aluminum Sulfate, high-grade Lb.
Ammonium Carbonate, domestic Lb.
Ammonium Chloride, white Lb.
Aqua Ammonia, 26°, drums Lb.
Arsenic, white Lb.
llarium Chloride Ton
Barium Nitrate Lb.
Barytes, prime white, foreign Ton
Bleaching Powder, 35 per cent 100 Lbs.
Blue Vitriol Lb.
Borax, crystals, in bags Lb.
Boric Acid, powdered crystals Lb.
Brimstone, crude, domestic Long Ton
Bromine, technical, bulk Lb.
Calcium Chloride, lump, 70 to 75% fused Ton
Caustic Soda, 76 per cent 100 Lbs
Chalk, light precipitated Lb.
China Clay, imported Ton
Feldspar Ton
Fuller's Earth, foreign, powdered Ton
Fuller's Earth, domestic Ton
Glauber's Salt, in bbls 100 Lbs.
Green Vitriol, bulk 100 Lbs.
Hydrochloric Acid, commercial, 20" Lb.
Iodine, resublimed Lb.
Lead Acetate, white crystals Lb
Lead Nitrate Lb.
Litharge, American Lb.
Lithium Carbonate Lb.
Magnesium Carbonate, U. S. V Lb.
Magnesite, "Calcined" Ton
Nitric Acid, 40° Lb.
Nitric Acid, 42° Lb.
Phosphoric Add, 48/50% Lb.
Phosphorus, yellow Lb.
Plaster of Paris Bbl.
Potassium Bichromate, casks Lb.
Bromide, granular Lb.
Carbonate, calcined, 80 @ 85%.. .Lb.
Chlorate, crystals, spot Lb.
Cyanide, bulk, 98-99 percent Lb.
Hydroxide, 88 ® 92% Lb.
Iodide, bulk Lb.
Nitrate Lb.
Permanganate, bulk Lb.
, flask 75 Lbs.
Red Lead, American, dry Lb.
Salt Cake, glass makers' Ton
Stiver Nitrate Oz.
Soapstone, in bags Ton
Soda Ash, 58%. in bags 100 Lbs.
Sodium Acetate Lb.
Sodium Bicarbonate, domestic 100 Lbs.
Sodium Bichromate Lb.
Sodium Chlorate Lb.
Sodiu
Sodiu
Sodiu
Sodiu
Sodiu
Sodiu
Potassiu
Potassiu
Potassiu
Potassiu
Potassiu
Potassiu
Potassiu
Potassiu
Quicksili
Cyanide Lb.
Fluoride, commercial Lb.
Hyposulfite 100 Lbs.
Nitrate, 95 per cent, spot 100 Lbs.
Silicate, liquid, 40° Be 100 Lbs.
Sulfide, 60%, fused in bbls Lb.
Sodium Bisulfite, powdered Lb.
Strontium Nitrate Lb.
Sulfur, flowers, sublimed 100 Lbs.
Sulfur, roll 100 Lbs.
Sulfuric Acid, chamber 66" Bt Ton
Sulfuric Acid, oleum (fuming) Ton
Talc, American white Ton
Terra Alba, American, No. 1 100 Lbs.
Tin Bichloride, 50° Lb.
Tin Oxide Lb.
White Lead, American, dry. Lb,
Zinc Carbonate Lb.
Zinc Chloride, commercial l.lt.
Zinc Oxide, American process XX '
V/i
@
3
11
@
u'/
15 'A
@
16
26
@
27
16V.
@
17
65.00
@
85.00
9'/,
@
11
40.00
in,
45.00
2.25
in.
2.50
9'/.
@
9>A
7'A
@
8>A
13 'A
@
15
nominal
75
@
85
25.00
@
30.00
4.25
in.
4.50
4'A
@
5
15.00
a
30.00
8.00
@
15.00
nominal
20.00
@
30.00
1.75
a
3.00
1.15
a
1.25
2>A
a
2'A
4.25
@
4.30
40.00 @ 65.00
1.60
2.00
nominal
83 'A
@
84
3.75
w
4.00
28
a
30
4.00
@
4.10
20.00
a
125.00
10
a.
10'A
20.00
a
25.00
56'A
a
57'/.
10.00
a
12.50
2.65
a
2.70
nominal
2.25
4.05
©
4.50
3.70
©
4.10
45.00
@
50.00
75.00
®
80.00
15.00
@
■ 17V
18.00
23'A
@
24'/i
75
®
80
9
®
9'A
ORGANIC CHEMICALS
Acetanilid, C. P.. in bbls Lb.
Acetic Acid, 56 per cent, in bbls Lb.
Acetic Acid, glacial, 99'/i%, in carboys Lb.
Acetone, drums Lb.
Alcohol, denatured, 180 proof Gal.
Alcohol, sugar cane, 188 proof Gal.
Alcohol, wood, 95 per cent, refined Gal.
Amyl Acetate Gal.
Aniline Oil, drums extra Lb.
Benzoic Acid, ex-toluol Lb.
Benzol, pure Gal.
Camphor, refined in bulk, bbls Lb.
Carbolic Acid, U. S. P., crystals, drums Lb.
Carbon Bisulfide Lb.
Carbon Tetrachloride, drums, 100 gals Lb.
Chloroform Lb.
Citric Acid, domestic, crystals Lb.
Creosote, beech wood Lb.
Cresol, U. S. P Lb.
Dextrine, corn (carloads, bags) Lb.
Dextrine, imported potato Lb.
Ether, U. S. P. 1900 Lb.
Formaldehyde, 40 per cent Lb.
Glycerine, dynamite, drums included Lb.
Oxalic Acid, in casks Lb.
Pyrogallic Acid, resublimed, bulk Lb.
Salicylic Acid, U.S. P Lb.
Starch, cassava Lb.
Starch, corn (carloads, bags) pearl 100 Lbs.
Starch, potato, Japanese Lb.
Starch, rice Lb.
Starch, sago flour Lb.
Starch, wheat Lb.
Tannic Acid, commercial Lb.
Tartaric Acid, crystals Lb.
OILS, WAXES, ETC.
Beeswax, pure, white Lb.
Black Mineral Oil, 29 gravity Gal.
Castor Oil, No. 3 Lb.
Ceresin, yellow Lb.
Corn Oil, crude 100 Lbs.
Cottonseed Oil, crude, f . o. b. mill Lb.
Cottonseed Oil, p. s. y 100 Lbs.
Menhaden Oil, crude (southern) Gal.
Neat's-foot Oil, 20° Gal.
Paraffin, crude, 118 to 120 m. p Lb.
Paraffin Oil, high viscosity Gal.
Rosin, "F" Grade, 280 lbs Bbl.
Rosin Oil, first run Gal.
Shellac, T. N Lb.
Spermaceti, cake Lb.
Sperm Oil, bleached winter, 38° Gal.
Spindle Oil, No. 200 Gal.
Stearic Acid, double- pressed Lb.
Tallow, acidless Gal.
Tar Oil, distilled Gal.
Turpentine, spirits of Gal.
METALS
Aluminum, No. 1, ingots Lb.
Antimony, ordinary Lb.
Bismuth, N. Y Lb.
Copper, electrolytic Lb.
Copper, lake Lb.
Lead, N. Y Lb.
Nickel, electrolytic Lb.
Platinum, refined, soft Ox.
.Oz.
4.90
@
5.00
1.35
@
1.37
5.50
@
5.75
98'/i
6.30
lov,
18.65
a
18.75
17'/,
@
—
20.40
a
20.50
99'/i
e
1.00
2.87
a
3.05
10
a
10'/,
a
nominal
Silver
Tin, Straits Lb.
Tungsten (WOi) Per Unit
Zinc, N. Y Lb.
FERTILIZER MATERIALS
Ammonium Sulfate 100 Lbs.
Blood, dried, f. o. b. Chicago . Unit
ml 50, ground, raw Ton
Calcium Cyannraid T Tnit of Ammonia
Calcium Nitrate, Norv\r.-c.i.iii 100 Lbs.
Caatot Mr.it Qnit
Fish Scrap, domestic, dried, f. o b. works. . .Unit
Phosphate, acid, 16 per cent Ton
Phosphate rock. f. o b. mine: Ton
Florida land pebble. 68 per cent Ton
Tennessee. 78-80 per cent Ton
Potassium "muriate," basis 80 per cent Ton
Pyrites, furnace size, imported Vint
Tankage, high-grade, f. o. b. Chicago Unit
i2»A a
13
3.30 @
3.35
23'A a
—
23'/, @
—
7 'A @
7 'A
55 a
56
nominal
87v. a
90
nominal
20.00 a
26.00
s , §
8'A
6.50
35.00
7.75
@ 6. 55
(A 40.00
16.00
10.00
17.00
nominal
3.25 a 3-50
5.50 a 6.00
345.00 @ 350.00
nominal
6.37Vi @ 6.40
The Journal of Industrial
and Engineering Ghemistry
Published by THE AMERICAN CHEMICAL SOCIETY
Volume X
MAY 1, 1918
No. 5
Editor: CHARLES H. HERTY
Assistant Editor: Grace MacLeod
Advertising Manager: G. W. Nott
ADVISORY BOARD
H. E. Barnard, H. K. Benson, F. K. Cameron, B. C. Hesse, A. D. Little, A. V. H. Mory, M. C. Whitaker
Published monthly. Subscription price to non-members of the American Chemical Society, $6.00 yearly; single copy, 60 cents
single copy to American Chemical Society members, 50 cents. Foreign postage, seventy-five cents, Canada, Cuba and Mexico excepted
Entered as Second-class Matter December 19, 1908, at the Post-Office at Easton, Pa., under the Act of March 3, 1879
All communications should be sent to The Journal of Industrial and Engineering Chemistry.
Telephone: Vanderbilt 1930 35 East 41st Street, New York City
Subscriptions and claims (or lost copies should be referred to Charles L. Parsons, Box 505, Washington, D. C.
ESCHENBACH PRINTING COMPANY, EASTON, Pa.
TABLE OF
Editorials:
Four Days More 336
Platinum Scraps 336
Publicity Work to be Continued 338
The Chemists' Club 338
Original Papers:
The Fertilizing Value of Activated Sludge. George G.
Nasmith and G. P. McKay 339
Equilibria in Solutions Containing Mixtures of Salts.
I — The System Water and the Sulfates and Chlorides
of Sodium and Potassium. Walter C. Blasdale 344
The Separation of the Chlorides and Sulfates of Sodium
and Potassium by Fractional Crystallization. Walter
C. Blasdale 347
The Use of "Mine Run" Phosphates in the Manufacture
of Soluble Phosphoric Acid. Wm. H. Waggaman
and C. R. Wagner 353
The Concentration of Potash from Raw Materials
Containing Only a Trace of This Element by Means
of the Electric Precipitation of Flue Dust and Fume
Cement Kilns. B. F Erdahl 356
Toluol from Spruce Turpentine. A. S. Wheeler 359
Arsenic in Sulfured Food Products. W. D. Collins. . . . 360
Some Constituents of the American Grapefruit
(Citrus decumana). Harper F. Zoller 364
Lakukatory and Plant:
An Inexpensive Ash Leaching Plant. W. D. Turner
and B. G. Nichols 374
Antimony Sulfide as a Constituent in Military and
Sporting Arms Primers. Allerton S. Cushman 376
r
RESSES :
Food Chemistry in the Service of Human Nutrition.
H. C. Sherman 383
Permanence as an Ideal of Research. S. R. Scholes. 390
The Dedication op Oilman Hall, University op Cali-
fornia 391
CONTENTS
Current Industrial News:
Machinery for France; Exports from Gold Coast;
English Pottery Industry; Soap Demand in Morocco;
Ferro-Concrete Shipbuilding; Railway Material for
Japan; Graphite for Boiler Scale; Swedish Gauges;
South African Iron Ore; South African Diamonds;
Shortage of Electrical Appliances; Margarine In-
dustry in Holland; Electrolytic Zinc; Trade Develop-
ments in Sweden; Rubber Industry in Japan;
Sorghum and Paper; Colloidal Nickel; Japanese
Industrial Developments; Mineral Deposits in
Malay States; Butter Substitute from Fish Oils;
Cod Liver Oil from Newfoundland; Indian Oilseeds;
Preservation of Pit Timber; Oil-Pressing Plant for
India; Russian Asbestos Industry; Roumanian
Petroleum; A Deoxidizing Alloy; Dye from Maple
Leaves; Instruments and Tools for Venezeula; Swiss
Electrochemical Industries; Oil-Break Switchgear;
British Board of Trade 394
Notes and Correspondence:
Preparation for Post-War Conditions in Great Britain;
Note on "The Fertilizing Value of Activated Sludge"
by Nasmith and McKay; Regulations Under the
Potash Leasing Act; Notes on "Free Carbon" of Tar;
The Growth of the Industrial Fellowship System;
American Dyestuff Manufacturers' Association;
Chemicals Division of National War Savings Com-
mittee Organized; American Ceramic Society; Tech-
nical Association of Pulp and Paper Industry;
Calendar of Meetings; Synthetic Materials— Correc-
tion 399
Washington Letter 4°3
Personal Notes 404
Industrial Notes 406
Government Publications 4°8
New Publications 4 ' .5
Market Report 4<°
336
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. s
LDITORIAL5
FOUR DAYS MORE
Not for the purpose of urging is this written, for
that is unnecessary; nor to explain, for this has been
capably done by those in charge of the promotion of
the Third Liberty Loan; but only to remind the chemist
who has not yet subscribed for his bonds that but
four days remain in which he can aid in the provision
of that "force to the limit" which President Wilson
has declared the policy of this country from this time
on until a just peace is declared.
LEND HIM A HAND I BUY LIBERTY BONDS !
PLATINUM SCRAPS
At the Kansas City Meeting of the American
Chemical Society the following resolution was
adopted:
"Resolved, That the attention of the National Council of
Defense be called to the scarcity of platinum under existing
conditions and to the great need of the metal, more particularly
in the prosecution of the war. We hold that its use at this
time in the production of articles of ornament is contrary to
public welfare. Therefore, we recommend that an appeal be
made to the women of the United States to discourage the use
of platinum in jewelry and that all citizens be urged to avoid
its use for jewelry, for photographic paper and for any other
purpose whatever, save in scientific research and in the making
of articles for industrial needs."
Since that time diametrically opposite campaigns
have been waging, without a decisive victory yet
assured on either side. The chemists have favored
Government control of the entire stock of platinum,
while the jewelers have fought strenuously to keep a
supply available for their trade. In defense of their
attitude, when the adoption of an amendment to the
war tax bill placing a tax of two hundred and fifty per
cent on the manufacture of platinum jewelry threat-
ened, the Jewelers' Vigilance Committee pledged sup-
port in these words:
"Having in mind the present needs of American industries,
educational institutions, and sciences for platinum and the
possible future requirements of the Government, the Jewelers'
Vigilance Committee, after giving the subject careful thought,
at the request of the Secretary of Commerce, has adopted the
following resolutions:
"WhERBAS, The Secretary of Commerce has requested the
Platinum Committee of the Jewelers' Vigilance Committee to
bring to the attention of the jewelry trade of the United States
(he advisability of conserving platinum in order that our Go\ era
ment may have larger supplies to draw upon for war purposes,
and
"WHERBAS, The jewelry trade has already expressed its desire
and determination to assist our Government to the extent of
its ability in bringing tin- war to a successful terminatio
"Resolved, Thai we pledge ourselves to discontinue and strongly
all manufacturing and retail jewelers of the
United States that they in a truly patriotic spirit discourage the
manufacture, sale and use of platinum in all bulky and heavy
pieces of jewelry. Be it further
"Resolved, That during the period of the war or until the present
supplies of platinum shall be materially augmented, we pledge
ourselves 1,1 discontinue and recommend that tin- jewelry trade
discourage the use ol tia] platinum findings or parts
of jewelry, such as scarfpin stems, pin tongues, joints, catches,
swivels, i sfactorily
serve. He it further
"Resolved, That the jewelrj trad by all means in
their power the use of gold in combination with platinum where* ei
proper artistic results may bei,obtained. Be it further
"Resolved, That copies of these resolutions be handed to the
Secretary of Commerce, to the trade press, and be sent to all
our trade organizations, and to the daily press, in order that
they may have the widest possible dissemination." — The Jewelers'
Circular, May 9, 191 7.
and quoted Secretary of Commerce Redfield, as follows:
"This is wise, patriotic, and unselfish action for which the
merchants and manufacturers are highly to be commended.
It will take time to work out fully its beneficial effects to the
country. It will disarm adverse criticism of the jewelry trade
in this respect and lead to general cooperation with them.
Such is the earnest desire of the Department. The jewelry busi-
ness is a part and an important part of our commerce. It has
acted fairly, its normal needs should be considered fairly. Plat-
inum is required for many uses. Even- such use has its just
claim. None may urge an exclusive demand. All have a part
in our common country, and the Government of that country
seeks through the Department of Commerce to secure for all a
due and proper share. To this end the considerate course
taken by the jewelers will directly contribute." — The Jewelers'
Circular, May 9, 1917.
Writing to Congressman Longworth, active in sup-
port of the tax measure, Meyer D. Rothschild, chair-
man of the Platinum Committee acting under the
s of the Jewelers' Vigilance Committee, stated:
;i: The Jewelers Committee who took up the ques-
tion of conserving platinum with the Department of Com-
merce and other Government departments voluntarily agreed
to cut out the use of this precious metal for heavier articles of
jewelry and for jewelry findings and unnecessary' parts, not-
withstanding the fact that they were convinced, and so stated,
that there was no shortage of platinum for war purposes.
"Eighth: The conferences with the Secretary of Commerce
and Government officials brought out the fact that there was
a persistent effort on the part of certain people to 'bear' the
price of platinum and to that end wilful mis-statements of fact
were being published and a regular press campaign undertaken
to discourage the buying of platinum by patriotic women, with
the avowed purpose of cheapening the price of platinum to
chemists, who have always been able to get all the platinum they
required at the market price, that is, at the same price that
jewelers and others had to pay for it.
"The resolutions passed by the Daughters of the Revolution,
and other like resolutions, can be readily traced to these mis-
statements of the actual requirements of platinum for war pur-
poses. The arguments used are so close to those used by you
on the floor of the House that a strong impression is created that
the misinformation you received about platinum must have come
from those sources." — The Jewelers' Circular, May 30, 1917.
At the Convention of the New Vork State Retail
Jewelers' Association, Mr. Rothschild made the follow-
ing statements:
"The selfish chemical interests which had started this attack
on our industry with the avowed and shameless purpose of
'bearing' the price of platinum in order to get it cheaper, now
began a misleading press campaign which the Platinum Com-
mittee met from day to day by press corrections and
statements of facts to the press and to jewelers. This cam-
paign culminated in an attempt by Congressman Longworth
to place a prohibitive war tax of 250 per cent on platinum
jewelry, which the Platinum Committee was happily in a posi-
tion to frustrate by the timely presentation of a letter from the
Secretary of Commerce, which was read on the floor of the House
of Representatives, defeating this effort to tax platinum jewelry
out of existence." — The Jewelers' Circular, May 30, 1917.
Coincidently, a vigorous advertising campaign was
carried on by wholesale and jewelers in
cally every city in the country, refer bach has
already been made in these columns. The well
the Women's National League for
the Conservation of Platinum to create a sentiment
against the use of platinum gave renewed
impetus to this advertising campaign.
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
337
Concerning the work of the Women's League, of
which Mrs. Ellwood B. Spear, of Cambridge, Mass., is
chairman, Secretary Charles L. Parsons writes:
"Platinum in my opinion should be 'tabooed' by all American
women who wish to see their country successful in this war and
successful after the war in keeping its lead in the industrial and
scientific developments. The opal has been considered unlucky.
Accordingly, it carried in the feminine mind little value as a gem.
I believe that without ever using the phrase, the Women's'
League for Conservation of Platinum has already begun to instill
into the minds of American women what really 'bad taste'
it is to wear a metal that looks like lead in rings, bracelets, etc.,
simply on account of its high price. I also believe that the
'slacker wedding ring' made of platinum will soon be a thing of
the past."
Then came the realization by the Government
authorities of the dire necessity of increasing the supply
of platinum for munitions manufacture and the conse-
quent order taking control of the raw material.
In view of the resolutions of the Jewelers' Vigilance
Committee quoted above, it is surprising to learn that
in March 1918, when the manufacturers of jewelry
were asked to offer to the Government at cost a con-
siderable part of their supply of unworked platinum,
a census of which had been taken, the response was
only ten per cent of the amount on hand, whereas at
least fifty per cent had been expected by the Govern-
ment officials. The situation gave rise to apprehension
on the part of the leaders
"* * * * that drastic action would possibly be taken by the
Government in the near future to get the platinum which they
believe the manufacturer should surrender." — The Jewelers'
Circular, March 27, 1918.
Commenting upon the evident accumulation of plat-
inum by certain manufacturers, The Jewelers' Circular,
March 27, 1918, reports an interview with Mr. C. H.
Conner of the War Industries Board, as follows:
"Mr. Conner also called attention to the fact that manufac-
turers might find themselves subject to serious loss inasmuch as
when the Government does commandeer the platinum, the
manufacturer who has bought since that time wiil not be pro-
tected against any loss, but will have to take for his platinum
the Government price of $105, irrespective of what he has paid
for it."
The following editorial discussion appeared in The
Jewelers' Circular of April 3, 1918:
"The platinum situation in the jewelry trade is not satis-
factory. The propaganda of the women fanatics asking the
public to give up platinum jewelry has not been contradicted
by the Government officials, who know it to be founded on
erroneous statements, because these officials are 'sore' on the
jewelers. The irritation arises from the fact that the jewelers'
voluntary offer of platinum to the Government is very small.
The smallncss of the offer is due to two reasons: (1) the way
that the so-called commandeering by order was handled and
put into effect by the officials at Washington, and (2) the actions
pf certain manufacturers whose selfishness and lack of fore-
sight have put the trade as a whole in a bad position with the
very officials whose cooperation is needed at the present time
BO counteract the malicious propaganda that is hurting our re-
tail trade.
"That approximately 5,000 ounces of platinum should be
reported among the manufacturers in the jewelry trade as of
February 1 and less than 500 ounces be offered to the Govern men t
when these manufacturers were called to give up caused offii ial
(to feel that the jewelers were not cooperating with the Govern
ment, but were selfishly looking to their own interests without
thought of the Government's ueeds, Of course, they did no1
take into consideration that the census of platinum «
of February 1 while the offer we tnadi as of platinum on hand late
in March; but another factor in theil attitude was due to thi ii
knowledge, of the speculation in platinum indulged in by a few
manufacturers and the rush by others to put platinum into
manufactured or half manufactured goods immediately after
it became known that the Government would need the raw
metal. This caused certain officials to believe that the manu-
facturing jewelers' pledges of loyalty were but 'lip service,'
and without meaning. * * * *"
Here it is interesting to quote from the report of
H. C. Larter, chairman of the Jewelers' Vigilance Com-
mittee at its meeting on April 2, 19 18:
' "We had hardly become organized when the agitation started
by the chemists of the country to eliminate the use of platinum
in the jewelry trade was promulgated. As you know, we promptly
took this matter up, in defense of the entire jewelry trade, and
at a large mass meeting a representative platinum committee
was appointed, and at its head, Meyer D. Rothschild, who for
nearly twelve months has successfully looked after the platinum
situation in the interest of our trade, and at the same time has
cooperated in every way possible with the Government.
"Unfortunately, for reasons beyond anyone's control — the
most important one of which, however, is the breakdown of
the Russian nation — the platinum situation is more confusing
and perplexing than ever.
"While the platinum matter, insofar as its connection with
the Government is concerned, is now out of the hands of this
Platinum Committee, the Jewelers' Vigilance Committee is still
interested in the adverse propaganda, started afresh with new
vigor because of the acute situation now existing throughout
the world in regard to this precious metal." — The Jewelers'
Circular, April 10, 1918.
Realizing that "something had to be done to over-
come the erroneous impression as to the jewelry trade
held by Government officials," organizations of manu-
facturing jewelers in all sections of the country were
appealed to by the Jewelers' War Service Committee
to call special meetings "to increase the offer of plat-
inum to the Government." Two meetings were held
in New York City, at which 400 ounces additional
were secured.
In an article written for The Keystone (a Leading
jewelry circular), April 1918, James M. Hill, of the U. S.
Geological Survey, states the relative supply and needs
as follows:
"* * * * In 191 5 there were approximately 44,000 ounces of
platinum in contact acid plants; in 1917. about 60,000 ounces,
and it is estimated that the industry must be further ex-
panded during 19 18 by at least fifty per cent to supply the sul-
furic acid to make the munitions necessary to carry on the war.
"The platinum for the nitrogen fixation industry is used in the
form of a very fine gauze, woven of pure platinum wire The
building of this industry has become necessary through the
great expansion in the demand for nitrates to be used in explo-
sives. The plants arc being built under the control of the Govern
ment and it is not expedient to give details concerning the
quantities of platinum required by them. It seems, however,
safe to say that the quantity runs in the thousands, ratlin than
in the hundreds of ounces,
"* * * * Yet it must always be remembered that platinum, the
metal most resistant to all chemical reagents, is par excellence the
chemist's metal for he can use it in nearly all steps of his work,
while with substitutes he must constantly hear in mind the
limitation Oi utensils made of other materials.
" * * * * In fact, it is believed that aside from the large amount
of platinum metals in the form of manufactured jewelry, a large
which is in private ownership, there is less than twenty
5vi I-' ''Hi oi ti 'mil -.toek of unmanufactured platinum
available for war needs.
"Thai these needs arc very real cannot he questioned bj
nr. 1 hoiking man. Tin question of what can lie .lone to meet
ed 1 very much alive and must in- solved shortly
war program of the United States is liable to suffer."
In the same issue of The Keystone, the Editor dis
the platinum situal ion ' g h anl
nd in terms which evince a clear comprehen-
338
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. s
sion of the gravity of the situation and of the jewelers'
responsibility therein.
"Let us not forget the urgency of the need for placing under
United States control as large a portion of the world's platinum
supply as possible. Crafty, forehanded Germany has been doing
her utmost, since the war began, to increase her supply of the
now doubly-precious and much-needed metal. Since the con-
clusion of her damnably insincere 'peace' contract with poor
Russia, she is in a fair way, through seduction or force, to ob-
tain access to the world's greatest source of the coveted material,
and thus not only take care of her own very urgent need but
also deprive the United States and her Allies of further importations.
"Hence, while the commandeering order recently issued by
l In- United States Secretary of War does not requisition platinum
jewelry nor in the least affect the side of any already made up,
the time may not be far distant when an appeal will be made or
an order found necessary to call in even the finished product
for use in essential purposes in prosecuting the war. What we
have to suggest, therefore, is perhaps as much colored with
prophecy as patriotism."
The story here narrated through excerpts from the
jewelers' publications constitutes no praiseworthy
chapter in the history of our war making. It does
furnish ample justification for the campaign inaugu-
rated by the chemists at Kansas City. Plainly the
handwriting is on the wall. Priority must be given
to munitions manufacture and scientific research.
PUBLICITY WORK TO BE CONTINUED
The work of the Press and Publicity Committee
of the American Chemical Society is to be con-
tinued. This policy was determined by the action
of the Directors at their Spring Meeting on April
13, 1918, whereby "it was voted that an additional
appropriation of $2,500, or so much thereof as may be
necessary, be made to the Publicity Committee and
that the Committee be continued."
This action has a twofold significance. In the first
place, it is clearly indicative of an increase in the
membership of the Society sufficiently large to dispel
the possibility of a decreased income due to war
conditions, for it was primarily upon this ground
that the recommendations of the Committee were
tabled at the December 191 7 meeting of the
irs. (This action was discussed editorially in
the January 1918 issue of Tins Journal.) In the
second place, it insures the continuance on an even
more efficient scale of one of the most important
activities of the Society. In justification of this ap-
praisal of the Committee's work, there is reproduced a
portion of the editorial above mentioned:
"We live in a democracy, and under such conditions sure
Foundations can be laid only in broad educational work from the
bottom upward. Our people through tln.it newspapers should
have opportunity t<> learn more of chemistry treated in a popular
: should be- brought into a more sympathetic relationship
with American chemists thro cord of their achieve
Such work is preeminently the function of the Ajcbric w
ll Society, an <a which has no propaganda
to promote othei than the welfare of this country through in-
creased appreciation of ch( mi
Asa result of the action of the Directors, the
mittee is now formulating plans for the continuance of
the work.
THE CHEMISTS' CLUB
At a meeting of the Trustees of The Chemists'
Club on April 5, 1918. it was voted that the following
communication and questionnaire should be sent to
each member of the Club:
The Board of Trustees, in view of existing conditions at home
and abroad, respectfully bring to the attention of all members of
The Chemists' Club, resident and non-resident, the importance
of complying with the following requests:
1 St. That the German Language shall not be used
in conversation in the Club.
2nd. That all disloyal criticism of the United
States Government, or its allies in the present
war, must be avoided in the Club.
3rd. That any member of the Club, resident or
non-resident, of whatever descent, and
whether an American citizen or not, whose
sympathies favor the enemies of this country,
or who cannot conscientiously comply with
the foregoing requests or who cannot be sure
of so conducting himself as to avoid giving
offense to his fellow members by any display
of hostility or disloyalty to the United States
or its allies, is requested to resign.
The Trustees also ask you to fill out and return not later than
May 1, 1918, in the accompanying addressed envelope, the en-
closed card asking for certain data, to enable them accurately to
answer inquiries from time to time made by the Government
authorities.
Floyd J. Metzger,
April 15, 1918 Acting Secretary
THE CHEMISTS' CLUB, NEW YORK
Name of Member. .
Address (Business) (Home)
Business ... (Firm)
Birthplace (Self) Year
Birthplace (Father) Birthplace (.Mother)
Citizen of United States Yes No
If Naturalized . When Where...
Citizen of
Sons in Service In Army In Navy ,
( Ither Members of Family in Service
This matter, we learn, had been under careful con-
sideration at several previous meetings of the Trustees.
The action taken officially establishes as a requisite
of membership in the Club unswerving loyalty to the
cause of this country and its allies, and will eliminate
all enemy sympathizers, the number of whom is small,
but whose presence, no matter how small the number,
is completely incompatible with that spirit of home
life which the term "club" implies.
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
339
ORIGINAL PAPERS
THE FERTILIZING VALUE OF ACTIVATED SLUDGE1
By George G. Nasmith and G. P. McKay
Received February 18, 1918
The most important problem remaining to be solved
in the disposal of sewage is probably that of econom-
ically dewatering the sludge. Since the discovery
of the activated sludge method, the necessity of
devising a method of dewatering this new type of
sludge has become even more urgent for the reason
that activated sludge has marked fertilizing proper-
ties, as Bartow and Hatfield2 have pointed out.
In the activated sludge method of sewage disposal,
finely divided air is blown through the sewage. After
some time the sludge which settles out is found to
possess remarkable properties when agitated with
fresh sewage by the same method of aeration. The
sludge has become "activated" and when blown
in contact with fresh sewage the organic matter
present in the latter is rapidly oxidized, practically
all the intestinal bacteria destroyed, nitrates elaborated,
and a stable effluent formed.
"Activated" sludge, however, like ordinary sludge,
contains 9 5 per cent of water, and still has to be
dewatered before it can be satisfactorily handled.
The treatment of sewage by this method is very
promising for if the fertilizing value of the sludge
is high, the revenue therefrom would help to pay the
cost of dewatering and disposing of the sludge. Fur-
thermore, it is a question of conservation of the first
magnitude, for if a fair proportion of the fertilizing
value of the excreta from our cities and towns could
be saved and turned back into the land it would be
a great factor towards solving our fertilizer problem,
particularly in conserving the supply of humus and
nitrates, and increasing the fertility and productivity
of the soil.
In December 191 5 a small experimental activated
sludge plant was started at the Toronto Main Sewage
Disposal Works, Morley . Avenue. Dr. Adams and
Mr. J. Scott, who at first operated the plant during
my absence in France, soon proved that Toronto
sludge could be readily activated, and the plant has
been in operation ever since. A good deal of prelim-
inary data have been obtained for our own information
in case the city of Toronto should ever decide to adopt
the method on a large scale. Among other things, we
have tested the value of activated sludge as a fertilizer.
Hatfield, in some experimental work to
value of activated sludge as a fertilizer,
r of experiments with the growth of
The activated sludge used by them
owing analysis: Total Nitrogen = 6.3 per
cent; P2O5 = 2.69 per cent.
By the use of one ton of this sludge per acre, equiva-
lent to 120 lbs. of nitrogen, to with 5 tons of
dolomite, '/« ton °f bonemcal, and 500 lbs. of potassium
sulfate per acre, they obtained a yield of 36 to 37V2
1 See communication from P. Uudnit-k in Xotcs and CofTCSpofl
" This Journal, S (1916), 17.
bu. of wheat per acre as against 13V2 bushels per acre
where the equivalent amount of nitrogen had been
added in the form of dried blood. The straw also
amounted to over two tons per acre as against less
than 3/4 of a ton of straw per acre where dried blood
had been employed as fertilizer.
In further tests as to the value of sludge as a market
garden fertilizer, these investigators used plots, each
2 ft. X 3 ft., which were treated with equivalent
quantities of sludge and dried blood per acre. They
obtained an increase in weight of 40 per cent in the
Fig. I — Showing Growth on Km
■ mental Plots, Jut* 18, 1917
lettuce and 150 per cent in the radishes, and the growth
was much more rapid in the beds fertilized with ac-
' sludge. They conclude from their
ments "that the nitrogen in 'activated sludge' is in
rilable form, and thai activated sludge is
Me as a fertilizer."
Bartow and Hatfield, in determining the amounl
of fertilizer to be employed, used as a basis the
of nitrogen present. For instance, they used in their
nts the quantity of activated sludge and dried
blood that would yield 120 lbs. of nitrogen per acre.
THE JOCKS AI. ()!■ INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 5
The amount of phosphate or other ingredients present
in the sludge was not considered.
THE VALUE OF FERTILIZERS
Experience has proved that the value of fresh
manure as a crop producer is from one-third to two-
thirds more effective than rotted manure, because
a certain proportion of the nitrogen and other in-
J,.^
kflU\ikk<iFriXi&akl
\8rcfliSfi
<UiSku.- H
>^$«
w$l
fKBnjfw^'SBSe\f
(J\^jft *>* v ^
^aSBBa
Rtf)1
•f*Wwl
WKPWW
Fig. II — Illustrating Table 1
gradients have been leached out of the latter and lost.
Manure has a greater fertilizing value than would be
estimated from the amount of nitrogen, phosphoric
acid and potash present. This greater value is due
to the large amount of humus present in the manure;
humus is not found to any extent in the commercial
fertilizers, which are commonly purchased on their
nitrogen, phosphoric acid or potash content.
Humus is partly decomposed organic matter, such
as decayed leaves. It is found in large quantities in
all fertile soils and is probably the most valuable con-
stituent present., because it is not only a source of
nitrogen, but it helps to keep the soil moist, loose and
well aerated, as well as to provide a medium for the
propagation of soil organisms so essential to the growth
of plant life.
The chemical constituents in a fertilizer are not
the only ones upon which its fertilizing value must
be determined. It would be possible to have the same
amount of potash, nitrogen and phosphate in two differ-
ent fertilizers and yet obtain entirely different
results upon plant growth. The availability of
the food material for the assimilation of the plant is
factor. Thus ordinary Septic sludge is not a
good fertilizer for immediate growth of plants, results
obtained the first year being poor. But the trans-
formation of the septic sludge taking place in the soil
frees the plant food material locked up in this sludge
and renders it available, so that it becomes an ex-
cellent fertilizer the second year after it has been
dug into the soil. The experiences of a number of
amateurs in Toronto who have been using ordinary
septic sludge for several years in their vegetable and
rose gardens, have quite established this fact.
The truest test of fertilizers is not their content of
nitrogen, phosphate or other chemical, but rather
the availability of the chemicals present as food for
growing crops and the actual increase in the yield
brought about by the fertilizer. Here again the
fertilizers must be differentiated according to their
ability to produce immediate results. We must de-
termine whether they are available through the grow-
ing season, whether they leave a residue of humus
and other materials in the soil, and whether they bring
about exhaustion of the mineral elements of the soil
or not.
Activated sludge, when air-dried, is a dark
brown, friable, perfectly inoffensive material with a
slightly earthy odor like that of decayed leaves. It
consists largely of humus, but contains much more
nitrogen, phosphoric acid and potash than does ordi-
nary barnyard manure. Furthermore, it is crowded
with millions of the nitrifying type of organisms so
essential to plant growth.
For the reasons given above as to the fertilizing
value of manure, we have taken this for our standard
of comparison and have not compared the fertilizing
value of sludge with commercial fertilizers on a nitro-
gen, phosphoric acid or potash basis.
The real single, final test of any fertilizer or manure
is the increase in the yield produced by it when com-
pared with an equivalent amount of barnyard manure.
Illustrating Table 2
We selected for our plot experiments a site on very
poor, humus-free clay soil, adjacent to our experimental
plant. The surface was scraped to free it of any or-
May, 1 91 8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
ganic matter present, and four inches of water-washed
sand were then thoroughly incorporated with the soil
to a depth of ten inches. This was done to permit of
aeration, to prevent the soil baking in the sun, and to
make the soil friable.
Six beds, each 10 ft. X 4 ft., were then laid out and
separated from the paths by boards placed edgewise
in the ground.
One bed was kept as a control, and no fertilizer added
to it. The second was treated with 27 lbs. of air-
dried horse manure, and the other four each with 27
lbs. of air-dried sludge (equivalent to 14V: tons to
the acre). This is summarized below:
Total
Total
Quantity
Nitrogen
P2Oi
Bed
Air-dried Fertilizer
Used
Per cent
Per cent
No. 1
None
0
0
0
No. 2
Manure
27 lbs.
1.90
1.00
No. 3
Activated sludge
27 lbs.
2.50
2.46
No. 4
Sludge from old bed
27 lbs.
1.10
0.85
No. 5
Humus — Brush filter
27 lbs.
1 .30
1.20
No. 6
Sludge — tanks
27 lbs.
1.21
1.24
On May iS, 191 7, the fertilizers were added and
thoroughly incorporated with the soil, and on May 21,
the seeds were planted in all the beds. Seeds were
used except in the case of tomatoes and Spanish
onions. A fairly thick planting was made so that
plenty of seedlings would be available when thinning
out, and a uniform number of strong seedlings of each
variety could be left in each bed.
As each row of vegetables was pulled from the several
beds at the same time, the complete plants, leaves and
all. were placed in bags, labelled and brought to the
laboratory. After the removal of adherent earth the
product of each bed was weighed; the tops, in the case
of root crops, were then taken off and weighed separately
I-V. IV- Illustrating Table 5
Fig. V — Illustrating Table 7
and the difference taken as the weight of the root.
Notes were also made as to the quality of the crop.
Before weighing, the crops were spread out on the
floor in their respective groups and photographed.
The photographs, however, gave only a general idea
of the difference in size of the various groups because of
the fact that the camera had to be tilted, in consequence
of which the rows closer to the camera appear larger and
the rows farther away smaller than they should be.
The plan adopted worked very well in practice and
gave, we think, fair comparative results.
Daily observations were made by the man who looked
after the beds, and who was himself a gardener, as to
appearance of the various vegetables, temperature,
rainfall and cultivation. When he cultivated one bed he
cultivated all the beds; if he watered one he watered all,
and used the same amount of water, and when he pulled
one variety he pulled that variety from all the beds.
In this way we tried to eliminate every factor which
might give any advantage to one bed over another,
and to remove every influence that might have had
any bearing on the growth of the plants except the
actual effect of the fertilizers themselves during the
i of one season.
The following are synopses of the results obtained:
Tabu i — Earlv Radishes
Acti- Morley N. Toronto
Con- v.iud Ave. . "- — »
trol Manure Shulm- Sludge Humus Sludge
Weight, total grama 92 *55 757 317 582 752
Weight roots— grams 59 350 490 200 417 518
Weiihtltop. crams 33 105 267 117 165 234
In. ]ii in roots over coii-
,r„l pir .cut 493 730 239 606 778
yield per acre— tons 5.04 7
Taule 2— Head Lettuce
Weight, total grams 31 238 484
in. rease over control |
,,,,, 667 1461
\ I. I.I pel acre — tons. 1-9 3.88 .. . ...
Table 3— LETTUCE, Grand Rapids
Weight, total grami 75 Missing 524 155 277 248
trol — per
c<.nt Mi i.ii S98 106 269 228
Yield per Bcrc— tons Misting
342
THE .Id RNAL OF INDUSTRIAL AND ENGINEERING I HEMISTRY Vol. 10, Xo. 5
357
377
531
39.4
47.2
107
160
437
2012
891
2945
1 1 69
304
3612
4770
472
283
28S
197
738
452
470
1006
2410
466
1425 1560 2695
327
700
3.9
420
527
Table 4 — Brans
Weight, total— grams 256 296 525
Increase over control — per
cent 15.6 105
Yield per acre — tons 1.78 3.16
Tablb 5 — Bi
Weight, total— grams 79 1796 3437 1
Weight, roots— grams 24 730 17.17
Increase over control — per
cent 2941 7137 1
Yield per acre— tons 5.85 13.90
TablB 6 — Late Radishes
Weight, total— grams 32 7.5 315
Weight, roots — grams 18 43 179
Increase over control — per
cent 139 894 1
Yield per acre — tons ... ...
Table 7 — Tomatoes
Weight, total— grams 29 422 1654
No. of tomatoes 2 9 15
Average weight of single to-
mato— grams 14'/j 47 1 10
Increase over control — per
cent 1355 5603
Yield per acre— tons 5.07 19.9
Table 8 — Carrots
Weight, total— grams 885 1680 1535
Increase over control — per
cent 96 80 66 82
Yield per acre — tons 20
Tablb 9 — Onions, Spanish (16 Bust)
Weight, total— grams 41 96 280 142 68
Increase over control — per
cenl 134 583 246 64
Yield per acre — tons 1.2 3.4
Table 10 — Onions, Red Weatherpield (8 Best)
Weight, total — grams 67 110 720 239 225
Increase over control — per
.... 64 974 256 235
Yield per acre — tons 1.3 8.7 ... ... 5.1
Table 11 — Onions, Danvers Yellow Globe (8 Best)
Weight, total— grams 67 124 232 260 184 169
Increase over control — per
cent 85 246 288 174 152
Yield per acre — tons 1.5 2.8 ... ... ...
NOTES ON TABLES I TO 1 1
table i — The radishes were planted May 21 and
pulled July 5, approximately six weeks later. The
same number of radishes was left in each bed.
The yields from the activated sludge and North
Toronto sludge were about the same, but 40 per cent
than that from the manured bed.
tables 2 and 3 — The two sets of lettuce, pulled
July 19, clearly showed the superiority of activated
sludge as a fertilizer. These beds yielded double the
weight of lettuce produced by the beds fertilized with
ordinary manure and other sludges. Activated sludge,
therefore, is a particularly good fertilizer for lettuce.
table 4 — The beans, one of the legumes, were pulled
August 7, anil did not show so wide a variation in the
beds as did the radishes and lettuce. Still.
ips from the beds fertilized wi1 l sludge
and with North Toronto sludge were 77 per cent
heavier than from the bed fertilized with ordinary horse
manure
rABLI I i , etS were pulled on August 16. Dur-
ing the period of growth the foliage on the beets in
1 sludge bed was much more luxuriant
than thai on the beets in any • plots. The
yield Oi from the beds fertilized
with ordinary manure, and the yield of roots 138 per
roronto was
considerably behind in this ease.
TABLE 6— The late radishes were not a success,
though a large increase over th was apparent
in all eases; they were distorted in shape and in some
cases rotted. The yield from the North Toronto
sludge plot was greatest, but 1 lie sludge from the old
beds, which had not been a successful fertilizer up to
this time, made a good showing and indicated that
aerobic action and nitrification of this sludge had taken
place in the earth, rendering this fertilizer available
as a plant food.
TABLE 7 — The tomatoes were picked October 2.
During the growing season the tomato plant in the acti-
vated sludge bed had been most vigorous; the tomatoes
had also ripened first on the beds treated with acti-
vated sludge and North Toronto sludge. The acti-
vated sludge bed gave the greatest number and the
greatest total weight of tomatoes. The activated
sludge gave a yield of 300 per cent in excess over that
of the manure bed, showing that activated sludge is
an ideal fertilizer for tomatoes. The yield from the
plot fertilized with North Toronto sludge was con-
siderably behind the activated sludge, though away
ahead of the manure plot.
Fig. VI -Ii.i.esTKATiNu Table 8
i ah li: 8 — The carrots were pulled on October 9.
Except in the case of North Toronto sludge, which
grew some huge carrots, the yields from the other beds
were all much the same as that from the bed ferti-
lized with ordinary manure.
tables 9, 10 and 11 — The onions were pulled Oc-
tober 0. and did not show phenomenal growth. Morley
Avenue sludge gave a slightly better result than acti-
vated sludge in the case of Danvers Yellow Globe,
May, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
343
Fig VII — Illustrating Tables 9, 10 and 11
showing that this sludge had latent fertilizing value. early in the year, but later on in the season ap-
Activated sludge was the best forcer in the case of peared to be more readily available for the growth of
Red Weatherfield onions, giving an increase in yield plant life.
of 554 per cent over the manured crop. conclusions
The yield of Spanish onions was practically the From the foregoing tabulated results it is clearly evi-
same in the case of the beds fertilized with North dent that activated sludge is a most valuable fertilizer.
Toronto sludge and activated sludge, but much greater When compared with the standard barnyard manure
than that from the manured plots. used by the farmer, our results show the following
In casting about for the reason why the sludge from increases:
the North Toronto sedimentation tanks gave US almost tncrease in Yield Due to Activated Sludge Over Barnyard Manure
as good results as activated sludge, we went back over Per cent
the method used in its preparation. LeuuceS. '.'.'.'. '.'.'. '.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'. 103.3
The sludge is pumped from the sedimentation tanks |eans 138 00
into drying beds. The water gradually flows away Toma^oet'5'1" " '.'.'.'.'.'.'. 29ko
into the drains beneath, so that in from 2 to 4 weeks Carrots No increase
. Onions, Spanish 191.0
the sludge is dry enough to dig out. During this Weatherfield 554.0
, . 6 . , . , b " « . i. , Danvers Yellow Globe 87.1
drying period it undergoes anaerobic action under-
neath the thick black, crust which forms on the surface. From the results obtained by us it seems to be
Eventually, however, it dries sufficiently for aerobic true that crops such as lettuce, where the foliage it-
action to take place in the spongy mass. The sludge self is eaten, or crops like beans, beets or tomatoes,
is then dug out of the beds, carried away on small which demand a heavy growth of plant and leaf if
dump cars and deposited in long heaps, where it lies the yield of roots or fruit is to be heavy, can be stimu-
exposed to the sun and air until finally removed. lated into very heavy growth by the use of activated
In all probability a series of nitrifying actions sludge. The increase in the yield of onions is also
somewhat similar to those which occur in activating great.
sludge occur accidentally in this method of drying For the growth of lettuce or tomatoes under glass,
h Toronto sludge, rendering it suitable for im- activated sludge should, therefore, prove to be a
mediate assimilation by plants. It would seem very most valuable fertilizer. In the case of radishes,
probable that any sludge dry enough to be spaded though the final weight was not materially greater,
would, if thrown into shallow heaps or spread out in the radishes matured much more rapidly, which is
layers on the ground, be converted by oxidation and just as valuable to the market gardener as if his crop
bacterial action from a form not readily assimilable were greater, for the quick growth is what is wanted.
by plants to one readily assimilable by them. The The same holds good of lettuce or beets in which the
same action would occur when sludge is dug into the growth was much more rapid than it was with the other
earth itself, and presumably more rapidly in a porous fertilizers tested. These points are now being tested
soil than in a heavy clay soil. This latter point by actual experiments under glass,
seems to be evident from results obtained from the It should be noted that the amount of air-dried
anaerobic sludge dug from the old Morley Avenue manure added, 14V2 tons per acre, is about the maxi-
sludge beds. This sludge made a very poor showing mum amount that could be used to advantage, and,
344
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. 5
therefore, in all probability the maximum crops cap-
able of being produced by the addition of manure
had been produced.
If this is true then the increase in yield due
sludge over ordinary barnyard manure is
very striking and at once places a high monetary value
on this material, for the value of fertilizers must be
directly proportional to the crop returns yielded by
them.
Department of Public Health
Division of Laboratories
Toronto, Canada
EQUILIBRIA IN SOLUTIONS CONTAINING MIXTURES OF
SALTS
I— THE SYSTEM WATER AND THE SULFATES AND
CHLORIDES OF SODIUM AND POTASSIUM1
By Walter C. Blasdale
Received March 20, 1918
The various processes suggested for increasing the
production of potassium-containing compounds involve
the separation of that element from associated salts
by fractional crystallization. The only satisfactory
method of obtaining a clear understanding of the possi-
bilities of making such separations is a study of the
phase-rule diagrams representing the equilibria which
exist in aqueous solutions between the salts to be sepa-
rated. Unfortunately much of the data necessary for
the preparation of such diagrams is lacking, and the
present paper represents the first of a series which have
been planned by members of the Department of Chem-
istry of the University of California for the purpose
of supplying what is believed to be much-needed infor-
mation. In carrying out the work here reported assis-
tance in the large amount of analytical work involved
has been rendered by students of the Department,
and special acknowledgment should be made to Messrs.
R. D. Elliott, A. H. Foster, D. Ehrenfeld and K. V.
King.
PREVIOUS WORK ON THE SUBJECT
The system designated in the sub-title consists of
four components, namely, water and any three of the
four salts concerned, which constitute a "reciprocal salt
pair." In addition to the four simple anhydrous salts
the only solid phases to be considered are ice, the
drate of sodium sulfate, which will be called
Glauber's salt, and the double sulfate of sodium and
potassium generally known as glaserite. This name was
first used by Penny to represent a compound corre-
sponding to the formula K-,Xai S( >,)•_■, but double sul-
ontaining somewhat different proportions of the
constituent salts were subsequently reported by Other
investigators and different names applied to them.
Yan't Hofl"- was able to show that it was possible to
prepare a series of solid solutions in which the per-
between ; i
oi. K, which justifies treating all of these compounds as
a single solid phase.
It was also shown by Yan't Holt and Reichcr5 that
it was possible to prepare a solution saturated with
1 This work has been supported by the Council ot Defense of the State
of California.
1 "Untcrs". u. Bildllna der ozeanischen Salzublugerung," p. 220.
1 Z. physik. Chem., 3 tins'". 482,
respect to glaserite, Glauber's salt, potassium chloride
and sodium chloride at a temperature of 3.7 °, and that
therefore this temperature represents the "transition
temperature" for the equilibrium
3KCI + 2Xa,SO,.ioH20^±:
K3Xa(SO,)2 + 3NaCl + 20 HjO,
in which all the formulae, except that of water, repre-
sent solid phases. A consequence of this fact is that
one of the two pairs of salts (in this case potassium chlo-
rideandGlauber'ssalt) can exist assolidphasesinequilib-
rium with solutions of the four salts at temperatures
below 3.7 ° only, whereas the other pair, i. e., glaserite
and sodium chloride, can exist as solid phases in equilib-
rium with such solutions only above this temperature.
If the temperature of the system is limited to the inter-
val between o° and ioo°, which represents the limits
of practical importance, so that ice is eliminated,
nine different univariant systems in which three solid
phases are present are theoretically possible. The
univariant systems which can be actually realized ex-
perimentally were first studied by Meyerhoffer and
Saunders,1 who fixed the transition temperature dis-
covered by van't Hoff at 4.4 ° instead of3.7°,and worked
out the phase-rule diagrams for the system at tempera-
tures of 0°, 4. 40, 160 and 250. In taking up the work
at this point it was thought desirable to repeat the de-
terminations upon which the diagrams for 0° and 25°
were based, and to obtain data necessary for the prepa-
ration of similar diagrams at temperatures of 50°, 750
and 1000.
EXPERIMENTAL METHODS USED
Saturation of solutions with respect to the different
salts was effected by stirring in an apparatus similar
to that used by Meyerhoffer until its composition re-
mained constant, which required from one to 4
days. The tubes for the determinations made at
o° were kept in a large thermostat capable of holding
sufficient ice to last for 5 days. For saturation at the
four other temperatures the necessary heat was sup-
plied to the thermostats by electric lamps immersed
in the water or oil of the bath; a large mercury regulator
kept the temperature of the 25 ° and the 50° baths
constant to within 0.20. and of the 75° and 100° baths
to within i.o°.
The composition of the saturated solution was ascer-
tained by removing portions of it in a weight pipette
previously heated to the temperature of the bath,
weighing and analyzing the solution. The chlorine
ion was determined by titrating a fractional part of
the solution with a standard solution of silver nitrate,
the SO4 ion by precipitating anil weighing as BaSO<,
and the potassium ion by separating and weighing as
K.l'tCl,.
As it seemed probable that the control of any pro-
cesses based on these diagrams could be most easily
effected by means of a hydrometer the specific gravities
of most of the solutions were also determined. The
method consisted in removing and weighing, by means
of a pipette which had been drawn out to a capillary
at the mark on its stem, a definite volume of the solution,
1 Z. rhysik. Chtm. 18 (1899), 45...
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
measured at the temperature of the bath, and compar-
ing the weight with that of the water delivered by the
same pipette at a temperature of 20°. The results are
probably accurate to within two units in the third
decimal place. No corrections were made for changes
in the capacity of the pipette due to varying tem-
perature nor for variations in the volume delivered by
it owing to changes in the viscosity of the solution.
THE DIAGRAM TOR 25°
The composition of the solutions saturated with one
or more salts at this temperature expressed in grams
of the various salts per ioo grams of water is given in
Table I.1 In order to represent these results graphically
the corresponding values, when expressed in terms of
mols of the various salts which have equal replacing
power per iooo mols of water, were calculated. These
data are given in Table II; they are plotted in Fig. i
Na.SOi.lOH o
Fig. 1 — The Equilibrium Diagram at 25°
with respect to four axes, representing Na2SO,i, K2SOj,
K2CI2 and Na2Cl2, respectively, and the various points
are connected by straight lines, although it is probable
Table I — Composition, in Grams per 100 G. op Water, op Solutions
Saturated at 25°
Saturated with NaCl
Ai NaiSO.
Bi KiSO,
Ci KC1
Di|NaCl 35.63
El NaiSOi and glaserite
Fi KiSO, and glaserite
G. K;SO. and KC1
Hi KC1 and NaCl 29.88
II NaCl and NaiSOi 32.16
Ji NaiSOi and Glauber's
salt 18.82
Ki NaiSOi, Glauber's salt,
glaserite 14 . 28
Li KCI, KiSOi, glaserite.. 6.78
Mi KCI, NaCl, glaserite. . 27.96
Ni NaCl, NaiSOi, glaserite 34.90
Saturated with NaiCli
Ai NaiSOi
Bi K,SO,
Ci KCI
Di NaCl 54.90
El NaiSOi and glaserite
Fi K1SO1 and glaserite
Gi K:SO, ami KCI
Hi KCI and NaCl 46.04
Ii NaCl and NaiSOi 49 . 56
Jl Na;SO( and Glauber's
salt 29.00
Ki NaiSOi, Glauber's salt,
glaserite 21.92
EtSOi, glaserite 10.45
Ui KCI. NaCl. glaserite.. 43.08
Ni NaCl, NaiSOi, glaserite 53.75
that most of these are curved slightly. It should not
be forgotten that this kind of a diagram actually repre-
sents the horizontal projection of a solid figure. Any
point on it may represent a number of solution
1 In the tables in this article the subscripts of A, B, C, ct<
the figure on which the points are to be found.
KCI
NaiSOi
KiSOi
Sp. Gr.
27.93
1.212
12.02
1.088
36.96
1.187
1.199
30.97
9.31
1.282
6.69
13.24
1.149
36.63
1.53
1.190
16.28
1.237
9.81
1.239
21.68
1.243
22.28
7.32
1.273
29.38
2.23
1.200
16.37
3. SI
1.250
2.25
11.03
1.266
R 1000
Mols of
Water, c
P SOLU-
TED AT
25°
K1CI1
NaiSOi
KiSOi
Sum
35.41
35.41
12.46
12.46
44.62
44.62
54.90
39.27
9.63
48.90
8.48
13.69
22.17
44.11
1.50
45.61
19.66
65.70
12.44
62.00
27.5
56.50
28.25
7.57
57.74
35 . 49
2.30
48.24
19.78
4.45
67.31
2.85
11.40
68.00
ferent composition, but if perpendiculars are erected
at the limiting points and given lengths proportional
to the total number of mols present in the saturated
solutions to which these points correspond, and if the
ends of these perpendiculars are properly connected,
any point which appears on the planes which limit the
resulting solid figure can have a single definite value only.
The diagram agrees in all essential features with
that given by Meyerhoffer, with the exception of the
position of the point J representing the composition of
a solution containing sodium chloride and sodium sul-
fate in equilibrium with solid sodium sulfate and
Glauber's salt. His determination places the position of
this point as W. That this is in error was clearly
shown by duplicate determinations and also by de-
termining the points a, b, c and d on the line IJ, and e
on the line AJ, that is, the composition of solutions
containing sodium chloride and sodium sulfate, and
saturated with either sodium sulfate or Glauber's salt.
The diagram indicates the composition of all possible
solutions which can be in equilibrium with the six dif-
ferent solid phases: viz., glaserite,. Glauber's salt, sodium
chloride, sodium sulfate, potassium chloride and potas-
sium sulfate. Since the composition of glaserite may
vary between certain limits, the position of all points
representing solutions saturated with respect to it
may show slight variations. In determining the com-
position of such solutions care was taken to add only
sufficient of the prepared salt to inoculate the solution,
that is, to cause the greater part of the solid glaserite
present to separate from the solution itself. This in-
sured the presence of solid glaserite of a composition
corresponding to the limiting value of the salt which
could exist in the particular portion of the diagram
concerned. No difficulty was experienced in inducing
the salt to separate under favorable conditions, even
without inoculation. It invariably appeared in the
form of coarse, granular crystals sometimes 2 to 3 mm.
in diameter, which showed under the microscope a
well-defined hexagonal symmetry, and were uniaxial.
Fig. 2 — Crystals of Glaserite
The typical habit, which makes it easy to distinguish
the salt from either potassium or sodium sulfates, is
represented in Fig. 2, of which A represents a specimen
prepared at ioo0 and B a specimen prepared at 500
from the two simple sull
THE DIAGRAM FOR 0°
The data for this diagram arc given in Tables III
and IV. The graphical representation given in Fig.
3 differs from that given by Meyerhoffer in two funda.
346
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 5
mental respects. First, the position of the point I,
representing the composition of solutions in equilibrium
with solid sodium chloride and solid Glauber's salt, is
located by Meyerhoffer at the
point marked W. That the point
I represents the correct composi-
tion of the solution was shown by
the preparation of two different
solutions whose analyses gave
closely agreeing results.
The second difference relates to
the location and size of the glas-
)iM erite field. The Meyerhoffer dia-
gram shows that the glaserite
field includes the point F and ex-
Fic. 3 — Thb Equilibrium - . . , .
diagram at 0° teilds over an interval between
the points marked X and Y. It
also makes the glaserite field extend between lines join-
ing the points Y and L and the points X and O.
Table HI — Composition,
I Grams per 100 G. op Water, op Solutions
Saturated at 0°
Na»SO.
4.62
NaCI
KC1
28.20
7.81
10.06
13.24
KiSO.
Saturated with
Ai Na.SO.
Bi KiSO.
C. KCI
Di NaCI 34.95
Fi Glauber's salt and
K.S().
Gl KjSO, and KC1
Hi NaCI and KC1 31.53
Ij NaCI and Glauber's salt 34.48
Li KiSO., KC1, glaserite.. 13.38
Nj NaCI, Glauber's salt.
KCI 32.08
Oi KC1, Glauber's salt.
glaserite 27.07
Pi KsSO., Glauber's salt,
glaserite 7.46
Table IV — Composition, in Mols per 1000 Mols op Wate
tions Saturated at 0°
6.30
1.70
4.73
2.78
3.62
3.24
Sp. Gr.
1.043
1.063
1.153
1.206
1.118
1.240
1.232
SOLU-
Sum
5.85
7.47
34.05
53.84
17.29
34.91
61.33
55.60
43.76
62.62
57.21
33.50
Saturated with NaiCli KiCli NaiSOi KtSO.
Ai NaiSO. ... 5.85
Bi K.SO, ... ... 7.47
Ci KC1 34.05
Di NaCI 53.84
Pi Glauber's salt and
K1SO4 ... 7.99 9.30
Gi KiSO. and KC1 33.66 ... 1.25
Hi NaCI and KC1 48.58 12.75
Ii NaClandGlauber'ssalt 53.28 ... 2.32
Li KiSO., KC1, glaserite . 19.41 21.48 2.87
Nj NaCI. Glauber's salt.
KC1 49.44 9.43 ... 3.75
Oi KC1. Glauber's salt,
■i.iserite 41.71 12.15 ... 3.35
l'j K.Sli,. Glauber's salt,
glaserite 11.50 16.00 6.0
Several attempts to prepare a solution whose com-
position corresponded to that represented by the point
X failed. All such attempts resulted in the formation
of a solution whose composition was represented by
'it F. when made cither from Glauber's salt and
glaserite or by the use of potassium sulfate and a large
■ •I Glauber's sail and inoculating with gl:
Although glaserite seems to be unstable at this tem-
perature in contact with any possible solution made
from the constituent salts, it might be expected to
exist as a solid phase iii contact with solutions which
also contain sodium and potassium chlorides, since the
m by which it is formed involves the dehydration
of Glauber's salt. No difficulty was experienced in show-
ing that glaserite was stable in contact with solutions
isition was represented by points slightly
to the left of the line I. (», and t he locations of the points
1 ), both of which represent solutions saturated
with glaserite, were found to agree with those fixed
by the work of Meyerhoffer. The determination of
the third point which establishes the form and size of
the glaserite field gave more difficulty. By starting
with solutions containing varying amounts of sodium
chloride and saturating with both Glauber's salt and
potassium sulfate, solutions represented by the points
a, b, c and d, evidently in the line FP, were obtained.
By starting with solutions containing both sodium and
potassium chlorides and saturating with Glauber's salt
and glaserite, solutions represented by the points e
and /, evidently on the line OP, were obtained, and by
saturating a solution of sodium chloride with potassium
sulfate and glaserite the point g was obtained. These
make it possible to fix with apparent accuracy the posi-
tion of the point P. The points h and i on the line OL
were fixed by a similar method.
The other parts of the diagram differ but slightly
from those found by Meyerhoffer. The complete
diagram differs from that for 25 ° in the disappearance
of sodium sulfate as a solid phase and the very much
reduced area occupied by the glaserite field.
THE DIAGRAMS FOR 50°, "5° AND IOO°
Since Glauber's salt loses its water of crystallization at
$$°, even when in contact with a saturated solution
of sodium sulfate, it cannot exist as a solid phase above
this temperature in equilibrium with aqueous solutions
of any of the salts here considered, and the only solid
phases to be considered at temperatures of 50°, 750
and ioo° are Na;S05. K:SO,. KCI, XaCl and glaserite.
The composition of the saturated solutions which
determine the equilibrium diagrams for these tempera-
tures are given in Tables V, VI, VII, VIII, IX and X,
and the corresponding diagrams (Figs. 4, 5 and 6). If the
diagram for 25 ° be compared with those for 50 °. 75° and
100° it will be seen that the progressive changes in the
positions of the points C, H, I, L, M and N are such as
Fig. 4 — The Equilibrium Diagram at 50°
might be predicted from the changes in the solubilities
of the four simple salts. The changes in the points
E and F depend in part upon the specific properties
of glaserite, but it correlate the change of
Ei to E) with the very great increase in the solubility
of sodium sulfate between 25" and 50°, and the changes
from E< to Es and E< with the slight decrease in the
solubility of this salt between 500 and 750. Similarly
the successive changes from Fi to F,, F5 and F,-. are
correlated with the increase in the solubility of potas-
sium sulfate between 2 5 "and 100 °. The striking feature
of these diagrams is the great increase in the size of
the fields representing the composition of solutions
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Fig. 5 — The Equilibrium
Diagram
AT 75
0
TableJV — Composition, in Grams p
er 100 G. of Water, of Solutions
Saturated at 50c
Saturated with
NaCl
KCI
Na2SO.
K2SOI
Sp. Gr.
At Na2SOi
44.84
1.301
B< K»SOi
43! 12
1?!09
1.110
C« KCI
1.198
Di NaCl
36\50
1.188
E4 NaaSO* and glaserite. .
45! 73
9!io
1.351
Fi K2SO4 and glaserite.. .
6.79
17.36
1.307
G< KCI and K.SO<
42! 24
1.84
1.212
Hi KCI and NaCl
29! 09
22.03
1.246
I, NaCl and NaaSO.
33.70
7!34
1.223
Li KaSO., KCI, glaserite.
4.68
35.06
2 .'59
1.203
Mi KC1, NaCl, glaserite. .
26.84
22.43
3 ! is
1.254
Ni NaCl, Na2SOi. glase
40.15
14.58
11.74
1.248
Table VI — Composition,
N MOLS P
ER 1000
Mols of
Water, of Solu-
tions Saturated at
50°
Saturated with
Na2Cl2
K2CI2
Na2SOi
K2SO1
Sum
A( Na-SOi
56.86
17.60
56.86
Bi K2SO,
17.60
C< KCI
52'. io
52.10
Di NaCl
56.24
56.24
E« NaiSOi and glaserite. .
58! 00
9!72
67.72
Ft K2SO1 and glaserite
8.61
17.95
26.56
Gi KC1 and K2SO«
51.03
1.90
52.93
Hi KCI and NaCl
44! 82
26.61
71.43
I« NaCl and Na2SO, . . .
51.93
9.26
61.19
U K2SO., KC1, glaserite .
7.21
42^36
2!67
52.24
Mi KCI, NaCl, glaserite. .
41.36
27.01
4.00
72.37
Ni NaCl, Na2SO<, glaserite
40.15
14.58
11.74
66.47
Table VII — Composition,
in Grams
per 100 G. of Water, of Solutions
Saturated at 75
Saturated with
NaCl
KCI
N32SO.
K2SO1
Sp. Gr.
A» Na2SOi
43.41
1.286
Bi K2SO.
20
80
1.120
C KC1
49! 70
1.204
D» NaCl
37! 75
1.183
Et Na2SO( and glaserite. .
42.06
ii
77
1.332
F» K2SO< and glaserite . . .
10.09
18
60
1.183
Gi KC1 and K2SC
48! 75
2
12
Hi KCI and NaCl
27.87
29.06
l!249
It NaCl and Na2SOi
35.46
6!67
1.210
Li K2SO., KC1. glaserite .
5.71
42! 58
2
83
1.223
Mi KC1, NaCl, glaserite. .
25.45
29.38
3.33
1.257
N« NaCl, NajSOi, glaserite
28.28
15.72
8.88
1.253
Table VIII — Composition
, IN Mols
per 1000 Mols of
Water,
of Solu-
tions Saturated at
75°
Saturated with
Na2Ch
K1CI2
Na!SO.
K2SO4
Sum
Ai NajSOi
55.03
55.03
Bi K2SO<
2i!so
21.50
Ci KC1
6o!o2
60.02
Di NaCl
58! 17
58.17
El Na2SOi and glaserite. .
53
M
12! i7
65.51
F» K2SO1 and glaserite.. .
12
BO
19.23
32.03
Gl KC1 and K2SO4
58! 90
2.19
61.09
Hi KC1 and NaCl
42! 94
35.11
78.05
Ii NaCl and NajSO.
54.64
8
48
63.12
Li K2SO., KC1. glaserite..
8.80
51.45
2!93
63.18
Mi KC1. NaCl, glaserite..
39.23
35.50
4
23
78.96
Ni NaCl, Na2SO., glaserite
43.57
18.99
11
26
73.82
Table IX — Composition,
in Grams per 100 G. of Water, op Solutions
Saturated at
00°
Saturated with
NaCl
KCI
Na2SO.
KiSOi
Sp. Gr.
Ai NaiSO.
41.68
1.264
!!• K.SO.
23! 44
1.134
Ci KC1
56! 20
1.217
Di NaCl
39140
1. 175
El N&2SO< and glaserite. . .
4 1 ! 70
ii!<s2
1.326
Pi KiSO« and glaserite. . .
13.57
20.51
1.213
Gi JCSO, and KCI
54!43
2.83
1.225
Hi NaCl and KCI
27! 39
35.16
1 . 253
Ii NaCl and Na,SO,
36.56
6.41
1.204
U KiSOi, KCI, glaserite .
3.19
5o!6l
i!24
1.233
M, KCI, NaCl, glaserite....
Ni NaCl, Na,S()«, glaserite
24.82
36.13
3!77
1.269
35.84
10.18
ii
mi
1.256
Fig. 6 — The Equilibrium Diagram at 100°
Table X — Composition, in Mols per 1000 Mols of Water, of Solutions
Saturated at 100°
Saturated with NasCU K2CU Na2SO< KiSOi Sum
Ae Na2SOi ... 52.86 ... 52.86
B. K2SOi ... ... 24.07 24.07
C5 KCI 67.90 ... ... 67.90
Ds NaCl 60.81 ... ... ... 60.81
Ee Na2SOi and glaserite ... 52.88 14.08 66.96
Fs K2SO. and glaserite ... 17.21 21.21 38.42
Gt K2SO< and KCI 65.76 ... 2.93 68.69
He NaCl and KCI 42.20 42.48 ... ... 84.68
Is NaCl and Na2SOi 56.33 ... 8.12 ... 64.45
he K.SO., KCI, glaserite . 4.91 60.41 ... 3.24 68.56
M« KCI, NaCl, glaserite. . 38.25 43.65 4.78 ... 86.68
N« NaCl, Na2SOi, glaserite 55.22 12.31 ... 11.37 78.90
with which solid glaserite is in equilibrium. Some
further details of these diagrams will be described in
the following paper.
University of California
Berkeley
THE SEPARATION OF THE CHLORIDES AND SULFATES
OF SODIUM AND POTASSIUM BY FRACTIONAL
CRYSTALLIZATION
By Walter C. Blasdalb
Received March 20, 1918
Relatively little use has been made in the industries
of data similar to that presented in the preceding article,
although the possibility of doing so was indicated by
van't Hoff1 and has recently been discussed by Hilde-
brand2 as applied to the utilization of the bittern of
sea water. In this paper the data referred to will be
utilized in suggesting and testing the efficiencies of
methods for the separation of certain pairs of salts
which yield a common ion, and for the recovery of
potassium salts from two classes of materials which
are of special importance to the states of the Pacific
Coast. The first is the ash of kelp, which is already
produced on a large scale in the state of California;
the second includes certain natural brines found in the
desert regions of California, Nevada and Utah. Many
of the latter contain small amounts of carbonates,
bicarbonates and borates which would make it neces-
sary to modify to some extent any process based upon
these data; others contain such large proportions of
these substances as to make an entirely new set of data
necessary.
I SEPARATION (IF POTASSIUM CHLORIDE PROM SODIUM
CHLORIDE
The behavior upon evaporation of solutions contain-
ing different proportions of these salts can be easily
1 "Zur Bildung der ozcanischen Salzablagerung." 1MB.
> This Journal, 10 (1918), 96.
34«
1 111: JOURNAL OF 1 \ I'l STRIAL AND ENGINEERING CHEMISTRY Vol. 10, No.
followed by means of a diagram based upon the data
given in the preceding article. In this diagram (Fig.
I) the weight of sodium chloride in the solution per
ioo parts of water is measured along the vertical axis,
that of potassium chloride along the horizontal axis.
he Separation of Potassium Chloride from Sodium
Chloride
The points Di, D2, D3, D4 and D5 represent the composi-
tion of solutions saturated with sodium chloride at o°,
25°, 50°, 750 and ioo0, respectively, the points Ci, C»,
Cj, C4 and d that of solutions saturated with potassium
chloride, and the points Hi, H2. H3. Hj and H5 that of
solutions saturated with both salts. The lines D1H1,
etc., represent the composition of solutions saturated
with sodium chloride in the presence of varying amounts
of potassium chloride in solution and the lines CiHi,
etc., that of solutions saturated with potassium chloride
which contain varying amounts of sodium chloride.
It is assumed that all of these lines are straight, and
although no actual measurements have been made, it
is probable that they are curves which differ but slightly
from straight lines.
A solution which contains 20 g. of sodium and 14 g.
of potassium chloride per 100 of water is properly
represented by the point p on the diagram. Since this
point lies within the space included by the broken line
Ci Hi Di it is unsaturated, even at 0°, with respect to
both salts. When such a solution is evaporated the
proportion of the two salts to each other does not change,
and the process of evaporation corresponds to move-
ment of the point p in the direction Op. If the evapo-
ration is made at 100° the solution will become satu-
rated with sodium chloride at the point of intersection
of the two lims op and DiH6. The composition of the
m at this point ran be ascertained graphically,
that is. by measurement of its position with respect to
tin' axis of reference, or by formulating the equations
representing the two intersecting lines (namely, x =
i-l-ii.v and .v = 3Q.4 — 0.3413)') and solving for the
unknown co6r method gave the
values 22.07 KC1 and 31.86 NaCl per 100 H20. The
amount of water which must be evaporated bet'
point is reached is easily calculated as follows:
Let it la- assumed that we start with 134 g. of tin- solution re-
ferred t.. above When ;, reached the rati., of NaCl to HjO
must have changed from 2Q ioo to 31.8 100. If x represents
the water which is evaporated, the following relation is true:
20 : 100 — x = 31.86 : 100
When solved for x we obtain 37.22 g.
If the evaporation is still continued, sodium chloride
will continue to separate and the solution must change
its composition in a manner represented by movement
of the point q to H5, at which point potassium chloride
will begin to separate. If the sodium chloride which
has separated is removed and the temperature reduced
to zero, the solution becomes supersaturated with potas-
sium chloride, but unsaturated with sodium chloride,
and hence potassium chloride will separate out, and the
composition of the solution will change to correspond
to that represented by the point r. If the potassium
chloride is now removed and the solution again evapo-
rated at ioo°,its composition changes to that repre-
sented by the point s, at which point sodium chloride
will again separate. The result of these operations
can be calculated by methods similar to that already
used, to be as follows:
Composition of Substances
Solution NaCl KC1 HiO eliminated
At the outset 20 14 100
At the point q 20 14 62.78 37.22 g.H:0
At the point Hi 10.91 14 39.72 {23°9|'h*0I
At the point r 10.91 5.14 39.72 8.86 g'. KCi
At the point s 10.91 5.14 31.83 7.89g.H:0
The series of changes representing movement of r to s,
s to Hs, and H5 to r, constitutes a cycle which can be
repeated as long as any solution remains, or the residual
solution can be added to a further quantity of fresh
solution. Cooling to 25 ° rather than o° would reduce
the efficiency of the process but little and might prove
to be more economical.
II SEPARATION OF POTASSIUM CHLORIDE FROM POTAS-
SIUM SULFATE
The possibility of separating these salts can be easily
shown by reference to Fig. II which is based upon the
data given in the preceding article. In this diagram
the weight of KCI per 100 g. of water is plotted on the
horizontal, that of KiSCn on the vertical axis, and the
lines BjGi, B2G2, etc., represent the solubility of
potassium sulfate in the presence of varying amounts
PlC 11 Tin: Separation of Potassium Sulfate from Potassium
Chloride
of potassium chloride, while the lines Ci Gi, etc., repre-
sent the solubility of potassium chloride in the presence
of varying amounts of potassium sulfate. When a
solution of the composition p is evaporated at 100°,
K;St >, will separate first at the point q and will continue
to separate in pure form until the solution has the com-
position G( at which point potassium chloride will
separate also. If the temperature is now reduced both
May, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
349
KC1 and K2SO4 will separate, and the composition of the
solution will change to correspond with that represented
successively by the points G4, G3, G2 and Gi. This
is a consequence of the fact that the solubility of neither
salt is increased by decreasing the temperature as with
the KCl-NaCl mixtures. If the solution of composi-
tion Gi or G2 is again evaporated at 100° it will first
become saturated with KC1 at a point on the C5G5
line very near to G6, and very little additional evapora-
tion will suffice to saturate it with K2S04 as well as
KC1 at the point G5. The proportion of KC1 which
could be recovered in pure form by this part of the pro-
cess would be too small to be of commercial significance,
but the mixture obtained by continued evaporation at
the point G5 would contain only about 5 per cent of
K2SO4, and might be used for many purposes without
further purification. Hence in dealing with these mix-
tures it is possible to recover in pure form only that
amount of K2SO4 which must be separated before the
ratio of K2SO4 to KC1 is changed to the ratio of 1 to 20.
Ill THE SEPARATION OF POTASSIUM SULFATE FROM
SODIUM SULFATE
The changes which take place during the evaporation
of solutions containing the two sulfates can be predicted
from Fig. Ill which is based upon the data given in the
preceding article. The vertical axis represents grams
of K2SO4, the horizontal, grams of Na2S04, per 100 grams
of water. The lines B1F1, etc., represent the composi-
tion of solutions saturated with K2SO4 in the presence
of varying amounts of Na2S04, the lines FiE2, F2E2, etc.,
Fig. Ill — Thb Separation of Potassium Sulfate from Sodium
Sulfate
solutions saturated with glaserite in the presence of
varying amounts of K2SO4 and Na2S04, the lines F1A1
and E2A2 solutions saturated with Glauber's salt in the
presence of varying amounts of K2SO4 and E3A3, etc.,
solutions saturated with Na2S04 in the presence of
varying amounts of K2SO4. A study of the diagram
suggests two possible cycles representing possible
commercial methods.
If a solution containing 20 g. Na2SC>4, 10 g. K2SO4
and 100 g. of water, corresponding to the point p, is
heated to ioo° and evaporated at that temperature,
glaserite will begin to separate at q, and the com-
position of the solution will change from q to Ej;
if the temperature is then dropped to 50°, glaserite
will separate along the line E5r, parallel to the line
representing the composition of solutions which con-
tain K2SO4 and Na2SOi in the same proportions as
in glaserite, but no Na2S04 will separate as such
since the solution is not saturated with respect to
this salt at 500 until it attains the composition E3.
If the temperature is now dropped to 25° a very little
glaserite and much sodium sulfate will separate, and
all of the latter will be in the form of Glauber's salt by the
time the solution reaches the point E2; if the tempera-
ture is dropped to o° a little glaserite and much Glaub-
' er's salt will separate along E2Fi, but at some stage in the
process all the glaserite should change into potassium
sulfate and Glauber's salt, although it is probable that
this change will be slow and perhaps incomplete unless
the glaserite separates as a fine precipitate, and unless
it is agitated with the residual solution. In making
use of this cycle it is evident that a potassium-rich
mixture should be removed at r and a sodium-rich
mixture at E2 or Fi.
The second cycle suggested would involve evaporat-
ing at 500 instead of 100 °, that is, from s to E3 and re-
moving the potassium-rich mixture, then cooling to
25 ° or o° and removing the separated sodium-rich
mixture. The comparative efficiencies of the two
methods can be calculated, by the methods already
discussed, to be as follows:
Substances Eliminated by Process I
H2O Na2SO. K!SO«
Between p and q 37.5
Between q and Es 17.01 1.03 3.79
Between E» and r 0.39 1.43
Between r and Ei 8.60 7.16 1.36
Between E2 and Fi 13.02 9.92 1.26
Left in Solution 23.86 1.50 2.16
Substances Eliminated by Process II
H20 NazSOj K2SO.
Between p and s 25 . 37
Between s and Ej 33.54 1.22 4.49
Between E3 and Ej 10.86 9.42 3.12
Between Ej and Fi 11.43 8.18 0.69
Left in Solution 18.80 1.19 1.70
These figures show that the total amount of K2SC>4
recovered by Process I in a concentrated form is some-
what greater than that recovered by Process II, also
that the proportion of K2S04 lost with the sodium-rich
mixture is less in Process I than in Process II. It is
also probable that under most conditions evaporation
at 100° would be more economical than at 50°. The
treatment of the residual solution by either of the two
processes would be more efficient than the treatment
'of the original solution. The effect of cooling to 25°
only would be to decrease greatly the proportion of
K2SO4 to Na2S04 in the residual solution and to increase
the amount of water which would have to be removed
by evaporation in the treatment of this residual solu-
tion.
The separation of pure K2S04 from the potassium-
rich mixture would involve large wastes of either power
or product, but it is probable that its K2S04 content
could be utilized as such without further concentration.
It is doubtful whether the sodium-rich mixture (espe-
cially 1 hat obtained by cooling to o°) could be profitably
treated for the recovery of the potash which it contains.
since it could not be concentrated to a greater degree
than would be represented by solutions saturated with
both sodium sulfate and glaserite, which at 100° would
correspond to the point Es.
IV THE SKPARATION OF SODIUM SULFATE I-'KUM SODIUM
(III 0RIDE
The diagram needed for the discussion of this ...
tion is shown in Fig. IV. The horizontal axis repre-
35°
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 5
sents grams of Na2S04, the vertical axis grams of NaCl,
per ioo g. of water. The lines Dili, etc., represent
solutions saturated with NaCl in the presence of vary-
ing amounts of Na2S04, the lines I2J2, I3A3, I1A4 and
I5A5 solutions saturated with Na2S04 in the presence of
NaCl, and I1A1 and J2A2 solutions saturated with
Fig. IV— Thk Se
Glauber's salt in the presence of Na2S04 and NaCl. It
will be assumed that a solution which consists of 20 g.
Na2S04, 10 g. NaCl and 100 g. H20 is to be treated.
The composition of this solution is represented by the
point p. When evaporated at 100° pure Na2S04 would
separate from q to the crystallization end-point at I5.
If the separated sulfate is removed and the solution
allowed to cool to 250, pure NaCl would separate until
the solution attains the composition r, or if allowed to
cool to 0°, both NaCl and Glauber's salt would separate
until it attains the composition I». If the former
procedure is adopted the separated NaCl could be
removed, the solution again evaporated at 100°, a
further quantity of pure Na2SOi recovered, am
cycle of changes repeated as in the separation of KC1
from XaCl, but it is obvious that the amount of pure*
salt separated would be small, and in view of the cheap-
ness of both salts not commercially feasible.
Cooling to o° would give a residual solution contain-
ing a relatively small proportion of Na2S04 and would
also eliminate a large amount of water as water of
crystallization. The efficiency of these processes
could be calculated quantitatively, but an approximate
idea can also be gained from a study of the diagram.
V— THE SEPARATION OF SALTS OF POTASSIUM FROM
MIXTURES FATES AND CHLORIDES
OF SODIUM AND POTASSIUM
preliminary discission— In applying the method
already used to the discussion of the more complex
mixtures here considered it becomes necessary to make
use of diagrams in which concentrations are expressed
in molecular equivalents, since the salts actually presert
are in part ionized, and the manner in which the un-
ionized basic elements and the acidic elements or groups
are actually combined is both variable and difficult
to ascertain. Hence the composition of all such solu-
tions will be expressed in terms of the number of mols
of Xa-..C12, K2C12, Na2S04 and K2S04 per 1000 mols of
water. The composition of any of these solutions can
be expressed in terms of any three of the four, and the
three actually used will be chosen arbitrarily. By
plotting the concentration with reference to two axes,
intersecting at right angles, as explained in the previous
paper, it is possible to prepare diagrams which properly
represent the composition of any such solutions. A
clearer idea of the uses of such diagrams can be gained
from a study of Fig. V which represents the equilibrium
conditions for the system here considered at 250. The
formulas which appear on the different areas represented
on this diagram indicate the composition of all possible
solutions which are saturated with respect to the salts
represented by these formulas. The lines separating
these fields represent the composition of solutions satu-
rated with respect to the two salts of the adjacent field,
and the points of intersection of these lines the composi-
tion of solutions saturated as to the two or three salts
adjacent fields. It should be noted that each
area represents the bounding surface of a solid figure,
and that all points within the space enclosed by these
surfaces represent unsaturated solutions. When such
a solution is evaporated the change in its composition
corresponds to the movement of the point representing
it in a straight line away from the origin. The point
at which this line intersects the surface of the solid
figure indicates the salt with which the solution first
becomes saturated and the composition of the solution
at that point. If the process of evaporation be con-
tinued the salt continues to separate, and the composi-
tion of the solution changes in a manner represented
by movement of the point of intersection along a line,
which is on the intersected surface, in a direction away
from the point representing saturation with^respect to
the salt concerned in water, that is, in the absence of
F10. V — The Separation of Complex Mixtures at 25°
all other salts. These lines will not in general be straight
lines, but in most cases the error involved in assuming
them to be straight will not be large. \.A
The points representing saturation with respect to
NasS0.,.ioH:O. lvSO,. K,C1S and Na,Cli are A,, Bj, C
and Di, and the series of lines radiating from these
points represent the "crystallization paths" of solutions
from which these salts separate during evaporation.
The point representing saturation with Xa2S04 is found
longing the line I2J2 until it intersects OAj.
The assumption is made here that if NasS04 could exist
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
35i
at 25° in equilibrium with water, and if its solubility
were changed by varying concentrations of NaCl be-
yond Jo at the same rate as between I2J2, its solubility
in pure water would correspond to the point R. The
point representing saturation with pure glaserite is
found by drawing from 0 a line representing solutions
containing K2S04 and Na2S04 in the ratio of three to
one (as in pure glaserite) and finding its intersection
with the line E2F2. Here it is assumed that if pure
glaserite could exist in equilibrium with water at 250,
and if its solubility were to be changed by varying pro-
portions of K2SO4 and Na;S04 uniformly along the line
E2F2, the composition of the solution with which it was
in equilibrium would be represented by the point S.
Having in this manner drawn crystallization paths
on all six of the surfaces bounding the figure, it is readily
possible to predict the crystallization paths after the
lines separating these surfaces have been reached.
It is obvious that solutions corresponding to points on
the N2M2 line, which are to the right of the line joining
D2 and S must change to correspond with the point
Ms, whereas those to the left of this line must change
to correspond with the point N2 when evaporated;
that is, there are two "crystallization end-points,"
M2 and Ns- Aside from the fact that the Glauber's salt
field is eliminated, the crystallization paths on the 100 °
diagram (Fig. VI) differ from those of the 25 ° diagram
mainly in the fact that there is only one "crystalliza-
tion end-point," namely M5. This is a result of the
fact that both N6 and M5 are to the right of the line
joining D5 and S.
THE SEPARATION OF POTASH FROM THE ASH OF KELP
From a study of the analysis of the ash of a typical
sample of Macrocystis pyrifera, which is the species of
kelp most largely used in California, made by P. L.
Hibbard,1 it would appear to be readily possible by
leaching with water at ioo° to prepare from such an
ash a solution containing 30 g. KC1, 10 g. NaCl, and 6 g.
Na2S04 per 100 g. of H20. The composition of this
solution, expressed in mols of K2CI2, Na2Cl2 and Na2S04
per 1000 mols of water, can be calculated as follows:
149.12 = 0.20.12
116.92 =
142.06
= 0.20.121 / 36.20 mols KsCl;
= 0.0855 ( * I80 = ) 15.39 mols NaiCh
= 0.0422 ( \ 7.60 mols NaiSO.
= 5.555 J \ 1000. mols H.O
The composition of this solution corresponds to the
point p, of Fig. VI, which represents the equilibrium
diagram at ioo°. It is obvious that, when evaporated,
glaserite, then glaserite and potassium chloride, will
separate until the composition of the solution corre-
sponds to the point M5. The total amount of H20,
glaserite and K2C12 which separate during the evapora-
tion can be calculated as follows:
Let x = H20, y = K2CI2, 2 = glaserite separated.
Then the following relations representing changes
in the composition of the solution as to K2, SO4, Cl2
and Na2 are obvious.
(1) 36.20— y — 1.
(1) 7.60— 2j
(3) 51.59— y
(4) 22.99 — 0.5 t
1000— x = 43.65 : 1000
1000— x = 4.7X : 1000
1000— x = 81.90 : 1000
1000 — i = 43.03 : 1000
When solved for x, y and z these equations give the
following values in mols:
H20 = 495.87, K2CI2 = 10.30, glaserite = 2.59
1 University of California Experiment Station, Bulletin 248, 142.
The residual solution could then be calculated to have
the composition in mols:
504.13 H20, 22.01 K2Cl2, 2.41 Na2S04, 19.28 Na2Cl2.
It is also of some interest to ascertain the amount of
H20 which must be evaporated before any glaserite
separates, the water which separates with the pure
Fig. VI — The Separation of Complex Mixtures at 100°
glaserite, and the water and K2CI2 which separate
along the line L5M5. These calculations are somewhat
long but the methods can be outlined as follows:
1 — Calculate the ratio which the K2C12 separating along the
line L5M5 bears to the H20 and to the glaserite separating simulT
taneously, assuming the rate is a uniform one.
2 — Calculate by means of these ratios the weights of H20
and glaserite which would separate after the K2C12 begins to
separate, from the total amount of K2C12 separated, and add the
amounts of H20, K2C12, NajSCX and Na2Cl2 which they represent
to the amounts of these salts present at Ms to obtain the amoimts
present at the point r.
3 — Subtract the glaserite lost between r and Ms from that
lost between q and Ms to find that lost between q and r and add
the amounts of K2C12, Na2SC>4, and Na2Cl2, which it represents,
to the amounts of these salts present at r to find the amounts
present at q.
4 — Determine the intersection of Op with the crystallization
path passing through r to get the coordinates of the point q
and from them the amount of water present at q.
5 — Subtract the sum of the amounts of water lost between
q and r and between r and Ms from that lost between p and Ms
to get that lost between p and q.
The results of these calculations gave when expressed in mols:
Loss between p and q = 182.0H2O
Loss between q and r = 151.16H2O + 2.955 glaserite
Loss between r and M5 = 162.71 H20 + 0.25 glaserite
+ 10.3 K.CI2.
If the solution is now cooled to 25 ° it will become
greatly supersaturated with respect to K2CI2 as is
shown by the position of Ms on the 25° diagram (Fig.
V). After the excess of KC1 has separated its composi-
tion will be represented by some point on the plane
C2H2M2L2G2. The determination of the position of
this point can be made by the following procedure:
1 — Calculate the total amount of K2CI2, glaserite and HjO
which must separate in passing from Ms to M2.
2 — Calculate the ratio which the amount of glaserite separating
along the line L2M2 bears to the amount of KsCU and of water
separating sinmltaneoualy, as uming that the rates are uniform.
3 — Calculate, by the use of these ratios, the weights of HjO
352
THE JOURNAL OF IS DUST RIAL AND ENGINEERING CHEMISTRY Vol. 10. Xo. 5
and K2C12, which separate after the glaserite begins to separate
at the point /, from the total amount of glaserite separated and
add the amounts found to the amounts of these substances present
at Mi to get the composition of the solution at /.
4 — Subtract the H20 and K2C12 lost between I and M; from
the amounts lost between M2 and Ms and add to the amounts
present at M; to find the amounts present at s.
5 — Determine the point of intersection of the crystallization
path tVn with the horizontal line Ms s, and from the coordinates
of this point determine the K2C12 present at the point s.
(1 — Subtract the sum of the amounts of K2C12 lost between
I and M2 and between s and I from that between Ms and M2 to
find the amount lost between Ms and s.
The results of these calculations can be summarized
as follows:
Loss between Ml and J= 10.28 K;C1:
Loss between j and I = 1 . 25 K:CI: + 21 .68 HiO
Loss between ( and Mi = 1 .20 K:C1:, 28. 15 HjO + 0.19 glaserite
It is not probable that these solutions could be evap-
orated at a temperature of 25° economically and the
only reason for calculating the changes which take place
in evaporating the solution from s to X2 was to ascertain
the composition of the solution at s, that is, at the point
at which all the KC1 which can be separated by cooling
to 25°, has separated. The most rational procedure
would be. to evaporate the solution of composition 5
at 100° for the purpose of eliminating salts of sodium.
By again referring to Fig. VI it will become apparent
that when this evaporation is made glaserite and XaCl
must separate, but it is not possible to predict a priori
which of the two will separate first. By using methods
similar to those already employed it can be shown that
the solution will first become saturated with XaCl
at the point u, that XaCl and H20 will separate along
uv and that H«0, XaCl and glaserite will separate
along i>Ms. These changes can be summarized as
follows:
Loss between J and a = 75.5.5 II: 0
I.oss between land) = 101.64 HiO, 6.09 XaiCli
Loss between V and Mi = 79.33 HiO, 4.66 NaiClj, 0.61 glaserite
This completes a cycle of changes similar to that de-
scribed in the separation of KC1 from XaCl, but one
which is less efficient than the former since some potash
is necessarily included with the sodium salts separated
at ioo°.
A comprehensive idea of the entire process as out-
lined may be gained by summarizing the changes during
the three important stages in terms of the weights
d salts expressed in grams.
Composition of solution at outsit 100 H-O. 30 KCI, 10 NaCl. 6 MaiSOi
Separated during evaporation to Mi 49.59 H.< I, 8 53 KCI. 3.36 glaserite
Separated during cooling to s 8.51 KCI
Separated during t\ ipM ition to Mi 25 63 II.i >. 6 98 NaCl, 0.79 glaserite
Left in residual solution 24. 74 HiO, 8.95 KCI. 6. 13 NaCl, 0.94 N
I III "1 POT \S11 PROM A Hi SERT URINE —
A sample of brine from a hole near the center of Death
Valley which was analyzed by A. R. Merz1 will serve
as an illustration for the application of the data of
the preceding article to this class of substances. The
of the analysis, expressed in grams per ioo cc.
of solution, was 3.00 KCI, 25.97 NaCl, 0.71 N
and 1.28 g. of undetermined salts. Although the
gravity is not given, a solution of this composi-
tion should give a value not far from 1.24 and the com-
position of the solution in grams per 100 g. of H20
> This Joubnal, S (1913), 23.
can be calculated to be 3.64. KCI, 30.92 XaCl and 11.56
Xa2S04. Calculated to mols per 1000 mols of water
these values become
4.40 K2C12, 47.60 Xa2Cl2, 1465 Xa2S04, iooo H20.
A solution of this composition would be represented by
the point m on Fig. VI, and when evaporated at ioo0
sodium sulfate must separate first, then a mixture of
sodium sulfate and sodium chloride, and finally glaserite
and sodium chloride corresponding roughly to move-
ment from m to n, from n to X5. and from Nj to Ms.
The change from m to X5 can be calculated to involve
the elimination of 814.2 mols of H20, 39.45 of Xa2Cl:,
and 12.45 of Xa2S0i; the change from X5 to M5 of 11 5. 5
H20, 6.79 Xa2Cl2 and 0.886 glaserite. This would
leave 70.3 mols of H20, 3.27 of Xa2Cl2, 3.08 of K-Cl-
and 0.34 of Xa2SO), which solutions could then be
treated by the cyclic process already described in dealing
with the ash of kelp.
The chief objection to this method of procedure is
the large amount of evaporation needed; this might
be decreased by utilizing solar evaporation to some ex-
tent. If, for example, it were permitted to evaporate
at 25 ° the solution would attain a composition cor-
responding to X2 of Fig. V as the result of the elimina-
tion of 614 H20, 31.25 Xa2Cl2, and 5.49 Xa2S04.
Further evaporation at this temperature would not
change the composition of the solution and it would be
necessary to continue the evaporation at a higher tem-
perature (preferably at ioo°) in order to concentrate
still further the potassium salts present.
A third possible method would involve cooling the
brine to 0° for the purpose of eliminating much of the
Xa2SO< and H20 as Glauber's salt before evaporation.
The composition of the original solution on the 0°
diagram (Fig. 3 of the previous article) is represented
by a point which shows that it is supersaturated at this
temperature with Glauber's salt and sodium chloride.
The composition of the solution after the excess of these
salts has separated must be represented by a point on
the line I3X3; it can be established by making use of
the following considerations:
1 — The original solution contains 4.4 K-C12, but (as shown
later) the solution loses 13S mols of water with the separated
Glauber's salt, hence the K2C12 content at the desired point must
be 4.4 -5- (1000 — 138) = 5.1 per 1000 H-O.
2 — Since the K2C12 changes from o to 13.18 between I» and
Ns, the desired point must be (5.1 -5- 13.18) times the distance
I3 — N'3 from I, This locates it at q, which required the presence
of 48.5 Na»Cli and 0.97 Na-SOi.
3 — The Glauber's salt which must separate in order to cause
N.i .S< >< to change from 14.65: 1000 to 0.97: 1000 can be found
by trial to be 13.80. Similarly the Xa.CU which must separate
in order to cause the NTa2Cls to change from 47 6 : 1000 to 48.5 :
1000, in spite of the loss of 138 mols of water associated with the
separated Glauber's salt, can be calculated to be 5.8.
This leaves a solution containing 41.S \..
K2C12, 0.85 Na Si i, and S62 H20 which can be treated
by methods similar to those used for the ash of kelp.
Of the three methods suggested for the treatment of
the brine the second gives promise of being the most
economical.
The application of similar methods of treatment to
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
the waters of Owens, Searles, Mono and other desert
lakes presents a more complex problem, owing to the
fact that these waters contain large percentages of
carbonates. It is not improbable that when the dia-
grams representing the equilibria, which must exist in
solutions which contain carbonates as well as sulfates
and chlorides of sodium and potassium, have been
prepared it will be found possible to suggest methods
by which the salts present in such waters can be profit-
ably separated into commercial products. It is also
possible that it may be found commercially feasible to
precipitate most of the C03 ion, either as NaHC03
or CaCC>3, from certain of these waters and recover the
potassium salts in the residual solution by the methods
already described.
University op California
Berkeley
THE USE OF "MINE RUN" PHOSPHATES IN THE MANU-
FACTURE OF SOLUBLE PHOSPHORIC ACID
By Wm. H. Waggaman and C. R. Wagner1
Received February 21, 1918
The increasing price of acid phosphate makes
it appear timely, if not absolutely essential, to
look to other methods of producing available phos-
phoric acid which will not only release to the muni-
tions industry part of the immense tonnage of sulfuric
acid now manufactured at the fertilizer plants, but
will also enable the farmer to continue to obtain
phosphates at a cost which will justify their applica-
tion to the soil.
The method which has received special attention
in this Bureau is that based on the smelting in an elec-
tric furnace of a mixture of phosphate rock, sand and
coke, whereby the phosphoric acid is volatilized and
subsequently collected by means of the Cottrell pre-
cipitator. The equations showing this reaction may
be represented thus:
Ca,(P04), + 3Si02 + sC = 3CaSi03 + 2P + 5CO
2p + S02 = P205
Ross, Carothers and Merz5 showed that the Cottrell
precipitator gave acid of such a high degree of con-
centration that the added cost of production by the
electric furnace method could be overcome in part
at least by the saving in freight charges over the lower
grades of commercial phosphates.
In order to obtain more definite data on the cost
of producing phosphoric acid by volatilization and
electrical precipitation this Bureau conducted some
work in cooperation with the R. B. Davis Company,
of Hoboken, N. J., over a period of several months.
In a recent report on this work Carothers3 showed that
phosphoric acid fP205) could be produced by this
method at a cost of 3.37 cents per lb., exclusive of
interest on investment, taxes and royalty. By using
the phosphoric acid thus obtained, however, to treat
another batch of phosphate rock, double superphos-
phate is formed, a prod lining three times
as much phosphoric acid as ordinary acid
■The writers wish lo express their thanks to I'rof Milton Whitney,
who suggested the work described in this paper.
■ This Journal, 9 (1917), 26.
■ Ibid., 10 (1918), IS.
and as Ross, Carothers and Merz1 have pointed out,
the making of double superphosphate brings down
the price of phosphoric acid produced by the vola-
tilization process very materially.
In order to compare the economic merits of the fur-
nace process with that of the old established sulfuric
acid method of making superphosphate, details of the
cost of the two processes are given below in Tables
I, II and III. In these estimates it is assumed that
washed rock will contain an average of 34 per cent
of phosphoric acid (P205) and that 90 per cent of this
is recoverable by the furnace method of treatment.
It is also assumed that the proportions of sand and
coke necessary to smelt the high-grade rock from the
different localities is practically the same.2 The esti-
mates on the cost of the furnace treatment are based
on Carothers' figures3 obtained at Hoboken, N. J.,
but they are modified on the assumption that the
process is carried on at the mines. Allowances, there-
fore, have been made only for the difference in the
cost of phosphate rock, sand and coke.
While the cost of labor and of power undoubtedly
varies considerably in different parts of the country,
a uniform charge has been made for these items through-
out. In the case of the labor and repairs necessary
in the manufacture of ordinary superphosphate a
charge has been made which is 50 per cent higher
than that prevailing in the South Atlantic States
prior to the war.
Since Carothers gives no estimates on the cost of
installing the furnace process, no interest, charges,
taxes and insurance are included in the cost data
for the acid phosphate process.
A comparison of the data given in Tables I and III
show that under the present abnormal conditions the
phosphoric acid in double superphosphate produced
by using the acid volatilized in the electric furnace
compares favorably in cost with that of ordinary
acid phosphate. This is particularly true when we
consider that in shipping such a concentrated product
as double acid phosphate the freight rates per ton
of phosphoric acid (P205) are considerably reduced.
Based on the conditions existing prior to the war,
this saving in freight charges should be more than
counterbalanced at the end of the war by a considera-
ble drop in the price of ordinary acid phosphate, due
to the release of an immense tonnage of sulfuric acid
no longer needed for the manufacture of munitions.
So in order that the furnace method may permanently
compete with the acid process of producing soluble
phosphates, the cost of the former must be materially
lowered.
There is, however, another and a very important
factor to be considered in connection with the furnace
method of producing phosphoric acid which makes
this method worthy of more serious consideration,
'Phis factor is the immense saving to bi
de pho i'li it.es and phosphatic material
1 hoc. cil.
1 \vh,[ n is not strictly correct, due to thl
composition of the different types of rock, it serves all practical put
" Carothers' figures an based OS ■< plant t.f 3000 kw. capacity pro-
ducing 2.147 tons l'/O, annually
354
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 5
TABLE I ) 1 CM • < • • OST (AT THE Minks) 1
Phosphate Rock 3.18
Sulfuric Acid (50° Be.) 3.44
Labor and Repairs
3.50
9.90(a)
1.30(6)
Total Cost
Dollars
11.13
34.06
8.61
53.80
Florida Pebble Phosphate
Cost
per Ton
1 '..!! .!
Quantity
Tons
3.18
3.44
Total Cost
Dollars
7.95
34.06
8.61
50.62
Tennessee Brown Rock Phosphate
Cost
Quantity per Ton Total Cost
Tons Dollars Dollars
3. IS 2.75 8.75
.5 44 9.90(a) 34.06
8.61
51.42
ii: Electric Furnace Method prom Various
Florida Hard Rock Phosphate Florida Pebhlk Phosphate Tennessee Hkown Rock Phosphate
Phosphate Rock 3.32
Sand 1 .50
Coke 0.75
Operating Expenses:
Electrodes,
Labor
Power
Total Cost.
Total
Cost
Dollars
11.62
0.37
6.00
3.32
1.50
0.75
Total
Cost
8.30
0.37
6.00
3.32
1.50
0.75
Cost
per Ton
Dollars
2.75
0.50
4.50
Items Ton
Phosphate Rock 0.98
PjOj in Form of 58° Be.
Acid 0.67(a)
Labor and Power
Drying
68.58
1.30(4)
0.25(6)
Total Cost
Dollars
3.43
45.95
2.68
0.52
Quantity
Ton
0.98
Total Cost ... 52.58
■ Equivalent to 1.08 tons of 58° Be acid.
(6) Cost per ton of material handled.
in the present system of mining and preparing a high-
grade rock for the market.
Since the fertilizer manufacturer finds it imprac-
ticable to acidulate rock containing more than 3 to 4
per cent of the combined oxides of iron and aluminum,
the phosphate miners have installed elaborate washing
plants in order to turn out a product high in phosphoric
acid and low in these objectionable impurities.
In the mining and concentration of Florida phos-
phate, all material passing screens of 3/i6-in. mesh
is discarded and washed out through a flume upon a
dump or waste heap. Of the total material mined in
these fields an average of not more than 1 5 per cent
is saved as marketable rock having a phosphate of
lime content ranging from 68 to 78 per cent. The
85 per cent of detritus which is washed away contains
the equivalent of from 32 to $s per cent of phosphate
of lime and represents an annual loss in phosphoric
acid fully twice as great as that marketed.
In the electric smelting of phosphate rock the pres-
ence of sufficient silica to produce silicates of calcium
is necessary in order to set free the phosphoric acid
contained in the rock. When using high-grade phos-
phates this necessitates the addition of a considerable
quantity of sand in order to obtain the proper silica-
lime ratio. Obviously, it would be very much more
practical from an economic standpoint to use, if possi-
ble, phospha1 J already containing sufficient
silica and alumina for smelting purposes than to sepa-
rate these materials by an expensive washing process
only to put them back again when the material is
charged to the furnace.
With this idea in view the writers undertook a num-
ber of experiments to test the feasibility of smelting
65.26
1.30(a)
0.25(a)
Total Cost
Dollars
2.45
43.72
2.68
0.52
Tennessee Brown Rock Phosphate
Cost
Quantity per Ton
Ton Dollars
0.98
0.67
Total Cost
Dollars
2.69
63.84
1.30(a)
0.25(a)
"mine run" material in the. electric furnace, thus
avoiding the expense and losses entailed in handling
and washing the rock.
For this .work samples of "mine run" material
were obtained from each of the following three locali-
ties:
1 — Hard rock phosphate and matrix from New-
berry, Florida.
2 — Pebble phosphate and matrix from Ft. Meade.
Florida.
3- — Tennessee brown rock phosphate from old dumps
near Mt. Pleasant, Tennessee.
The analyses of these samples of phosphatic ma-
terial are given in Table IV:
<d Waste
Florida Pebble Tennessee
Phosphate Brown Phos-
nd Matrix phate Waste
Per cent
1 .49
14.23
29 . 85
Hard Rock
and Matrix
Constituent Per cent Per cent
CO, 2.22 1.53
SiO, 14.37 45.99
P.Ot 30.69 15.38
AI1O1 + FttOi 5.03 7.50
CaO 42.07 22.79
F 3.68 1.58
Total 98.06 94.77
Since the most practical ratio of lime to silica for
use in the smelting of phosphate rock is approximately
i to 1.44 it will be seen from the analyses given in
Table IV that all of these "mine run" samples require
additions of either sand or phosphate rock in order
to produce a charge suitable for furnace treatment.
It is the opinion of the writers, however, that none
of the samples is representative of the field from
which it came, the Florida hard rock and matrix and
the Tennessee waste material being higher, and the
May, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY 355
Florida pebble1 sample lower in phosphoric acid than on the "mine run" samples and that required for a
the average "mine run" material from these fields. charge made up with high-grade washed rock, but it
In order to obtain a charge of the desired composi- seems unlikely that there would be much difference
tion the phosphatic material from the pebble region in these figures. In fact the lowering of the melting
of Florida was reenforced with a washed rock con- point of the former charge due to its higher content
taining 32 per cent of P205 and 7 per cent of Si02. of iron and aluminum oxides should more than counter-
The Florida hard rock and matrix and the material balance the extra number of thermal units required
from the Tennessee dump heaps were mixed with a high- to raise the temperature of the increased quantity
grade, white sand and sufficient coke was added in of slag.
each instance to bring about the necessary reduction In calculating the figures given in Tables VI and VII,
in the smelting operation. Approximately 500 lbs. showing the cost of producing phosphoric acid (P205)
of charge were made up in each instance, and smelted from "mine run" material by means of the electric
in the electric furnace for 3 hrs., the phosphoric acid furnace, a 90 per cent recovery is assumed in order to
volatilized being collected by means of the Cottrell make the figures comparable with those of Carothers1
precipitator. Since the charge used was relatively on high-grade washed rock.
small and the period of run was comparatively short, By comparing the figures given in Table VII with
no attempt was made to determine the quantity of those of Table III, it will be seen that the cost of
P206 volatilized from the weight of acid collected, producing one ton of P203 by smelting "mine run"
but at the end of 3 hrs. the furnace was tapped and phosphate in the electric furnace would be materially
the amount of phosphoric acid (P205) still remaining lower than that of treating high-grade phosphates
in the slag was determined by analysis. The amount which have undergone an expensive mechanical wash-
volatilized was thus obtained by difference. ing and screening process to prepare them for the
The figures showing the efficiency of this furnace market. If the sample from the pebble regions of
treatment as applied to "mine run" rock are given in Florida had been of better grade — and from the
Table V. writer's knowledge of the Florida deposits, it seems
Table »V— Quantity of Phosphoric Acid (P2Os) Volatilized from a tu,t ^ocf nf the "mine run" rorV will rennirp nn rP
Charge Made Up of "Mine Run" Phosphates when Smelted in the Inal" mosx ol Ine mine run TOCK will require no re-
Electric Furnace for 3 Hrs. enforcement with higher grade phosphate rock — -the
PjOs age of cost of producing one ton of P205 from "mine run"
Exdulife fto. in Remain0' ^i""" material in the various fields would be from $3.75 to
Phosphatic Materia! co^F aXL si£Xr *Stod" $6.50 less than from high-grade phosphates.
Used in Charge Per cent Per cent Smelting Per cent Although it would be necessary to wash and screen
Hard Rock and Matrix 22.0 0.50 1.8 98.2 _ . 7^ . , . , , . ... ., ,
Land Pebble and Matrix... i9.i 0.66 3.0 97.0 sufficient phosphate rock for treatment with the phos-
Tennessee Waste Material . . 21.3 0.67 2.7 97.3 , • -j , . • j u ti. I 4.-1* ».•
phone acid obtained by the volatilization process,
While the figures given in Table V show a higher the use of the electric furnace at the phosphate mines
volatilization of P20» from the "mine run" material would save the vast bulk of phosphate now discharged
than from the high-grade rock used in the commercial upon the waste heaps and thus greatly prolong the
operations at Hoboken, N. J., such results would prob- life of the phosphate mines. Whether or not this fac-
Table VI — Estimated Cost (at the Mines) of Producing One Ton of Phosphoric Acid (P2O6) by the Electric Furnace Method from "Mine Run"
Phosphates
Florida Hard Rock and Matrix Florida Pebble and Matrix Tennessee Brown Phosphate Waste
Cost Cost Cost
Quantity per Ton Total Cost Quantity per Ton Total Cost Quantity per Ton Total Cost
Items Tons Dollars Dollars Tons Dollars Dollars Tons Dollars Dollars
Phosphate and Matrix 3.62 0.50 1.81 4.89 0.50 2.45 3.73 0.75 2.80
Washed Pebble for Reenforcing .. ... 1.12 2.50 2.80
Sand 1.64 0.25 0.41 .. .. ... 1.64 0.50 0.82
Coke ^ 0.75 8.00 6.00 0.75 8.00 6.00 0.75 4.50 3.37
Operating Expenses 50.59 .. .. 50.59 .. .. 50.59
Total Cost .. 58.81 .. .. 61.84 .. .. 57.58
Table VII — Estimated Cost (at the Mines) of Producing One Ton of Available Phosphoric Acid (PiOs) in the Form of Double Superphosphate
by Treating High-Gradb Phosphate Rock with Phosphoric Acid from "Mine Run" Material
Florida Hard Rock Phosphate Florida Pebble Phosphate Tennessee Brown Rock Phosphate
Cost Cost Cost
Quantity per Ton Total Cost Quantity per Ton Total Cost Quantity per Ton Total Cost
Items Ton Dollars Dollars Ton . Dollars Dollars Ton Dollars Dollars
Phosphate Rock 0.98 3.50 J. 43 0.98 2.50 2.45 0.98 2.75 2.69
P1O1 in the Form of
58° Be. Acid 0.67(a) 58.81 39.40 0.67 61.84 41.43 0.67 57.58 38.58
Labor and Power 1.30(6) 2.68 .. 1.30(6) 2.68 .. 1.30(d) 2.68
Drying 0.25(6) 0.52 .. 0.25(6) 0.52 .. 0.25(6) 0.52
Total Cost ... 46.03 .. ... 47.08 .. ... 44.47
inivalent to 1.08 tons of 58° Be. acid.
OSt per ton of material handled.
not be obtained in an actual run over a protracted tor would counterbalance the lower cost (under normal
■1 of time when conditions would not always be conditions) of producing soluble phosphate by treat-
favorable. No data were obtained which would ad- ment with sulfuric acid would probably have to be
mil of a comparison between the power consumed definitely determined by actual experience.
' More representative samples of pebble phosphate and matrix showed v g DRPARTMBNT OP Aoriculturb
■ composiiion more nearly corresponding to the proper furnace charge. bureau of Soils, Washington, D. C.
but there were not sufficient quantities of these materials to smelt in the
furnace. * Loc. cil.
3 56
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. s
THE CONCENTRATION OF POTASH FROM RAW MATE-
RIALS CONTAINING ONLY A TRACE OF THIS
ELEMENT BY MEANS OF THE ELEC-
TRIC PRECIPITATION OF FLUE
DUST AND FUME CEMENT
KILNS
By B. F. F.KDAm.
Received. June 25, 1917
With a view of securing more definite information
regarding the concentration of potash from flue dust
and fume cement kilns, a series of experiments was
made during the past 6 mo. at a cement plant using
limestone and blast-furnace slag as raw materials and
powdered coal for fuel.
During the period of experiments outlined herein
an electric precipitation system was installed; 4 pre-
cipitators were put in operation successively, one
applied to each kiln. The plant has 4 kilns 150 ft.
long and 10 ft. in diameter. The precipitation system
was installed primarily to abate the dust nuisance
and recover the dust for clinker. It occurred to the
writer that the system at the same time might serve
as a concentrator of potash volatilized from the kilns.
In order to find the potash content of the limestone,
the slag, the coal ash resulting from the fuel, the clinker
and the precipitated dust, a series of analyses was
made of weekly average samples during the past 6 mo.
From these analyses it was found that the potash
content of the limestone and clinker remained constant;
the potash content of the slag varied from 0.28 per cent
to 0.69 per cent, of the coal ash from 1.20 per cent
to 1.52 per cent; the potash in the precipitated dust
increased with each addition of a new treater to the
system of kilns.
The latter fact suggested the idea that the precipita-
tor system may serve as a concentrator of volatilized
potash.
The amount of potash going in with the raw material
during a week was figured from the registered dumps
of the raw material scales and the amount of potash
produced from the coal ash was figured from the amount
of coal used to burn the number of barrels of clinker
corresponding to the raw material passing through.
A fairly representative week showed the following
results:
Limestone contained 0.06 per cent KiO, existing most likely as insoluble
feldspar. KA1I W •
Slag contained 0.69 per cent KiO. existing mainly as soluble K1CO1 and
KaSOt, the former derived from the coke ash. the latter precipitated
from KsCOj by vapors of SOt and HjO in the blast furnace.
Coal ash contained 1.20 per rent K:0. existing as soluble KiCOj.
Clinker contained 0 14 per cent KjO.
With these percentages for the week in question
were calculated the number of pounds K20 going
in with the raw material and coal and the amount of
KjO coming out with the clinker, the difference giving
us the number of pounds volatilized potash for the
week, thus:
Limestone curried in ... 3084.30 11-
irritd in 31082 89 !i
sh carried in 1756.00 11-
Volatilized 10.891
■•scd in percentage = 70 ulized
Tin- writer lias considered the difference between the
amount of potash fed to the kilns with the raw material
and coal and the amount leaving the kilns with the
clinker as volatilized potash. Strictly speaking, some
of the potash, however, goes over as non-volatilized
with the dust blown from the kilns by the draught
before the mixture reaches the volatilizing zone. The
dust thus carried over is not any richer in potash than
the corresponding mixture and the amount of potash
in it is in relation to the total potash content in the
mixture as the regular stack loss is to the whole raw
material charge. The non-volatilized potash, there-
fore, represents a small amount compared with the
volatilized and as a distinction between them will
not influence the subsequent calculations, it is omitted.
The highest efficiency as to volatilization of potash
is dependent on many factors. The writer's personal
experience based on analyses of clinker, clinkerdust,
clinker balls and rings under varying kiln conditions
seems to point out as the main factors for producing
the highest possible percentage of volatilized potash:
i — A kiln temperature of 25500 F. or higher.
2 — A neutral or slightly over-limed mixture, facili-
tating the formation of a small nut sized clinker which
in turn would make easier the liberation of potash
possibly enclosed in the clinker.
3 — A low percentage of sulfur in the slag and the
coal, decreasing the formation of S02 which in turn
would tend to precipitate less of the more difficultly
volatilizing K2SO4, leaving the greater part of the potash
as K2C03.
From the preceding data it will be seen that some
potash, in spite of normal kiln conditions, will re-
main in the clinker, but at the same time it must be
remembered as an important fact that this loss is prac-
tically constant. This leads to another conclusion,
namely, that the potash once volatilized is easily vola-
tilized again. The writer had occasion to verify this
through the successive erection of the four treaters.
The potash content of the dust returning to the kilns
increased with the addition of precipitators and as
the result the charge to the kilns became richer in
potash but the potash content of the clinker remained
constant. It is, therefore, evident that a precipita-
tion system returning all the dust from the flue gases,
assuming 100 per cent efficiency, would conserve all
the potash volatilized. At the clinker end the potash
cannot escape over and above a certain constant amount
mentioned above because of the volatilization tempera-
ture in the clinkering zone; at the stack end the potash
will be returned by the electric precipitator; practically
the efficiency is not absolute; normally a recovery of
approximately 96 per cent is obtained; the dust es-
caping is richer in potash than the average dust pre-
cipitated; this material is not coal ash but conforms
to the general analysis of dust returned to the
with the exception of its potash content. The fact
that this escaping dust is richer in potash than the pre-
cipitated seems to be a consequence of operating an
electrical precipitation installation. The heavier dust
is easily collected, while the recovery of tine fume
s a more difficult problem. As the potash
volatilized in the kilns is largely present in the form of
fine fume it naturally follows that the escaping ma-
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
357
terial will be richer in potash than the material col-
lected.
In order to discover the laws governing the accumu-
lation taking place, a dump of the raw material scales
was taken as a unit for the purpose of calculation.
A dump at the plant where and during the week these
investigations were conducted was a representative
one and consisted of 1500 lbs. of limestone and 13 14 lbs.
of slag, while the fuel necessary to burn this to a clinker
produced 42.7 lbs. ash.
Accordingly a dump represents:
From limestone 0.90 lb. KiO
From slag 9.07 lbs. KiO
From coal ash 0.51 lb. KjO
Totai, 10.48 lbs. KsO
As the volatilized potash escapes back through
the kilns with the speed of the gases and cools off
below its condensation point some of it strikes and
adheres to the walls of the back end of the kilns and
the walls of the kiln housings and gas coolers, while
some will solidify in small particles and intermingle
with the dust. The former part will deposit while
the latter part will act as dust and later be returned
to the kilns. It is, therefore, convenient to dis-
tinguish between the deposits and the circulating dust,
as they are following different laws as to accumulation.
In deposits closest to the clinkering zone the K2S04
naturally will be prevalent, while there are indications
that the potash in the circulating dust is mainly
K2C03. It is hard to tell how much of the volatilized
potash will deposit and how much will be left in the
■circulating dust. The writer has assumed that 3/io
will deposit. This, however, is an arbitrary figure
used for the purpose of determining the law of this
potash accumulation.
Regarding the dust escaping through the electric
field or stack loss, it amounted to approximately
1500 lbs. in 24 hrs. for each precipitator or to 36,000
lbs. for the week the investigation was made, during
which time the precipitators recovered approximately
•96 per cent of the dust passing through them. A
representative average sample of this escaping dust
is for practical reasons extremely hard to get. The
best sample the writer could "obtain analyzed 1.20
per cent K20, but this result is most likely too low.
Conceding this, the potash content of the escaping
1 will show a lower limit in the subsequent calcu-
lations than really will exist. This circumstance,
however, will not change the principle in the laws of
potash accumulation, so the above result will be used
\ in calculations below. Accordingly, the stack loss
I for the week in question amounted to 432 lbs. K20.
(In other words, of 25,240.89 lbs. volatilized K20,
432 lbs., or, expressed in percentage, 1.7115 per cent,
were lost through the stacks in spite of the precipitators.
With these preliminary data at our disposal we
will follow the volatilized potash in its circuit through
the precipitation system and elicit the laws of accumu-
lation.
In order to make clear the distribution of the potash
and its recirculation the results at the different stages
are tabulated below.
It will be necessary to recollect that the potash
once volatilized is all volatilized again; that 29.74 per
cent of the total potash in a unit of 10.48 lbs. K20
remain in the clinker; that V10 °i the volatilized potash
are assumed depositing in the back end of the kilns,
the kiln housings and the gas coolers; that 1.7115 per
cent of the volatilized potash is lost through the stacks.
98a °£ °i . -ggS o.Se 0^22 .Sm«-
«£S «a» «-gJ| 53°-- «"2 M--2a. Q-aS
oJIO "Sg^ lUj a SH oa.2 •=*§ M2|
-05 -| t" s|g „"3.2j» -'£.2- 0=-:^ =«m
o~°"£ oil '^«m'I'0o'3 int>' «>°SJ5 111
Cycle Efe'iS E«" o>3-2 &Wk3 H~£S ?5SS |a2
No. << < > a < ^ <•
1 10.48 3.1168 7 3632 2.2090 5.1542 0.1260 5.0282
2 5.0282 + 10.48 3.1168 12.3914 3.7174 8.6740 0.2121 8.4619
3 8.4619 + 10.48 3.1168 15.8251 4.7475 11.0776 0.2708 10.8068
4 10.8068+10.48 3.1168 18.1700 5.4510 12.7190 0.3110 12.4080
Gathering from this table the results on the in-
crease of potash in the returning dust and in the de-
posits in the back end of the kilns, the kiln housings
and the gas coolers and further the results on the loss
through the stacks we have:
Returning Dust Deposits Stack Loss
Lbs. Lbs. Lb.
Cycle No 1 5.0282 2.2090 0.1260
Cycle No. 2 8.4619 3.7174 0.2121
Cycle No. 3 10.8068 4.7475 0.2708
Cycle No. 4 12.4080 5.4510 0.3110
According to the results for the returning dust we
find an increase of 3.4337 from Cycle 1 to Cycle 2,
2.3449 from Cycle 2 to Cycle 3 and 1.6012 from Cycle
3 to Cycle 4. The total of these increases carried into
infinity — or what may be considered infinity for all
practical purposes — will form a series like this:
2 = 3-4337 + 2.3449 + 1. 6012 + 00
This series is a converging geometric progression in
which the coefficient between the terms is approxi-
1000
mately — — . Without any appreciable error we may
1465
100
for use in our calculations call the coefficient
147
In studying the series we will observe that the in-
crease is getting smaller all the time and is approach-
ing a limit. The reason for this is the separating out
of the deposits and the stack loss. In order to find
the limit of the increase we may put down the follow-
ing equation:
ioo\
— ; - 3.4337
Z = —77- ~= IO-7394
M — 1 100
147
Starting out in the progression with 3-4337 while the
total available increase is 10.7394, it is evident the
returning dust — with the amount assumed depositing
and the figured stack loss — will increase only 3.1276
times its original amount.
When the last treater in our system started up,
the returning dust contained 1.47 per cent K80. The
laws of the progression above may be applied to this,
using as coefficient, or we may simply multiply the
■47
percentage by 3.1276, thus:
IOO\
,, J — '•'»'
4/ - = 1.47 X 3-1276 = 4-6o
100
1
147
353
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. 5
Accordingly, the limit of the potash content in the
returning dust should be 4.60 per cent, but it must be
remembered that the increase is mainly governed by
the amount deposited. As previously stated, 3/io is
only an arbitrary figure, so the returning dust may
run higher or lower in potash, according to the size
of this figure; but nevertheless we will on the whole
get the benefit of the volatilized potash one way or
the other, with the exception, of course, of the stack
loss.
The writer used this way of calculating under the
successive erection of precipitators.
When 2 precipitators had been in operation for a
reasonable length of time the limit of the increase,
taking into consideration the extra loss through the
stacks not connected up, was figured to be 0.58 per cent
K2O and analysis strikingly corroborated this; when
3 precipitators had been in use for a fair length of
time the limit with the same consideration as above
was figured to be 1.47 per cent K20 and again analysis
strikingly corroborated the figured result; finally when
4 precipitators had been in operation for a reasonable
length of time the limit was figured as above to be
4.60 per cent K20 — analysis again giving corroborating
result. For depositing figures in these, three cases
were used, respectively V10, 2/io and Vie
The deposits in the back end of the kilns, the kiln
housings and gas coolers follow a different law as to
accumulation from that of the circulating dust. Study-
ing the cycles we see that 2.2090 lbs. K20 are de-
posited during Cycle 1 and note they stay there; during
Cycle 2. 3.7174 lbs. are brought in and so on.
Accordingly the series for the deposits will be:
5 = 2.2090 + 3.7174 + 4-7475 + 5-45IQ+ °°
forming a progression, the total of which goes beyond
limits. The amount deposited each time, however,
is approaching a limit. There is an increase of 1.50S4
between Cycles 1 and 2, 1.0301 between Cycles 2
and 3, and 0.7035 between Cycles 3 and 4. In order
to find the highest possible amount to be deposited
at one time we may use the series:
2 = 1.5084 + 1. 0301 +0.7035+ »
100
Here again the coefficient is , approximately, for
x47
reasons previously mentioned, and accordingly we
have:
S =
„ /ioo\
1.50S4I 1 — 1.5084
\ 147'
100
147
= 4-7177
As we started out in the progression with 1.50S4, we
will observe that the highest available deposits for one
cycle will be 3.1276 times the original amount and
consequently we have:
2.209
2 =
°(10°)
100
147
— 2.2090
= 2.2090 X 3.1276 = 6.9090
The series for the deposits will therefore look thus:
2 = 2.2090 + 3.7174 + 4.7475+5.4510+. . . .6.9090= »
This theoretically means that the deposits will go on
until the system is clogged up. When that will take
place practically is just a matter of conjecture as our
depositing figure, V10, is an arbitrary one and may be-
considerably smaller. Also some of the deposited
cakes may loosen from the walls and drop into the-
conveyers for the returning dust and in that case,.
what we lose in deposits we will get back in the cir-
culating dust.
The work on locating and analyzing deposits is still
in progress. Up to date they have been found to be
richer in potash than the circulating dust. Deposits
containing 6 per cent K20 have been found at the en-
trance of the gas coolers.
Regarding the stack loss it will be seen from the
cycles that it also will increase. In order to find the
largest amount going out we note the increase in loss-
from Cycle 1 to Cycle 2 to be 0.0861, from Cycle 2
to Cycle 3, 0.0587, and from Cycle 3 to Cycle 4, 0.0402.
The series for the stack loss will accordingly be:
2 = 0.0861 + 0.0587 + 0.0402 + °°
This is also a converging geometric progression in which
100
the coefficient is — , approximately, for reasons stated.
147
previously.
Consequently we have as before:
0.0861
CO
\I47/
147
0.0861
= 0.2693
Starting out in the progression with 0.0861 while
the highest loss is 0.2693. it follows that the highest-
possible loss of potash through the stacks will be
3.1276 times the original amount.
For a sample taken before the last precipitator was.
connected up the writer found 1.20 per cent K.O
in the dust escaping from the stacks. This value is
conceded too low, as previously mentioned, but being
the only figure at hand it will be used in our final
calculation and accordingly we have as before:
>(I0°)
V147/
= 1.20 X 3.1276 = 30
In view of this we may look for a loss of K2O passing
through the stacks in spite of the precipitators, a loss
steadily increasing up to a certain limit. This limit
probably should be the same as the limit for the re-
turning dust. Some time after the last precipitator
started up, but before the limit could have been reached,
the writer found a sample of escaping stack dust to
analyze 3.65 per cent K20.
This potash in the dust and deposits exists mainly
as soluble K2C03 and KjS0«, making the dust and de-
posits suitable fertilizing material.
MARY
1 Under normal kiln conditions about 30 per cent
of the potash in the raw material and the fuel will
remain in the clinker while 70 per cent will be vola-
tilized.
May, 1 918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
359
II — There will occur an accumulation of volatilized
potash in the back end of the kilns, the kiln housings
and the gas coolers which in time may clog up the
system.
Ill — Under normal precipitator conditions the cir-
culating dust will increase in potash up to a certain
limit, the increase being governed by the amount
deposited and the efficiency of the precipitators and
following the laws of a converging geometric progression.
IV — In spite of fairly ideal precipitator conditions
there will occur a loss of potash through the stacks,
a loss steadily increasing up to a certain limit and also
governed by the amount deposited and the efficiency
of the precipitators and following the laws of a con-
verging geometric progression.
Universal Portland Cement Company
Duluth, Minnesota
TOLUOL FROM SPRUCE TURPENTINE
By A. S. Wheeler
Received March 25, 1918
The heavy demand for trinitrotoluol is taxing the
resources of the country in toluol, and any new source
for the latter requires careful investigation in the hope
'of increasing the supply. It has been suggested that
[spruce turpentine, a waste product of the sulfite
[process of making sprucewood paper pulp, might
serve as an important source of toluol. Spruce tur-
pentine is remarkable in that it consists largely of one
aromatic hydrocarbon, cymol (cymene). It has been
attracting interest in several quarters in recent years.
;The French chemists Boedtker and Halse1 subjected
[the crude turpentine and also pure cymol to the Friedel-
[Crafts reaction with benzol and obtained high yields
lof toluol and cumol. On account of the importance
!of the reaction I have attempted to repeat their best
experiment in order to confirm their findings and offer
pn this paper a preliminary report, giving the results
of the first two experiments.
Boedtker and Halse reported on four experiments
as follows: (1) 150 g. crude 90 pep cent cymol (spruce
[turpentine itself), 1 kg. benzol and 30 g. aluminium
[chloride boiled 6 hrs. on the water bath. Products:
I52 g. toluol, 75 g. cumol. (2) 100 g. cymol, pure,
B kg. benzol and 20 g. aluminium chloride boiled 6
hrs. Products: 41 g. toluol, 85 g. cumol. (3) 100 g.
cymol, pure. 1 kg. benzol and 10 g. aluminium chloride
3>oiled 8 hrs. Products: 31 g. toluol, 67 g. cumol.
■(4) 90 g. cymol, pure, 900 g. benzol and 4.5 g. alumin-
ium chloride boiled 10 hrs. Products: 44 g. toluol
■80 per cent), 68 g. cumol (85 per cent yield). (The
ifigurc, So per cent, is an error. A recalculation shows
^hat this ought to be 71 per cent, the theoretical yield
being 61.8 g.) A Vigreux column was used in the dis-
tillations but no statement is made as to the number
of fractionations and no figures are given for the boiling
points of the fractions. Further, it is not known what
the authors mean by pure cymol. A number of boiling
points have been given for this compound but Schor-
ger* seems to have prepared a pure product. This
1 Bull. sot. chim., |4] 19 (1916), 444.
' J. Am. Chem. Soc, 39 (1917), 2671.
was due to the observation that concentrated sulfuric
acid removes impurities which have defied a variety
of active agents. As late as 191 6, Bogert and Tuttle1
worked with an impure cymol.
In the two preliminary experiments reported below
the purification of the cymol was not carried to the
extreme limit. The Champion Fiber Company, of
Canton, North Carolina, is generously furnishing the
spruce turpentine for this investigation. The first
experiment was carried through by the author. The
second, or parallel, experiment was carried through
from the beginning to the end by Mr. E. P. Wood,
a senior student in chemistry and I wish to thank him
here for his careful work.
The spruce turpentine was purified by first subject-
ing it to distillation in superheated steam, the vapor
being carried through hot 10 per cent caustic soda and
then condensed in the usual way. The crude turpen-
tine was pale red, but the condensed oil was brilliant
and water-white. The caustic soda assumed a reddish
color. Seventy per cent of the oil passed over into
the receiver but a newer shipment is giving a larger
yield as high as 87 per cent. If caustic soda is not used
the distillate is lemon-yellow in color. The oil was
separated from the water and shaken several times
with 0.5 per cent potassium permanganate, then 20
times with one-sixth its volume of concentrated sul-
furic acid. The first addition of sulfuric acid assumed
a very dark color, later washings a red color and finally
a pale yellow color. Schorger states that pure cymol
gives no color with this acid. The oil was then shaken
with water several times, dried with calcium chloride
and finally boiled with metallic sodium. It was dis-
tilled with a Glinsky still head and the main portion,
boiling at 177-177.5°, was employed in the reaction.
The benzol was a sample of Baker's C. P. It was
dried over calcium chloride and boiled with metallic
sodium. The aluminium chloride was freshly prepared
by passing dry hydrochloric acid gas over hot aluminium
filings.
EXPERIMENT I
90 g. cymol, 900 g. benzol and 4.5 g. aluminium
chloride were boiled together on a water bath for 10
hrs. The solution became dark red. The fractiona-
tions of the product were carried out with a 3-section
Young still head, with results as follows:
1 79-80"
2 80-81°
3 81- 83"
4 83- 95°
5 95 U0C
6 110-131°
380
242
184
Volume
1 Cc.
7 113-141° 15
8 141-151° 11
9 151-154° 47
10 155-200° 6
11 200°+ 3(o)
(a) Fluorescent.
The second distillation was begun with Fraction
No. 4 and gave the following results:
Fraction Temperature Volum<
No. Interval Cc.
1 80-83° 80
2 83-95° 50
3 9S-100° 3
4 100-105° 2
5 105-109° 4
6 109-113° 15
7 113-115° 11
No
[\ inp-t
Interval
8 115-120°
9 120-131°
10 131-151°
11 151-154"
12 154-156°
13 156-170°
14 170° +
Accumulations occur at the vicinity of the boiling
points of toluol, 110°, and cumol, 153°.
I J. Am. Chem. Soc, 38 (1916), 1352.
360
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 5
A sample of No. 6, 109-113°, was easily and smoothly
converted into trinitrotoluol (TNT), according to the
method recommended by Hoffmann.1 The crude
product, washed with hot water, melted at 76-78°.
After one recrystallization from a mixture of alcohol
(9 parts) and benzol (1 part), pale yellow needles,
melting sharply at 80-80.5°, were obtained in excellent
yield.
EXPERIMENT II
88. 5 g. cymol, 885 g. benzol and 4.5 g. aluminium
chloride were boiled together on a water bath for 10
hrs. A 3-section Young still head was used in the
first fractionation and a 5-section Young still head in
the second.
ti-II
Temperature
Volume
Fraction
Temperatu
So.
Interval
Cc.
Xo
Interval
1
.. 79- 81°
501
7...
.. 141-1M0
'
.. 81- 83°
299
8...
. 151-154°
3
.. 83- 95"
151
9...
. . 154-170°
4
.. 95-110°
21
10...
. . 170-180°
5
.. 110-131"
16
11...
. . 180-200°
h
.. 131-141°
16
12...
. . 200° +
For the second distillation, Fraction No. 2 was
started with.
1
. 80-81°
249
7.. .
. . 115-120
,'
. 81- 83°
126
8...
. . 120-131
.1
. 83- 95°
62
9...
. . 131-141
4
95-108°
6
10. . .
. . 141-149
-1
. 108-112°
22
11...
.. 149-154
r>
. 112-115°
8
12...
.. 154° +
The accumulations again show toluol and cumol.
The amounts are less in both experiments than those
claimed by Boedtker and Halse. They gave no state-
ment as to the purity of their products so that ques-
tion is in doubt. On our part some necessary step
may still be lacking for maximum yields. The investi-
gation is being actively pursued. Boedtker and Halse
introduced in each of their experiments two variants
so that it cannot be said which variant changed the
results. It will be noted that 17 molecules of benzol
were used for one molecule of cymol. It is hoped to
materially reduce this proportion. The mechanism
of the reaction will be studied in order to determine
whether the cymol furnishes the methyl or the tolyl
group for the toluol. It is noted that the published
work on the nitration of cymol and of cumol is of an
unsatisfactory character and these reactions are being
reexamined.
CON>
Spruce turpentine yields toluol when subje
the combined action of benzol and aluminium chloride.
The other product, cumol, is not a waste product
since it may be oxidized directly to benzoii
This will save a like amount of toluol now used to make
benzoic acid.
1'm\i:rsitv op North Carolina
Ciiaim:i. Hal, N. C.
ARSENIC IN SULFURED FOOD PRODUCTS
liv \\ . D. Collins
1918
IN 1 K. im CTION
It has been recognized for a long time that appreci-
able quantities of arsenic might be taken up by food
1 Bureau of Mines, Technical Paper 146 (1916).
products through treatment with sulfur dioxide fumes
obtained by burning sulfur which contained arsenic.
The most notable case of contamination of food
products with arsenic was the well-known instance
of poisoning at Manchester, England, caused by ar-
senic in beer. The investigation that followed showed
that the arsenic in the beer came from the use of glu-
cose or brewers' sugar which was made from starch
by the use of sulfuric acid which contained large
amounts of arsenic. Analyses of some of the samples
of sulfuric acid showed as much as 2 per cent of arsenic
as AS2O3. Samples of the glucose contained from 0.01
up to nearly 0.1 per cent of arsenic. Samples of the
beer in question contained up to 1.0 or 1.5 grains of
arsenic per gallon of beer, and some even as high as
3 grains per gallon. The average medicinal dose c#
arsenic mentioned in the U. S. Pharmacopoeia is 2
mg. or one-thirtieth of a grain. In the report of the
English Commission which investigated these cases
of arsenical poisoning, it was recommended that liquid
food materials should be considered adulterated if
they contained as much as 0.01 of a grain of arsenic
per gallon, and that solid food materials should be
considered deleterious if they contained as much as
0.0 1 grain of arsenic per pound. The results of the
investigation showed that it was entirely possible to
keep the arsenic below these limits in all the materials
used in the production of the beer and in the other
food materials which were investigated at that time,
provided care was taken to keep the materials free
from arsenic.
In connection with an investigation of the subject
of arsenic in wines, Dr. H. D. Gibbs,1 in 1905. suggested
arsenical sulfur as one of the possible sources of arsenic.
Several samples of the Japanese sulfur which he ex-
amined showed amounts of arsenic up to several
hundred parts per million. Dr. VT. W. Stockberger,*
in a bulletin published in 1908, suggested that sulfur
was probably the cause of the presence of appreciable
amounts of arsenic in certain samples of sulfured hops.
It appears to be recognized by the dealers in sulfur
that it is desirable to use for bleaching hops and dried
fruits sulfur which is free from arsenic. It is probable
that certain users of sulfur have made some effort
to obtain sulfur which contained no arsenic.
In 1914, as a result of objections made to some ship-
ments of hops from the United States to foreign por
on account of the fact that the hops were said to cor
tain more arsenic than was permissible, the Depa
ment of Agriculture investigated again the questic
of the source of arsenic in dried hops. Dr. Stockberge
of the Bureau of Plant Industry, visited the hop
growing districts and collected samples of unsulfure
hops, sulfured hops and samples of the sulfur used
He also collected samples of sulfur used on the hop
in the shipments which were rejected on account
excessive arsenic. Two samples of sulfur from thii
lot showed 3:0 and 356 parts of arsenic per million
The writer made a study of various methods for th
determination of small quantities of arsenic in sue
1 J.
•V. S Dcpt. of A>:r., Bureau of Plant Industry. Bull. 1S1 O908),
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
361
materials as hops and sulfur and after reaching a satis-
factory method, as described below, determined the
arsenic in samples of sun-dried hops, kiln-dried hops
and sulfur.1
METHOD OF ANALYSIS
The use of the Gutzeit test for the quantitative de-
termination of arsenic has been discussed by Sanger
and Black,2 Smith,3 Allen and Palmer,4 and recently
by Beck and Merres5 of the Kaiserlichen Gesund-
heitsamt who found Smith's method entirely reliable.
Many references to the literature are given by these
authors. On account of the difficulties found in
applying the various methods described, it seems worth
while to describe fully the details of the method found
satisfactory for the examination of hops. It is mainly
a selection of some of the procedures described by
C. R. Smith.
OUTLINE OF METHOD
The method depends upon the action of arsine upon
a salt of mercury. The arsine is produced by reduc-
tion of an arsenious compound by nascent hydrogen
obtained with zinc and an acid. -In the colorimetric
method the arsine acts along a strip of paper impreg-
nated with mercuric bromide, and the amount of
arsenic is measured by the brown color produced.
In the gravimetric method the arsine acts on mercuric
chloride in solution and the mercurous chloride ob-
tained on boiling is weighed.
PRECAUTIONS
To obtain consistent results in the colorimetric
method where comparison is made with standard
stains, it is essential that the rate of evolution of hydro-
gen and of arsine be the same in all cases for a given
amount of arsenic. Smith recommends cooling the
generator in making standard stains to obtain results
comparable with those obtained with samples contain-
ing salts in solution. Allen and Palmer advise using
more acid when salts are present. Smith's precipita-
tion method seems more certain to give a uniform
amount of salts in the generator. The arsenic is pre-
cipitated as ammonium magnesium arsenate together
with ammonium magnesium phosphate by adding about
2 g. of a soluble phosphate to the solution of sample
and then precipitating with magnesia mixture and am-
monium hydroxide. This precipitate is large enough
to mask small differences in the amounts of salts so
that solutions for standard strips and for the samples
will have practically the same conditions in the genera-
tor if the same amount of acid is used to dissolve the
precipitate. In testing substances which will give a
precipitate in ammoniacal solution with the ammonium
magnesium phosphate, allowance must be made for
the extra amount of salts which will be in the generator.
In order that the rate of evolution of arsine may be
the same in all cases, it is necessary that the arsenic
be reduced to the arsenious condition before zinc is
1 Thi: detailed results of the analyses are Riven in U. S. Dcpt. of Agr.,
Bull. 668, "The Presence of Arsenic in Hops " W. W. StockljerKcr and W. D.
Collins
» J. Soc. Chem. lnd., 26 (1906). I I I v
• U. S. Depl of Akt . Bureau of Chemistry, Circular 102 I 191
' Orig. < ",..m. xih Inter. Conn. Apfl. < htm , 1 (1912), 9-17.
• Arb. toil. Cesundh., 60 (1916), 38-49.
added. The choice of reducing agent and of acid de-
pends upon the amount of arsenic present, and for the
best results the proper combination must be selected.
When hydrochloric acid is used in the generator it
is not easy to secure sufficiently slow evolution of gas
to make a strongly colored stain if enough acid is used
to 'Complete the reduction of the arsenic. This diffi-
culty is overcome by using sulfuric acid, but if potas-
sium iodide and stannous chloride are used for reduc-
tion with sulfuric acid, it sometimes happens that
reduction of sulfuric acid to hydrogen sulfide takes
place and the determination is lost. It is possible,
however, to fail to reduce all the arsenic to the arsenious
state without the use of potassium iodide if much more
than 0.1 mg. of arsenic, as As203, is present. For
small quantities, reduction with stannous chloride
(0.5 g.), with 1 g. sodium chloride and 10 cc. sulfuric
acid in a volume of 75 cc, gives consistent results.
For larger quantities which are to be determined
gravimetrically, so that the rate of action need not be
the same in every case, reduction by stannous chloride
and potassium iodide in hydrochloric acid solution is
best.
The surface area of the zinc will affect the rate of
action. Care must be taken to use always the same
number of pieces of zinc of the same size. The amount
of iron in the zinc will affect the rate of solution and,
therefore, the appearance of the stain.
The capacity of the apparatus and the amount of
liquid used in the generator will affect the appearance
of the stain.
For obtaining a test for a very small quantity of
arsenic, as to distinguish between 0.5 and 1 microgram,
it may be best to use a small generating bottle; but
for quantitative measurement of amounts from 5 to
50 micrograms a larger generator gives more uniform
results, though the time required is longer.
The temperature of the reaction affects not only
the rate of evolution, but, as pointed out by Allen,
the temperature determines the amount of moisture
in the gas evolved and so affects the appearance of
the stain. Differences of one or two degrees in tempera-
ture are not likely to have any measurable effect on
the stains, but as much as io° may have a decided
effect.
APPARATUS
The accompanying diagram shows the form and
dimensions of the apparatus used.
REAGENTS
THE SENSITIZED STRIPS OF DRAWING PAPER, II Cm.
long by 2.0 or 2.5 mm. wide, are prepared by soaking
for one hour in a 5 per cent alcoholic solution of mer-
curic bromide. The excess solution is wiped off and
the strips dried on glass rods.
acids and zinc may be purchased practically free
from arsenic.
SODIUM CHLORIDE is usually free from arsenic, but
samples of reagent sodium chloride have been found
to contain measurable amounts.
01 chloridi i" liabli i" contain traces oi
arsenic. This !"■ removed by beating the solution
of the salt in hydrochloric acid with pieces of metallic
362
THE JOURNAL OF INDUSTRIAL AND ENGIN EERI \(, CHEMISTRY Vol. io, No. 5
- Drawing paper 2.2X110
mm. soaked 1 hour
per cent alcoholic
euric bromide and dried
Level of liquid
Stick zinc
ig. I — Apparatus for the
GUTZBIT TBST A3 MODI-
FIED by C. R. Smith
tin and a piece of platinum wire or foil. Heating the
solution for several hours will usually remove the
arsenic. The solution is di-
luted, filtered, and made to
such a volume that i cc. con-
tains 0.5 g. stannous chloride.
THE SODIUM OK AMMONIUM
phosphates found in the
laboratory may contain ar-
senic. The microcosmic salt
used in examining hops was
purified by making a concen-
Giass wool moistened trated solution strongly acidi-
with 5 per cent ieadfied with hydrochloric acid,
acetate solution J
adding mercuric chloride solu-
tion and passing in hydrogen
sulfide gas to saturation. The
paper wet with s solution was left about 24 hrs.
nt lead acetate so- w;th occasional stirring by a
stream of hydrogen sulfide.
The precipitated mercuric sul-
fide, which carried with it the
arsenic as sulfide, was filtered
out. The solution was boiled
-20 cc. concentrated to remove hydrogen sulfide,
sulfuric acid in 120cc. ^ bromine water was added
in slight excess. After filter-
ing, if necessary, the volume
was made such that io cc.
contained 2 g. of the micro-
cosmic salt.
magnesia mixture — The general laboratory stock
of magnesium salts are liable to contain arsenic. This
can be eliminated by treating a solution of the salt
with hydrochloric acid and arsenic-free zinc. There-
action may be allowed to proceed for a day, with gentle
heating. After filtration ammonium hydroxide and
hydrochloric acid are added alternately till there is
no precipitate when the solution contains an excess
of ammonia. The volume is adjusted so that a con-
venient amount, 15 or 20 cc, will give an excess when
used to precipitate 2 g. of the phosphate.
vessels — It is generally known that arsenic may
be taken up from some glass vessels by solutions, es-
pecially when heated. It is advisable, therefore, to
use porcelain, as far as possible, for heating solutions
to be tested for arsenic. Tests of solutions of reagents
soon after treatment to remove arsenic rarely gave
any indications of the presence of arsenic, while after
standing a month in flasks the same solutions often
showed measurable amounts of arsenic, which may have
been absorbed from the glass.
STANDARDS
With all precautions there will still be some irregu-
larity in the length of stains due to variations in width
of paper strip, in size and condition of pieces of zinc,
in volume of solution, strength of acid, volume of air
space above solution in generator, in size of tubes hold-
ing lead acetate paper and moistened glass wool,
possibly also in the sensitiveness of the paper. All
these possibilities of error are covered by Smith in the
suggestion that at least three concordant stains should be
obtained before a value is selected. In testing a num-
ber of samples of hops over several weeks' time, it
was found advantageous to make a few standard stains
each day with the day's lot of samples. Portions of
standard arsenic solution were treated with bromine
to oxidize the arsenic and the solution so prepared was
treated in exactly the same manner as the solutions
prepared from the samples. At the end of the experi-
ments a number of standard strips had been made cover-
ing all the range of values which had been found. The
end of the brown stain on each side of a strip was marked
to the nearest millimeter and the average of the lengths
on both sides was taken as the length of stain corre-
sponding to the amount of arsenic which was precipi-
tated. The accompanying curve, which shows all
the values obtained for standard stains, shows the
relation between the length of stain and the amount of
arsenic, and indicates the errors which may be made
in single determinations.
c. r. smith's coi.orimetric method applied to hops
To determine arsenic in hops the samples were
oxidized carefully in porcelain casseroles with concen-
trated nitric and sulfuric acids. After the vigorous
action with nitric acid was over, sulfuric acid was added
and oxidation completed by heating over a small
flame with additions of small amounts of nitric acid
till fumes of sulfuric acid w-ere given off with no blacken-
ing of the solution. As has been pointed out by various
writers, arsenic will be reduced and lost if the or-
ganic matter chars and the solution gives off sulfur
dioxide.
Fro. II — Rblation^Bbtwbsn Amounts of Arsbnic 'and Length of
Stains Obtained in Onb Sbribs of Tests
Small amounts of bromine water were added to make \\
sure of the oxidation of the arsenic. The arsenic was
precipitated by the use of 2 g. of microcosmic salt, H
an excess of magnesia mixture and ammonia to com- I
plete the precipitation. After standing over night
the precipitate was filtered, washed once with 2.5 per
cent ammonia, and then dissolved in about 50 cc. of
dilute sulfuric acid containing 10 cc. of the concen- H
trated acid. After solution of the precipitate and
washing of the filter, the volume was about 75 cc. [j
One gram of sodium chloride was added and the solu- '
tion heated nearly to boiling, about oo° C. One cc. :
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
3(>3
of solution containing 0.5 g. stannous chloride was
added and the warm solution stirred occasionally for
10 min. The solution was now cooled, 10 cc. more of
concentrated sulfuric acid added and the mixture
again cooled. The liquid was now transferred to a
4-oz. bottle and made up to a volume of about 120 cc.
When the stopper was in place the air space was about
20 cc. The bottles were placed in a pan of water and
brought to a temperature of 200 C. Four pieces of
stick zinc were now added. Two pieces were new
and were 18 mm. long and 7 mm. in diameter. Two
of the pieces had been used in previous determinations.
The stopper carrying the tubes with the lead acetate
paper, glass wool saturated with lead acetate, and the
mercuric bromide paper were put in place immediately
after the addition of zinc. Practically all of the stain
was formed in one hour, but the strips of paper were
regularly left for 3 hrs.
The samples of hops were divided into portions of
about 18 g. In order to eliminate errors from the
presence of arsenic in reagents and vessels, a sample
of one gram of hops was digested with the same amounts
of sulfuric and nitric acids and bromine as were used
for the 18-g. sample. The digestion mixture of each
sample was filtered. That from the 18-g. sample
was made up to 200 cc. and volumes of the 200 cc.
solution were taken corresponding to 1 g., 6 g. and n
g. These aliquots were precipitated in the same
manner as the solution from the digestion of the i-g.
sample. After the stains were made by treating these
samples in the generator, the lengths were measured.
The difference between the length of the stain for the
i-g. sample and the stain obtained for Vis of the 18-g.
sample indicated the amount of arsenic obtained from
1 the digestion reagents. By reading on the curve the
1 amounts of arsenic corresponding to the stains ob-
1 tained for the i-g., 6-g. and 11-g. sub-samples, any
I error from the reagents used in precipitation could be
eliminated. The difference between the 6-g. sample
I and the i-g. sample was taken as the amount of ar-
senic in 5 g. of hops, and the difference found between
lithe 1 i-g. sample and the i-g. sample was taken as
the amount of arsenic in 10 g. of hops.
About 1000 tests were made in the course of this
'5| work and the treatment outlined above gave in nearly
H all cases satisfactory stains of which the length could
B be measured with certainty and the results which were
H obtained leave little doubt as to the amount of arsenic
present in the samples which contained as much as
B0.5 p. p. m. The average of several concordant re-
I suits is probably within 10 per cent of the true value
for quantities of 3 or 4 p. p. m.; the samples con-
■ tained as little as 0.1 or 0.2 p. p. m.; the amount of
■ arsenic obtained from the reagents and vessels used
in the work was greater than that present in the sample,
so that there is some uncertainty as to whether the
amount reported as 0.2 really means any arsenic at all.
If it were desired to settle the question as to whether
the sample taken contained no arsenic or 0.1 p. p. m.,
it would be worth while to spend more time in making
sure of the purity of the reagents.
ARSENIC IN SULFUR
To determine the arsenic in samples of sulfur, 1 to
IS g- of sulfur were treated with from 5 to 25 cc. of
bromine as described by W. Smith1 for the estimation
of selenium in sulfur. The sulfur bromide and bromine
were shaken cautiously in a separatory funnel with 2
or 3 portions of from 20 to 40 cc. of bromine water.
From 90 to 95 per cent of the arsenic were found in the
bromine water portion at the first separation and, ex-
cept with large amounts, two separations gave all the
arsenic, together with the selenium which was present,
and some sulfuric acid. The bromine water extracts
were united, filtered and the excess of bromine re-
moved by passing air through the solution. The ar-
senic was precipitated by the use of phosphate solution
and magnesia mixture. The precipitate was collected
on a filter, washed once with 2.5 per cent ammonia
and dissolved. If the amount of arsenic was small
it was determined colorimetrically as in the case of
hops. If a larger amount was present the precipitate
was dissolved in 25 cc. of dilute hydrochloric acid (sp.
gr. 1. 10) and the arsenic reduced by heating for 10 min.,
after the addition of 1 cc. of solution containing 0.5
g. stannous chloride and 2 cc. of solution containing
°-37S g- potassium iodide per cc. The selenium was
largely precipitated at this point, carrying with it
much of the arsenic. If the precipitate is not filtered
out the arsenic is all recovered. More hydrochloric
acid was added to bring the total amount of concen-
trated acid up to 28 cc. The solution was washed into
the generating bottle which had a capacity of about
140 cc, and the volume was made to about 120 cc.
Six pieces of zinc were now added and the gas passed
into mercuric chloride solution, as described by Smith.
Glass wool moistened with lead acetate solution served
to keep back hydrogen sulfide. The generator was
cooled to about 10° C. at first, so that the action would
not be too violent. After 2 or 3 hrs. the mercuric
chloride solution with the precipitate was boiled gently
one-half hour. When cool, the precipitate of mercurous
chloride was collected on ignited asbestos in a Gooch
crucible, washed with alcohol and dried at 110°.
After weighing, the crucible was ignited to drive off
the mercurous chloride and weighed again to give the
weight of precipitate. The results by this method were
as satisfactory as those given by Smith in his descrip-
tion of the method.
RESULTS
The sun-dried hops contained from 0.1 to 0.2 part
of arsenic (As203) per million, the sulfured hops from
0.2 to 26 p. p. m., and the samples of sulfur gave from
3.6 to 356 p. p. m. The relation of the different lots
showed very clearly that the contamination of the
hops must have come from the arsenic in the sulfur.
This naturally led to consideration of the possibility
of contamination of dried fruits which are treated with
sulfur fumes. Samples of peaches and apricots col-
lected at a local store gave 0.2 to 2.0 parts of
per million parts. Samples of peaches which had been
collected for another purpose contained from 0.7 to
' This Journal, 7 (1915), 849.
364
THE JOURNAL OF IXDUSTRIAL AND ENGINEERI NG I HEMISTRY Vol. IO, No. 5
2.0 parts of arsenic per million. Samples of dried
apples which were in storage gave from 0.1 to 0.5 part
of arsenic per million. Mr. R. S. Hiltner, who was
engaged in an investigation of the drying of fruit from
other points of view, kindly furnished 10 samples of
sulfured peaches and apricots and samples of the sulfur
used in treating them. The samples of dried fruits
contained from 1.4 to 3.4 parts of arsenic per million.
The samples of sulfur contained from 5 to 50°
parts. The source of the samples of sulfur was not
known. The samples of sulfur which were studied in
connection with the occurrence of arsenic in hops were
all Japanese sulfurs.
In connection with this subject, some samples of
Japanese sulfur were collected at the port of San Fran-
cisco and examined for arsenic. They contained from
55 to 700 parts of arsenic per million. Through the
kindness of Mr. Philip S. Smith, of the U. S. Geological
Survey, samples of sulfur were obtained from six of
the companies producing sulfur in the United States.
It is generally recognized that sulfur obtained from the
largest source of supply in the United States is free
from arsenic. The sample from this source, and all
the other samples examined, showed no arsenic, or less
than one part of arsenic per million.
Thus it appears that food products which are treated
with sulfur fumes from sulfur which contains arsenic
are liable to contamination with arsenic. In the case
of hops the use of sulfur containing an amount of
arsenic of about 100 p. p. m. will, on the average,
introduce about three parts of arsenic per million parts
of dried hops. It appears probable that if sulfur
which contained less than ten parts of arsenic per million
were used for sulfuring hops or dried fruits, it would
be almost impossible to detect any contamination of
the sulfured products with arsenic. It also appears
that the native supplies of sulfur in this country are
free from arsenic and if used for sulfuring food products
would make it certain that no contamination with
arsenic could result from the sulfur. The amount of
sulfur burned for curing food products is a compara-
tively small proportion of the total amount used. The
greater part, which is used in making lime-sulfur mix-
ture for spraying and dipping and as powdered sulfur
for dusting vines of different kinds, would, of course,
introduce no appreciable contamination of arsenic
into the food products, even if the sulfur did contain
large amounts.
Food Investigation Laboratory
Bureau op Chemistry, u. S. Department of Agriculture
Washington, D. C.
SOME CONSTITUENTS OF THE AMERICAN GRAPE-
FRUIT (CITRUS DECUMANA)1
By Harper F. Zoller
Received January 14, 1918
INTRODUCTION
The adoption of the grapefruit in America as a
valuable food accessory has spread with amazing
* Abstracted before the Spring Meeting, American Chemical Society,
Kansas City, Mo., April 1917. The major portion of the work was carried
on in the chemical laboratories, Kansas State Agricultural College, Man-
hattan, Kansas,
rapidity, so that now it is possible to obtain this fruit
in season in practically every remote village in the
United States or Southern Canada. This whole-
sale distribution has necessitated an industry which
bids to become of greater vastness than either the
lemon or orange industries, if proper market conditions
and disposal of wastes can be secured. The fact
that a successful season in the citrus industry depends
upon favorable weather conditions and orchards free
from certain pathological plagues, indicates that citrus
by-products are sure to become an important factor.
In the sorting and grading of the thousands of tons
of grapefruit, representing a season's crop, many tons
of culls are allowed to rot for the want of an economical
disposal. Certain of the producing companies are
seriously contemplating the isolation of certain of the
by-products, and one or two companies have engaged
in extractions on a minor scale. I am of the opinion
that with a proper knowledge of the important con-
stituents their commercial production would become
profitable and the trades would be supplied with the
raw materials which they demand. It seems probable
that extended analysis of the grapefruit must have been
made by chemists in the employ of the citrus fruit
companies, but if these have been made they have not
been published at large. It is my purpose in this
paper to present some research data on the nature
and quantities of certain of the more important con-
stituents of the American-grown grapefruit from
different sources, with the idea that it should prove
valuable to those intimately connected with the
citrus orchards in the South and West.
HISTORICAL AND COMMERCIAL ASPECTS
Before proceeding with the data it would be well
to consider briefly the historical and botanical sig-
nificance of the grapefruit. Textbooks on botany,
scientific journals and current publications are re-
markably free from allusions to this fruit.1 Hume
says. "No fruit of importance now grown in the United
States has such a meagre American literature as the
pomelo. Nor is this strange when we remember
the fact that it is only within the last fifteen years or
so that the pomelo has been regarded as a commercial
fruit."1 * But it is strange that since Hume's edition
of his bulletin in iqoi much less literature has ap-
■ In searching through the Library of Congress for early literature on
the citrus fruits, with the hope of gaining an insight into the past history
of grapefruit, I was fortunate enough to 6nd Giovanni Batiste Ferrari's
book on the "Hesperides" published in Rome in 1646. This work, con-
sisting of over 800 pages, and replete with full-page woodcuts of the various
species of citrus, proved to be the most complete record of the citrus fruits
of the Orient to date. It is not surprising that we find herein described
the varieties of the different species from many of the islands of the Pacific
^including Java), Bgypt, Greece, India and Italy. While Ferrari classifies
the species similar to the grapefruit under Aurantium, it is not unlikely that
one of the following most closely resembles the grapefruit as we know it:
Aurantium Dulci Cortict et Sinsnsi, p. 430; Aurantium Pomum, or Pomum
Adam. p. 309; Aurantium Maximum, p. 437. It is difficult, from the de-
scription and woodcuts, to say definitely just which one most closely re-
sembles our typical American fruit. Perhaps the three are not distinct
species, one or more may be hybrid varieties. It is clear that Aurantium
Dulci Corlict and Aurantium Pomum (Adam's Apple) are variously con-
sidered as the "forbidden fruit" of the early Orientals; at least so con-
sidered by Ferrari, Johannes Commelin (Xederlantze Hesperides, 1676)
and Gallesio (Loc. cil.); and most reasonably, because of their extreme
bitterness.
• Numbers refer to References iu Bibliography, p. 573,
May, 1 918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
36;
peared in proportion to the increased importance of
the fruit. Articles have occasionally appeared in
horticultural journals and experiment station records,
dealing primarily with cultural and rough analytical
aspects: the analyses reporting edible portions of
fruit, number of seeds, amount of acid, total solids,
sugar, and ash. Citation of these will be made later.
That the present name (grapefruit) originated from
the fact that the fruit commonly occurs on the trees
in large clusters, somewhat resembling clusters of
grapes, is well known. But it is not so well known
that the term "pomelo" has been applied and adopted
by the U. S. Department of Agriculture, American
Pomological Society, Florida State Horticultural So-
ciety, etc. The English of Ceylon and India call it
pomelcw, a name probably derived from the Latin
words "pomum melo" — the melon apple2 — though it
may have been corrupted from pompelmoes, the
Dutch name first applied by Rumphius in 1750.3
The latter seems more probable since all incidents
point to the Dutch East Indies, on the Island of Java,
as the original home of the grapefruit. To the French-
and the Germans it is known as pompelmouse and
pompelmuse, respectively. The term shaddock has
crept into the literature as a synonym for grapefruit
in honor of a certain British sea-captain who is said
to have introduced the fruit into the West Indies from
Java early in the eighteenth century. It is interesting
to note that in Java, which is the acknowledged home
of the grapefruit, there are two varieties.4 5 One is
small, bitter though edible, and grows in enormous
clusters on trees from 10 to 20 ft. high situated in the
lower coastal regions of the island. The other variety
is much larger (often from 10 to 20 lbs. per fruit),
intensely bitter, with a dark-yellow to red pulp. It
grows at much higher altitudes, abundantly on the
Bandong plateau, and is known there as the non-
edible variety. The bitter principle in both varieties
is identical,4, 6| 6> 28 which would lead to their classi-
fication as sub-varieties under Citrus decumana* This
non-edible fruit, because of ite prolific growth and
large flowers, was a source of "neroli-oil" or oil of bitter
orange for a number of years to the inhabitants of
Europe and Asia. Both varieties are being extensively
cultivated in Southern Europe and Asia at present for
food and commercial products.
It is likely that the term shaddock applies more
specifically to the above larger and "non-edible"
variety (Hume). The smaller variety is the one that
I most of us are familiar with though it is not unlikely
[ that the larger variety has also been introduced into
the West Indies as well as the United States and
Mexico. One is safe in saying that the term shaddock
will never become generally known as synonymous
with pomelo, or grapefruit. This large non-edible
fruit may be placed on the market in a few years as
a hybrid of cither orange or lime, since several of the
unpalatable varieties, after undergoing hybridization
with other citrus species, have been transformed into
very agreeable fruit, commonly known as grapefruit.
It is quite doubtful whether the term pomelo will
ever become generally used outside of scientific circles,
any more than the term maize will ever supplant the
more agreeable word corn. Shamel9 writes that pomelo
has never been accepted by the public or fruit trade
and seems to favor the term grapefruit. Hume,
though loyal to pomelo, also expresses his doubt as
to the common acceptance of the term pomelo. In
discussing the probable origin of the term grapefruit
he quotes Risso and Poiteau10 who say, "The author
of the Flora of the Antilles has equally observed the
pomelo cultivated in Jamaica, where the inhabitants
call it grapefruit The fruits are gathered in
clusters of from 15 to 18 on the branch, each of the
size of the fist, spherical, firm, with a slightly rough
skin of sulfurish yellow." It seems to me that it
would be unwise to try to dissuade the public from the
term grapefruit, since "usage determines preference"
to a large degree and the term has become so firmly
rooted in the common vernacular. However, one will
agree that it is misleading. The term grapefruit will
be adhered to in the following.
Just at what particular date the grapefruit was
introduced into this country is not known. While
the state of Florida claims the first fruit, it must not
be forgotten that the fruit has flourished in Mexico
for decades past. While Mexico has proved to be
better suited for the production of larger and more
luscious grapefruit, and evidences of citrus orchards
of extremely early date exist, it is not improbable
that the Spaniards first introduced the fruit into
Mexico or Central America.* If one relies upon the
reminiscences of the horticulturists to aid him in de-
termining the early history, or even the existence,
of the grapefruit in America he is bound to be dis-
appointed. Occasional allusions to it as a pomological
curiosity, though debased food-material, can be found,
indicating that it had at least been noticed in the
latter half of the nineteenth century. Watson,11
in writing of citrus fruits, mentions that, "The shaddock
is a still larger fruit, in form more resembling the
orange, curious, but worthless." This was in 1859,
while in 1885, Spalding12 remarks, "Meanwhile the
pumalo and its congeners when allowed growing space
continue to load themselves down with fruit as large
as footballs. They are matters of wonder and that is
all." Downing, also in 1885,13 in discussing the
grapefruit under the name of shaddock, writes: "The
pulp is sweetish or sub-acid and the juice is rather re-
freshing. It is, however, more showy than useful,
and certainly makes a magnificent appearance in a
collection of tropical fruits." Many other writers on
horticultural topics do not mention it even in writings
of the present day. It is noteworthy to learn that
a very recent book, "La Culture des Citrus," by
Guitet-Yauquelin (191 7), contains only a brief para-
graph on this subject, while we are indebted to the
French for some of the earliest botanical classifica-
tionSil«.W,W,17
* Gallesio, in bis "Traitc du Citrus," 1829, p. 344, discusses the in-
troduction of citrus fruits into the Americas through Mexico, and further
speaks of its reception by King Montezuma While he does not explicitly
state that grapefruit was among the varieties introduced, he docs indicate
that he is acquainted with the fruit, for on page 326 he describes the
Auranlium decumanum" as the sole variety of the pompelmouse (also
known as " pomme d'Adam").
366
THE JOURNAL OF INDUSTRIAL AND ENGINEERING ( HEMISTRY Vol. 10, Xo. 5
While Florida and California practically comprise
the entire source of grapefruit in the United States,
it is astonishing to learn that an amount equal to one-
half of the United States crop is imported for our
consumption. According to Vaile,11 the following
shipments of grapefruit have been determined: Florida,
1915, 8,000 carloads; California, 1015, 250 carloads;
Puerto Rico, 1913, 500 carloads; Cuba, 191 2, 250
carloads. The present shipments run considerably
above these values, since hundreds of acres of 5 yr.-old
orchards are coming into production each year, and
a tree, once producing, continues to produce abundantly
for several years if not incapacitated by frost. Mexico
is liable to become a contending -factor in the grape-
fruit market in a very short time.* The Mexicans
have found to their satisfaction that the grapefruit
industry can take the place of the long-tried orange
and lemon industry. These latter Mexican-grown
fruits cannot compete with the better varieties of
oranges and lemons grown in this country, while the
grapefruit seems to thrive prolifically in the higher
and warmer altitudes of central Mexico, the climatic
conditions in Mexico comparing favorably with those
on the Island of Java. All the energies of the citrus
growers in Mexico are now being bent towards a suc-
cessful prosecution of a grapefruit commerce. Ac-
cording to Hume,19 the first shipment of grapefruit
from the state of Florida occurred sometime during
the years 1880 to 1885 and were sold in New York
and Philadelphia, netting the shippers 50 cents per
barrel.
Numerous varieties of grapefruit have resulted from
the efforts of the citrus growers and horticulturists.
As previously intimated, hybridization has played an
important r61e in this development. Shamel,20 Rea-
soncr,21 Hume-'- and Bulletin No. 8, Division of Po-
mology, United States Department of Agriculture,
give lists of the several varieties with brief descrip-
tions. Hybrids of grapefruit with the orange, tangerine
and grapefruit from various countries exist. The
chief aim apparently is to produce a fruit with a mini-
mum of bitterness and few seeds. The Marsh Si
is an example of a hybrid grapefruit with few seeds,
though it retains the bitterness of the original grape-
fruit. This is extensively cultivated in California
and Florida, and appears on the market in quantities.
Since it ripens in California during May to July and
in Florida during February to March, it acquires
additional importance from a commercial standpoint.
The Duncan is another variety possessing few
together with much bitterness. In fact, these are
about the only varieties possessing a small quota of
seeds. The average number of seeds in the other
varieties is well above forty. The effort to remove or
mask the bitterness is not so well rewarded. A few
varieties have lost the bitterness, and at the same time
they have lost all that characterized them as grapefruit.
* Shamel9 and WallschlaeKer,« call attention to Quarantine Regulation
No. 5 of Feb. 8, 1913. and subsequent, which forbids the entry into the
United States of Mexican grapefruit. This is done to safeguard against
citrus fruit pests It would seem that such a regulation is unn.
the conclusions of Aaron Aaronsohn" arc to be taken in all seriousness,
for he writes "The grapefruit possesses marked resistance to some of the
numerous parasites of other citrus species."
A fruit exhibited as grapefruit but without the "qui-
nine" bitterness should no longer be looked upon as
a grapefruit, any more than a flower growing on a bush
without thorns should be considered a wild rose.
Pfeffer,23 DeVry,24 Bias,25 Hoffmann,26 Lebreton,"
Will,28 Hilger,29 von Rijn,31 and others, as long ago
as 1828-1870, found that the bitter glucoside existing
in the "pompelmoes"' from Java could be found in
no other citrus fruit. Likewise, they found that
neither hesperidin nor isohesperidin, glucosides com-
mon to certain other citrus fruits, could be found in
"pompelmoes" (grapefruit). My research confirms
these earlier findings. It is not uncommon to find
statements in the literature which are not in keeping
with these facts — Kraemer.30 Truly it may be ex-
pected that in some of the more divergent hybrids
one may find a commingling of the glucosides charac-
teristic of each parent stock. Whether or not this is
true should be determined with utmost expertness
in connection with the citrus culture, for upon the
glucosides depends the primary differentiations of the
They undoubtedly control the sugar con-
tent, flavor, and possibly the color of the fruit through
their reversible reactions. The acid content of the
fruits (citrus), while varying in amount in each species,
is attributed almost entirely to citric acid, so we do
not look to this for the basis of differentiation.
THERAPEUTIC VALUE
The dailies and periodicals of promoters in citrus
fruit sections abound in attractive quackery on the
beneficent medicinal properties of all citrus fruits,
and especially grapefruit. This remedial property is
being assigned to everything present in the fruits —
the "alkaloids" said to be present, the citric acid, the
potassium phosphate in the pulp, and the oils in the
peel. If it is upon the oil present that we must de-
pend for this elixir, then a tablespoonful of pure
gum-turpentine will furnish the same amount of
remedial as an entire crate of citrus fruit, providing
' he peel and all. If it is due to the phosphoric
acid as phosphate, as»Dygert2 would have us believe,
then a glass of cow's milk would be equivalent to a
dozen grapefruit in this life-giving entity. If it
due to the alkaloids present in the citrus fruits, then
they have no therapeutic value, for no alkaloid has
been detected in any of the citrus fruits regularly
marketed in this country, and it is not likely that an
alkaloid exists in any of the citrus family.
In LeLong's bulletin,32 much to my surprise, the
following statement appears: "The special alkaloid
of most varieties of the pomelo contains a bitter princi-
ple, which, while its medicinal virtues are conceded,
has not yet, I regret to say, been defined by chemical
examination. Neither is it safe to consider it quinine
for there are scores of vegetable bitters which are
not quinine. The presumption is that it is a unique
bitter principle peculiar to this fruit." It would
not seem so strange if such a statement came from
one who was supposed to be unacquainted with the
citrus fruits. The bitter principle of Citrus deeumana
urately investigated nearly forty years ago,
and its relation to similar principles found in other
•May, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
367
citrus species compared and published. Specific ci-
tations to the literature on this subject will be found
later under the heading "Glucoside or Bitter Prin-
ciple." R. T. Will33 calls attention to the glucosides
appearing in the peel of the orange "principally in
certain conditions of ripeness." He mentions hes-
peridin, isohesperidin and aurantiamarin, and con-
tinues as follows: "Aurantiamarin is the principle
which gives the orange its bitter flavor; it is very similar
to quinine in its physiological action and charac-
teristics." Since Will did not state the specific variety
of orange in which these three glucosides are supposed
to appear, his allusion to them is of little value. It
is only necessary to review Tanret's34 isolation and
investigations of isohesperidin to find that it is a
very bitter glucoside and occurs in certain varieties
of the orange. Likewise aurantiamarin occurs in
the Aurantii A mart Cortex3* as the bitter substance,
and probably occurs in some hybrids of this variety,
though not necessarily in all hybrids. Hesperidin
possesses a slight sweetish taste and has been isolated
from a number of the aurantiaceae. Now while it
is possible for all three of these glucosides to be found
in a certain variety of orange, it is not a common phe-
nomenon and it would be interesting to know to which
hybrid Will refers. It is wrong to imply, furthermore,
that oranges in general are characterized by these
three glucosides.
As to the physiological action of aurantiamarin and
its similarity to quinine, I was unaware that any
pharmacological study of this particuar glucoside
had been inaugurated, and since no references were
mentioned I am justified in relegating his statement
to the same realm as those of the following.
Some of the leading home economics teachers of
the country delight to revel in the curative properties
of grapefruit, due "to the quinine or similar alkaloid
which it contains." In Dygert's "Crops that Pay"
we find, "A cool juicy pomelo before breaktast is one
of the pleasantest and surest antidotes imaginable
for malaria;" though as previously stated, Dygert
rather suggests that we should look to phosphoric
acid for its medicinal value. LeLong32 writes, "For
medicinal purposes it (grapefruit) leads all the citrus
fruits, and its value from this point of view is as yet
unknown." Sub-tropical and tropical countries are
prone to offer grapefruit or similar citrus as a safe-
guard against malaria, and publications from these
sources contain similar advice.
We have undoubtedly come to this impression of
the therapeutic value of grapefruit through a false
sense of security. Perhaps our educational system
of former years was responsible, in a measure, for
Greek, Roman, and Italian literature is crowded
with references to the remedial beneficence of "hes-
perides and citron fruits." Gallesio and Ferrari
(see footnotes) both frequently so state and give
references to specific passages. For example, Virgil37
writes:
"The Median fields rich citron fruits produce,
Tho' harsh the taste, and clammy the juice;
Blest antidote! Which when in evil horn,
The step-dame mixes herbs of pois'nous power.
And crowns the bowl with many a muttered spell,
Will from the veins the direful draught expel.
Large is the trunk, and laurel-like its frame.
And 'twere a laurel, were its scent the same;
Its lasting leaf each roaring blast defies,
Tenacious of the stem its flow'rets rise;
Hence a more wholesome breath the Medes receive
And of their sires the lab'ring lungs relieve."
LeLong32 comes to the real truth when he says that
we do not know upon what its real value depends.
In the glaring array of these insecure impressions we
must admit there is very likely a constituent in the
true grapefruit which has valuable properties. Like-
wise certain others of the citrus species may possess
constituents of therapeutic value. That is all that
we can say with definiteness.
I have experimented empirically with some purified
naringin from grapefruit with this end in view, and
while some of the results are encouraging from a thera-
peutic standpoint, I cannot now report more until
a more thorough pharmacological test is finished.
The latter is being conducted with naringin which
I have isolated and purified.
EXPERIMENTAL
The investigations reported herein covered the
greater part of a period of 30 mo., which included
three grapefruit seasons. Before planning the work,
I satisfied myself that in the published investigations
of American grapefruit, very little, if anything, could
be found relative to the constituents of the peel and
seeds. In proceeding with the work I became aware
that during storage (i. c, the period between picking
and placing in the hands of the consumer), especially
when the period extended a couple of months into the
Spring, the juice suffered a marked change in flavor.
This observation initiated another series of analyses
of the acid-sugar ratio of the juices of fruit found on
the market in late Fall and early Spring. In the
examination of the seeds several remarkably interesting
factors revealed themselves, factors which have un-
doubtedly considerable influence on the naringin
(glucoside) content of the fruit. The analysis of the
seeds and their biochemical relationship to the re-
mainder of the fruit merit a separate treatment, and
hence no further mention of them in this report will
be made, except to call attention to the fact again,
that a sane disposal of the bulky seeds, the culls
and the spoils is a factor of no small mien in the handling
of the by-products.
I have compiled a brief table of the typical analyses
of grapefruits found in various bulletins from ex-
periment stations and in other publications. It
shows the character of investigations which have been
reported hitherto. It also serves well to show the
relative quantities and characteristics in various
varieties of grapefruit grown in different countries,
this correlation being important. In Table I, I have
indicated as far as possible the analyst and publisher
of the data.
The order in which the following research will be
considered is as follows:
I — Constituents of peel, or rind: (a) Oil, or es-
sential oils; (b) glucoside, or bitter principle; (c)
pectin.
368
THE JOURNAL OF INDUSTRIAL AND ENGINEERING < HEMISTRY Vol. 10. No. 5
II — Constituents of juice, or pulp: (a) acid;
(6) sugars.
Ill — Constituents of seeds (not herein reported).
It must be emphasized that these "constituents"
mentioned above are not the only constituents to be
found in the grapefruit. Others were found to exist,
and many more are present, though in minute quanti-
ties and very likely of no consequence from a by-
products standpoint. For instance, a quantitative
and qualitative analysis of the ash from the pulp
in case of II was conducted upon two varieties with
the idea of ascertaining the amounts of sulfates and
phosphates present. While the quantity of sulfates
was negligible, the phosphate value was in proximate
agreement with those presented by Hume,19 and,
hence, are not given in my results.
Table I
P E *
> — ■- o
*l- s s 1 °! s g£s 8 8
Description £<0 lj— 3~ ^,u •CB< 5s- U'*1- g5" Cft
op Fruit < ft ft < ■< in « £ft
Philippine Islands(o).. 930.0 34.0 61.0 0.63 1.06 6.26 8.86 0.66 ...
California ((>)
(1) 477.0 30.0 69.2 0.39 .. 3.116.22 0.58 ...
. 391.0 27.0 73.0 0.39 4.77 7.37 0.56 ...
(«)
(1) 574.0 28.7 71.0 .. 1.28 .. 7.50
(2) 561.0 34.9 62.5 .. 1.51 .. 7.40
Florida(rf)
Royal 541.0 27.2 69.3 .. («) .. (J) 0.30 0.040
Peraambuco 742.7 28.0 68.5 .. (<0 .. (/) 0.29 0.056
Manville 487.6 20.9 74.7 .. (e) .. (J) 0.26 0.054
Aurantium 430.9 28.3 68.6 .. («) .. (f) 0.22 0.053
Walters 721.3 28.2 68.6 .. (e) .. (/) 0.32 0.049
Triumph 534.631.865.2 .. («) .. (/) 0.290.050
(1) Analysis of standard seedless fruit (10 seeds).
(2) Analyses of seeded variety (59 seeds).
(3) Some writers consider the pulp as that portion of the citrus fruit
other than the peel and seeds, i. e., the edible portion; some consider it as
the segmented sections; others, as the juice only.
(<j) Pratt and del Rosario, PhiUipint J. Sci., Stc. A, 8 (1913), 76.
Evidently this fruit is not of a true grapefruit, but must be similar to
the Cuban fruit described by Chace, Tolman and Munson, U. S. Dept.
of Agriculture, Hureau of Chemistry, BulL 87, p. 13.
(b) Colby, Cat. Agr. Exp. Report. 1892-93, p. 256.
(c) Quoted by Shamel, California Citrograph, Xo 6 (1916), p. 3.
(d) Hume:1 in this bulletin Hume makes no reference in the tables to
the sugar or acid content.
(e) if) Chance, Fla., grapefruit analysis, gives the following values
for the acid and sugar content of three different fruits, respectively: 1.26,
0.90, 1.58; for total sugars: 6.30. 7.88 and 8.41.
(Further note.) The potash content amounts to 10-25 times that
n! the PlOl content; these values indicate ihe total fruit content, while
iu the case of the seeds the values for these constituents are 1000 per cent
greater than for either peel or pulp.
The varieties of grapefruit which fell to my lot for
examination depended chiefly upon the choice of mid-
continental fruit wholesalers, and included Marsh
Seedless, Duncan, Indian River, Excelsior, Peraam-
buco and DeSoto. The Atwood Grapefruit Company,
of Manavista, Fla., graciously supplied me with
several fine fruit, which, though I am uncertain, were
probably of Walters. Indian River or Hall variety.
The peel and fiber of all varieties were markedly
bitter; if a comparison were to be drawn, the Marsh
Seedless and another unknown variety would be classed
as the least bitter. Hume and Others do not consider
the Marsh, because of its flavor, etc., as a true grape-
fruit and they are undoubtedly right. I have used
it in my analysis merely because it possessed an insoluble
amount of the bitter constituent, and also because it
is to be found so extensively in the market both in
early Fall and late Spring.
ANALYSIS OF PEEL OK RIND
essential oils — For the separation of the essential
oils large quantities of peels were obtained at frequent
intervals from the hotels and eating-houses in this
community. These peels were sorted and only those
which were fresh and which represented the Indian
River, DeSoto and Excelsior were used for oil analysis.
They were thoroughly washed and all juice-sac tissue
was removed. It was noticed that the distribution
of the oil-sacs in the pericarp varied considerably
in the different varieties, some being especially rich
in oil, others comparatively poor. The oil content
of the grapefruit furnished by the Atwood Company
was noticeably deficient. Marsh Seedless averaged.
from 0.75 to 1.0 per cent of light-colored oil which
resembled orange oil more than any other oil.
The cleaned peels were cut by a revolving food
chopper into pieces averaging a centimeter in cross-
section. Trial methods of isolating the oil were tried.
A small hand-press cider extractor was employed,
yielding a liquid emulsion of solids, oil and water.
When this emulsion was allowed to stand for several
hours there was a slight separation of the oil on the
upper surface but it was always turbid and intensely
bitter. Centrifuging and freezing were tried to free
the oil from the accompanying material and while it
was in a measure successful, it would be unadvisable
on a large scale. Precipitation of the astringent
material, pectose and resins by means of gelatin and
tannic acid solution gave a somewhat clearer oil,
but its flavor was repugnant.
Extraction of the oil by means of volatile solvents
gave a good yield of oil but was laborious, and in
case of the solvents employed (acetone and ethyl
alcohol) the bitter glucoside and resins were ex-
tracted at the same time. In order to purify the oil,
distillation under reduced pressure, or with steam,
would be necessary. The former would affect the
original character of the oil, while a combination of the
two would give a good product.
The method finally adopted and which resulted in a
perfectly clear, slightly-yellow oil was as follows:
The finely cut peel w-as introduced into a roomy con-
tainer with an equal weight of water. Slight suction
was applied by means of a water-pump furnishing
a steady reduction of pressure. Live steam was then
drawn through the suspended peel and condensed in
a suitable condensing apparatus connected with the
suction (see F in Fig. I). Steam distillation was
continued until the condensate was free from turbidity,
which point indicated that the oil was entirely re-
A second receiver was connected with the
suction in series with F, and this second receiver was
submerged in brine-ice mixture in order to entrap
any of the oils which might tend to be drawn past F.
Buffers of glass-wool were placed in the second re-
ceiver as an addi; ution. A slight amount
of oil was recovered this way, but with a suitable
condenser no extra receiver would be necessary. The
oil separated on the surface after a few minutes'
standing, ami was drawn off. The remaining traces
wen removed from the distillate by centrifuging.
From 0.4 to 1.1 per cent of oil per fruit or, by weight,
2.5 to 6.0 g. were obtained. Less than one-half
this amount would probably be recovered industrially.
May, 19 18
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
369
A decrease in the aldehyde content of the oil during
storage is manifested.
100 g. of the steam-distilled oil, collected under
diminished pressure as indicated above, were washed
several times with 50-cc. portions of normal Na2C03
solution, then with water, and finally dried with an-
hydrous sodium sulfate. The oil in this condition
had the following physical properties: Odor, strongly
that of citral; color, clear greenish yellow; refractive
index at 20° C. = 1.4750 and 1.4785; optical rota-
tion in 100 mm. tube at 200 C. = +72.5 and +7S.5;
specific gravity at 20° C. = 0.845 and 0.860.
Fig. I
100 g. of the washed and dried oil were distilled
from a flask fitted with a Hempel column under a
constant pressure reduced to 12 mm. The distilling
flask was immersed in a bath of cottonseed oil and
the temperature very gradually increased. The dis-
tillate was collected in the following fractions. The
boiling point of each fraction was determined and the
approximate results are also given in this table.
Fraction B. P. Weight Boiling
No. Range Grams Point
1 48-52° 2.4 158°
2 52-58° 71.5 172°
3 58-70° 14.2 178°
4 70-85° 1.3 181°
5 85-100° 4.8 200°(a)
6 100-115° 3.6 230°
la) Rapidly rising to 225°, then dropping rapidly and browning.
factions 2 and 3 were mixed together for qualitative
analysis, also Nos. 5 and 6, since the range in either
case is similar.
identification of a-Pi.\ENE— Fraction 1 and the
[fixture of Fractions 2 and 3. Pinene was tested for
|in these separate fractions by the nitrosyl chloride
method described by Wallach38 and Ehestadt,3' and
its presence in both mixtures established by the
melting point of the obtained pinene-nitrosochloride,
102 and 103 ° C. The largest yield was, of course,
from Fraction 1. Crystals of pinene-hydrochloride
were also prepared from Fraction 1 which melted
at 1 3 2 ° C .
identification of i-LiMONENE — A portion of the
mixture of Fractions 2 and 3 distilled under atmos-
pheric pressure gave a distillate which was collected
at the approximate temperature of pure limonene,
1 75° C. The solution was strongly dextro-rotatory,
+ 38 in a 100-mm. tube at 200 C. As further proof,
5 g. of crystalline limonene-tetrabromide were pre-
pared which melted at 104° C. Limonene was also
detected in Fraction 4, though in small amount.
TEST FOR ALDEHYDES IN LIMONENE FRACTION IO g.
of the limonene fraction from distillation of the mixture
of Fractions 2 and 3 were treated with semicarbazide-
HC1 and sodium acetate41 for the production of ketone
or aldehyde semicarbazides. None were found, al-
though a slight positive indication of their presence
was obtained by means of Schiff's reagent. Test
for aldehydes in Fractions 4, 5 and 6 were all positive,
Nos. 5 and 6 yielding the largest quantity.
TESTS FOR ALCOHOLS IN LIMONENE AND OTHER
fractions — By acetylation methods the limonene
fraction indicated only a possible trace of alcohols.
Fraction 4 indicated at least 10 per cent of its weight
as of alcohols, calculated as linalool [(CH3)2C : CH.-
CH2.CH2.C(OH)(CH3).CH : CHS]. The mixture of
Fractions 5 and 6 indicated more than a trace of alco-
hols, 4 per cent of their combined weight, calculated
as geraniol [(CH3)2C : CH.CH2.CH2C(CH3) : CH.-
CH2.OH].
identification of linalool — Fraction 4 consisting
of a little over one gram was shaken in a small glass-
stoppered flask with an excess of 5 per cent sulfuric
acid. After a short time crystals of terpine hydrate
(CioH2002.H20) separated, which melted at 1160 C.
The oxidation of linalool to citral was impossible
in this connection, since citral is in the succeeding
fraction in large quantity, and probably also present
in No. 4, judging by the odor and by the test under
aldehydes.
identification of citral — While citral was known
to be present both from the odor and from the boiling
point of the last two fractions, in the latter case suffer-
ing decomposition, it was further identified by its
semicarbazide preparation. The semicarbazone, pre-
pared according to Zelinsky,42 melted sharply at 1650.
identification of geraniol — One gram of Frac-
tion 6. before mixing with 5, was shaken vigorously
with 5 per cent aqueous H2S04 and after standing for
one hour the acid was neutralized with 10 per cent
NaOH. Upon further standing crystals of terpine
hydrate separated which melted at 116° C. It was
assumed that none of the linalool appeared in Fraction
6, since its boiling point is slightly below 2000 C.
at atmospheric pressure, while Fraction 6 boils under
the same conditions at approximately 2300 C.
0THEK constituents — While the washed oil showed
a small saponification number no attempt was made
to determine the esters present. It might be expected
that both linalyl- and geranyl-acetate are present,
from the analogy of this oil with the other citrus fruit
oils.
37°
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. S
From the analysis and the distillation figures it
would seem that the constituents present in the oil
examined are in about the following proportion:
J-I.imonene 90-92 per cent
Citral 3-5 per cent
a-Pinene 0.5-1.5 per cent
Geraniol 1 . 0-2 . 0 per cent
Linaiofil 1 . 0-2 . 0 per cent
Citronellal Some
Linalyl and Geranyl Esters Some
The oil has a very pleasing odor and flavor and when
30 per cent by volume of pure ethyl alcohol is added
it seems to keep as well as either lemon, orange or
lime oil. Its properties seem to place it between the
lemon and the orange in value.
Glucoside, or bitter principle — The residue re-
maining in the container after steam distillation of
the peels was fibrous and intensely bitter. Several
liters of the residue were pressed through bags of
cheesecloth and the liquid allowed to stand for several
days, while the oils were being analyzed. The fibrous
mass remaining in the cheesecloth bags, after expressing
the juice, was found to be free from bitterness. It was
apparent that the hot water was sufficient to extract
the "bitterness." A few days after the above liquid
had stood at room temperature I was surprised to
find a rapid fermentation in progress. Numerous
rosettes of small crystals were forming on the sides of
the glass container near the bottom, while several
centimeters of a white snowy product had collected
on the bottom. Microscopical examination of this
snowy mass revealed multitudinous spine-like crystals,
with here and there some unbroken rosettes. It was
finally found that these crystals could be separated
from the remaining liquid by pouring through a funnel
in which a tuft of absorbent cotton was placed. Most of
of the yeast cells filtered through, though slowly, of
course. The crystals and contaminating yeast cells
were taken up with hot water (900), just enough water
being used to dissolve the crystals; the solution was
then filtered through filter paper and allowed to re-
crystallize. After repeated recrystallizations from
water and finally from alcohol the product was assumed
to be pure. The fermented solution from which the
first crop of crystals appeared was still strongly bitter,
and only when the solution was placed in ice water
did more crystals separate; the bitterness had then
decreased to a noticeable trace. Doubtless the alcohol
formed during fermentation was responsible for the
retention of the bitter principle, since it is quite soluble
in cold alcohol diluted with water and refuses to crys-
tallize from this mixture even when lowered to the
freezing point.
The following method was devised tor the direct
urn of the bitter principle from the chopped,
fresh peel. An extraction apparatus according to
Fig. II was set up. Tin < .1 held the finely
chopped peel from 15 large grapefruit. A small tuft
of ^lass wool was placed in the bottom of the percolator
to prevent the return tube from I iped up.
One and one-half liters of 96 per cohol were
placed in B. C contained water for the bath. The
operation is automatic and simple after the first dump-
ing of A. Ten hours are sufficient for the complete
extraction of the glucoside from each charge of peel.
Of course, the oils, resins and other substances are
extracted along with the glucoside, but no pectose
material is present in the extract. To facilitate the
evolution of a continuous current of alcohol vapor
from B, a glass tube of 0.5 to 1.0 cm. bore is sealed at
one end and inverted in the round bottom flask. The
vapor expanding in this tube causes a continuous suc-
cession of bubbles, which tend to prevent both bumping
and froth. The extract from B is then poured into
^mu
' of Fig. I. /■; is again used for a water bath,
the temperature of which must not remain above 80 °.
D is connected with a Hopkins condenser with a glass
seal, and the condenser in turn connected with a re-
ceiver to which suction to the pressure of 10 mm. may
be applied. A fine capillary tube with stopcock extends
to the bottom of D to regulate the distillation by means
of a free current of air. The alcohol and oils are col-
lected in F and may be used for the extraction of an-
other charge of peel without redistilling.
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
The residue in D should be a golden yellow syrup,
which is taken up in water and treated with a few
cubic centimeters of 25 per cent basic lead acetate
solution to precipitate out the material other than
naringin, the glucoside. The mass is filtered without
suction and the excess lead removed with hydrogen
sulfide, from hot solution. The clear filtrate from the
PbS precipitate is allowed to stand for a few hours,
when the white rosettes begin to form on the sides of
the containing vessel, analogous to those from the fer-
menting liquor. Mild shaking induces instantaneous
crystallization which fills the container, and from which
considerable heat is evolved. Purification is accom-
plished as previously mentioned.
The white crystals are monoclinic, glistening, and
when compacted are light cream in color. They are
exceedingly fluffy so that the quantitative yield ap-
pears larger than it really is — from 0.2 g. to 1.6 g. per
fruit. The crystals are soluble in water at 20° to the
extent of one part in 8000 of water, though even at
this dilution it is intensely bitter. This emphasizes
the fact that it is of a greater degree of bitterness than
quinine, for which it has so often been mistaken. Only
a few of the physical and chemical properties will be
recorded in this paper, for a subsequent paper will
treat more fully of the glucoside.
After the determination of its physical constants,
elementary analysis, and chemical reactions together
with the physical and chemical properties of its hydro-
lytic products, I was certain that I was working with
the same compound that deVry4 discovered in 1857,
in the flowers of the grapefruit trees in Java. DeVry
states that it occurs in all parts of the Citrus decumana
though to a much greater extent in the freshly opened
flowers. While both he and Hoffmann,5 and later
Will,28,40 conducted classical researches on this gluco-
side, they state that they obtained their raw product
from the residue remaining in the distillation pots at
Java after removing the "neroli-oil" from the flowers
of the grapefruit tree by steam distillation. Both
deVry and Hoffmann were unable to find this same
bitter substance in the flowers or fruit of any of a host
of other citrus fruits, including the bitter orange.
Hoffmann6 applied the name "naringin" to the gluco-
side which deVry and he investigated. Will28 retained
the same term in his investigations with Tiemann.7
The term originated, according to Hoffmann,* from the
Sanskrit word "naringi" for orange.
Solutions of naringin in ethyl alcohol and water
are levorotatory; the molecular rotation in alcohol
at 180 C. is — 65.2. Its empirical formula as deter
mined from carbon and hydrogen combustion, as well
as from a study of its cleavage products, appears to be
C2iH260ii.4H20 (air-dried). Over sulfuric acid it loses
3 molecules of water, and when dried at 1200 C. it
loses the remaining molecule of water. In the latter
state it is in the form of an impalpable powder, colored
a faint tinge of yellow. When naringin is hydrolyzed
with dilute (5 percent | IIC1 or H2S04, it forms a mixture
of rhamnose and glucose, though the quantity of glu-
* Hoffmann' in his paper gives credit to Professor Fluckiger for the
suggestion of the derivation. PIQcIdger was interested in dcVry's carl;
investigations of naringin.
cose is much smaller than that of rhamnose. At the
same time a highly crystalline solid separates, insoluble
in water, and was found to be the phloroglucinol ester of
/>-hydroxy-cinnamic acid. Methods of isolation and
analysis, together with proof for arriving at the above
conclusion regarding its constitution, cannot be pre-
sented in this paper, but will be followed by a more
detailed and theoretical discussion in a succeeding-
number of the Journal of the Society.
In passing, let me call attention to the behavior
of the glucoside which governed the choice of the ex-
traction method above for its isolation from the peel.
When the air-dry naringin is heated in a receptacle
over a free flame it melts at about 83° C, and forms
a syrupy mass which turns brown on gently increasing
the temperature to ioo° C, above which violent evolu-
tion of H20 vapor takes place and a hard, glassy,
dark brown mass results. This mass is yet bitter
but dissolves with difficulty in water. Now, on the
other hand, when a water solution of the naringin
(pure crystals) is boiled, it rapidly turns yellow to
brown, the bitterness gradually disappears and when
evaporated on a steam bath a resinous mass results,
possessing the odoriferous principles of caramelized
sugars together with those of coumarin and certain
pliLnols. No naringin could be extracted from the
mass. Likewise, when the peel was ground, dried
at no0 C, and lixiviated with water, very little naringin
was obtained. Hence in the separation of the gluco-
side from the fresh fruit, temperatures above 80° C.
should be avoided. In the steam distillation of the
peels some of the naringin is hydrolyzed by the steam,
though the temperature in the distilling flask seldom
registered above 85 ° C; stronger suction would pre-
vent this decomposition.
The quantity of glucoside in the grapefruit examined
was approximately as follows:
Table II
Weight of Quantity of Naringin
Variety of
Age of
Fruit
from Peel Only
Fruit
Fruit
Grams
Gram
Indian River
Fresh Market
770
0.62
Old* Market
715
0.35
Walters
Fresh Fruit
682
0.50
4 raos. at 15° C
695
0.24
Marsh. Seedless
Fresh Market
539
0.36
Old Market
570
0.08
i It is difficult to give the age to any great degree of exactness. "Old*
signifies that the fruit was ol the same variety as the fresh market, but
that it had been kept for some time between analyses, in order to determine
the effect of deterioration on the bitterness. The Walters was secured di-
rectly from a fruit exchange and some of the frtiit kept at constant tempera-
ture for the time specified.
From the table it is quite evident that there is a
diminution in the naringin content during storage,
more noticeable in some varieties than in others.
What has happem-d In the glucoside is revealed when
the sugar content of the pulp is examined over a like
period. Of course, it is not argued in this paper that
the increase in sugar content of the pulp during
able solely to the glucoside, in the Eace ol the
large pectosi content. Bu1 a portion ol i1 may be de-
i by the aid ol thi
enzymes presenl in the fruit. Certain &&
"pink 'i h develop simultaneously with the
decrease in na in sugars an
able to the glucoside, when the reactions of this sub-
stance are bettei underst
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. S
pectin — None of the citrus fruits grown for com-
mercial purposes are so rich in pectose materials as
the grapefruit. The navel orange ranks second in
this respect. Some citrus, of no commercial value
hitherto, contain more pectin at certain stages of
growth.
The isolation of pectin during this investigation
was merely a subsidiary proposition, and was initiated
solely because of the coming commercial importance
of pectin as a filler for preserves, jellies, desserts, ice
creams, etc. A suitable source of pectin among the
by-products industries, where other substance besides
pectin may be isolated to lessen "overhead" expenses,
would be welcome. R. T. Will33 has indicated the
possible isolation of pectin, among other products
from oranges. This has been received only half-
heartedly by the citrus by-products people, owing to
the fear of no demand for the material. It is, therefore,
up to home economics and domestic science investi-
gators to help create the demand by more widely
heralding the suitableness and value of this natural
constituent of many fruits. It is likewise up to the
by-products companies to more effectively study the
isolation of pectin so that a pure, dry, soluble and mer-
chantable product may be obtained. Cooperation be-
tween the above-mentioned laboratories is urged.
No attempt was made to study the theory of pectin
formation or its chemistry, for scores of contributions
on this subject are to be found in biochemical litera-
ture. Mention should be made of its colloidal nature
and emphasized, because its isolation and purification
must be conducted according to the knowledge of
colloidal phenomena. The tenacity with which pectin
clings to many of the substances existing along with
the pectose complex points to the importance of the
above statement, and failure to remove these contam-
inating substances will mean lack of purity.
After the peels had been extracted with alcohol for
the removal of naringin, according to Fig. II, they were
placed in water and boiled for 3 hours. This boiled
mixture was then decanted through cheesecloth and
expressed by hand. The expressings together with the
filtrate were boiled for another hour, filtered through
absorbent cotton, which filled the apex of a fluted
filter paper in the funnel, and then evaporated by means
of reduced pressure to a fairly thick syrup, or viscous
liquid. Three processes were employed from this
point to purify the pectin: u) Reprecipitation by
alternately pouring into redistilled 95 per cent alcohol,
and reconcentrating the water-dissolved precipitate by
means of reduced pressure mentioned above; (2)
freezing and centrifuging to remove excess of water,
without causing decomposition of the pectin body,
after precipitation in alcohol and dissolving in water;
(3) agitated dialysis* in a collodion membrane sus-
pended in running distilled water, of the water-dis-
solved precipitate after the first alcohol precipita-
tion. It might be mentioned that dialysis was also
conducted on the pectin solution obtained after con-
centration by reduced pressure, without alcohol
* By agitated dialysis I mean the introduction of a stirring device in the
collodion dialyzing cell in order to hasten and cause a more complete
dialysis.
precipitation. In all cases the pectin, after final
concentration, was evaporated in vacuum at tempera-
tures not exceeding 40° C. and resulted in grayish
yellow scales easily soluble in water and closely re-
sembling agar in color and texture. Mr. C. A. Utt,
of the Kansas State Food Laboratory, was interested
in working over the liquid remaining from the spon-
taneous fermentation of the steam-distilled peels,
after the naringin had precipitated, for the recovery
of pectin. He also worked with some of the fresh
peels and by means of alcohol precipitation alone,
after previously boiling with water, obtained a product
with scarcely any bitterness. It is possible to isolate
the pectin from grapefruit without retaining any
of the original bitterness. In the boiling process,
a fact to which I have called attention before, the
naringin is slowly destroyed. Since working with the
pectin an instance has occurred to me wherein I be-
lieve it would be very desirable, after purification,
to remove the last traces of water from the substance
by freezing it and then subjecting it to a very high
vacuum. It is a question, however, whether this
would be possible on a commercial scale. It would
yield an excellent product providing it was econom-
ically feasible.
The amount of pectin isolated from the peel of 10
grapefruit (Indian River) weighing 1560 g. was some-
thing over 65 g. regardless of loss. Ten grapefruit
of the same variety obtained two months later in season,
the peels of which weighed 1450 g., yielded about 40
g. of pectin. One would expect the pectin content
to decrease markedly during storage. I am firm in
the opinion that, if the fruit were examined at the time
of picking for market, the average of recoverable
pectin from all varieties of grapefruit would be con-
siderably above 10 per cent of peel weight. Naturally,
the thinner the peel, the poorer the fruit is in pectin.
ANALYSIS OF PULP OR JUICE
In the preparation of thepulp previous to the analysis,
the following method was adopted: Ten average fruit
of each variety chosen were picked out and weighed.
Five of the fruit of each variety were then stored at
nearly constant temperature (150 C.) for a period of
3 mo., and then analyzed according to the same pro-
cedure as for the first set. Table III will indicate
the varieties analyzed. The fruit were peeled by hand,
divided into segments, and the segments freed from
as much of the "pith" as possible without rupturing
the juice sacs. The segments from each five fruit
were then ground in a large mortar with sea-sand in
order to free the juice from the fiber and all washed
into a flask graduated to hold 5 liters and made up to
the mark.
citric acid — Five 50-ec. portions were removed
from the above standard volume, and titrated with
standard A'./io NaOH in the presence of phenolphthal-
ein. The average of these 5 determinations were
calculated to crystallized citric acid (HjC6H507.H:0)
and expressed in grams of acid per fruit.
reducing sugars — 100 cc. of the prepared juice
were measured into a 200-cc. volumetric flask. 5 cc.
of 20 per cent basic lead acetate solution were added,
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERJNG CHEMISTRY
3 7 3
followed by 10 cc. of alumina cream, and the mixture
made up to volume with water and filtered through a
fluted filter with a small tuft of absorbent cotton in the
apex. Reducing sugars were determined in aliquots
of the filtrate with Fehling's solution, following the
method of Munson and Walker, and were expressed
as dextrose in grams per fruit.
It was necessary to clarify the solution in order to
remove the sac fibers and other suspended material.
Because of the presence of a small amount of naringin
in the juice it is inadvisable to determine the sugars
polarimetrically, since naringin is not removed by
clarification.
sucrose — Aliquots of the clarified juice were hy-
drolyzed according to the usual method (acid hydrol-
ysis) and the total invert sugar determined, after neu-
tralization with Na2C03, by the method of Munson
and Walker. The total invert sugar less the reducing
sugars, multiplied by 0.95, was used to express the
sucrose present in grams per fruit.
Table III
Approx.
Age of
Fruit
Av. wt. Av. wt. Citric Reducing Sugars
per Pulp per Acid per Sucrose as Dextrose
Fruit Fruit Fruit per Fruit per Fruit
Grams Grams Grams
430 290 2.77
440 308 1.85
Gran
6.20
Variet
Fruit
Marsh Seedless. .
Marsh (stored) . .
Atwood Grape-
fruit Co. Fruit. 1 680 460 5.98 11.24 14.84
(stored) 4 670 440 3.40 15.15 19.60
In looking at Table III one finds an increase in
both sucrose and reducing sugars during storage,
while the citric acid decreases. It might be thought
that the increase in sugar content could be explained
on the assumption that there is a considerable loss of
moisture from the pulp during storage. But such a
loss of moisture would have to be enormous to account
for the large gain in sugars, and no such loss was
noticed since the fruit were weighed both before and
after storage. Furthermore the citric acid decreases
could not be accounted for on the same assumption.
Again it might be said that soluble pectose material
dialyzing through the sac walls might explain the
increase in sugar content of the juice, but while this
might explain the increase in reducing sugars it could
not explain the sucrose increase. One must look to
the continuation of the function of the enzymes of
the fruit during storage in order to account for both
of these phenomena, the sugar increase and the acid
decrease, as well as the naringin and pectin decrease.
From the large sugar, pectin and glucoside content
it might be profitable to transform these into easily
fermented sugars, and by fermentation of the entire
grapefruit, after processing, obtain an economical
yield of alcohol for commercial purposes. The citric
acid present, if slightly increased by added mineral
acids, would be serviceable for the hydrolysis of the
glucoside and pectose material to available sugars.
From one ton of grapefruit, considering the preformed
sugars alone, one would be able to obtain 10-15 gal.
of proof spirit, calculations being based upon green
weight of fruit.
The values for the sugar content of Marsh Seedless
as shown in Table III are somewhat lower than the
sugar content found at various times before and after
this series of analyses were performed. While the
fruit were purchased for Marsh Seedless it is possible
that they represent another variety. From Colby's
analysis (Table I) it would seem that the above values
represented another fruit. However, the same char-
acteristic rise in sugars is noticed in the true Marsh
Seedless.
SUMMARY
I — A brief condensed history of the grapefruit is
given in an endeavor to trace its introduction into
America. It appears that it was grown in Mexico
before introduction into the United States. Attention
is called to Ferrari's classification of citrus.
II — Lack of previous analyses of constituents is
shown, other than general routine analysis.
Ill — Issue is taken with the various promulgators
of the medicinal value of grapefruit for having made
no attempt to actually ascertain upon what constit-
uents, or possible constituents, the heralded thera-
peutic value depends. Mention is made of the writer's
experiments with naringin for this purpose.
IV — Analysis of the peel showed recoverable amounts
of essential oils (principally Hmonene, citral, pinene
and alcohols), the glucoside naringin, and pectin. Im-
portant properties of naringin are shown and serious
consideration of naringin as of real significance in the
differentiation of Citrus decumana from other citrus
species is urged.
V — Grapefruit culls may factor in the production
of a satisfactory grade of pectin for various purposes
if correct methods are employed in its isolation.
VI — The citric acid, naringin and pectin content of
grapefruit decrease during storage; reducing sugars
and sucrose increase.
VII — Attention is called to the possibilities of
industrial alcohol production from the whole culls.
VIII — Naringin and the "bitter principle" of grape-
fruit are synonymous.
BIBLIOGRAPHY
1— Hume, Fla. Agr. Exp. Station, Bull. 68 (1901), 388.
2— Dygert, "Crops That Pay," 1903, p. 3.
3— GaUesio, "Traits du Citrus," 1811.
4 — DeVry, Jahresber. far Pkarmacognos, 132, 1866.
5 — Hoffmann, Bet., 1876, p. 685; also Hoffmann, Arch, der Pharmacie,
14, (1879), 139.
6 — Dehn, Z. Rubenzucker lnd.. 1868, p. 564; also Denn, Z. Chem.,
103, 1866.
7— Tiemann and Will, Ber., 14 (1881), 979.
8 — Author's article on classification of grapefruit to appear soon.
9— Shamel, California Cilrograph, I, No. 5, p. 19, and No. 6. p. 3, 1916.
10 — Risso and Poiteau, "History and Culture of Oranges," 99, 1872.
1 1 — Watson, "The American Home Garden," 1869, p. 363; also quoted
by Hume."
12 — Spalding, "The Orange in California." 1886, p. 89; also quoted by
Hume.'
13 — Downing, "Fruits and Fruit Trees in America," 1886, p. 579; also
quoted by Hume.'
14 — Gallesio, "Traite du Citrus," 1811.
15 — Lebreton, J. de Pharmacie el des Sciences Ace, 14 (1828), 377.
16 — Toiteau, Individual papers.
17 — Risso et Poiteau, "Histoire Naturclk des Oranges," 1818.
18 — Vaile's report quoted by Shamel, in Monthly Bulletin, Com. Hort.
of Calif., 6 (1916), 239; Wallschlaeger, "World's Prod, and Com. in Citrus
Fruits and By-Products," in Bull. 11 (1914) of Citrus Protective League of
Calif.
19— Hume, Loc. cit.
20— Shamel, Monthly Bulletin Com. Hort. of Calif., 6 (1916), 239.
21 — Reasoncr, Division of Pomology, U. S. Dcpt. Agr., Bull. 1.
22 — Hume, "Citrus Fruits and Their Culture"
23— Pfefler, Botan. Z., 1874, p. 481.
24 — DeVry, Loc. cit.
25— Bias. Z fiir Chem . 1869, p. 316
I 111- JOURNAL OF INDUSTRIAL AND ENGINEERING < EEMISTRY Vol. 10. No.
26 — Hoffmann, Loc. cit.
27 — Lebreton, Loc. cit.
28— Will, Ber., 18 (1885), 1311; 20 (1887), 294.
29— Hilgcr, Ibid., 9 (1876), 26.
30 — Kraemcr, "Text on Pharmacognosy."
31— Von Rijn, "Die Glycoside," 1900.
32— LeLong, "Citrus in California," 1900.
33 — Will, This Journal, 8 (1916), 78.
34 — Tanret, Compl. rend., 102 (1886), 518.
35— Tanret, Ibid., 102 (1886) 1518; also Kraemer, l.o
36 — Aaronsohn, "World's Production in Citrus Fruits," Trans, from
Jewish Agr. Exp. Sta., Palestine, Bull. 1 (1914), 7.
37 — Virgil, Gcorg book II, vers. 126-.
38— Wallach. Liebig's Annalen, 216, 251.
39— Ehestadt, Refit, of Shimmel is- Co., April 1910, p. 164.
40— WU1, Ber., 20 (1887), 1186.
41 — Mullikan. "Identification of Pure Organic Compounds," Vol. I.
42— Zelinsky, Ber., 30 (1897), 1541.
U. S. Department op Agriculture
Washington, D. C.
LABORATORY AND PLANT
AN INEXPENSIVE ASH LEACHING PLANT
By W. D. Turner and B. G. Nichols
Received March 25, 1918
The industrial chemistry department of the Missouri
School of Mines has erected a small plant for the
leaching of wood ashes, and at this time when the
potash industry is receiving such frequent mention,1
a brief description of this installation will be of some
interest. The work was started for its pedagogic
value but developed to a point where it assumed small
commercial dimensions.
APPARATUS
To apply the countercurrent lixiviation principle
vertical columns of buckets were arranged. A column
was supported on two upright "two by fours," 10 ft.
. long and spaced 20 in. apart, fastened directly to the
floor at the base and braced to the ceiling at the top.
At a point 30 in. above the floor and at intervals of
16 in. above this, spikes were driven part way into
these uprights and projected outward about an inch
to serve as brackets to support cross-rods of 3, s-in.
sq. iron bars from which the buckets could be sus-
pendei
The leaching buckets consisted of ordinary 60-lb.
wooden lard tubs, in the bottom of which a dozen or
more holes were bored. The original handles were
removed from these tubs and were replaced by heavier
iron loops bent from '/Vin. round iron rods and fastened
to the buckets by driving the ends through boles
drilled in the sides of the tubs and bending them up
into place. For the water reservoir at the top a
bucket was similarly prepared with only one hole
in the bottom provided with a loose wooden plug by
means of which the flow of water could be regulated.
To catch the liquor at the bottom a tub without holes
was used. The column thus consisted of a liquor
receptacle standing on the floor, above this a series of
S leaching buckets, and at the top a water reservoir.
This column constituted a complete unit. The second
unit was constructed beside the first, letting one "two
by four" serve in both columns. The two units were
identical except that all the bracket spikes in the
second were four inches higher than in the first to
prevent interference in changing the ashes. The third
column was again like the first, and so on.
The liquor was causticized in an ordinary oak barrel
into which a .uncut of live steam could be conducted
to heat and stir the contents, and from which the clear
liquor could be siphoned after the mud had settled.
1 This Journal. 10 (1918), 6, 96, 106, 109, etc.
For concentrating the liquor a cast-iron, seamless steam-
jacketed kettle was used, though for an isolated in-
stallation both this and the causticizing operations
could be carried out in open flame-fired kettles. The
final evaporation or fusing of the potash was carried
out in an ordinary caustic pot.
OPERATION
At the start of operations the bottom of each leach-
ing bucket was covered with about 3 in. of excelsior,
which later packed down to an inch, and over this was
spread a layer of old toweling or other cloth. The
buckets were then filled to the top with ashes and were
lifted into place in the columns by means of a small
block and tackle which could be suspended from a hook
in the ceiling in front of each column. Water was
then filled into the reservoir and was allowed to drip
through the successive buckets until the ashes in all
were saturated. A measured quantity of water,
equivalent to half the weight of the ashes in one
bucket, was then placed in the reservoir and was
allowed to drip through the column, forcing out an
equivalent amount of liquor into the receptacle at the
bottom. When the top bucket had ceased to drip,
it was removed by means of the block and tackle and
was dumped. The excelsior and cloth which came out
with the spent cake were replaced, and the tub was
again filled with fresh ashes. Each of the remaining
buckets was now raised successively to the next higher
bracket and the fresh ashes were placed at the bottom.
Water equivalent to i'/2 times the weight of the ashes
was now placed in the reservoir and was allowed to
drip through. This was sufficient to saturate the
fresh ashes and force out about half their weight of
liquor. This operation of renewing the ashes was then
repeated as often as the reservoir could be emptied.
The liquor from the leaching columns was placed
in the causticizing barrel until this was about three-
fourths full. The calculated amount of lime was
then added and the mixture boiled for about an hour
by moans of the live steam jet. It was then allowed
to cool and settle and the supernatant liquor was
siphoned into the concentrating kettle. The lime mud
at the bottom was then spread over the fresh ashes
at the bottom of the leaching columns, so that any
potash which it still contained was leached out as it
passed up through the successive steps to the top.
By this moans the customary countercurrent lixivia-
tion of the lime mud was obviated.
The concentration of the liquor was continued until
most of the sulfate which it contained separated out
May, 1918
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
375
as a granular deposit. The liquor was then drawn off
into the caustic pot where it could be evaporated to any-
desired concentration or could be fused if necessary.1
To obtain a clean product without the necessity for
calcination, the potash in a part of the liquor was
converted entirely to sulfate by neutralizing with com-
mercial sulfuric acid. This operation was carried out
in an ordinary oak barrel arranged so that acid could
be siphoned into it directly from a carboy. Before
neutralizing, the leach liquor was concentrated until
Diagram of Leaching Column
solid carbonate began to appear. It was then drawn
off into another container where it was allowed to
settle and cool. The clear, saturated solution was
then placed in the barrel and the acid allowed to
run in until neutral to litmus. This caused a violent
reaction and resulted in the precipitation of a large
per cent of the potash in a clean, pure, finely divided
crystalline mass. This was allowed to settle, the
supernatant liquor was returned to the concentrating
kettle, and the crystals dried in a centrifugal machine.
1 Martin, "Salt and Alkali Industry," p. 45.
By this means almost all of the organic matter was
removed and the potassium sulfate obtained was nearly
pure and colorless, the sodium remaining behind as
carbonate in the concentrating kettle, and the organic
matter remaining in the liquor.
DATA AND RESULTS
It was found from preliminary experiments that the
rate of flow through the ashes was dependent mainly
on the area of the cross-section from which the liquor
could drain, but was practically independent of the
depth. The buckets which were used were 16 in. in
diameter at the top and i21/2 in. at the bottom, and
were 1 1 in. deep. These dimensions gave an area of
drain of about 490 sq. in. and a capacity of about
35 lbs. of ashes when loosely packed. Through this
body the necessary 7 gals, of water would percolate
in about 4 hrs. or less under favorable conditions.
It was thus practicable to make three changes per day,
making the total capacity of each column about 105
lbs. Since oak ashes average about 11 per cent
potassium salts the yield from each column was about
10 or 11 lbs. of potash salt per day. One man could
change one column in about 10 or 12 min., so that he
ought to handle easily 4 columns per hr. or a total of at
least 15 columns, allowing 4 hrs. between changes.
A few average analyses will give a measure of the
efficiency of the apparatus. Analysis of the ashes in
the vicinity of the School of Mines shows about 4.25
per cent hydroxide, 4.50 per cent carbonate, 2.90 per
cent sulfate and 0.02 per cent chloride. If all con-
verted to sulfate this will yield over 15 per cent; if
causticized it will yield about 7.8 per cent hydroxide
and 2.9 per cent sulfate. Tests on the liquor from the
top bucket just before discarding it showed: sulfates
a mere trace and total alkali figured as potassium
hydroxide 0.3 per cent. But this final liquor is
saturated with calcium hydroxide, so that the actual
potassium hydroxide content is not 0.30 per cent but
about 0.06 per cent to 0.08 per cent. The percentage
recovery is therefore 99 per cent or more of the avail-
able salt.
For causticizing, a dilute solution of the material
to be treated is necessary, and it will be noted that the
solution as it drains from the bottom bucket is just
about at the right concentration. Analyses on this
liquor show about 3. 75 per cent sulfate, 5.50 per cent
hydroxide, and 5.75 per cent carbonate. This will
yield about a 10 per cent solution of caustic potash
when completely causticized, a strength which is
recommended as most economical.1 For this con-
version the liquor from one bucket will require (allow-
ing a 50 per cent excess) about 1 lb. of quicklime.
Thus the average amount of sludge to be returned to
each bucket from the causticizing barrel will be less
than 2 lbs. and may be spread over the surface of the
ashes without detriment. It is probable even that
this sludge converts some potassium carbonate to
hydroxide during the leaching process.
Typical results may be tabulated as follows:
' F. H. Thorp, "Outlines of Industrial Chemistry," p. 84.
376 ////•; JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 5
Table of analyses quantity and of a sufficiently satisfactory grade to
Leach After Final Final ^ J .
Ashes Liquor Causticizing Hydroxide Sulfate assure the country an adequate native supply.
Substance Percent Percent Percent Percent Percent . . . . . a ., , ,. ,
Su|fate 2.90 3.36 3.14 Trace 99.05 .Antimony occurs in nature chiefly as the tersulfide
\^'h *•*> Ill g.25 g4 Nil (Sb2S3) in the mineral stibnite and to a smaller extent
chloride 0.02 0.02 ... jn combination with other metallic sulfides under a
Leach i Liouor for a Typical Run Just Before Chancing the Tubs variety of names. Such as bournonite, pyrargyrite.
Total aiiaii "(as "kj'coi), kermesite, etc. For the purpose of this paper, how-
percent 0.33 1.99 3.59 6.88 12.30 ... . ~- . c ., ,• • . .,
ever, it will be sufficient to confine the discussion to the
Sodium1 and Potassium in Product . , . . , , .. ..
NajSOt KiSO( Moisture consideration of the more or less pure stibnite ores
Percent p"7ce4nt Peyejit that occur in nature. As these ores are rarely free
• Sodium by difference. from a siliceous gangue, it is necessary in the prepara-
m m.uary tion of the material for use as a primer constituent
. ... . , , , . , , ., , to melt or liquate the ore out of contact with the air.
A small, inexpensive ash-leaching plant is described -..,.. , . , o ^
.. , '. . , , . ,. . . .. . Stibnite, when pure, melts at approximately 550 C.
in which the principle of countercurrent hxiviation is , , . . , ...
..... . . ... , In the process of melting, a certain amount of metallic
applied, with certain resulting advantages: r . , ,° it fi .
.... . ... , , . , antimony is separated from the melt and goes to the
1 — Minimum initial expense and low upkeep. , ., , , , , -,•
T .. „,, , , ,. bottom, while, on the other hand, the siliceous gangue
2 — Low operating cost. 1 he leach liquor requires no . ... , _ ' . , ,
.. . , , ., .. impurities rise to the top. On cooling down the melt,
concentration before causticization and the caustic , v , , . ,. , , ,.
, . . ^ ,• • ■ x- therefore, the intermediate layer represents the liquated
sludge requires no separate hxiviation. . ,, , ,.,,,,, r ,, ,
TT. , ~. . t, antimony sulfide which should be carefully separated
3 — High efficiency. Recoverv is 00 per cent or , , J , , .
, from the other two layers and represents the raw ma-
„., -i^- t^i_i r-u terial of the antimony sulfide used as a primer con-
4 — Rapid manipulation, .bach column furnishes a ,„ „ . , , , . ,
. . j c c 11 * a 1 1 r stituent. If during the process of melting down, the
spent charge and a unit of full-strength leach liquor . 6 f 6 *
, , antimony sulfide comes into contact with oxygen of
every four hours. .... , . ,. ,
the air. it is to a greater or less extent oxidized and
Missouri School op Mines . ,
Rolla, Missouri the material is not pure sulfide of antimony but con-
tains an indefinite proportion of oxide, and possibly
ANTIMONY SULFIDE AS A CONSTITUENT IN MILITARY ^ ^ the f°™ of °^}^ intimately associated
AND SPORTING ARMS PRIMERS1 w tersulfide which has not been oxidized or
By allerton s. Cushma n» burned.
Received March 29, 1918 T^le work of liquating the crude ores is principally
Toward the end of the year' 19 1 6 and throughout done in China and JaPan before the material is im-
191 7, the production of military ammunition for all Ported lnto the Umted States- Wlth the result that
arms began to be tremendously speeded up in the heretofore there has been but little control of this
United States. At the same time, the overseas com- Process and the antimony sulfide available in the open
merce of the world was interfered with by trade con- market has shown a wlde variation in its chemical
ditions incident to the war and shortage of ships. The analysis and therefore in its quality. Textbook and
result of this combination of circumstances produced periodical literature on the subject of specification of
a very unusual condition with regard to the chemical antimony sulfide as a constituent of primer mixtures
constituents used the world over in the manufacture 1S for the most Part meager and often misleading and
of military primers of all kinds. inaccurate. It is usually the custom to direct that the
For years past tersulfide of antimony has been Puritv of the antimony sulfide in question shall be
used in almost every type of primer and is considered determined by analyzing the material for antimony
a necessary ingredient thereof, although the percentage bv anv of the weU-known volumetric methods and then
quantity used in various formulas varies within wide calculating the percentage of antimony to the basis
ranges. The principal sources of antimony tersul- of the tersulfide (Sb2S3) which in a sample of pure stib-
fide for this purpose are the crude stibnite ores nite should fiSure out verv close to 100 per cent.
which are found native in many parts of the world, A number of chemists have become aware of the
including England, Canada, United States and Alaska. fact that analyses and calculations made on this basis
Nevertheless, the principal supply of tersulfide of very frequently led to results running over 100 per
antimony as far as the United States is concerned is cent, which was assumed to be due to the fact that
from Japan and China and at the present time prin- some slight amount of free antimony accompanied
cipally from China. It is probable that the segrega- the antimony sulfide. On the other hand, when cal-
tion of this business into the hands of the nations of culations were made on the same basis of analyses
the Orient is largely due to cheap labor, so that if and came out less than 100 per cent, it was consid-
on account of any condition incident to the war it ered that this showed an unsatisfactory grade of
became difficult or impossible to import antimony purity in the material.
sulfide from overseas, the result would be that the The fact that the antimony determination is easily
price of the crude materials would advance. Native an(i quickly made, while the determination of sulfur
antimony sulfide could then be produced in sufficient >n the material has been considered a difficult and
1 Published by permission of the Chiei of ordnance. unsatisfactory determination, has probably been the
' Lieutenant-Colonel. Ordnance Department. I principal Cause of this State of affairs.
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
377
The assumption has always been made by explosives
chemists that the material required for making efficient
primers was pure tersulfide of antimony (stibnite) of
as high a degree of purity as the market or methods of
treatment of the original ores would make it possible
to obtain. It has at no time, as far as the writer of
this paper is concerned, been suspected that very possi-
bly, if 100 per cent pure stibnite was available on a
large scale, it would not lend itself so efficiently to the
manufacture of high quality primers as does the ordi-
nary liquated crude antimony sulfide which can be
made practically available in large commercial quanti-
ties. In fact, the whole question as to the proper
grade or condition of the antimony sulfide for the com-
mercial production of high-grade primers has been so
obscured by theory, opinion, rumor and loose state-
ment that it has been almost impossible for a worker
in this field to make any definite decision with regard
to this important subject.
The primer, as its name implies, is expected to in-
itiate every explosion which takes place from the first
burning of the propellant powder to the final explo-
sion of the shell, if such explosion is designed to take
place, when it arrives at the final place where detona-
tion is required. It is therefore quite apparent that
the success of ammunition, and very often the final
decision in war, must hang directly upon the efficient
and proper functioning of the greatest possible number
of all primers loaded. It is apparent that the efficient
functioning depends upon the proper selection of the
constituent materials which enter into the priming
mixture.
There are, of course, a number of different types
of primers and quite a wide variety of selection is
made in different types of constituent chemicals, but
since antimony sulfide is common to almost all primers,
for the purpose of this paper, no discussion of the
other chemicals aside from antimony will be included.
As far as antimony sulfide is concerned, it can be
reiterated that the book references as to the quality
which should be sought are generally vague and un-
authoritative. As an example of this, it will be suffi-
cient to cite the paragraph with which antimony sul-
fide is dismissed in the latest (1017) edition of Mar-
shall's compendium on "Explosives, Properties and
Tests," Volume II, page 686:
"This material is found native in England and other countries; it has a
density of 4.63 and the pure substance melts at 555°. At high tempera-
tures it is volatile. The crude ore is refined by melting out the antimony
sulfide, which then forms bluish gray lumps with a metallic luster and very
brittle. It is also produced artificially, but in Germany it is forbidden to
use in explosives the artificial product, or such as contains iron. It is abso-
lutely essential that it should be free from sulfuric acid, as this has a very
deleterious effect on the stability of explosive mixtures containing a sulfide
and a chlorate, such as cap compositions. When treated with aqua regia
it should not leave a residue of more than 0.5 per cent. It should be ex-
amined to see that it is not adulterated with sulfide of lead or iron, and
that it contains little arsenic. The value of the substance as a constituent
of cap compositions seems to be due largely to its hardness and crystalline
form, which render the compositions sensitive to blows and friction."
It will be noted that the above paragraph gives
very little information on the subject. The im-
pression is given by the paragraph that what is wanted
is practically pure stibnite and, above all, that it should
be free from sulfides of lead or iron and contain little
arsenic. It further states that the residue after treat-
ment with aqua regia should not amount to more than
0.5 per cent. It will be the object of this paper to
show, as the result of an extended and exhaustive re-
search, that none of the statements made in the above-
, mentioned paragraph are based upon facts and that
they are mainly incorrect. As a matter of fact, it may
fairly be doubted whether any antimony sulfide used
throughout the world in primer compositions at pres-
ent would be found to leave a residue after treatment
with aqua regia of not more than 0.5 per cent. In
fact it would probably be impossible to obtain such
material in large commercial quantities, even if such
a specification were essential.
As a matter of fact, very good primers can be made
with antimony sulfide containing up to 5 per cent
residue insoluble in aqua regia. This residue, as
would be expected, is mainly siliceous and the objec-
tion to its presence can only be because, just to the
extent that it is present, it reduces the proportionate
quantity of active sulfide of antimony. Moreover,
high percentages of silica in the form of grit will wear
away the charging tools which are part of the machines
which are used in the manufacture of the finished
primer. Certain primer mixtures are loaded dry, in
which case the presence of any considerable amount
of gritty silica will lead to explosions in the presses,
which, though not of a very serious nature and which
are always expected to occur to a certain extent, are,
of course, not desirable.
For this reason it is well to select antimony sulfide
with as low silica content as possible, but very excellent
primers can be manufactured if properly compounded,
in which the silica content of the sulfide runs from
2 per cent to 3 per cent, which is within the bounds
of practical accomplishment on a large commercial scale
of operation.
The statement that the antimony sulfide should be
free from sulfides of lead or iron, can be shown to be a
totally unnecessary specification, for this paper will
set forth the results of investigations in which sulfide
of lead and iron have been entirely substituted for
antimony sulfide, with the results that very excellent
primers have been made from these materials. It is
not logical to assume that if excellent primers can be
made with these sulfides, with the exclusion of anti-
mony, small quantities of such sulfides existing as
an impurity in the antimony sulfide would necessarily
be deleterious. As a matter of fact, such textbook
statements naturally increase the anxieties and difficul-
ties which press upon the explosives chemist in the
proper specification of constituent materials for primer
mixtures. This subject will be returned to in detail
in a later portion of this paper.
It should suffice, however, at this place, to point
out that if authors preparing textbooks on explosives
would be careful to include only such information as
is based upon authoritative evidence with citations to
the literature, the whole question of production of
ammunition on the sudden large scale demanded by
modern warfare would be made easier for all concerned
in its manufacture.
378
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 5
Probably the most important point, and one that
has been most discussed and debated with reference
to the proper grade of antimony sulfide for use in
primers, has reference to its degree of purity as gov-
erned by the amount of actual antimony tersulfide
present, irrespective of outside impurities. By this
is meant the degree of oxidation of the sulfide which
has taken place in the process of liquation. It has
been this point which has led to quite extreme differ-
ences of opinion among explosives chemists and on
which but little evidence and data were available until
the investigation set forth in this paper had been
concluded.
Up to October 191 7 specifications for ground anti-
mony sulfide as used at Frankford Arsenal prescribed
that the ground material shall on analysis show a
percentage of antimony sulfide not lower than 98
per cent of Sb2S3. In the light of present knowledge,
this specification was irrational and impossible. The
specification was based on the percentage of antimony
found and did not take into consideration the per-
centage of sulfur present or rather the amount of oxide
or of sulfide that had been formed in the process of
liquation.
Liquated Chinese antimony sulfide comes into the
market under the trade names of "crude" or "needle"
antimony. As the earthenware pot furnaces in which
the liquating is carried out are presumably never
quite air-tight, the product is to a greater or less ex-
tent oxidized and contains oxygen in the form of oxide
and oxysulfide. Numerous careful analyses of the
antimony, sulfur and oxygen content of various sam-
ples of "needle antimony" made at Frankford Arsenal
show that this material as prepared for primer manu-
facture throughout the United States and Canada
approximates around 80 per cent Sb2S3, 18 per cent
Sb;03, and 2 per cent aqua regia insoluble. Just how
the oxide is associated with the sulfide in the needle-
shaped crystals of liquated antimony sulfide must
remain for the present a matter of conjecture. It is
apparent that there may be several possibilities: the
oxides may be present as oxysulfide or oxide either in
the form of a solid solution (eutectic) or as mixed
crystals. A careful microscopic research would de-
termine this point if it were considered worth while.
In the meantime, however, it is known that if pow-
dered "needle antimony" is boiled or washed in a ten
per cent solution of tartaric acid and immei
washed with water and dried, the product will analyze
with a higher percentage of antimony sulfide. Tar-
taricacid has then fore been used as a method
of analysis for determining the amount of oxide pres-
ent in s nple. As a method of analysis, how-
ever, the tartaric acid extraction is extremely crude
and in. 1 not only is antimonious oxide in a
crystalline form difficultly soluble in the acid, but also
the crystalline sulfide is not entirely insoluble. Mani-
uly correct method of determining the
percentage present is by igniting the sample in a com-
bustion tube in a stream of pure, dry hydrogen sul-
fide and collecting and weighing the water formed.
It is evident, however, that both the tartaric acid
and the ignition in hydrogen sulfide treatments furnish
a method which might be adapted to the commercial
scale of operation if it were desirable or necessary to
attempt to increase the percentage of actual Sb2Sj
present. In fact, treatment with tartaric acid has
already been recommended by several workers, who are
interested in the manufacture and inspection of primers,
as a method of washing and purifying ground "needle
antimony" intended for use in the manufacture of
military primers. That such a method of treatment
would involve not only an additional amount of trouble-
some and expensive work, but also grave danger, can-
not be denied.
In a program of manufacture which comprehends
the production of millions of primers per day, such a
treatment of the ground antimony sulfide for use in
the mixtures would be a serious consideration to any
manufacturer, whereas, if all of the reacting tar-
taric acid is not perfectly and completely washed out
of the material before re-drying, a new danger is in-
jected into an already difficult and dangerous process
of manufacture. If, however, it could be proved
necessary to add this additional treatment to the
preparation of high-grade antimony sulfide for the
purpose intended, neither the expense, time nor danger
would constitute a sufficient reason for not carrying
out the process.
The question is, is it necessary and to what extent?
Will experimental data collected by an exhaustive
investigation serve to show that better primers can
be manufactured with antimony so treated than with
the commercial grades of Chinese "needle antimony"
which are at the present time available for the pur-
pose?
It was with these considerations in mind that the
investigation which is the subject of this paper was
undertaken and the results of which investigation will
now be set forth. It is obvious that such an inves-
tigation must not confine itself merely to the problems
of analytical chemistry involved, but must also carry
the problem into the actual manufacture of military
primers and to the subsequent problem of drying,
loading and proving. This can be carried out efficiently
only when the chemical laboratory is working in the
closest coordination and cooperation with the small
arms manufacturing department and with the proof
house where the actual ballistic records of different
experimental lots of primers can be put to the last
and final test in all types of small arms, including the
0.45 caliber pistol and revolver and the 0.30 caliber
for rifles and machine guns of all types at present
used in the service.
ANALYSIS
It has already been stated that it has been hitherto
the common practice among most of the purveyors
and consumers of antimony sulfide to specify and
grade the material on the basis of purity calculated
from the percentage of antimony found on chemical
analysis, instead of from the percentage of sulfur.
It is now known that this practice was wrong and
has led to great confusion of thought and opinion
May, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY 379
As an instance of this, the following is quoted from manufacture, does not run better than approximately
the announcement of a leading dealer in ground anti- 80 per cent actual Sb2S3. The following questions
mony sulfide: immediately suggest themselves:
"Antimony sulfide (needle). Guaranteed metallic antimony minimum I Would it be of material advantage to the end in
70 per cent-equivalent to about 98 per cent sulfide. Lump or 150 mesh." yjew tQ usg ar,timony sulfide of a higher degree of
As a matter of fact, this particular brand, based on purity?
the sulfur content of 22.36 per cent, really con-' 2— Would it be practical and worth while to at-
tained about 80 per cent Sb2S3 and 18 to 19 per cent tempt to treat the 80 per cent sulfide in order to in-
Sb203. crease its purity, and if so, what impurities are the
The chemical methods which have been used in ones to be considered harmful?
the determination of sulfur, may be roughly divided In order t0 get yight on these questions, the investi-
into (1) fusion, (2) evolution, (3) wet oxidation, (4) gati0n was directed to the study of treating ground
electrolytic. The most consistent and accurate re- samples of antimony sulfide with tartaric acid solu-
sults are obtained by digestion of the finely ground tions 0f varying strength under varying conditions,
sample in bromine and carbon tetrachloride with sub- After numerous experiments it was found that a
sequent dilution, filtration and precipitation of barium 10 per cent soiution of tartaric acid was as effective
sulfate. Consistent results have also been obtained for the purpose in view as stronger solutions and,
with bromine and acetic acid as the oxidizing further, that in order to get the maximum results
medium. without producing decomposition of the antimony
Designating these methods as "A" and "B," respec- sulfide itself, boiling for 30 min. is required. If
tively, the following check results have been obtained cold digestion is resorted to, 5 or 6 days are required
in the course of this investigation. All other methods to approximate the maximum extraction of oxide,
for the determination of sulfur have been rejected as On the other hand, the purest Japanese sulfide free
leading to inconsistent results. The samples included from oxide yields 1 per cent extract on 30 mins. boil-
in the table were as follows: F. A. 42 and F. A. 88, ing and 4 per cent on 3 hrs. boiling in 10 per cent acid
representing material purchased to a specification when 150-mesh samples are being used. In the same
very similar, except as to granulation, to the dealer's time F. A. 88 antimony sulfide yielded 16 per cent
grade quoted above. and selected Chinese lump 6 per cent extract in the
It may be stated at this place that many millions 30-min. test.
of eminently satisfactory primers have been manu- The above work has shown very clearly that while
factured from the lot of antimony sulfide represented treatment with tartaric acid does remove a consid-
by these samples. There have also been manufac- erable portion of oxide that is present as oxide, it does
tured many millions of primers from this same lot not remove oxysulfide and, moreover, it is shown
that were defective. In the defective ammunition, that even the purest antimony sulfide is to some ex-
however, the granulation of the antimony sulfide tent decomposed by the acid. It is, of course, obvious
was not correct and other subsidiary causes of the that while the oxide impurity is being lowered, all
defects were discovered. acid insoluble impurities present, such as silica, are
The sample marked C. L. was a picked sample of being increased. The danger of the introduction of
Chinese lump from a consignment recently imported. tartrates into the final product is objectionable. The
The sample J. S. was pure stibnite from the Ichino conclusion drawn by the author as the result of this
Kawa Mine, Iyo, Japan, where magnificent groups of part of the investigation is that tartaric acid treat-
brilliant crystals up to 20 inches in length of very high ment of antimony sulfide intended for use m mih-
purity are found. The results of the analytical work are tary primers should not be permitted,
given in Table I: It is apparent from what has been stated that com-
Table j mercial liquated antimony sulfide is never a pure prod-
Method A Method b Acid insoluble uct containing antimony and sulfur in the propor-
Sampie ^Pe? e'en?"1 ^"er" cent"* EofSL tions of Sb2S3, but is always contaminated with oxy-
p. a. 42 22.36 22.37 2.5 gen, which it absorbs while in the molten state. Muni-
22:08 tions laboratories have heretofore generally based
F. A. 88 22.53 22.69 2.5 their specifications on purity calculated from the
c. L 2T.34 26.42 0.2 amount of Sb,Sa figured from the percentage anti-
2642 2g jo None mony found, instead of from the percentage of sulfur.
J'S' This practice is shown to be wrong. As a
Calculating the percentage of Sb2S3 present in fact, most commercial needle antimony sulfide will run
F. A. 42 and F. A. 88 from the sulfur content found, from about 8oto85p., - til .,, bual SbjS, and ma
we get 78.4 and 79.1 per cent, respectively, instead tained to So pel cenl i ry ex-
of approximately 98 per cent calculated from the cellent primers can b wil be demon-
antimony content. strated in th( U
The above-described work establishes the fact that The correct analyses oi "iples of anti-
granulated Chinese "needle antimony," such as has mony sulfide in v turers of mili-
been in common usage for many years in munition tary primers are given in Tabic II:
380 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 5
Tablb II -Analyses o» Antimony Tersulfide (Needle Antimony) nAincxir- ^i-ctc
Anti-Sul-Sas Oxv- BALLISTIC xtblb
TeT p« Svfr Pw ' Per P™ 'ivrd APe'rnic The quality and ballistic accuracy of small arms
cent cent cent cent cent cent cent cent ammunition depends upon a number of factors. If
F. A. 88 69.6 22.6 79.1 2.8 4.6 0.06 Trace None ... . ., . ., , , . ,, ,
p a 42 70 o 22.4 78 4 2 i o 06 Trace None it be assumed that the powder, cases and bullets are
;;;;::, ;;; &8 «:» ":$ Sis' °:.°4 TraCe None °- K- in a given lot, erratic ballistic results are in-
l\ ,;""!'!;, .'.nit 22.0 Ve'.lV.? variably ascribed to the primers. The primer is un-
,"' ' ' , , ??■£ -m * it „ H questionably the heart of the cartridge and is de-
rreated SbtSt) . . 71. 8 24. 5 75. 81. 6 ... ^ J °
Dealer b 70.o 2.2 pended on to initiate the functioning of each and every
Pure Japanese Stibnite.. . 71.4 28.5 99.9 0.00 , _ . , A. . , ,,
shot. In its turn the functioning of the primer per se
The method of determining sulfur adopted by the involves a number of factors, each one of which in
Frankford Arsenal Laboratory as giving fairly quick an ideal primer (if such a thing indeed existed) must
and accurate results is as follows: not only be right in itself, but must coordinate with all
Treat 0.5 g. of the powdered sample in a covered No. 2 beaker or small the others in just the right way. Small arms primers
Bask v ith a mixture of i cc. n,o. 9 cc. siaciai acetic and 6 cc. liquid bromine arc made 0f an intimate mixture of reacting chemicals,
at r i temperature; let stand overnight. In the morning add 20 cc. cone. . . . . . . . ..
HC1 and warm gently for half an hour. Remove the cover and evaporate which mixture IS then machine-pressed into Small
to 'soft dryness" on steam bath. Take up with io cc. cone, nci and a brass or gilding metal cups foiled with a paper disc,
little water. Add 2 g. of : tartaric acid and dilute to ISO cc with hot water. ,, , ;, inserted and the primers dried,
To the warm solution add 0.5 g. powdered aluminum, a little at a time, f
until the antimony is precipitated as metal. Filter at once and wash the after which they are ready for the loading operations,
precipitate with hot water. Allow the filtrate to cool. Dilute to about The chemical mixture or composition varies widely
600 cc. and precipitate BaSOi by adding 25 cc. of a 10 per cent solution . ., . . «. . j. , . . . . .,
of Bacu from a burette m lne different formulas developed by the separate
, , , . , munition manufacturers and governments. It is
The method used for the determination of anti- ... . . .. f ,, ■ . • . «.
,_ , . r ,, not the intention of this paper to enter into a discussion
mony in needle antimony sulfide is as follows: , ., .. , c . „ .. c ,-a . m „
1 J of the comparative defects or merits of different well-
Weigh accurately 0.3 g. of sample and brush carefully into an 800 cc. . . . . . ,. , , .
Krienmeyer. Add 35 cc. HO (op. gr. l . 19) and let stand in the cold for known primer mixtures, many of which have been
thirty (.50) min., after which the hydrogen sulfide is expelled by heating on patented. It may be Stated briefly, however, that
the water bath. Then add 20 cc. cone. iici. 20 cc. cone. ii,so. and ioo primer compositions divide roughly into two types —
cc. water. Boil 15 to 20 min. to drive off all SOa and H..S; dilute to about \ . r , t,'i •
600 cc. and cork up with a connection to a bottle of Na,COi and cool under detonating and burning. In the detonating type
tap quickly. Titrate at once to first pink with A7io k Mno, standardized mercury fulminate, lead azide or some similar sub-
against Bureau of Standards' sodium oxalate, prepared according to Sorensen, stance fai fa ^ y ^ detonated by & perCUSSive
or run a blank against C. P. metallic antimony. J J r
™, ., - , . j , .« j . ... , . , blow is made the base of the composition. In the
The method selected for the determination of lead , , ■ , , ,,
, . c ,, burning tvpe we have to consider more or less well-
and iron is as follows: , , , . , . ,
„ . . , balanced mixtures of fuel and oxygen-carrying con-
WeKh 5 g. of sample into a small beaker and treat with 60 cc. HNOl • , - j
(sp.gr. i.4). when sh,s. is completely decomposed, take down to moist stituents. For the oxygen carriers the main de-
dryness; add 5 cc. cone, iinos, dilute to ioo cc. and filter through a double pendence is potassium chlorate with sometimes an
filter (595 S. S.). Wash free from acid and determine lead in the filtrate , ,-.• in r . .v
,.• ,« „«,, ,, ,> r- . . a v,-. , additional small quantity of barium or some other
by adding 10 cc. HiSOi (1 : 1). Evaporate to dense white fumes on any 1 J
suitable hot plate; cool, add water and filter the Pbso. on a prepared nitrate. The fuels selected are usually sulfur or some
Gooch crucible Wash in diluted aSO» (1-100), once in alcohol, and dry at sulfide Or Sulfo Salt with Or without the addition of
250° C. for one hour. Cool and weigh. PbSO. X 0.6831 = Pb.
_ ,...,-. „ carbon or carbonaceous material.
Transfer the lead filtrate to a 600 cc. beaker, boil off alcohol; then add
3 g. of ammonium chloride and heat the solution to boiling. Precipitate The one striking thing about primer composition
the iron with a slight excess of ammonium hydroxide. Cover and boil in general throughout the world is that they almost
for 5 min Remove the cover and let settle for 20 min., filter on a fast ' ■ i i .■ c
running paper and wash well with diluted ammonia (1-5). Wash well invariably O.n.all, SOuie proportion of antimony
three times with hot water. Redissoive the iron with is cc. iici (i-i), sulfide regardless of whether they are representative
usi„,- this acid to rinse the beaker. Add 2 g. of nii.ci and a few drops of 0f the detonating or burning type. The author is
HNOs. Reprecipitate the iron and filter. Wash three times in diluted am- , ... . , , , .
l, twic with hot water. Dissolve the iron off the paper with 20 cc. familiar with only one modern primer composition
of H.SO. (1-1) into a small Erlenmeyer Add 1 g. of 20-mesh zinc, warm which WaS made Up without antimony Sulfide, but
on a hot plate and when dissolved titrate with N/30 KMnO. to a permanent th;s hag nQt been ft success and it ;s understOod that
pink.
„..,,,, ,, the manufacturers have recently modified it by an ad-
1 lu- method used for determining oxygen in needle ,. . , ,_ , : .
., . .... dition of antimony sulfide to the formula.
antiui'im sulfide is as follov _. . ,, , .
Since antimony sulfide is so generallv admitted to
One grain of the finely powdered sample is weighed into a porcelain .
boat and heated in a glass combustion tube In a stream of pure, dry hydro- be a necessary ingredient of good primer COmpOSl-
gen sulfide. After all air has been displaced, the combustion tube is heated tionS, the question at Once Suggests itself aS to JUSt
uHv a, firs, and finally to the fusion point of the sulfide, about S50« wh t rflle j. , • ^ functioning? On this Sub-
C. Care must be taken not to allow the temperature to rise much above . F °
the melting point, aa SbjSi emd SbiOj volatilize ..t hlghei temperntures. ject there has been much difference of opinion on the
The water formed in th oiiected in an absorpUon mbe in the part of various authorities. It must be very generally
usual manuei iimi iftei ilro 11 sultide with dr\* air, is ■ j .» . • 1.1 , 1 1"
weighed Blank, should be run on pure tlbnite to caUbr.teth<app.»tiu. conceded that in order to burn the powder properly,
.,., 1 , , , 1 11 a primer should function at the instant it receives
1 lie determination <>t aqua regia insoluble lmmin- , ., , , _ .
, , 1, 1 1 , , t 11 the percussive blow of the firing pin without showing
ties in antimonj sulfide is dcliTmined as follows: ...... . ■
„,,.., , . Mnn . , . , ,„„ delay action leading to hangfires. ' In particular, it
Wei| [h 5 g. of sample into a 400 cc. beakci and tieat with 200 cc. aqua ' •• .
regia (1 part UNO,, .1 parts 111 1) Keep on hot plate for one half hour Should also show a high heat of Combustion, a good
to complete solution and expulsion of all us. Kilter on well-packed as- depth of penetration, not too violent explosion and
bestos Gooch. Wash free from acid and onee with alcohol. Dry at 250° C. i j _*:__ „f „ v. j
.,„.... , . , „ , , ". . large gas production of such a nature as to produce
and finally ignite to volatilize any separated sulfur. Cool, weigh and re- e> e. f """ul' '"' "" r'^
port as insoluble in aqua regia. a long flash of flame. Above all, it must possess
May 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
381
properties which will prevent its deterioration in stor-
age and in service and must be of a sufficient but not
too high sensitiveness.
Now it is possible that the presence of antimony
sulfide affects all of these desired qualities, although
not all to the same degree. There are in addition to
the above, three other possible functions of antimony
sulfide in primer compositions.
1 — The hard, smooth grain of the needle crystals
may act the part of a friction agent similar to that
produced in certain primer compositions by the in-
troduction of powdered glass.
2 — The needle grains may hold apart or insulate
the more reactive chemical agents in the mixture and
thereby control sensitiveness and reduce tendency
to deterioration.
3 — The needle antimony may act in part or as a
whole as a contact or catalytic agent and modify the
explosive reactions.
It may be admitted that for one or all of these reasons
antimony sulfide or its equivalent is a necessary con-
stituent of all primer mixtures. Since it is known
that the present source of supply of needle antimony
is from China and Japan and since it is not without
the bounds of possibility that at some time or other
importations might be interfered with, it is important
to determine whether antimony sulfide of a grade of
purity which could be produced in this country would
be equally as effective as the imported material and
also whether other domestic mineral sulfides which
occur in sufficient abundance could be substituted in
an emergency.
The answers to these questions can be obtained
only by making up lots of experimental primers, load-
ing them into ammunition and making the usual
ballistic tests for muzzle velocities, barrel pressures,
sensitiveness and freedom from misfires and hang-
fires.
It is not necessary in this paper to discuss in detail
all the required ballistic specifications that finished
small arms ammunition has to meet, but the following
requirements are quoted from Ordnance Pamphlet No.
544:
"On inspection and tests of finished cartridges, the standard velocity
at 78 feet is 2640 foot seconds. 1 he mean velocity must not vary from these
standards by more than 30 f. s (2610 f. s. - 2670 f. s.) in the model of 1903
rifle. The mean variation in velocity must not exceed 20 f. s. in the model
of 1903 rifle.
"The maximum pressure must not exceed 52,000 lbs. per square inch
in the model of 1903 rifle."
It will be seen from the above that if the powder
cases and bullets are quite right, the primer must
burn the standard charge of powder in such a manner
as to produce a muzzle velocity of about 2640 ft.
seconds at a pressure not to exceed 52,000 lbs. per
sq. in. If a primer is weak from any cause, pressure
and velocity will run low. A good primer will tend
toward maximum velocities with minimum pressures.
If pressures run high for normal velocity, discussion
is in order to determine whether the powder or the
primer is at fault. It is apparent, therefore, that a
primer can be too strong and that the narrow limits
of satisfactory functioning present the most perplex-
ing problems to the primer manufacturer.
One method by which the manufacturer seeks to
gain information and control of his production is by
means of the drop test by which samples usually
about one-half per cent of output are shot. All mis-
fires must be accounted for or the lot of primers repre-
sented by the sample rejected and destroyed. Per-
haps the greatest value of the drop test lies in the fact
that in expert hands it can be used to measure the
comparative sensitiveness of different lots and types
of primers and it serves to keep the character of the
functioning continually under observation. When
improperly used and interpreted there is no test
more confusing or misleading. Unfortunately, the
type and arrangement of drop testing machines has
not been standardized. Each manufacturer pursues
his own method of testing and there are many con-
flicting opinions in regard to specifications for sensi-
tiveness.
The object of this paper is to set forth the results
of tests made to determine to what extent the degree
of purity of the antimony sulfide used in the primer
composition effects the sensitiveness of the finished
primers. All other variables such as the granulation,
or grain size of the antimony, were kept constant and
based on the standard practice used by the author
at Frankford Arsenal in the manufacture of the ser-
vice F. A. 88 primer. The sensitiveness test selected
for this investigation was the minimum height of fall
of a 3-oz. weight with firing pin attached that would
just begin to show misfires. The primers under test
were inserted with all necessary precaution in a steel
die. The regular F. A. 88 primer was made the stand-
ard for comparison. The composition of the F. A. 88
primer will not be given in this paper, but it may be
stated that it is of the non-fulminate or burning type
and that it is made so as to contain 17 per cent of
specially grained needle antimony sulfide. The anal-
ysis of the needle antimony has already been given in
Table II and it will be noted that it is not by any
means pure, but contains about 18 per cent of oxide.
The fact that F. A. 88 is a highly efficient and
satisfactory primer under service conditions, proves
conclusively that needle antimony containing about
80 per cent actual Sb2S3 is sufficiently pure for primer
manufacture.
The first question that naturally arose was: What
results would be obtained if the F. A. 88 primer was made
up using pure stibnite in the place of crude needle
antimony? Through the cooperation of the National
Museum, a sample of pure crystalline antimony sul-
fide (stibnite) was made available. The results of
the sensitiveness test were as follows:
F. A. 88 regular
3-oz. weight
100 O. K. at 19.5 in.
100 O. K. at 19.0 in.
97 O. K. 3 misfires at 18.5
Tablk III
F. A
tli pure stibuite
oz. weight
100 O. K. at 19.5 in.
at I'J .0 in.
100 O. K. at 18.5 in.
96 O. K. 4 misfires at 18.0 in.
The above results show that pure stibnite increased
the sensitiveness about 'A in- f°r the 3"oz- weight.
Carefully calibrated indentation tests have shown
that a weak-spring gun with 1.1 -lb. pull corresponds
to a 22-in. drop, so it is shown that the slight increase
382
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 5
in sensitiveness gained by the use of pure stibnite
would not justify the expense of obtaining it on a com-
mercial scale.
first EXPERIMENT — The ballistic proofing of finished
ammunition is the best test of the primer, and there-
fore experimental lots of hand-loaded ammunition
were made up and fired for pressure and velocity in
the usual way. The results of the competitive firings
between F. A. 88 (regular) and F. A. 88 (pure stib-
nite) are as follows:
Table IV
F. A. 88 (Regular) F. A. 88 (Pure Stibnite)
Powder charge in each shot 48.8 grains
Shot Velocity Pressure Shot Velocity Pressure
No. Ft.-Secs. Lbs. No. Ft.-Secs. Lbs.
1 2649 50150 1 2646 48700
2 2660 44850 2 2649 48200
3 2681 49850 3 2646 47750
4 2656 46750 4 2649 48450
5 2646 46350 5 2672 45900
6 2665 46800 6 2651 46650
7 2646 48400 7 2655 46150
8 2656 45750 8 2656 47700
9 2646 46400 9 2632 46650
10 2644 46250 10 2635 47150
Mean 2655
Powder, primers, bullets,
47155
2649
47330
An examination of the above table will convince
anyone familiar with the ballistics of small arms am-
munition that as far as these firings were concerned,
there is nothing to choose as between the primers
made with needle antimony sulfide of about 80 per
cent purity (Sb:S3) and those made with stibnite 100
per cent purity (Sb2S3).
second experiment — Starting with pure 100 per
cent stibnite, it was decided to try the effect of the de-
liberate addition of 18 per cent of soft powdered yel-
low antimonous oxide thoroughly mixed with the
granulated stibnite. It was further decided to make
up another lot with the needle antimony sulfide
which had been purified with tartaric as described in a
previous paragraph. The results of the ballistic tests
are given in Table V and are comparable with those
given in Table IV.
Table V
F. A. 88 — With pure antimony F. A. 88 — With antimony sulfide
sulfide plus 18 per cent SbiOj treated with tartaric acid
Standard powder charge 48.8 grains
HOI
Velocity
Pressure
Shot
Velocity
Pressure
No.
Ft.-Secs.
Lbs.
No.
Ft.-Secs
Lbs.
1
2722
49350
1
2720
46500
2
2714
49350
2
2723
48200
3
2701
46950
3
2694
46400
4
2698
48650
4
2697
47900
S
2689
46050
5
2716
49450
6
2694
48500
6
2626
48500
7
47050
7
.... 2702
47150
8
2709
47900
8
.... 2700
47900
9
2667
47300
9
2697
47050
2694
47550
10
2694
47100
2695
47865
2697
47615
Powder, primers, bullets, cases, O. K.
When we compare the above results with each other
and with the results given in Table IV, there is little
to choose bet wren them. All four scries are ballis-
tically satisfactory. On the drop test, all primers
shot 0. K. at 21 in. I', is very clearly indicated that
ence of 1 8 per cent of antimonous ox
it occurs as a natural impurity or as a deliberate in-
on with pure antimony sulfide, need not be a
source of atu ! manufacture of military primers
good mixture is being used.
THIRD EXPERIMENT— It will be remembered that in
an earlier paragraph of this report a statement was
quoted from Marshall's book on explosives1 to the
effect that sulfides of lead and iron were objectipnable
in cap primer compositions. The statement was not
qualified as relating to the fulminate type exclusively,
and it was felt that a mere statement unsupported by
data was unconvincing. The easiest way to get at
the desired information seemed to be to make up
lots of F. A. 88 primers in which the antimony sulfide
was entirely replaced in one lot by crystalline lead
sulfide (galena) and in another by crystalline iron sul-
fide (pyrite). Fairly pure samples of these two min-
erals were obtained, granulated and sieved to the
standard grain of the antimony sulfide ordinarily
used in the F. A. 88 primer.
The results obtained were somewhat surprising as
the author had thought that the primers would prove
themselves to be defective and show tendencies to be-
ing either too sensitive or not sensitive enough. Why
antimony sulfide was originally selected by explo-
sives chemists as the only possible sulfide for use in
primer compositions and why the impression prevails
that the antimony sulfide used must be of very high
purity is not explained by the results of this investiga-
tion.
Table VI
F. A. 88-
-Made with lead sulfide
F. A.
88 — Made with
iron sulfide
(galena) instead of antimony sulfide
(pyrite
i instead of antimony sulfide
Standard powder
charge 48
8 grains
Shot
Velocity Pressure
Shot
Velocity
Pressure
No.
Ft.-Secs. Lbs
No.
Ft.-Secs
Lbs.
1
2697 46150
1. . .
2696
49050
2
2700 46900
2...
2689
46750
3
2713 48200
3...
2725
48350
4
2715 49200
4. . .
2692
46550
5
2688 47400
5...
2708
49450
6
2723 47500
6...
2703
48050
7
2715 50050
2720
48600
8
2692 46650
8...
2703
46250
9
2697 46650
9...
2694
48700
10
2700 46750
10...
2708
46650
Mean . .
2704 47545
2704
47840
Powder,
primers, bullets, cases, O
. K.
The drop test sensitiveness of the foregoing lots
of primers was satisfactory for the lead sulfide at
21 in. The iron sulfide was a trifle more insensitive
at 22V2 in., whereas 22 in. is the calibration factor
corresponding to the 14-lb. weak-spring gun. As
far as shooting quality is concerned, the iron sulfide
and lead sulfide primers showed up in these tests
slightly superior to the regular F. A. 88 primer. Re-
tests were made in nearly all series of shots given in
the above tables, but as essential checks were obtained
in all cases, for the sake of brevity, only the first ten
shots fired in each series have been tabulated.
In making up all experimental lots, the greatest
care was taken in regard to the granulation of the anti-
mony sulfide and its substitutes. It is well known
that the sensitiveness and stability of primer mix-
tures is affected by the grain of the antimony which
should not be too coarse or too fine. In all the above
described work equal quantities of three sieve sizes
were used. The ground material was passed through
sieves so as to divide in 100- to iso-mesh, 150- to 200-
mesh, and through the 200-mesh. Equal quantities
en weighed and the whole very inti-
mately mixed. These precautions of even graining
should always be carefully followed in carrying on
' Loc at.
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
383
comparative tests on primer mixtures of varying com-
positions.
SUMMARY
This paper has set forth some of the results obtained
in the course of a long and exhaustive research on a
large number of primer compositions and forms of
finished primers. Much of this work is of too confiden-
tial a nature at the present time to justify publica-
tion, but it is believed that the data as given here will
be of benefit to many workers in this field without dis-
closing information that would be harmful.
For some time past there has been some anxiety
felt in regard to adequate supplies of very pure anti-
mony sulfide. This paper should, it seems, serve in
some measure to allay this fear.
CONCLUSIONS
I — The purity of liquated1 "needle antimony"
should be determined from the sulfur content. The
method of basing purity on the antimony content is
shown to be incorrect.
II — The method of purification of "needle" anti-
mony which depends on treatment with tartaric acid
is shown to be unjustifiable, if not actually dangerous.
Ill — The methods for the complete analysis of anti-
mony sulfide are set forth.
IV — "Needle" antimony sulfide of an approximately
80 per cent purity, containing about 18 per cent of
oxide, is shown to be as efficient for the manufacture
of primers as approximately 100 per cent stibnite.
V — Sulfides of lead and iron are shown to work
satisfactorily when substituted for antimony in a
non-fulminate primer.
VI — It is indicated from V that the presence of sul-
fides of lead and iron existing as impurities in anti-
mony sulfide would not be harmful, textbook state-
ments to the contrary notwithstanding.
VII — The conclusion is drawn that in case of defi-
cient supplies of overseas antimony sulfide, domestic
ores would serve every purpose and that other more
abundant minerals might be substituted. Further
investigation as to stability of primers made with other
mineral substitutes for antimony sulfide would be de-
sirable before attempting their use on a large scale.
VIII — The fact that primers made with lead sul-
fide (galena) and iron sulfide (pyrite) showed a higher
velocity for a normal pressure than those obtained
with regular antimony sulfide, is interesting and sug-
gestive but by no means conclusive as a much more
extensive experimental program would have to be
carried out before any definite conclusion could be
reached.
In concluding this paper the author desires to ex-
press his great appreciation of the interested and able
assistance which he obtained in carrying out the ex-
perimental part of this work from Mr. J. K. Miller
and Mr. Sydney N. Greenburg, Explosives Chemists,
employed at Frankford Arsenal.
Philadelphia, Pa.
ADDRL55L5
FOOD CHEMISTRY IN THE SERVICE OF HUMAN
NUTRITION1
By H. C. Sherman
Received March 26, 1918
At the suggestion of your President I propose to speak this
evening of the application of food chemistry to problems of
human nutrition with special reference to the economic aspects
of our present food situation, i. e., to consider how in the light of
our present knowledge we can best combine adequacy of nutri-
tion with economic use of food — remembering, too, that economic
in this connection and at this time should mean not only the
wisest expenditure of money for food from the standpoint of the
consumer, but also such conservation of the food resources of
the entire country as shall enable us to furnish our Allies and our
armies abroad with the largest possible share of those foods which
are adapted to their needs and suitable for exportation.
Briefly and somewhat crudely, the material requisites of an
adequate diet may be summarized under five heads. It must
(i) provide sufficient amounts of digestible organic nutrients to
yield the necessary number of Calories of energy; (2) furnish
proteins in ample amount and of suitable sorts; (3) supply ade
quate amounts and proper proportions of the ash constituents,
salts or inorganic foodstuffs; (4) furnish enough of those as yet
unidentified substances, the food hormones or so-called vit-
amines; (5) it must include a sufficient amount of material of
such physical character as to ensure the proper handling of the
food mass and its residue in the digestive tract.
Since we are here to deal with the chemical rather than physical
aspects, discussion may be limited to the first four of these requi-
sites Logically each of these four categories calls for subdivision.
1 Lecture delivered before the Harvey Society, Academy of M. .lie ln< .
New York City, January 12, 1918.
As sources of energy the carbohydrates, fats, and proteins
function interchangeably to a very large but not to an unlimited
extent. If our understanding of the relation of the energy value
of food to the energy requirement of the body is to be complete we
must study the intermediary metabolism of each of the organic
foodstuffs and its relation to the energy exchange, including the
problem of its specific dynamic action.
Similarly the problem of protein requirement divides itself
into a group of problems having to do with the requirements of
the body for each of 15 or 16 amino acids which constitute the
building stones of the body tissues, and which are less widely
interchangeable than are the energy values of the different food-
stuffs.
The ash or mineral matter comprises at least 10 chemical
elements not contained in simple proteins, fats, and carbohy-
drates and which are not only not interchangeable but are in
some cases actually antagonistic in function Under ordinary
conditions and with our usual ample use of table salt the only
mineral elements requiring special consideration from the stand-
point of adequacy of nutrition are phosphorus, calcium, and
iron.
The vitarnine or hormone value of foods is due to at least two
substances distinguished by McCollum as the Fat-Solubl
the Water-Soluble B.
It cannot be denied that the rapid progress of our knowledge
of nutrition during the past few sreai has tended to complicate
rather than simplify our conceptions of f<""l values and nutritive
requin ments. But while the problem lias become more complex
it also has become clean 1 because we now for the lirst time have
good reas. in to believe that all of the substances needed for normal
nutrition have been recognized and can be reckoned with even
3«4
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No.
though the chemical identification is in some cases not yet com-
plete.
It is most fortunate that the recent progress of research in
nutrition, so largely the work of our own countrymen, has brought
us to this stage in our knowledge of nutritive requirements in
time for us to apply it to the problem (now for the first time really
urgent in this country) of making a more economical use of our
national food resources.
The efficiency with which economy in the use of food and con-
servation of the food supply can be combined with entire ade-
quacy of nutrition is chiefly dependent upon the extent to which
we can state the various essentials of an adequate diet in quanti-
tative terms.
THE QUANTITATIVE STUDY OF THE ENERGY REQUIREMENT baS
been so recently summarized and so fully discussed before this
Society by the very men to whom we are chiefly indebted for its
progress in recent years1'2'3* that to review the subject here would
involve unnecessary repetition. Suffice it to say that all authori-
ties are now in substantial agreement as to the principles of the
energy metabolism and the fundamental facts as to the energy
requirement of the body — particularly of the normal adult. So
well do different investigators agree in their estimates of the
basal metabolism of normal men, that it seems safe not only to
accept their average results as expressing the basal energy re-
quirement with a satisfactory approach to exactness, but also
to tabulate together the measurements made in different labora-
tories upon the energy output under various conditions of work
and rest so as to furnish a table of "hourly factors" from which
the day's energy metabolism and therefore the day's food re-
quirement so far as it is measured in terms of energy may be
computed. Reduced to a common basis of 70 kilograms (154
pounds) of body weight and averaged in round numbers, the
data thus compiled are as follows:
Table I — Hourly Expenditure of Energy by Average Sized Man
[70 Kilograms (154 Pounds) Without Clothing] Under Dif-
ferent Conditions of Activity. (Approximate Averaces Only)
Calories
Sleeping 60-70
Awake, lying still 70-85
Sitting at rest 100
Standing at rest 115
Tailoring 135
Typewriting rapidly 140
bookbinding 170
"I.iKht exercise" (bicycle ergoraeter) 170
Sboemaking 180
Walking slowly (about 2!/i mi. per hr.) 200
Carpentry 240
Metal working 240
Industrial painting 240
"Active exercise" (bicycle ergotneter) 290
Walking actively (about 3V« nii. per hr.) 300
Stoneworking 400
"Severe exercise" (bicycle ergorneter) 450
ing wood 480
Running (about 5'/< mi. per hr ) 500
"Very severe ■ vrgometer) 600
l;or a healthy man or woman of normal physique the energy
'■iit f"i" -( hours can be calculated from the number
of hours spent in each degree of muscular activity, using the
hourly rates of energy expenditure indicated in the table and
reducing or increasing the total according as the body weight is
lessor more than 7" kilograms.
If the degree or intensity of muscular activity is consistently
interpreted, the results thus calculated will be found entirely
consistent with the generally accepted estimates of the food re-
quirements of people oi differing occupations.
The available data on the energy requirements of growing
children vary over a sonicwli.it wider range so that average
figures arc more difficult to give and less accurate to use. Du
Bois has constructed a curve of basal metabolism per square
meter of body surface at different ages, but the condition predi-
* Numbers refer to corresponding numbers in "Bibliography." p. 390.
cated for the measurement of basal metabolism — complete
quiescence on an empty stomach — is so remote from the usual
status of a healthy growing child, that it is necessary to make
large assumptions in arguing from the rate of the basal metab-
olism to the total requirement for a day of normal activity.
Estimates of the energy requirements of healthy children must
therefore allow for considerable individual variations. It is
necessary in making food allowances for individual children to
exercise much judgment as to the activity of the child and also
as to whether he is maintaining not only a normal rate of growth
in weight but also a desirable ratio of height and weight, in other
words a desirable degree of fatness.
Table II — Food Allowances for Healthy Children*
Age
Years
Under 2
2-3
3-4
4-5
5-6
6-7
7-8
s-'J
9-10
10-11
11-12
12-13
13-14
14-15
15-16
16-17
Boys
900-1200
1000-1300
1100-1400
1200-1500
1300-1600
1400-1700
1500-1800
1600-1900
1700-2000
1900-2200
2100-2400
2300-2700
2500-2900
2600-3100
2700-3300
2700-3400
-Calories per Day-
Girls
900-1200
980-1280
1060-1360
1140-1440
1220-1520
1300-1600
1380-1680
1460-1760
1550-1850
1650-1950
1750-2050
1850-2150
1950-2250
2050-2350
2150-2450
2250-2550
Indeed the maintenance of an optimum degree of fatness
(which as Symonds has shown is very near the average of healthy
Americans) is usually the best evidence that the energy value
of the diet is well adjusted to the needs of the individual. "Count-
ing the Calories" in the food eaten is not necessary as a means
of establishing the adequacy of the customary food intake if this
is already established by the obvious condition of nutrition of the
individual concerned — but if there be any question of prescribing
the food — of rationing either an individual or a community —
then adequate energy value of the ration is the first thing which
should be considered, for only when the energy supply is adequate
can the "tissue building" constituents of the body and of the
food be conserved to the best advantage.
the protein requirement has not been so accurately and
conclusively measured as has the energy requirement. Chit-
tenden's well-known investigation of over a decade ago5 remains
the largest single contribution to this subject and the criticisms
evoked at the time by his advocacy of a standard for protein
consumption only a little higher than the rate of catabolism
shown by his observations — corresponding to 44 to 53 g. of pro-
tein per man of 70 kg. per day — are perhaps as suggestive as
any which have been offered. Notable among these criticisms
were Meltzer's argument6 that the usual high rate of protein
consumption constitutes an important factor of safety which it
would be a mistake to forego by reducing the protein content of
the ration to a figure near the minimum requirement, and Bene-
dict's criticism' of the low protein diets as likely to be accom-
panied by a less complete digestive utilization of the non-protein
food. In connection with the latter point it is interesting to
note that Mills" found a better utilization of subcutaneously
injected fat when the experimental animals cats were fed a
high protein diet than when they were fed on low protein or fasted.
Mills suggested that this might he because the high protein diet
furnished more lipase in the body, and Falk and Siguira* found
that their castor bean) lipase preparations were composed
essentially of protein material, as had already been shown in the
case of purified preparations of pancreatic and malt amylases. I0,u
Since the criteria of purity ordinarily used in chemical research
are not applicable to unstable colloidal substances like the di-
gestive enzymes, it is easy to say that such enzyme preparations
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
may be far from pure. It has been suggested that the protein
matter of which these enzyme preparations chiefly consist may
be only an impurity or a "carrier," while the "real enzyme"
is something of wholly unknown chemical nature. There is,
however, no positive evidence in support of this latter suggestion.
On the other hand, there is much evidence which, while not con-
clusive, is direct and positive in character, tending to show that
the common hydrolytic enzymes, such as those concerned in the
utilization of foodstuffs, either are proteins or contain protein
matter as an essential constituent. Probably therefore the food
protein must furnish material for body enzymes as well as for
body tissues.
Table III — Forms of Nitrogen in Protein Materials and Enzyme
Preparations
(Expressed in Percentage of the Total Nitrogen in the Material)
Pan- C astor
Hemo- creatic Malt Bean
Forms of Case- Edes- glo- Amvl- Amyl- Li-
Nitrogen in(o) tin(a) bin(a) Hair(o) ase(a) ase(6) paseW
Arginine N 7.4 27.0 7.7 IS. 3 14.6 14.2 24.7
Histidine N 6.2 5.8 12.7 3.5 6.0 5.4 6.2
Lysine N 10.3 3.9 10.9 5.4 7.4 5.5 4.3
Cystine N 0.2 1.5 ? 6.6 2.5 4.9 3.1
Amino N of Filtrate 55.8 47.5 57.0 47.5 50.4 52.4 49.4
Non-Amino N
of Filtrate 7.1 1.7 2.9 3.1 4.6 4.5
Ammonia N 10.3 10.0 5.2 10.0 8.1 7.9 12.1
Melanine N 1.3 2.0 3.6 7.4 5.3 5.6 3.3
(a) Van Slyke (1910).
(6) Sherman and Gettler (1913).
U) Falk and Siguira (1915).
Both this consideration and the more familiar one that indi-
vidual amino acids furnished by the food proteins may serve
as precursors of body hormones,12'13 naturally tend toward
caution in the acceptance of a low protein standard, especially
since the proteins have been shown to vary widely in their amino
acid make-up and in their nutritive value when fed singly,
especially in experiments upon growing animals.14,16
These differences in nutritive value among proteins, especially
as correlated with chemical structure by Osborne and Mendel,
are of the greatest importance, but we should be careful not to
mistake them as justifying a reactionary attitude or even a need-
less degree of timidity in accepting and applying the results
of experiments upon the amount of protein required for normal
human nutrition. Rather they furnish us the information neces-
sary to enable us to plan economical use of protein wisely and
with confidence.
The best guide to the amount of protein actually needed in
the food of the adult is to be found in the rate of nitrogen out-
put when the intake is restricted to an amount barely sufficient
or not quite sufficient to maintain equilibrium.
The nitrogen output on a diet markedly deficient in protein
and involving a large loss of body nitrogen may be less than the
nitrogen requirement since a large nitrogen loss from the body
might not be convertible to equilibrium by the addition of an
equal amount of food nitrogen to the intake; but where there is
nitrogen equilibrium on a low protein diet it seems safe to con-
clude that such diet is meeting all the demands of the normal
nutrition as far as protein is concerned. Also when the nitrogen
output is only very slightly greater than the intake it seems per-
missible to regard the output as approximating the actual re-
quirement. It might perhaps be argued that even a small loss
of nitrogen from the body might, if long continued, be serious,
possibly on the ground that the extra nitrogen of the output over
that of the intake may conceivably represent the catabolism of
some particular important amino acid which the food docs not
supply in sufficient amount and whose continued loss would be
detrimental. The experimental evidence, however, does not
seem to support such a pessimistic view. In experiments, for
example, in which gelatin is the sole protein we do not find a
merely small loss of body nitrogen which might be mistaken for
approximate equilibrium, but a loss large enough to indicate
plainly that the food protein in such a case is inadequate. Sim-
ilarly in the well-known experiments of Osborne and Mendel in
which rations containing a single protein are fed to experimental
animals, the feeding of zein rations results in prompt and con-
siderable losses of body nitrogen and body weight.
It is therefore very unlikely that a diet which maintains ap-
proximate nitrogen equilibrium is so deficient either in the kind
or amount of protein which it contains as to make it a source of
danger even if long continued. On the contrary, a small negative
balance usually means simply that the body has not yet com-
pleted the adjustment of the rate of output to the rate of intake.
In most such cases it is altogether probable that the continuance
of the low protein diet would soon lead to nitrogen equilibrium
and that in taking the output as a measure of the requirement
we are quite on the side of safety and are probably overestimating
the real protein requirement.
We have therefore thought it worth while to bring together
the data of all experiments of which we found record in which the
dietary conditions and the nitrogen balance were such as to indi-
cate that the output of nitrogen might be reasonably construed
as approximating the actual nutritive requirement. In order
to minimize the personal equation in interpretation, we have
uniformly excluded all experiments showing a loss of nitrogen
greater than 1 gram per day. There remained 86 experiments
upon adults showing no abnormality of digestion or health, in
which the diet was sufficiently well adjusted to the probable re-
quirement and the nitrogen balance showed sufficient approach
to equilibrium to make it appear that the total output of nitrogen
might be taken as an indication of the protein requirement.
These experiments are taken from 20 independent investigations
in which 41 different individuals (37 men and 4 women) served
as subjects. For purposes of comparison the daily output of
total nitrogen in each experiment was calculated to -protein and
this to a basis of 70 kg. of body weight. Reckoned in this
way, the apparent protein requirement as indicated by the data
of individual experiments ranged between the extremes of 20.0
and 79.2 g., averaging 49.2 g. of protein per man of 70 kg. per day.
Thus the average falls well within the range of Chittenden's
estimate of the amount of protein required for normal nutrition
when the energy value of the diet is adequate.
Examination of the data recorded in the original papers indi-
cates that the wide differences in amounts of protein catabolized
in the different experiments cannot in these cases be attributed
primarily to the kind of protein consumed nor to the use of diets
of fuel values widely different from the energy requirements.
Apparently the most influential factor was the extent to which
the subject had become accustomed to a low protein diet.
In view of the fact that individual proteins when fed singly,
especially to growing animals, have shown striking differences in
nutritive efficiency, it may seem strange that in the experiments
hitherto made to determine the protein requirement of man, the
kind of protein fed has not had more influence upon the amount
required. There is, however, no real discrepancy between the
two sets of findings. Experiments like those of Osborne and
Mendel, for example, were for the object of comparing individual
proteins isolated even from the other proteins which always
accompany them in natural or commercial food materials, and
were conducted largely upon rapidly growing young animals in
which there is an active synthesis and retention of protein so
that a deficiency in the supply of any amino acid which ii n
quired in the construction of body protein is apt to be
and plainly reflected in a diminution or cessation of growth.
On the other hand in experiments, the purpose of which is not to
compare proteins but to measure the normal protei 1 1 requi
the diet is naturally made up, not of isolated proteins 01 ev< a ol
single or unusual foods, but (ordinarily at least) ol
tions of staple foods as are believed i" i' prea ul rmal di< t,
so that even a relatively simpli i it 1 . »i 1 arranged f<" the purpos
of such an experiment would probably contain :i numbei <>f 'lit-
386
THE JOURNAL OF INDUSTRIAL AND ENGINEERING ( II EM I ST RY Vol. 10, No. 5
ferent proteins, among which any peculiarities of amino acid make-
up would be apt to offset each other, at least to a considerable
extent. Moreover, the experiments of the group now under dis-
cussion have been made entirely upon adults whose protein re-
quirement was limited to that of maintenance. In such cases
there is no longer a demand for amino acids to be built into new
tissue but only to maintain the equilibrium which already exists
In tween amino acids and proteins in the full grown tissues. Any
of the amino acids whose radicles are contained in tissue proteins
may be expected to contribute something to the maintenance of
such an equilibrium whereas there can be no growth unless all
the necessary amino acids are present. In the protein metabolism
of growing children or nursing mothers the influence of food selec-
tion would probably be much more pronounced — and even in
the case of adult men protein requirement will probably be
found to be considerably influenced by food selection when ex-
periments suitably planned to test the question are carried out.
The inadequacy of gelatine as a sole protein food and its in-
feriority to meat or milk protein when substituted beyond a
certain proportion is well known. A series of experiments, de-
signed to demonstrate differences in nutritive efficiency for man
of the protein supplied by different staple articles of food, was
carried out by Karl Thomas'6 in Rubner's laboratory and the
striking results reported have been widely quoted, often on Rub-
ner's authority. These results, however, have as yet failed of
confirmation, and on some important points have been so directly
refuted by later workers using longer experimental periods, as
to make it appear that Thomas' plan of experimenting and mode
of interpretation were not entirely suited to the solution of the
question at issue.
Thomas thought he had demonstrated that meat protein was
greatly superior to bread or potato protein for the maintenance
of body tissue; but Hindhede17 finds no such difference, being
able to maintain normal nutrition with either bread or potato
nitrogen in relatively small amounts.
Rose and Cooper18 have also demonstrated the high value of
potato nitrogen in the maintenance of nitrogen equilibrium, and
a few experiments in the writer's laboratory19 have tended to con-
firm Hindhede's finding that nitrogen equilibrium may be main-
tained on a relatively low intake of protein in the form of bread.
Of at least equal practical importance are those experiments20
which show the maintenance of nitrogen equilibrium over a long
period on low protein diet in which bread was the chief source of
protein but was supplemented by small amounts of milk.
At a time when compulsory rationing is being seriously dis-
cussed and when we know that in any case economic conditions
are forcing the majority of people to an increased use of the less
expensive foods which may mean that a larger proportion of the
protein consumed is not of the kinds having highest nutritive
efficiency, it becomes important to consider somewhat more
closely the question of the utility of the so-called incomplete pro-
teins in nutrition, and the protein-sparing action of the fats and
carbohydrates which may operate to conserve the protein supply
by diminishing protein catabolism. In order to do this we should,
I think, recognize that protein metabolism is not an affair of
ite processes anabolism and catabolism — ■
but is rather to be conceived as involving a series of reversible
reactions or of approximate equilibria in the body. The tissues
always contain protein and amino acids which in a grown man
arc constantly in approximate equilibrium, represented by
Amino acids <; > Protein.
The suppl) "i amino acids in the tissues is constantly being
augmented bj the digestivi products brought by the blood, and
ime time is constantly being depleted by deaminization.
If amino acids are brought to the cell more rapidly than they are
removed or deaminized, the concentration of amino acids is
d and this must tend to push the above reaction toward
the right, i. e., to check the rate of protein catabolism or to con-
serve the protein of body tissue, and vice versa. Similarly the
intake of ammonia salts under proper conditions may check the
deaminization of amino acids and thus indirectly take part in
the maintenance of nitrogen equilibrium. But ammonia may
also contribute to the actual formation of amino acids in the body
as shown by Embden and Knoop and by Dakin and this probably
furnishes us the best explanation now available of the protein-
sparing action of carbohydrates and fats as illustrated in the
accompanying diagram.
e. g.. Stearin
/ \
Stearic acid Glycerol
CARBOHYDRATE
Glucose
\ I
By /3-oxidation to Glyceric
(finally) carbon aldehyde j
dioxide and \
Amino acids
(among
which)
Alanine
water
Methyl glyoxal
\
Lactic acid ■ t-NH3
/
Pyruvic acid-
\
By oxidation to (finally) carbon
dioxide and water
Since pyruvic acid appears to be regularly formed in the metab-
olism of carbohydrate and of the glyceryl radicle of fats, and
ammonia is always being formed in protein catabolism (by
deaminization of amino acids ), and since the ammonium salts
of a-ketonic acids, such as pyruvic acid, are convertible into
amino acids which are building materials for body protein, we
have here a mechanism by which an intermediary' product of
carbohydrate metabolism (pyruvic acidj takes up a "waste
product" of protein metabolism (ammonia) and turns it back
into protein material again. Thus carbohydrate, in undergoing
metabolism, "spares" protein, not only by serving as fuel so
that protein need not be drawn upon for this purpose, but also
by furnishing material which in combination with ammonia
(.otherwise a waste product can actually be converted in the body
into some of the amino acids of which the body proteins are com-
posed and with which they are in equilibrium. This explains
how an increased intake of carbohydrate, with resulting increase
of pyruvic acid, naturally leads to increased synthesis of amino
acids and thus to a tendency toward protein storage, or, to ex-
press the same thing in somewhat different terms, tends to push
the reaction, Amino acids ( * Protein, toward the right.
According to present theory, most, if not all, of the energy of
the carbohydrate becomes available through oxidation processes
which involve the intermediate production of pyruvic acid, an
1 ketonic acid whose ammonium salt is capable of conversion
into amino acid. Of the fat only the glyceryl radicle (about one-
twentieth of the fuel value is oxidized through pyruvic acid,
while the fatty acid radicles, representing about nineteen-twen-
tieths "f the energy of the fat. arc metabolized through /3-oxida-
tion processes which yield, so far as we know, no product whose
ammonium salt is convertible into amino acid in the body.
Hence, complete withdrawal of carbohydrate, even though sub-
stituted by sufficient fat to yield an equal number of calories,
must be expected to result in increased excretion of nitrogen.
Under war conditions, while we may have to economize in the
use of sugar, there will probably be at least an equivalent pres-
May, 19 18
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
387
sure for economy in the use of fat so that the energy requirement
will tend to be met largely by the use of starchy foods, such as
potatoes, cornmeal, and oatmeal. Hence there should be at
least as high a proportion of carbohydrate in the war diet as in
that of peace and the full protein-sparing effect should be realized.
Now- that we have a chemical explanation of the protein-spar-
ing action of carbohydrates and fats which is based on reactions
which have been definitely demonstrated to take place in the
organism, we see that only a few of the simplest amino acids can
be conceived as synthesized by this mechanism and yet we know
from the results of many feeding experiments that the "sparing
action" of carbohydrates and fats is a large factor in conserving
the protein of the body or of the intake. In harmony with this
we find that "incomplete" proteins, furnishing some but not all
of the amino acids of which body proteins are composed, may still
play a very important part in the protein metabolism of main-
tenance.
McCollum in 191 1-1 called attention to the rather surprising
nutritive efficiency of zein in cases in which only maintenance
was involved, and offered the suggestion that "repair" processes
may not involve the disruption and reconstruction of entire pro-
tein molecules. The same idea may be expressed from a slightly
different point of view by saying that having in the cell under con-
ditions of maintenance an equilibrium, Amino acids < Protein,
between protein and a whole group of amino acids, the catabolism
of protein will be diminished by increasing the concentration
of any (even though not all) of the amino acids into which the
protein molecule tends to be resolved.
Thus food proteins which do not furnish all of the amino acids
needed for the construction of body tissue and which therefore
could not properly be made the chief reliance in the feeding of
growing children or of women during pregnancy or lactation,
may still be depended upon to a very large extent for the ordinary
maintenance of adults.
Nor does it seem necessary to assume that because of the dif-
ferences in nutritive value among proteins, a very large margin
for safety must be allowed above the average amount found in
the 86 experiments cited above This would be true only if the
diets in these experiments had been selected from among materials
whose proteins are of more than average value, which in general
is not the case. In fact in the low protein diets used in these
experiments there was often if not usually a more than average
proportion of bread or other grain protein so that, if anything,
the experiments tend to overstate the amount of protein which
an ordinary mixed diet must furnish in order to cover the require-
ments of normal protein metabolism in the adult. Under these
conditions it seems abundantly liberal to allow when planning
for an economic use of food, a protein "standard" 50 per cent
higher than the average estimate of the actual requirement
(which as already shown is probably an overestimate). Such a
50 per cent margin for safety would lead to a tentative standard
allowance of about 75 g. of protein per man per day. The
requirements of children for protein as well as other tissue-build-
ing material will be considered as proportional to their energy
requirements and therefore much higher per unit of weight than
in the case of adults.
the phosphorus and UAi.cirM rkijuikkmenTS have in the past
been much less studied than the protein requirement, although
in principle they are equally well adapted to investigation by
the method of quantitative comparison of intake and output.
Such experiments as could be found in the literature ha
summarized elsewhere '-- In general it may be said that the re-
sults were not sufficiently numerous or concordant to give us
much confidence in the validity of the average and that as a basis
for general conclusions regarding phosphorus and calcium re-
quirement in human nutrition they were open to the further
criticism of having bi ilmo 1 exclusively upon male
Experiments upon women therefore were plainly
needed, and since the effects of the monthly cycle upon phos-
phorus and calcium metabolism had not been studied, it was
especially desirable that the determination of intake and output
should continue for an entire month without intermission. Four
young women, graduate students and research workers in the
writer's laboratory, have served as subjects in such experiments,
taking diets uniform from day to day for 28 or 30 days, consecu-
tively, with quantitative determinations of intake and output
of nitrogen, phosphorus and calcium balanced in experimental
periods of 3 or 4 days each. Three of the four subjects have each
made two such series of experiments. From the data of all these
experiments there does not appear to be any distinct monthly
cycle in the total quantitative metabolism of either phos-
phorus or calcium; nor was the output of either of these
elements in the menstrual flow large enough to materially
affect the average daily metabolism for the entire month. From
this standpoint the material lost in menstruation is essentially
blood and as such is important to the estimate of the average
daily requirement for iron, but is of very minor consequence
in the phosphorus and calcium metabolism.
The determination of phosphorus and calcium balances in 3-
or 4-day periods for 28 or 30 days without intermission gave
therefore in each case a series of 7 to 10 experiments of unusual
value for the purpose of studying the requirement, since the
diets were so arranged as to furnish the desired numbers of calories
and amounts of protein with quantities of phosphorus and calcium
small enough to test the ability of the body to establish equilib-
rium on the amounts furnished, and to show to how low a level
of phosphorus or of calcium metabolism' the body could adjust
itself.
The minimum requirements thus found, computed, for con-
venience of comparison and application, to a basis of 70 kg. of
body weight, correspond respectively to 0.91, 0.72, 0.83, 0.89 g.
phosphorus and 0.49, 0.38, 0.44 g. calcium "per man per day."
Averaging these results with those of several other experiments
made in this laboratory upon both men and women, and with all
comparable data found in the literature, indicated a mean re-
quirement per 70 kg. of body weight of 0.88 g. phosphorus and 0.45
g. calcium per day.
Considering both the number of experiments contributing to
the average and the range of results in each case, it would seem
that our present knowledge of the quantities required for normal
nutrition is probably about equally accurate as regards protein,
phosphorus, and calcium. This being so, we have as much reason
to set phosphorus and calcium "standards" as to set a "standard"
for protein, and it seems logical to allow as much margin for safety
in the one case as the other. The accompanying table summa-
rizes the data on which these estimates of "requirements" and
"standards" are based and shows also the relative frequency of
American dietaries which fall below the standard or even the
bare minimum requirement in each case.
Table IV — Nutritive Requirements and Actual Intake
"Per Man per Day"
Protein Phosphorus Calcium
Number of experiments 86 87 S3
"Requirement" grams «».««»
pJuiK 20.0-79.2 0.52-1.19 0.27-0.78
Average.'. . .' 49.2 0.88 0.45
"Standard" (50% above "require-
75 grams 1 .32 grams 0 . 68 gram
[mounts in 246 oil
,i 106 grams 1.60. grama 0. #4 gram
Below "Standard" 7 per cent 29 per cent 52 per cent
Requirement" Less than 1
percent 4 percent 16 pi
quirement" it total food
None 2 per cent 12 per cent
It must be stated with all possible emphasis that the words
"requirement" and "standard" are used here only for lack of
better terms and that they have not and cannot have the un-
mal significance which is apt to be attached to them.
McCollum's recent work" emphasizes the fact, which earlier
i t lie metabolism ol calcium and iron,4'»had illustrated,
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 5
that the amount of any one nutrient required will depend to a
considerable extent upon the amounts of other nutrients furnished.
In taking the average of the minima of various investigations as
an estimate of the "requirement" we do not mean that just this
amount will be literally required in each case. The very ex-
periments from which this average is derived are sufficient to
show that the minimum or requirement varies with the subject
and the diet if not with other conditions. Similarly in taking
an amount 50 per cent above the average minimum as a"stand-
ard" it is by no means intended to imply that this amount will be
always the most desirable. On the contrary a larger amount
might easily be advantageous, especially in the case of calcium
as a safeguard against failure of completely normal absorption
in the digestive tract.
Thus the quantitative statements of what are here called "re-
quirement" and tentative "standard" must not be literally in-
terpreted nor rigidly applied. They arc, however, directly
useful as a concrete basis for classifying the results of dietary
studies as to whether they contain liberal or scanty amounts
of the element in question. An intake less than the so-called
requirement does not necessarily mean a continuing deficit leading
finally to disaster in every individual case, but does mean that
there is always this danger wherever such low intakes are habitual.
In individual cases in which intake and output are quantita-
tively determined and the inability of the subject to establish
equilibrium is demonstrated, there can be no doubt that the
intake is inadequate for the subject and conditions of the experi-
ment and such a deficiency with reference to any particular ele-
ment (calcium, for instance) may be established with entire
certainty by the laboratory evidence without awaiting the de-
velopment of any pathological symptoms.
Of the 246 dietary studies here referred to, 144 were originally
recorded by the United States Department of Agriculture and
have recently been subjected to more detailed analysis and com-
putation, especially as regards the mineral elements, in connec-
tion with the investigations upon mineral metabolism at Colum-
bia University; 102 were collected and studied in detail by Miss
Gillett, working under the joint auspices of the University and
the New York Association for Improving the Condition of the
Poor. Nearly all of the latter were from New York City. Of
the 144 government studies, 54 were made in New York City,
46 in other large cities, 44 in small cities or towns and rural regions.
In every group calcium is the element most often deficient and
of which the average intake shows the least margin of safety-
above the bare requirement. It is particularly interesting to
note the agreement of this result with that of McCollum2* who
has found in his studies of laboratory' animals that it is largely
if not chiefly because of insufficient calcium that such animals do
not show normal nutrition on rations derived too largely from
seeds. American dietaries, both urban and rural, tend to con-
sist too largely of the products of seeds (breadstufls, etc.), meats,
sugar and fats, all of which are poor in calcium — and too little
of milk and vegetables which should be used in larger proportion
both for their mineral constituents and for the vitamines which
they furnish.
As might be expected in view of New York City's great size
and the difficulty and expense of bringing in adequate supplies
of perishable foods milk for instance, having to be brought from
7 states and from distances souk times as great as 400 miles or
more — the New York City dietaries show a smaller average
calcium content than those of other cities, while the small towns
and rural regions show the best average.
Most of the New York City dietaries recorded by the United
States Department ol Agriculture were observed in 1 895-1 806;
by the time of the Association for Improving the Condition of the
Poor investigation in 1914-1915 the average calcium content
had improved about 14 per cent Undoubtedly this is chiefly
due to the increased per capita consumption of milk which is
known to have occurred during this 20-year period, and which in
turn is no doubt largely attributable to the good influence of the
public and private agencies which have been working in New York
City for a better understanding of the importance of milk by the
general public, largely due to the efforts of the dietitians, visiting
nurses, and other visitors of the social and relief organizations,
and the teachers of domestic science in the public schools. That
the calcium content of the dietary' is very closely related to the
amount of milk used and that the latter can be influenced by
education are both well illustrated by data of the New York City
investigations which have been presented elsewhere." By
analysis of the data of the 44 dietaries studied in small towns and
rural regions it was found that here also the adequacy of calcium
intake depended chiefly upon the amount of milk consumed,
adequate calcium being found, on the average, only in those
dietaries which contain at least one-third of a quart of milk per
mau per day.
These results indicate very' strongly that the average American
dietary' contains a much more liberal margin of protein than
of either phosphorus or calcium, and that while the danger
of a protein deficiency is rarely serious the danger of a defi-
ciency of phosphorus or calcium is more important. Phosphorus
deficiencies are plainly more frequent than are deficiencies of
protein, and calcium deficiencies are more frequent still. The
old assumption that adequate protein may be taken as meaning
adequate supplies of all tissue-building material is found to be
wholly misleading. Adequate energy intake is, in practice, more
apt to ensure adequacy of mineral elements, but even if all of the
246 dietaries had been brought to a basis of 3,000 Calories per
man per day, 12 per cent of them would still have furnished
less than the average "requirement" of calcium.
the iron requirement is much less definitely known than that
for phosphorus or calcium. From the few experiments^'28 which
now appear trustworthy, it would seem that the actual require-
ment may average about 0.010 g. and the corresponding standard
be placed at 0.015 S- "per man per day." On this basis it would
appear that the danger of a deficient intake of iron on freely
chosen diet is less than in the case of calcium but much greater
than is the danger of a deficiency of protein.
STANDARD ALLOWANCES OF PROTEIN, PHOSPHORUS, CALCIUM
and ikon for children's dietaries — It will of course be under-
stood that in all these statements regarding adequacy of family
dietaries or of food allowances for a family or a community, the
child's requirement for protein, phosphorus, calcium or iron is
reckoned as proportional to his energy requirement and there-
fore as much more than proportional to his weight. Starting
with the food allowances for healthy children already proposed
in terms of Calories it may be convenient to reckon the require-
ments of children or of families containing children as follows:"
Protein 2.5(a) grams per 100 Calories
Phosphorus... 0.048 gram per 100 Calories
Calcium 0.023 gram per 100 Calories
Iron 0. 0005 tram per 100 Calories
(fl)Which should be mainly in the form of milk protein in the dietaries
of growing children.
the "vitamine" requirement cannot be stated in terms of
actual weights of Fat-Solul le A and of YVater-So'.uble B, but
the percentages of certain foods rich in the one or the other of
these essentials which suffice to make an otherwise satisfactory
diet adequate for normal growth and reproduction have been
determined experimentally fot several food materials by Osborne
and Mendel and by McCollum and his associates19 so that we
BOW know in a general way the relative richness of several of the
chief types of food in each of these dietary essentials and can
take account of this factor of food value in considering the prom-
inence which should be given to each type of food in planning an
adequate and economical diet. It is very interesting and im-
portant to find how generally the types of food rich in calcium —
milk ej;;~s. vegetables — are rich in vitamines as well, so that in.
May, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
389
safeguarding against deficiency of the element most likely to be
deficient, we at the same time secure an ample intake of the food
hormones or vitamines.
TO APPLY KNOWLEDGE OF NUTRITIVE REQUIREMENTS IN THE
choice OF food any one of several plans may be followed.
1 — The actual quantity of each essential element could be
calculated for every proposed combination of staple food ma-
terials, but this method would be too cumbersome for general use.
2 — Since in the past it has been customary to treat protein
as the tissue-building material of the food and since we now know
that dietaries containing enough protein do not necessarily con-
tain enough of other building materials such as phosphorus and
calcium we might seek to remedy the situation with a minimum
revision of past habits of thought by so specifying the kind of
protein as well as its amount as to ensure that adequate protein
supply shall really ensure (what we formerly erroneously assumed)
an adequate supply of all essential elements. Thus in specifying
that the protein in the dietaries of growing children shall be
mainly in the form of milk, we ensure not only a good form of
protein but an adequate supply of calcium, of phosphorus, and
of both types of vitamines as well.
3 — Again, since food values are commonly stated in terms of
Calories and the 100-Calorie portion of food is becoming a
more and more familiar unit, it is possible by building up a
dietary of such units and specifying the number to be drawn from
each type of food, to ensure that in covering the energy require-
ment an adequate supply of protein, of each of the inorganic
elements, and of each type of vitamine shall also be supplied.
This is perhaps the most satisfactory procedure in those cases
in which the balancing of the diet is attained by careful planning
of each meal from day to day, and its application has been
greatly facilitated by the publication of the excellent series of
meal plans for which we are indebted to Mrs. Rose.30
4 — Still another method of balancing the dietary and ensuring
an adequate supply of each essential nutrient without undue
expenditure or extravagant consumption in any one direction
is to follow a food budget, or, in other words, apportion the money
expended for food among the different types of food materials.
This plan, while less logical from a scientific standpoint than
those previously mentioned, has the merit of simplicity, of re-
quiring no use of technical terms, and of facilitating comparison
with food statistics which are as apt to be reported in money
value as in weights and measures and in any case are much more
readily reducible to money value than to food value when the
latter is construed as broadly as we now must construe it to cover
all the constituents of food which we know to be essential to
normal nutrition.
food supplies OF American Families — The results of inquiries
by the United States Bureau of Labor Statistics in over two
I thousand families and of very accurate records obtained by the
United States Department of Agriculture and the New York
Association for Improving the Condition of the Poor in over
two hundred households carefully chosen as representative of
different economic groups, are quite consistent in showing that
of the total expenditure for food about one-third is for meats
[ and fish, about one-tenth for milk, one-twentieth for eggs, one-
tenth to one-sixth for breadstuffs and other cereal products,
■bout one sixth for butter and other fats, sugar and other sweets,
about one-sixth for fruit and vegetables, and one-twentieth to
one-tentli for all other foods and food adjuncts. This estimate
of the relative prominence of different types of food is confirmed
by the statistical estimates of the values of annual products of
ood industries of the United States after allowing
for imports and exports.
Are the habits of food consumption which those statistics reveal
the ones which we must consider the best in the light of our pres-
ent knowledge of nutrition? if they are capable ol modifii atioo
for the better, can this lie accomplished in a manner consistent
with our responsibilities in the present world food situation?
I think there is no doubt whatever that the average American
dietary can be modified to meet all the wishes of the Food Ad-
ministration and be materially improved at the same time.
We are asked by the larger use of perishable foods including
such grain products as are more perishable than wheat flour to
"save," or reduce, our consumption of wheat, meat, fats and
sugar. It is in fact precisely because of the free use of meat,
sugar, fat and white flour in American dietaries that so many of
them are deficient in one or more of the mineral elements, par-
ticularly calcium, so that the partial substitution of other foods
for each or any of these four will tend directly to remedy the
commonest defect in the nutritive value of our food.
That the mineral and vitamine content of the average Ameri-
can dietary can and should be improved by the larger use of milk
and vegetables, even if this means a decreased consumption of
meat, is now well recognized by students of nutrition. Because
of the economic limitations under which the food for most families
must be provided, the use of so much as one-fourth to one-third
of the food money for meat practically results in too great a
limitation of the consumption of fruit, vegetables and milk.
Even if there were no war we should teach a lessened use of meat
and sugar in order that more milk, vegetables and fruit may
be purchased and consumed. Since sugars and fats are prac-
tically devoid of inorganic foodstuffs or of water-soluble vitamine,
as well as of protein, a diet in which the use of purified sugars
and fats is reduced and the same number of Calories supplied by
an increased use of other food material, is almost sure to be im-
proved as regards its calcium, iron and phosphorus content as well
as made richer in protein and vitamine.
True, the substitution of other fats for butter may diminish
the intake of "Fat-Soluble A," but if the diet contains as much
of milk and green vegetables as is desirable, this need not be a
cause for anxiety. The saving of meat, sugar, and fats by sub-
stitution of other foods seems therefore to be wholly desirable
from a selfish nutritional, as well as from the ethical and the
national economic standpoint.
The duty placed upon us by the present food emergency, to
eat less meat and more of such perishables as milk, vegetables
and fruit, is therefore precisely what the recent advances in our
knowledge of food and nutrition have shown to be for our best
interest in any case.
It seems a good general rule for families of any level of income
or standard of living (1) to spend at least as much for milk as
for meat, (2) to spend at least as much for vegetables and fruit
as for meats and fish. By redistributing the expenditure of a
typical family of low income reducing the allowance for meat and
increasing those for fruit and vegetables (together) and for milk
so as to make the expenditures for these three items equal, a food
supply much better according to our present knowledge of nutri-
tion could be obtained without any increase in cost.
If it be objected that many people "simply cannot buy"
milk at present prices, it should be said in reply that while every
increase in the cost of milk to consumers is greatly to be regretted
and should be avoided if possible, yet milk at any price which it
has yet reached or is likely to reach is a better investment than
meat. Lusk's admonition to the housewife to "buy three quarts
of milk before buying a pound of meat" is still good advice not-
withstanding the general rise in prices. Any family thai can
afford meat at all can bettei afford milk.
11 may perhaps be asked wheth< 1 we should not use less milk
in order that more in»i lie leiised foi shipment alnoad
Under present conditions it is unlikely that such an attempt
would work out as intended In relativi I cases are city
milk dealers equipped with plants for the production of canned
condensed milk. More generally the market milk business and
the making of canned condensed milk are distinct industries,
usually centered in separate localities and with present difficulties
39°
THE JOURNAL OF INDUSTRIAL AND ENGINEERING ' II l-.MISTRY Vol. 10, No. 5
of transportation and high prices of beef (and of cattle feed)
there is great danger that a diminution of demand for market
milk would lead to slaughter of the cow rather than to her ship-
ment to a distant milk-condensing region.
In general the milk condenseries compete with butter and cheese
factories rather than with city milk dealers so that if we wish to
increase the supply for the condensery we should diminish our
consumption of butter rather than of milk.
We arc asked by the Food Administration both to economize
in the use of meats, sugar and fat, and to consume less wheat.
To the extent that the saving of white wheat flour means an
increased use of the coarser flours and of oatmeal and potatoes
in breadmaking (or potatoes in place of white bread) this also
will result in an improvement in the mineral and vitamine con-
tent of the diet. To the extent that wheat flour is replaced by
cornmeal, we may anticipate no appreciable gain or loss in
nutritive value.
The rat-feeding experiments of McCollum, often continued
for the lifetime of the experimental animal and sometimes through
more than one generation, have shown that the corresponding
products from the different cereal grains are very similar in their
nutritive properties, and preliminary experiments in our own
laboratories, upon the substitution of corn protein for wheat
protein in human nutrition, tend toward the same conclusion.
In these experiments it has been found that nitrogen equilib-
rium can be maintained, and apparently all the requirements
of the protein metabolism fully met, by low protein diets in which
at least four-fifths of the protein is from wheat or wheat and corn
(maize) and that the results are apparently as good when maize
is substituted for a considerable part of the wheat as when wheat
furnished all of the grain protein.
Beginning this discussion with a reference to the material
requisites of an adequate diet we have so far not felt called upon
to specifically discuss psychological aspects, but we have not
forgotten that "aside from all questions of physiological need,
eating has an immense vogue as an amusement." In the present
world food situation we would perhaps be justified in asking that
people regard food primarily as a source of nutrient and only
secondarily of entertainment, since it is possible for us to find
our entertainment in "amusements" which do not involve de-
priving our friends abroad of their daily bread. But particularly
in this very matter of the use of other things than patent flour
in breadmaking we have been so often and emphatically warned
that any change must be considered from the standpoint of
psychology as well as nutrition that it may not be out of place
to ask whether American psychology will be always and alto-
gether on the side of conservatism as against conservation. It
is commonly assumed that our national psychology is and always
will be opposed to any change in the color or flavor of our familiar
white wheat bread. But is this necessarily true? Is there not a
psychology of conviction, of ethics, of patriotic emotion if you
will, as well as a psychology of habit and prejudice? As our
people come to realize more fully and more keenly the needs of
OUT friends abroad, a pure-white, all-wheat loaf may possibly
cease to be regarded as the standard of excellence and desirability
and a bread tasting of corn or tinted by oatmeal may come to
seem a more worthy staff of life.
BIBLIOGRAPHV
I— Lusk: "Science of Nutrition." 3rd Ed., 1917.
m i "Metabolism during Inanition,"
1906-1907, p. 170, and Publications of the Carnegie Insl
3 — DuBois: "The Respiration Calorimeter in
Harvey Lectures for
R <ishingtoH.
Clinical Medicine,"
Harvey Lectures for 1915-1916, p. 101, and papers in the Archives of Internal
Medicine.
4 Gillett: "Food Allowances for Healthy Children," published by
New York Association for Improving the Condition of the Poor.
5 — Chittenden: "Physiological Economy in Nutrition and The
Nutrition of Man."
6 — Mcltzer: "The Factors of Safety in Animal Structure and Animal
Economy," Harvey Lectures for 1906-1907, p. 139.
-Sherman and Schlesinge
Sherman and Gettler:
-Willcock and Hopkins:
-Osborne and Mendel:
7 — Benedict: "The Nutritive Requirement of the Body," American
Journal of Physiology, 16 (1906), 409.
8 — Mills: Archives of Internal Medicine. 7 (191 1), 694.
9 — Falk and Signira: Journal of the American Chemical Society, »T
(1915). 217.
Ibid.. 34 (1912). 1 104. 37 (1915). 1305.
Ibid.. 35 (1913). 179.
Journal of Physiology. 36 (1906), 88.
Journal of Biological Chemistry, 17 0914),
328.
14 — Osborne and Mendel: "Feeding Experiments with Isolated Food
Substances," Publications of Carnegie Institution of Washington, 1911, and
subsequent papers in the Journal of Biological Chemistry.
15 — Mendel: ' Nutrition and Growth," Harvey Lectures for 1914—
1915, p. 101.
16— Thomas: Arehiv fur Anatomic und Physiologic, 1909, p. 219.
17 - Hindhede: Skand Arehiv fur Physiologic, 30, p. 97, 31 (1913-14),
259.
18— Rose and Cooper: Journal of Biological Chemistry, 30 (1917),
201.
19 — Sherman and Osterberg: Unpublished.
20— Sherman and Wheeler: Unpublished.
21 McCollum: American Journal of Physiology. 89 (1911), 215.
22— Sherman. Mettler and Sinclair: U. S. Dept. Agriculture. Butt.
2J7, Office of Experiment Stations; Forbes and Keith: Ohio Agricultural
Experiment Station, Tech. Series, Bull. 6 (1914).
23 — McCollum and Simmonds: Journal of Biological Chemistry,
passim.
24— Von Wendt: Skand. Arehiv fur Physiologic, 17 (1905). 211.
25 — Sherman: Office of Experiment Stations, TJ. S, Dept. Agricul-
ture, Bulletin 18S. p. 37.
26 — McCollum, Simmonds and Pitz: Journal of Biological Chemistry.
27 — Sherman and Gillett: "A Study of the Adequacy and Economy of
Some City Dietaries." published by New York Association for Improving
the Condition of the Poor.
28 — Sherman: "Chemistry of Food and Nutrition." 2nd Ed., 1918.
29 — McCollum: "Supplementary Dietary Relationships Among
Natural Food Materials." Harvey Lectures for 1916—1917.
30 — Rose: "Feeding the Family."
Columbia University
New York City
PERMANENCE AS AN IDEAL OF RESEARCH1
By S. R. Scholes
Truth, beauty, and goodness are accepted as the ideals for-
human endeavor. Of these ideals, truth is the special goal of
the man of science, and he must lead in its discovery and es-
tablishment. And among scientific men, it is the chemist who
must discover the truth about the changes that occur or may be
made to take place in the composition and constitution of material
things.
The outstanding attribute of truth is its eternal character,
it endures, it is permanent. We deny the notions of the early
chemists who held the phlogiston theory, because it did not stand '
the test of time. We call Lavoisier the Father of Modern
Chemistry because his master concept of the quantitative char-
acter of chemii i is endured and become stronger
through the years. Permanent-., is the criterion of ideas, in our
is in any other; but this test should be applied more -
not only to ideas, but to things, to the utilities that
chemistry produces, that justify it to the world.
If right ideas are permanent, so also must be the material
things into which natural resources are made, if they are to be -
worthy of final acceptance Vgainst this ideal of permanence
stands the great natural tendency of all things to disintegrate -
and decay — to pass into a useless state. The action of the ele-
ments, of abrasion and vibration, erosion and corrosion, disinte-
gration ami destruction continually operate to nullify the labors -
of man and to bring to naught His best material achievements.
i \ ample, is the strongest and most adaptable of our
ing materials, but it yields to the action of the atmos-
od eventually falls into useless rust With few except
1 Summary °f Address delivered at the October 1917 meeting of the -
Pittsburgh Section of the American Chemical Society. Reprinted from ,
The Crucible, the monthly of the Section,
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
39i
tions, all our materials follow similar courses, so that the ultimate
triumph of decay is voiced in many a pessimistic proverb.
Here is a challenge to the chemist. How to meet it seems a
problem more worthy of his effort than is the extension of the
number of substances, regardless of their lasting character, or
even the establishment of new laws of chemistry, except as they
have a bearing on the question of permanence : to make steel
in large quantities, not only strong and cheap but resistant to
rust, vibration and other destructive forces; to protect wood
from the attack of air and moisture, of insects and fungi; to make
glues and cements that will last as long as the substances they
bind together; to make dyes that will not fade, and paints and
varnishes that will retain color and protective power; to develop
rubber so that its useful life is years instead of months; to im-
prove clay products, mortars, and Portland cement until they are
indifferent to heat and cold, dryness and moisture; to discover
new treatments for textile fabrics that will greatly increase their
strength, and resistance to wear and the agencies of decay,
and even to fire itself while preserving all their useful character-
istics ; to improve paper so that the printed page may have some
of the lasting qualities of the carven tablets of antiquity; to take
from glass some of its fragility — these are among the aims that
our research must seek, if our science fulfills its highest mission.
In addition to the value of such results merely as ideals, there
would be tremendous economic gains, and, as a corollary, a vast
improvement in the condition of the race. So long as the forces
of ruin hold their present sway over our best and strongest
materials, so long must a large part of the available human
energy be expended in repairing and rebuilding. If such dupli-
cation of effort could be eliminated, not only would the wealth
of the world increase much more rapidly, bringing us more of
the useful things for our enjoyment, but the economic leisure
of all men would be extended, with all the beneficial results
which sociologists can hope from that desideratum.
We are already making progress and considerable research
is now under way as everyone knows, along these lines. Most
of the work remains to be done and the initiative rests with the
chemists who can understand both the necessity and the promise
of research; who have intelligent dissatisfaction with present
achievement and imaginations trained to picture ideal materials
and to plan for their manufacture.
Here in this great manufacturing district, where huge quanti-
ties of engineering materials are made and fabricated, the call
for such research is doubly emphatic. It is not only a call,
but an opportunity to win fame and fortune together with the
deep satisfaction of having rendered real and lasting service.
H. C. Fry Glass Company
Rochester, New York
THE, DEDICATION OF GILMAN HALL, UNIVERSITY OF CALIFORNIA
The University of California celebrated its semicentenary
during the week March 18 to 23, 1918, with an appropriate and
interesting program of events, one of which was the dedication on
Friday, March 22, of a new building for chemistry which as it
now stands is the front wing of the future Chemistry Building
of the University. It was erected at a cost of $220,000; measures
190 by 60 feet; has four floors, a basement and a sub-basement;
and constitutes a departure from the architecture of the new
University in being built of reinforced concrete.
The addresses delivered at the dedication exercises, at which
Professor Edmond O'Neill, of the University of California, pre-
sided, are printed in full below. — [Editor]
INTRODUCTORY ADDRESS
By Edmond O'Neill, Professor of Chemistry. University of California
We meet to-day to dedicate this building. It is called Gilman
Hall, in honor of Daniel Coit Gilman, the first President of the
University, from 1870 to 1874. Under his administration the
University was organized, the Faculty enlarged, and the course
of instruction amplified. Unusual for the administrators of his
day, he believed in the importance of science, and it was through
his efforts that the College of Chemistry was established and the
first laboratory built.
Afterwards, as the first president of Johns Hopkins University,
he had a larger field for his administrative genius, and we all
know the impetus given to science as the result of the establish-
ment of Johns Hopkins, of the eminent leaders of science that
were gathered in its halls, and of the influence of its sons in so
many American universities. For these reasons it is eminently
fitting that this building should commemorate his name, and the
words Gilman Hall will ever serve to bring back his personality
and the services he rendered to this University.
The dedication of a building is like the launching of a ship.
The architect, or the designer, must plan his building, or his ves-
sel, keeping in mind the experience of the past, endeavoring
to correct errors, planning improvements, giving rein to his
imagination to create a new design more beautiful, or more
harmonious, or better fitted for its purpose. And then comes the
period of building when the architect or designer sees his dream
take form, when the artisans fashion the stone and the steel and
the wood, each workman a specialist in his task, each craftsman
doing the work that lies before him, in apparent confusion and
aimlessness. But gradually the structure shapes itself, the casual
onlooker can understand the meaning of the seeming disconnected
efforts, can recognize the outlines of what it is meant to be, and
finally the building or the ship is finished and ready for its pur-
pose.
The launching or the dedication is a gala day, a day of festivi-
ties and celebration. The vessel glides down the ways festooned
with banners and streamers, with the sound of music and the
plaudits of the assembled multitude. The dedications of great
buildings are carried out with pomp and ceremony. Are those
ceremonies and festivities merely in commemoration of the com-
pletion of a great work? Only in part. It seems to me that it
is more a mark of what the future will bring. The ship sails
away to foreign shores, with its passengers and cargo, bearing
new materials and new ideas to other parts of the world and re-
turning with a freight of material and spiritual things for our
enlightenment and betterment; and so it is with this building.
We commemorate its completion, we recall to our mind the labors
and devotion of the architect and advisers and builders of this
beautiful structure. But still more, this dedication is to mark the
promise of the future. Year after year students, instructors and
investigators will work in these laboratories, teaching the ex-
perience of the past, expounding the knowledge of the present,
and unveiling the mysteries of the future. Future generations
will throng this hall; professors and students, mutually helpful,
pioneers in science exploring new fields, attacking new problems,
solving the riddles of the Universe.
To-morrow is the fiftieth birthday of the University, The
founders of the College of California are not here to witness the
development of their little college. I remember as a boy going
to the evening lectures of Professor Carr. the first professor of
chemistry, where he presented the elementary principles of
chemistry, illustrated with experiments. Although it was fifty
years ago, I remember the lectures and experiments as though
they occurred yesterday. It fired my imagination ami
insight into the charm and interest of science Little
did I think then that fifty years later I would assist in the dedica-
tion of a chemical laboratory, many times larger, many times
more costly, than the entire college of those days. Would that
,"
THE JOURNAL OF INDUSTRIAL AND ENGINEERING I HEMISTRY Vol. 10. No.
the men of those times could be present here this week, to see
the great tree that has grown from the little seed they planted
in the sixties.
The development of the Department of Chemistry may be
divided into three periods: the first period from 1870 to 1890,
the second period from 1890 to 1918, and the third period to-day.
The beginning of each of these epochs is marked by the erection
of a new building.
South Hall, the first edifice on the Campus, was to a large
extent devoted to chemistry. The original plan was to build it
entirely of granite, but owing to lack of money the granite was
used only to the first floor, the remainder being of brick. But
the building was good. Only the best material was used. Iron
straps, for bracing and binding, were freely used and the building
has stood the test of time, weather, earthquakes, and use, for
nearly fifty years, and it is as sound and good as it ever was.
The cost, when labor and material were a fraction of what they
are now, was $180,000. The architect was David Farquharson.
The furnishing and equipment were of the highest quality. The
interior furnishings were of California laurel; the laboratory
desks were of black walnut; the hoods were made of plate glass.
Everything was of the very best, and the laboratory when com-
pleted was far superior to any in America and unexcelled by any
in the world. The faculty was small, the students few in number,
but the spirit was fine. Of the chemistry instructors of those
days two have passed away, Professors Rising and Christy.
Professors Stillman and Slate are still with us. Under their
inspiring and enthusiastic leadership, together with the smallness
of the classes, and the lack of distracting avocations and activities,
now unhappily so prevalent, we could devote ourselves to study
and reflection and discussion in a leisurely way which now no
longer is possible. The closeness of association of professor and
student, so often referred to by the old graduates, was the rule.
The small college in the midst of uninhabited fields of Berkeley
had a charm that can never come again.
The University grew, and with it the Department of Chemistry.
In spite of the erection of a number of other buildings, South Hall
became too small for the accommodation of the chemistry stu-
dents and, in 1890, the Regents erected the adjacent Chemistry
Hall, devoted entirely to chemistry. The late Clinton Day,
an alumnus of the College of California, was the architect. The
cost was $62,000. Additions were made from time to time until
the cost as it now stands amounts to about $100,000. This
structure marks the second stage in the development of the Col-
lege of Chemistry.
Just as the building was devoted to chemistry alone, so the
course of instruction in the College was narrowed to specialized
chemistry. In the early days the College of Chemistry served
the purpose of a College of Natural Science, which at that time
did not exist. Students interested in general science enrolled
in the College of Chemistry. The creation of the College of
Natural Science, now merged with the College of Letters, as the
College of Letters and Science, gave the general science student
greater freedom in the choice of his studies, and the Col
Chemistry could devote itself to its more special instruction.
This condition continued until the advent of Professor Lewis
in 191 2, when the graduate and research departments were or-
ganized. The conditions of the seventies were reproduced, the
graduate school taking the place of the early College. The small
numl icr of students, the group of young and enthusiastic instruc-
tors, the close relations in the laboratory and the seminar, serve
as a reminder of the old laboratory in South Hall.
This building, in a material way, brings back recollections of
the seventies. Like South Hall, it has its deep foundations, its
massive wall, its tons of steel reinforcement. It will prove a
monument to the architect, John Galen Howard, and to the
State of California, who, as in 1870, provided the great sum of
money for its erection.
Rut this structure, beautiful and genuine as it is, its varied
and costly equipment, with electric furnaces that will melt plati-
num or granite, its liquid hydrogen plant, by means of which we
will approach the absolute zero, its delicate measuring instru-
ments which will show a variation of 0.00001 degree, will all be
valueless if they are not put to real use. Real use will require
real men. If a company of instructors and students imbued with
the true spirit of research, with genuine love for learning, with
intelligence and will, with enthusiasm and persistence, with
patience and industry, will devote themselves to solving the
secrets of science, the mysteries of nature, then this building will
serve its purpose. I can safely say that within this hall is
gathered such a company, and it is with the confidence of this
knowledge that we assemble here to-day to dedicate this building
to its high purpose of advancing knowledge, to reach a little
further into the unknown, to teach the truth, and to help mankind
in its quest for happiness.
We have spoken of the spirit of the old laboratory in South
Hall, of the fine relations between instructor and student, and
of the charm of the environment. One of the men who exempli-
fied this spirit is with us to-day, John Maxson Stillman, student
in the College of Chemistry, 1 870 to 1 874, Instructor of Chemistry
in the Uriversity of California, 1875 to 1882, later Professor of
Chemistry and Vice President of Stanford University, now Pro-
fessor Emeritus. Dr. Stillman is a most fitting representative
to take part in the dedication of this building. I wish to take
this opportunity of paying a personal tribute to him in the part
he played in the early University. He has been identified with
the development of chemistry in California since the beginning.
His influence as a teacher has been wide-spread and far-reaching.
With respect and affection, I present him to you and will ask him
to tell us something about the early University and what this
dedication means to him.
ADDRESS
By John Maxson Stillman. Professor Emeritus of Chemistry.
Leland Stanford University
Permit me first to express my appreciation of the courtesy
extended to the University I represent and of the honor conferred
upon me by the authorities of the University of California, in
inviting me to participate in the dedication of this new and
splendid temple to Chemical Science
As a representative of the Department of Chemistry of Stan-
ford University, 1 take pleasure in extending to the University
of California and to our friends and colleagues of the Department
of Chemistry our heart-felt congratulations upon this important
addition to the equipment and therefore to the efficiency of chem-
ical training in the University.
I voice the sentiments of my colleagues of Stanford in express-
ing our hope and confidence in an ever-increasing development
and an ever-widening influence of this department upon the
growth of chemical science in America.
It is, however, not only as a representative of a sister institu-
tion that I am deeply interested in the occasion which brings us
together here. When, forty-live years ago, the University first
established itself at Berkeley, laboratory instruction in chemistry
was first systematically undertaken, anditwasmy valued privilege,
as assistant, and later as instructor, to have participated in the
work of the pioneer period of this Department of Chemistry.
It is not an easy matter to span this gulf of years with full
realization of the different conditions prevailing then and now
— conditions affecting not merely the facilities of this University
for the teaching of chemistry, but the relations of chemical
education to public demand and appreciation. Indeed, it is
difficult to now realize the great difference in the relations of
university ideals in general to the popular comprehension which
underlies public support, as they obtained then as they now exist.
May, 191S
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
393
The last published catalogue of the University shows a student
body in the Colleges at Berkeley numbering 6780 students. In
the first year at Berkeley the total registration was 191.
The latest register shows a teaching force in the Chemistry
■ Department of eight professors, one lecturer, five instructors,
and fourteen assistants, or thirty altogether. In 1873 to 1874
there was but a single professor, Professor Willard B. Rising,
who came to the work fresh from several years' training in the
best laboratories of the old world and who brought with him
methods and ideals of chemical training abreast of the time. He
was assisted that first year by but three undergraduate assistants,
seniors in the College of Chemistry. While the spacious labora-
tories of chemistry have been in recent years continuously over-
crowded by their almost thousands of workers, the two modest
laboratory rooms in old South Hall were in those early years never
overcrowded by their few dozens of students.
And these comparative figures are indicative of, and to a great
extent a measure of, the changes that have taken place in the
public appreciation of the value of university ideals, and of the
importance of chemistry to the public welfare.
The career of the chemist in those days offered few inducements
and little of promise. The Pacific Coast in particular still lingered
in the epoch of exploitation of its rich natural resources in gold
and silver, grain, cattle, and timber. The occupation of chemist
meant to the general public little more than that of assayer of
gold and silver, or pharmacist. Outside of mining, the chemical
industries were few and were conducted primitively and on tra-
ditionally established lines. Indeed, the chemical industries
of the whole United States were largely contented to depend upon
the scientific and technical achievements of Europe.
Those were years of sacrifice and of many trials for the little
band of teachers with advanced concepts of university education
and for their relatively few but very earnest supporters in Cali-
fornia. Isolated by distance from sympathetic co-workers in
the Eastern States, struggling against public apathy, and battling
against attempts to obstruct their aims or to divert from the
young University its needed financial support, their disappoint-
ments were frequent and their discouragements many.
So much the greater honor to those who nevertheless against
Jail opposition kept the course of the University ever steadily
onward toward the highest ideals, until such time as the people
of California, recognizing at last the value of the service rendered,
rallied loyally and generously to its support.
A great leader of those who formulated and fought for high
university standards was he who from 1872 to 1875 held the office
of President of the University, Daniel C. Gilman. Though but
1 for three years he was with us, those were critical years. The
Organization of Johns Hopkins University, the unique position
it very soon commanded among American universities and the
hrestige it so long maintained are the lasting monuments to the
high ideals and the organizing ability of President Gilman. And
if not so conspicuously, no less effectively, was his influence exerted
in the infancy of the University of California.
The clear judgment, the sound ideals of scholarship, and the
friendly encouragement of President Gilman awakened and nour-
ished the ambitions of many of the students of those early years
to persevere in attaining the most thorough training obtainable
'for the educational career, when conditions generally were dis-
heartening to such aspirations.
And so it appeals to me as very appropriate that this new labora-
tory, devoted to the extension of chemical knowledge, should bear
the name of Gilman, our pioneer leader, whose far seeing vision,
and whose wise initiative laid broad and deep the foundations
upon which, under enlightened leadership, the splendid super-
structure of our State Universitj I ted.
I have a letter from President Gilman written forty years ago
which will not be without interest to-day.
Baltimore, February 16, 1878
My dear Stillman:
There are no letters (except family letters) which give me
so much pleasure as those I receive from California, and within
a few days I have been favored with excellent varieties of the
species, from your pen and Mr. Stearns'. My last previous
letter was from Prof. Rising I have had many printed
papers referring to the progress of the University of California,
including the notes of Mr. Bacon's proposed gift, the Report of
the Regents, the lectures of Prof. Becker, etc. In all these signs
of growth and progress I rejoice with all my heart. I have always
believed that the good forces in California would overcome the
bad elements, and that we should see a university on the Berkeley
slopes, strong and sound, helping on all the interests, social,
industrial, political, literary and scientific. It is a great pleasure
to me to see on the Register, which has also come lately to hand,
the names of former students enrolled among the instructors.
The faculty of a college, as it seems to me, should be in part com-
posed of alumni of the institution and in part from men trained
elsewhere. The former know the situation — its good points
and bad, they love their Alma Mater and are quick to defend and
advance her interests. The latter bring in good ideas from other
institutions and prevent the concern from moving in too firm a
routine. As I write, your name and Jackson's and Christy's,
and Slate's, and Rowell's and Parkers' and Hinton's and ever so
many more occur to me as those on whom the University might
well rely. Royce would be a great addition to your company.
He has certainly a very remarkable mind and is I think likely to
become a man of great distinction Give my kind re-
gards to all your comrades and believe me ever your friend.
Sincerely,
D. C. Gilman
It is at a momentous time in our national history that Gilman
Hall is opened for research and instruction. But it is also an
auspicious time. For do we not all see now, as we have never
seen before, that America must never again be satisfied to be
dependent upon any other nation for the vital necessities of
national life, either in her industries or in the scientific knowledge
upon which these are founded ? Yet it is in the chemical field that
in the past our unpreparedness has been most flagrant. The
many serious problems, which in this time of war are tasking to
the utmost the chemical skill and science in this country, are not
more serious and not more numerous than those which will call
upon chemical science in the strenuous years to follow, when
peace shall some time come to this war-torn world.
May Gilman Hall, under direction of its wise faculty and with
the loyal support of the people of California, contribute in gen-
erous measure to the solution of the future problems confronting
the chemists of America. For the American people are at
last fully aware that the security and the prosperity of this nation
is dependent in no small measure upon the self-dependent charac-
ter of its chemical science and chemical industries.
Professor O'Neill then introduced the next speaker as follows:
Dr. Stillman represents the old University. Since his time a
new generation has come into the field to carry on the work. We
older men must lay down our burden to be taken up by the
younger ones.
Dr. Lionel H. Duschak is a fitting representative of this younger
group. A graduate of Michigan and Princeton, Superintendent
of the Berkeley Division of the Bureau of Mines, a specialist in
physical chemistry, he will serve in the ranks of chemists and
carry forward the banner of the scientist. For a long period yet
to come, he and his contemporaries will see the uses to which this
building "ill be put, will watch the work that will be done in it,
and will make use of the results and discoveries made in this
laboratory. As a representative of the younger generation of
chemists, 1 present Dr. Duschak.
ADDRESS
By Lionbl Hbrman Duschak, Superintendent, Berkeley Station,
U. S. Hureau of
As a representative of the younger men who are engaged in
chemical work, I deeply appreciate the honor of being invited
to participate in the dedication of Gilman Hall. We have
194
THE JOURNAL OF INDUSTRIAL AND ENGINEERING ( HEMISTRY Vol. io, No. 5
watched with a real interest the recent growth and progress of
the Chemical Department of this University and note with
gratification that its needs for better facilities have been met by
this excellent new building. May I extend to the University
and the Chemical Department our congratulations on the event
which gives rise to this ceremony?
It will occur to all of us that this occasion is one of particular
significance to our part of the chemical world. Standing as a
permanent addition to the chemical group, Gilman Hall is a
milestone marking an important step in the development of the
chemical work of the University. I wish to indicate by a few-
words what this development may mean to us. The underlying
thought which I wish to convey to you is suggested by consider-
ing for a moment the relation of this University in its entirety
to the commonwealth. I shall not attempt to define this, but
wish only to call your attention to certain facts which have im-
pressed me. As a part of this University we find colleges of
mining and agriculture, which in many States form separate,
and all too frequently, competing institutions. We find courses
in music, in commercial education and in other branches which
are frequently offered only in special schools. We observe a
quick response on the part of the University to growing popular
interest in any new line of endeavor. This is not to be inter-
preted in any sense as a concession to faddishness, but rather
as an evidence of virility, of alertness, of a desire to assist in
realizing the greatest good from each new activity by giving it
the benefit of the scientific study and technical direction available
in the great University workshop. This University has main-
tained to an unusual degree a close and helpful contact with the
complex and ever-changing activities of the life about it.
May we not take it for granted then that this splendid new-
building will be used by the Chemical Department for correspond-
ing efforts in its own particular field; that the increasing chemical
activity within the University implies a corresponding increase
in the helpful influence which will emanate from this center to
the broad and varied fields of chemical activity without?
Research in so-called pure science has been aptly referred to
as the foundation upon which all scientific work rests. One
should not think of this foundation, however, as a mass of con-
crete lying cold and inert in the earth, but rather as the trunk of
a great tree, which is constantly pushing forth its roots into new
and impenetrated earth, tapping new sources of vital energy.
We shall expect first of all then that the activities in this new
building will supply leadership in the field of theoretical chem-
istry, a field in which this Department already occupies a prom-
inent place. This leadership will come in part from the trained
men continually going out from the University.
Consideration of the practical value of a theoretical advance
is rarely, if ever, the compelling motive of the investigator.
He has a less material vision before him. To-day, however, no
one regards it as a degradation of science that such practical
application should be made. It is an interesting fact that some
of the recent and highly fundamental theories and conception
of physical science have received direct practical application.
As an example, the new type of X-ray apparatus developed at
the research laboratory of the General Electric Company may
be cited. In fact, chemistry would enjoy but a restricted exist-
ence and would probably suffer decay were it not making its
rich and varied contributions to the daily needs of the world.
The ideal and the material must go hand in hand, and in this
new building, which is being dedicated to-day, there is abundant
evidence that both aspects of chemistry will be given due atten-
tion. The variety and extent of the material resources of the
Pacific Coast are more or less well known. Their utilization
has only just begun. In unlocking the great storehouses of this
region the chemical pioneers will look to the University for assis-
tance in many ways. In this connection it is well to remember
that as we pass from experimental work for a theoretical purpose
to that with material ends in view, we usually approach opera-
tions of an extremely simple character. The basic principles
will be obvious and well understood and the technician's skill is
more particularly required in detecting and controlling what
may superficially appear to be details of small importance. The
solution of a seemingly minor problem may bring major
results.
Members of the Chemical Department will be proud to recall
later on that much of the equipment for experimental work of a
more practical character was first used in the study of problems
having to do with the utilization of local materials in meeting
the needs of our country in the present great conflict.
The relation of chemical work within the University and that
without should not be one-sided. We on our part wish to stand
in the most friendly and helpful relationship to the Department,
to assist where possible, to the end that it may achieve the largest
measure of usefulness. With the idea of friendly cooperation
and mutual helpfulness in mind, the dedication of this new and
splendidly equipped building has an almost individual significance
to each one of us.
In the years to come there will grow up about Gilman H
rich memories like those which now enshroud its older com'
pardons. In this new era just beginning the Chemical Depart-
ment will continue true to its early ideals and traditions and will
carry forward the standards so splendidly maintained throughout
the past.
CURRENT INDUSTRIAL NLW5
MACHINERY FOR FRANCE
Shortage of labor has shown that modern methods of bread-
making are comparatively little employed in France, in spite
of the country being one of the largest consumers of bread in
the world. Even in tin big cities the ancient and unhygienic
method of hand kneading is still adopted. It is now urged
that mechanical breadmaking is essential, seeing that a reduction
of 50 per cent in the labor employed could be effected thereby.
In certain quart' 'li.it the French Government
should do what has been don« by certain Smith African Govern-
, forbid bakers to carrj on except by machinery, and
it is suggested that establishments turning out bread on a large
- nl aftei the war in a similar
way to the smaller baker who would thus lie transformed into
a tradesman merelj lot tin sale of the article. There should,
then, lie a good market open to manufacturers of breadmaking
machinery. A. McMn 1 \\
EXPORTS FROM GOLD COAST
During the years 1915 and 19 16 the exports of nuts and oil from]
the Gold Coast were as follows:
1915 1916
Quantity Value Quantity Value
KolaNuts 8,677, lOOlbs. $196,815 6,760,898 lbs. $652,8301
Copra 770 tons >t>4,105 633 tons ? "1.9:0
I'.ilin Nuts 4,064 tons 5_\S2,560 5.857 tons $429.4951
Palm Oil 330,990Kals. $128,845 450.360gals. $191.4951
The decrease in kola nuts is probably due solely to the difficulty!
of getting the product shipped to its principal market, Nigeria.]!
A record total value for copra was reached in 1916. Considerable!
progress has been made by companies engaged in developing the
palm oil trade and their activities give promise of a revival
the industry. The increase in palm kernels and palm oil cor-j
responds approximately to the decrease that occurred in 1915I
and is due to the stimulus given by the increased price and de
nian.l in Buropi
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
395
ENGLISH POTTERY INDUSTRY
According to the Chemical Trade Journal, 62 (1918), 32, the
output in the North Staffordshire pottery industry was consider-
ably reduced last year, owing to depletion of staffs and difficulty
in obtaining raw materials, some of which are now costly. The
English potters have had the home and oversea markets largely
to themselves and selling prices have shown considerable in-
crease. Greatly augmented business has been opened up in South
America. It is thought that the china-clay combine in Corn-
wall and Devon must lead to more expensive china. Manufac-
turers have been notified of an advance of 33 V3 per cent. Im-
portant research work has been done and is proceeding at the
Stoke Pottery School. It is stated that experiments to manu-
facture hard paste porcelain from English materials to compete
with the German hard paste porcelain, hitherto a great rival to
English pottery, have reached a practical stage and bodies
have been prepared and supplied to manufacturers in order
that the latter may experiment in making this class of china. — M.
SOAP DEMAND IN MOROCCO
A report published recently in the Bo/etin de la Cdmaras de
Comercio (Madrid) calls attention to the favorable opportunity,
which to-day presents itself, for the supply of soap to the
Spanish Moroccan market provided an effort is made to suit
customers' demands. The kind mostly asked for is blue and
white mottled soap packed in cases containing 64 bars, each
weighing 780 g. Although the price in normal times was $5
per case, a case is now obtained with difficulty for $14. The
annual consumption of soap in Spanish Morocco is some 2,500
to 3,000 metric tons. There is also a good demand for stearine
candles in cases containing 100 packets (of from one to twelve
candles) each weighing 287 g. A case at present brings $13 to
#14.— M.
FERRO-CONCRETE SHIPBUILDING
A company, says Engineering, 105 (1918), 65, has been formed
in Denmark for carrying on the Alfsen method of ferro-concrete
shipbuilding. Suitable sites have been secured on the Limfjord,
at Norre Sundby, and close to the Cooperative Cement Works.
The undertaking will be started on a fairly comprehensive
scale and under satisfactory auspices, and it is the intention
to build not only lighters but sea-going vessels up to 1000 tons
dead weight. Mr. Alfsen is a member of the Board. The
Alfsen method will also be adopted by a company, with a capital
of $275,000, which is constructing a yard at Arendal on Tromoen
especially laid out for the building of ferro-concrete vessels of
looo tons dead weight. A company in Sweden has been formed
for building vessels of the same class, and the original Alfsen
I yard in Norway, the Porsgrund Cement Works, is about to
increase its capital by some $195,000.' — M.
RAILWAY MATERIAL FOR JAPAN
Japan, says the Times Trade Supplement, will be one of the
countries eager to import railway material of all descriptions
after the war, as it is extremely unlikely that the several de-
velopments of this nature contemplated in that country can be
PUTJed out with locally manufactured supplies. The proposal
for the construction of a light underground electric railway at
Tokyo has been discussed again, the overcrowding in the Tokyo
tramways having called attention to its desirability. The
Scheme is preferred to the establishment of an omnibus service
by reason of the narrow streets. A line, <i mil. in length, is
proposed, but it is recognized that it will take 5 yrs. before such
a system is completed. There has also been a revival of the
scheme for increasing the gauge of the Japanese government
railways. — M.
GRAPHITE FOR BOILER SCALE
A very finely powdered graphite, says the British Clay Worker,
placed in a boiler immediately after it has been cleaned circu-
lates with the water and rubs against the steel to which it im-
parts a graphite polish on which scale does not readily form.
When the initial quantity is regularly followed up by smaller
ones, the graphite by mechanical motion gradually softens and
disintegrates any old scale that may still be present and, if new
scale thereafter forms, and it always will to some extent, it forms
with that scale so that all may be easily broken up and re-
moved. Inferior grades cannot with safety be allowed in steam
boilers. — M.
SWEDISH GAUGES
It is stated in Machinery, n, 470, that bar gauges of the
Johansen type are already being made by the Pitter Venti-
lating and Engineering Company, Woolwich, England. The
bars can be made to an accuracy of ±0.00001 by female labor
on special lapping machines at a high rate of production. It is
of interest to mention that the first set tested by the National
Physical Laboratory, London, was satisfactory in flatness,
parallelism and hardness and "wringing," and that 33 per
cent showed no appreciable error in dimensions. — M.
SOUTH AFRICAN IRON ORE
The Mining World, 94 (1918), 180, states that considerable
deposits of iron ore have been located in Ermelo district. It is
said to be of great purity, assays of nearly 70 per cent having
been obtained. A large tonnage is being made ready for trans-
port to Vereeniging where it will be tested by the Union Steel
Corporation. If the results are satisfactory it will be possible
to get the necessary machinery required for the erection of an
up-to-date steel producer plant which will render South Africa
largely independent of outside supplies. So far the Steel Cor-
poration has principally smelted scrap and imported pig iron,
but the existence of a large quantity of good iron ore with an
ample supply of the necessary flux in the neighborhood should
lead to the Union producing all the steel required by the colony
and perhaps other parts of Africa. — M.
SOUTH AFRICAN DIAMONDS
From a report the total output of diamonds from the diamond
mines in South Africa for the year 1916 was 1,403,514 carats
valued at $16,966,555. This total is exclusive of the result
of debris washing which accounts for 8,362 carats valued at
$51,705- The average value of the diamonds produced by
the mines during the year was $9.60. Taking the average
price realized per carat for the first quarter of the year against
that realized in the last, we find an increase from $8 to about
$11 — a rise of almost 40 per cent. That the average price
per carat of both mine and alluvial stones in 1916 was the highest
since Union, is a striking fact, says the report, bearing con-
clusive testimony to the success of the sound policy of con-
trol exercised during the disturbing influences of the war. With
regard to the alluvial diggings, the report of the Cape inspector
shows that the output for 1916 was 98,879.75 carats of tin- vuhie
$3,271,380. The great increase over 1915 is apparent when it
is stated that the previous year's production was 61,933.25
carats valued at $1,296,060. The average price realized for
the alluvial product for the year 1916 was $31.80 again I
for 1915. The 1916 average transcends all records, al least
for recent years, the highest figure having been $29 in [912.
Taking the last quarter of 1916 by itself, the average price
realized was no less than $30. In view of the above liKiuis,
the year has been one of extraordinary prosperity in the digging
generally. — M.
396
THE JOURNAL OF INDUSTRIAL AND ENGINEERING ( II I:\I1STRY Vol. 10, No. ;
SHORTAGE OF ELECTRICAL APPLIANCES
According to the South African Mining Journal, electrical
materials are becoming very scarce in Johannesburg. The prices
of key-sockets and switches have sharply advanced of late.
Lamps coming on the market are quickly absorbed and all kinds
of cable material are particularly difficult to obtain. On the
other hand, the demand for motors has fallen off somewhat as
the municipality is not in a position to supply newcomers. — M.
MARGARINE INDUSTRY IN HOLLAND
The 1916 Yearbook of the Chamber of Commerce at Rotterdam
states that 30,000 metric tons of animal and vegetable mar-
garine are consumed every year in Holland and that the ratio
of export is normally five times that of consumption, or 150,000
tons out of a production of 180,000 tons, 1916. Practically
all vegetable and animal fats can be used in making margarine.
The principal fats are: vegetable — cottonseed, peanut, sesame,
soya bean, palm kernel, rapeseed, linseed, Kapok seed and
copra; animal — oleo oil, oleo stock, tallow, neutral lard, imi-
tation neutral lard, butter and milk. Salt water is always
mixed with the various ingredients. Deodorizing machinery
has been developed in Germany and Holland to an extraordi-
nary degree so that many oils and fats of no use elsewhere
can be introduced without harm. There are about 30 principal
margarine manufacturers in Holland but, of these, several
have recently been bought up by Jurgens Margarine-fabriken
Oss with headquarters in North Brabant. — M.
ELECTROLYTIC ZINC
News from Australia states that the electrolytic plant now
established at Risden, Tasmania, has proved the possibility
of the application of the electrolytic process to Australian ores
and concentrates for the production of zinc. The chairman
of the Electrolytic Zinc Company states that the present plant
has a capacity of 15 tons per day which can be increased ten-
fold. Competition between the technologists of the Risden
electrolytic process and the Port P'rie retort furnacing process
has already produced metallurgical improvements. Leading
members of the staff believe that, with the new conditions,
they will beat the results already obtained from the older pro-
cess. The outcome of these operations will, it is said, vitally
affect the Empire's zinc industry. — M.
TRADE DEVELOPMENTS IN SWEDEN
The British Attache at Stockholm reports that two im-
portant chemical factories have been amalgamated in a new
company which has been established at Stockholm for the manu-
facture of aniline dyes and drugs. Negotiations are said to be
proceeding for the purchase of or cooperation with other Swedish
companies. The capital of the new company has been fixed
at about $3,000,000. Other industries and inventions which
are projected or are being developed in Sweden at the present
time include the following: the manufacture of train oil from
fish liver, and fish meal from fish waste; the establishment
by the Swedish Government of a whale industry for state ac-
count; the production of fats and oils from coast animal sub-
stances and the exploitation of a recently discovered method
of making aluminum from clay deposits. Electrolytic copper,
as well as nickel and cobalt are to be produced by a new Swedish
firm whose works are to be erected at Vasterus. It is also
reported that preparations are being made to establish an
oil industry to utilize Swedish deposits, and experiment^ an
said to have yielded very promising results. Some large financial
groups are interested in this enterprise. — M.
RUBBER INDUSTRY IN JAPAN
It is stated in the Board of Trade Journal that two well-known
firms, one American and the other Japanese, have established
a joint company in Yokohama for the manufacture and sale
of rubber goods in Japan as well as in the Far Eastern countries.
The Japan company, it is reported, owns rubber plantations
in the Federated Malay States. The new company will have
capital of about $1, 250,000 and plans are already in hand for
the erection of a four-storied factory building on the Yokohama
site which has been acquired. At the outset, the general run
of mining and industrial goods will be manufactured, as such a
line represents the largest volume of business in Japan at the
present time. The saving effected by manufacturing goods in
Japan itself is estimated at 30 per cent on landed goods. Later
on, the company intends to manufacture motor-car, ricksha
and cycle tires, specially compounded to withstand road con-
ditions in Japan. In addition, rubber boots and shoes, rain-
proof materials; vulcanite for battery jars, telephone switch-
boards, fountain pens, etc.; also druggists' sundries, surgical
instruments and sporting requisites. American experts will
supervise the production of the goods and the company's patents
and processes are to be utilized in the Japanese works. — M.
SORGHUM AND PAPER
The French chemist, Andre Piedalla, has presented to the
Paris Academy of Agriculture, a report showing the marvelous
utility of this grass, which according to minute researches made
by him supplies sugar, fodder, paper, dyes for textiles, and flour.
The grass is indigenous to equatorial Africa and thence was
carried to Egypt, India and China. In the fifteenth century,
it was found growing in Italy, in Genoese and Venetian territory.
In 1850 it was recommended to agriculturists in France but,
at that time, it was not considered of sufficient value to interest
cultivators. The Temps recently devoted a lengthy article to
this once despised grass. Its yield of sugar is very considerable
in appropriate climates; thus in China it yields 0.7 ton per acre.
The fibers, rich in cellulose, yield 2 tons paper pulp per acre and
Mr. Piedalla has produced from the pulp a superb paper of daz-
zling whiteness. In addition, the leaves serve admirably as fod-
der, the roots are useful for the production of alcohol and the
seeds supply starch, nitrates and fatty matter that give a grayish
flour of good taste, easily mixable with the usual breadstuffs.
and it is enveloped in gluten which furnishes excellent coloring
matters. As regards paper pulp, says the Paper Maker, it can
be said that experiments dealing only with the utilization of
sorghum date from many years back and seem to have given
excellent results. The employment of sorghum for this purpose,
however, seems to have made no progress and this, seemingly,
for reasons independent of its value as a pulp-producing com-
modity.— M.
COLLOIDAL NICKEL
Suspensions of colloidal nickel can be prepared in various ways.
From the oxides and certain salts nickel is reduced to the dry
state by hydrogen at 2000 C. In a recent paper in the BerichU
d. deulschen client. Gesellschaft, C. Kelber states that he tried
this reduction by hydrogen in solutions. He dissolved nickel
formate together with gelatine in glycerine, heated the solution
to 200 or 210° C. and passed a current of hydrogen through this
solution The latter assumed a brownish color which did not
turn turbid when exposed to the atmosphere and could be mixed
with alcohol. Water precipitated a chestnut-brown colloid
which, when purified in the centrifugal apparatus and dried at
ordinary temperature, gave a colloidal nickel soluble in acidulated
water, dilute acetic acid, glycerine, and alcohol — M.
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
397
JAPANESE INDUSTRIAL DEVELOPMENTS
The chemical industry has made wonderful advances in Japan
since the outbreak of war. According to the Chemical Trade
Journal, 62 (1918), 134, no less than twenty new companies
are said to have been formed with a capital of $15,025,000, and
twenty-eight factories are under their control. Among their
chief products are ammonium sulfate, potassium chlorate, sodium
peroxide, iodine, fatty and stearic acids, caustic soda, bleaching
powder, potassium sulfate, potassium carbonate, sulfide of sodium,
chloride of sodium, nitric acid, glycerine, oils, dyes, drugs,
fertilizers, disinfectants, and phosphorus. Large stocks of
potassium chlorate are on the market and the price has accord-
ingly fallen. One company is producing indirect dyes for domestic
needs exclusively, while direct dyes are being produced for the
export trade. Another company claims to have produced ultra-
marine equal to that formerly obtained from Germany. For
the manufacture of paints, three new companies have been formed
with capital of $450,000. Their chief products are zinc and house
paints, paints for ships' bottoms, antiseptic paints, rust-preventing
paints and paint-substitutes. Six companies have been estab-
lished with a capital of $8,250,000 for the production and refining
of mineral oils. Fish grease is to be used for the manufacture
of soap and glycerine by a recently formed company, while
crude sulfur from a recently exploited mine is being refined by
a special process. — M.
MINERAL DEPOSITS IN MALAY STATES
Mining engineers, who have recently visited the southern
Siamese Malay States, have come to the conclusion that one of
the richest mineral areas in the world is to be found there. In
addition to wolfram, rich deposits of tin alluvium are found in
the valleys and gullies of all the hills in which wolfram has been
found. According to Eastern Engineering, in most of the hills
the number of wolfram lodes already located exceeds ten and
in all of them tin has also been found. Plenty of water with
sufficient head is said to be available for washing out the tin in
the rainy season and there are possibilities for storing water in
reservoirs for the dry season. There is a waterfall close by with
sufficient head to develop electric power for working a large
number of mines. In northern Siam, mineral areas adjoining
the new railway extension have been opened. Lead and anti-
mony ores are the minerals worked, the lead being mixed with
zinc and containing some silver. — M.
BUTTER SUBSTITUTE FROM FISH OILS
The attention of the British Board of Trade has been di-
rected to a report appearing in a Norwegian paper to the effect
that a process has been discovered in Norway by which butter
substitute can be manufactured exclusively from Norwegian
fish oils. The production of the substitute will, it is stated,
be undertaken by a refinery which alone can produce sufficient
to cover the requirements of the country. The Provisions
Director will purchase the fish oils required. In addition to
whale oils, all kinds of fish oils and particularly oil from herrings
will be used. — M.
COD LIVER OIL FROM NEWFOUNDLAND
• Owing to the fact that the large quantities of cod liver oil pro-
duced in Newfoundland as a by-product in the fishing industry
were of inferior quality to that produced in Norway, the New-
foundland oil was not greatly esteemed in this country for medic-
inal purposes. Now, however, a great improvement in the
quality of Newfoundland oil has been effected through the
Government's action in sending a Norwegian expert to instruct
the Newfoundland refiners in the methods of preparing the finest
oil. The result of these measures has been to considerably im-
prove the quality of Newfoundland oil and it is claimed that this
oil is now equal to the best Norwegian oil. — M.
INDIAN OILSEEDS
The current number of the Bulletin of the Imperial Institute,
London, contains an interesting report dealing with the Indian
trade in oilseeds. It appears that the Indian production is
worth annually about $250,000,000 and the export value of
oilseeds and oilcake amounts to about $92,500,000. Great
Britain is now India's best customer for these articles although,
before the war, Germany had secured a monopoly for certain
classes of Indian oilseeds. This was due to the fact that her
specially controlled market enabled her to buy the most valuable
seeds, the products from which were eventually exported in the
form of margarine and other edible fats. The recent great in-
crease in the manufacture of margarine in England may possibly
alter the state of this permanently. The report referred to, we
may add, contains full information regarding the Indian oilseed
resources, the world's production, and demand for oilseeds, and
the part which India plays as a source of supply. The Bulletin
is published by J. Murray, Albemarle St., London. — M.
PRESERVATION OF PIT TIMBER
In view of the importance in present circumstances of prevent-
ing wastage in pit timber as much as possible, the British Depart-
ment of Scientific and Industrial Research has issued a bulletin
in which Prof. Percy Groom suggests some preventive and
remedial measures against decay. He points out that the fungi
which are for the most part responsible for the decay often clothe
the surface of the wood with a fluffy or cottony material (spawn)
which rapidly spreads and may be conveyed through the air and
attack other wood. These fructifications should be removed
and burned. For dealing with the spawn the men should carry
a swab, cloths and a pail of antiseptic solution; the antiseptics
suggested are creosote, zinc chloride and copper sulfate — the last
should not be used if the mine is rich in iron. This treatment,
once begun, should be systematically pursued and an attempt
made to render the wood immune to infection, perfect protection
being ensured only by impregnating the wood throughout. Iron
sulfate is not recommended as an impregnating agent. — M.
OIL-PRESSING PLANT FOR INDIA
Although it has not been practicable to purchase modern oil-
pressing plant from abroad, owing to war exigencies, the Board
of Industries in the United Provinces is assured that oil pressing
there has been accepted by capitalists as one of the most promis-
ing fields for development after the war. It is already a well
established domestic industry. Works extensions are proposed
as soon as they become practicable, while other capitalists have
intimated their readiness to put up modern oil mills when con-
ditions for the purchase of plant are favorable. — M.
RUSSIAN ASBESTOS INDUSTRY
The gradually increasing demand for asbestos, says the Mining
Journal, is reflected not only in the opening up of new deposits
such as those in South Africa, but also in the more active working
of older fields. Considerable increase was shown in the Russian
output previous to the war and although for the time being
any further development has been stopped, in view of the con-
siderable areas in which asbestos occurs, the future is regarded
as important. The chief centers from which the present produc-
tion is obtained are situated in the Urals. The output for recent
years is as follows:
Ysar Tons Ybar Tons
1907 10,451 1912 18,818
1908 13,130
1909 16,584
1910 13,467
1911 17,423
In addition to the Ural deposits, there are partially worked oc-
currences in the governments of Irkutsk and Yenisei M
1913
19,287
1914
17,297
1915
10,780
1916
9,030
398
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 5
ROUMANIAN PETROLEUM
A German oil authority lecturing recently at Bucharest stated
that the fuel value of Roumanian oil was very high, viz., 11,000
calories per kg., as against 8,000 calories for the best Welsh
steam coal. Germany, hitherto, has obtained oil from her ally,
Austria, which country in 19 13 produced well over 1,000,000 tons
of crude. The Motor suggests that Germany evidently expects
an enormous development of the Diesel engine. Thus, it is to
be expected that Germany will make an attempt to get a grip
011 all the oil sources she can and so render herself independent
of coaling stations. An 8,000-ton ship with Diesel engines,
it is estimated, can make a trip from England to Japan and back
on 700 tons of oil only. — M.
A DEOXIDIZING ALLOY
The above alloy consists of manganese, aluminum and mag-
nesium and is said to be particularly suitable for deoxidizing iron
and other metals. The presence of aluminum, which is easily
combined with magnesium and in which manganese is soluble,
permits of the formation of a ternary alloy which can easily be
obtained without impurity and without loss. It forms a very
powerful oxidizing agent. In preparing this alloy the aluminum
and magnesium are first combined, the manganese being then
added.— M.
DYE FROM MAPLE LEAVES
The British Consid at Seoul has forwarded a report dealing
with the so-called "Shinnamu" dye, obtained from the leaves of
a species of maple tree. As the result of investigation conducted
at the Central Laboratory of the Government, it is stated that
the dye is looked upon as a superior one and that it has attracted
the attention of people in various districts where the leaves have
been gathered and the manufacture of the dye has been entered
upon. No success worth speaking about has, however, been
obtained, owing to the lack of expert knowledge and the small
scale on which operations have been conducted. In the vicinity
of_Kaijo (Song-do) a large quantity of leaves is available and the
manufacture of the dye on an adequate scale is being planned.
There has also been experimental planting of the species of maple
tree referred to which is peculiar to Korea, being found almost
everywhere in that country. — M.
INSTRUMENTS AND TOOLS FOR VENEZUELA
Venezuela, says the Times Trade Supplement, which is one of
the South American States benefited by the war, is about to
launch upon a modified but comprehensive campaign of new-
building construction. There will, therefore, be a demand be-
fore long for many kinds of small machines, engineering instru-
ments, artisans' tools and contractors' machinery'- The Govern-
ment is also engaged upon a survey of a number of new highways
and here again the usual appliances for road construction will be
called for. Among the more urgent demands are the following:
windmills, portable boilers, rock-crushers, carts, wagons, in-
dustrial railways, wood-working machinery, appliances used
among mines and small industrial plants. Already a number of
road-rolling machines have been imported. There is an opening
for small stone crushers ami split log drags, such as are used in
the United States for the maintenance of roads having an earth
surface. In 1914 the value of imports in the matter of instru-
ments taken into the republic for the use of artisans and laborers
alone, was about $80,000. Manufacturers would do well to get
into touch with some of the larger importing firms in Caracas, of
whom there are 17 who act as agents for foreign manul.u tun 1 9
There are several important foundries, sawmills and lumber
dealers at Caracas, Cagna, Puerta Cabello and Maracaibo.
Communications should be addressed in Spanish, as English
is little understood. — M.
SWISS ELECTROCHEMICAL INDUSTRIES
According to a report in the Chemical Trade Journal, 62 11918),
184, on the commerce and industry of Switzerland, the calcium
carbide production rose from 60,000 tons in 1915 to 70,000 in
1016. The exports to different countries in 1915 and 1916 were
as follows:
1915 1916
Germany 46,200 tons 46,200 ion*
France 2,200 tons 20 tons
Belgium 3,900 tons 690 toiu
Netherlands 2,200 tons 20 ton*
Total exports 55,400 tons 58,000 ton
Value $2,500,000 $3,860,000
The output of calcium cyanamide was doubled during 1916,
the production being nearly 25,000 tons. The production of
carborundum and other abrasives was also nearly doubled, rising
from 800 to 1500 tons. Figures on the aluminum production
are not given, but the exports increased from 9,400 tons in 1915
to 1 1 ,400 tons in 1916. The nitric acid works at Chippis and in
Bodis produced sufficient acid from atmospheric nitrogen to
cover the demand of the federation. The output of caustic soda
from the works in Monthey has risen from 1000 tons in 1913 to
2,500 in 1916. New chemical works opened at Aaran for the
manufacture of hydrogen peroxide and at Bex for electrolytic
copper sulfate of ferrosilicon; the works in Visp and Bodis ex-
ported 20,000 tons, the whole of the production in the previous
year amounting to only 14,000 tons. — M.
OIL-BREAK SWITCHGEAR
A descriptive list issued by the British Thompson, Houston
Company, of Rugby, England, deals with a totally enclosed
switch for circuits of small capacity up to 700 volts. The
standard forms are non-automatic, double or triple pole for 60
amperes, and automatic double or triple pole with series trip
coils for 3 to 60 amperes. The automatic switches can be fitted
with time lags and low voltage releases, if required, the low volt-
age release coils being wound for 100 to 700 volts, as necessary.
The switches are opened and closed by the single motion of the
operating handle, with which a quick make-and-break action is
obtained, and they cannot be left in any position but full on or
off. The tripping mechanism is so designed that, if the switch
opens automatically, the operating lever remains in the closed
positions. The automatic trip is, therefore, of the free handle
type, and an indicator, independent of the handle, shows when
the switch has opened automatically. Large clearances are al-
lowed between all live parts and there is no earthed metal in the
neighborhood of the contacts. The switches can be arranged for
mounting on a wall, or can be carried on pedestals, either plain or
containing bus bars, isolating switches, cable boxes and starting
rheostats. — M.
BRITISH BOARD OF TRADE
During the month of February, the British Board of Trade
inquiries from firms in the United Kingdom and abroad
regarding sources of supply for the following articles. Firms
which may be able to supply information regarding these things
are requested to communicate with the Director of the Com-
mercial Intelligence Branch, Board of Trade, 73 Basinghall St.,
London, E. C.
Machinkkv and Plant:
Can-making plant to produce the
standard conical tins as used for
corned
Wirt- iMiamellins plant
Brush-making machine, pulling sys-
ppooed to tr.lv
Machinery lor making toy marbles
Plant for caustic soda production,
electrolytic process
Muchincry for making manioc flour
from cassava roots
Plant for manufacture of sealing wax
Badges, regimental letter, made of
celluloid or celluloid and paper.
not metal
Celluloid poultry rings
Flower bead necklets
Hair curlers and wavers
Levigated iron
Stoves suitable for burning wood
fuel
Zirconia 'firms holding stocks)
M
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
399
NOTES AND CORRESPONDENCE
PREPARATION FOR POST-WAR CONDITIONS IN
GREAT BRITAIN
The British Ministry of Reconstruction has published a com-
plete list of the various commissions and committees that have
been set up, both within that ministry and within other ministries
and departments of the British Government, to deal with ques-
tions which will arise at the close of the war. The commissions
and committees, which have been appointed at various times
since the war began, now number 87 and fall into 15 groups
as follows:
1 — Trade Development
2 — Finance
3 — Raw Materials
4 — Coal and Power
5 — Intelligence
o — Scientific and Industrial Research
7 — Demobilization and Disposal of
Stores
8 — Labor and Employment
9 — Agriculture and Forestry
10 — Public Administration
1 1 — Housing
12 — Education
13 — Aliens
14 — Legal
1 5 — Miscellaneous
Some of the committees and commissions of these groups
dealing with chemical questions are:
Trade development — Committee on the Chemical Trades — To
advise as to the procedure which should be adopted for dealing
with the position of the chemical trades after the war, with a
view to the creation of some organization which should be ade-
quately representative of the trade as a whole and by means
of which the trade may be enabled hereafter to continue to
develop its own resources and to enlist the closest cooperation
of all those engaged in the chemical industry.
Board of Trade Committees on the Coal, Electrical, Engineering,
Iron and Steel, Nonferrous Metal, and Textile Trades — To con-
sider the position of these trades and industries after the war,
with special reference to international competition, and to re-
port what measures, if any, are necessary or desirable to safe-
guard that position.
raw materials — Central Committee on Materials Supply — ■
To consider and report upon (1) the nature and amount of the
supplies of materials and foodstuffs which, in the committee-s
opinion, will be required by the United Kingdom during the
period which will elapse between the termination of the war
and the restoration of a normal condition of trade; (2) the
probable requirements of India, the Dominions, and Crown
Colonies for such supplies at the close of hostilities; (3) the
probable requirements of belligerents and neutrals for such
supplies at the close of hostilities; (4) the sources from which
and the conditions under which such supplies can be obtained
and transported, and, in particular, the extent to which they
might be obtained from the United Kingdom or within the
Empire or from allied or neutral countries; (5) the question
whether any measure of control will require to be exercised in
regard to the nature and extent of any such control.
Committee on Edible and Oil-Producing Nuts and Seeds — -To
consider and report upon the present condition and the pros-
pects of the West African trade in palm kernels and other edible
and oil-producing nuts and seeds, and to make recommendations
for the promotion in the United Kingdom of the industries
dependent thereon.
Nitrogen Products Committee — (1) To consider the relative ad-
vantages for this country and for the Empire of the various
methods for the fixation of atmospheric nitrogen from the point
of view of both war and peace purposes, to ascertain their relative
costs, and to advise on proposals relevant thereto which may ln-
submittcd to the department. (2) To examine into the supply
of the raw materials required, e. g., pure nitrogen and hydrogen,
and into the utilization of the by-products obtained. (3) Sum
lOBU "f the processes employed depend for their success on the
provision of large supplies of cheap power, to ascertain where
and how this can best be obtained. (4) To consider what steps
can with advantage be taken to conserve and increase the national
resources of nitrogen-bearing compounds and to limit their
wastage. (5) To carry out the experimental work necessary
to arrive at definite conclusions as to the practicability and effi-
ciency of such processes as may appear to the committed to be
of value. (6) As a result of the foregoing steps, to advise as to
starting operations on an industrial scale.
coal and power — Coal Conservation Committee — To con-
sider and advise (1) what improvements can be effected in the
present methods of mining coal with a view to prevent loss of
coal in working and to minimize cost of production; (2) what
improvements can be effected in the present methods of using
coal for production of power, light and heat and of recovering
by-products with a view to insure the greatest possible economy
in production and the most advantageous use of coal substance ;
(3) whether with a view to our maintaining our industrial and
commercial position, it is desirable that any steps should be
taken in the near future, and if so, what steps, to secure the de-
velopment of new coal fields or extensions of coal fields already
being worked.
Mining, Power Generation and Transmission, Carbonization,
and Geological Sub-Committees — The question of the applica-
tion of carbonization to the preparation of fuel for industrial
and commercial purposes.
Committee on Supply of Electricity — To consider and report
what steps should be taken, whether by legislation or otherwise,
to insure that there shall be an adequate and economical supply
of electric power for all classes of consumers in the United King-
dom, particularly industries which depend upon a cheap supply
of power for their development.
intelligence — Imperial Mineral Resources Bureau Com-
mittee— To prepare a scheme for the establishment in London
of an Imperial Mineral Resources Bureau ( 1 ) to collect informa-
tion in regard to the mineral resources and metal requirements
of the Empire; and (2) to advise what action, if any, may appear
desirable to enable such resources to be developed and made
available to meet requirements.
scientific and industrul research — Fuel Research Board —
To investigate the nature, preparation and utilization of fuel
of all kinds, both in the laboratory and, where necessary, on an
industrial scale.
Cold Storage Research Board — Appointed to organize and
control research into problems of the preservation of food prod-
ucts by cold storage and otherwise.
Standing Committees on Engineering, Metallurgy, Mining,
and Glass and Optical Instruments — To advise the council on
researches relating to the lines of activity named and on such
matters as may be referred to the committee by the Advisory
Council.
Joint Standing Committee on Illuminating Engineering — To
survey the field for research on illumination and illuminating
engineering, and to advise as to the directions in which research
can be undertaken with advantage.
Mine Rescue Apparatus Research Committee — To inquire into
the types of breathing apparatus used in coal mines, and by ex-
periment to determine the advantages, limitations, and defects
of the several types of apparatus, what improvements in them
are possible, and whether it is advisable that the types used in
mines should be standardized, and to collect evidence bearing
on these points.
Abrasives and Polishing Powders Research Committee — (1) To
conduct investigations on abrasives and polishing powders
with a view to their preparation and use as one factor in ac-
celerating the output of lenses and prisms for optical instruments,
not only for peace requirements, but in connection with the war.
(2) To investigate the preparation and properties of abrasives
and polishing powders.
Food Research Committee — To direct research on problems
in the cooking of vegetables and meat, and in bread making,
to be undertaken by two scholars of the committee of council.
Electrical Research Committee- -A committee of direction ap-
pointed in connection with certan researches affecting the elec-
trica] industry.
Committee for Research on Vitreous Compounds, and Cements
and Prisms— To conduct researches into the prepara-
operties, and mode of employment of cements for lenses
and prisms; to prepare ;i reference list of vitreous com]
imposition, densities, refractive indices, and dispersive
powers.
Tin and Tungsten Research Board—The Cornish Chamber of
Mims has been invited to nominate a representative of the
landlords and a representative of the mine owners to serve
on the board. A committee of control appointed in connection
1 j lain researches into tin and tungsten.
Lubricants and Lubrication Inquiry Committee To prepare a
indum on the field for research on lubricants and lubrica-
tion, which will contain an analysis of tin- problems involved,
with a suggested scheme of research, which would be
most likely to lead to valuable results.
400
THE JOURNAL Of 1NDI STRJAL AND ENGINEERING CHEMISTRY Vol. io, No. I
Chemistry of Lubricants Subcommittee — To collect and review
the existing information relating to the chemistry of lubricants
and lubricating oils.
Zinc and Copper Research and Inquiry Committee — To collect
and review the existing information as to the copper and zinc
industries upon which future research must be based, to formulate
proposals for carrying out the research suggested by the Brass
and Copper Tube Association of Great Britain into the best
methods of making sound castings of copper and brass for tube
making and to prepare an estimate of their cost; and to report
to the Advisory Council.
agriculture and forestry — Forestry Committee — To con-
sider and report upon the best means of conserving and de-
veloping the woodland and forestry resources of the United
Kingdom, having regard to the experience gained during the war.
education — Committee on the Teaching of Science — To in-
quire into the position occupied by natural science in the edu-
cational systems of Great Britain, especially in secondary schools
and universities, and to advise what measures are needed to
promote its study, regard being had to the requirements of a
liberal education, to the advancement of pure science, and to
the interests of the trades, industries, and professions which
particularly depend upon applied science.
NOTE ON "THE FERTILIZING VALUE OF ACTIVATED
SLUDGE" BY NASMITH AND McKAY
Editor of the Journal of Industrial and Engineering Chemistry:
We have reviewed with much pleasure the timely and interesting
contribution by Messrs. Nasmith and McKay on the subject
of "The Fertilizing Value of Activated Sludge" and feel that
its publication would be of direct value. However, we wish
to point out in particular two fallacies in this paper which
should not be perpetuated by being quoted from one publica-
tion to another.
First is the result obtained by Bartow and Hatfield in which
activated sludge gave a higher yield proportionately than dried
blood in their fertilizer experiments. This is contrary to all
experience and known facts regarding dried blood, which is con-
sidered the most valuable of commercial organic ammoniates. The
explanation for this discrepancy is probably in the abnormal
conditions under which the experiments were carried out as com-
pared with actual agricultural conditions, namely, in the use of
a sterilized soil or of washed sand in stiff clay soil, thus killing
off or materially reducing the ammonifying and nitrifying organ-
isms which are so necessary to the success of organic ammoniates.
Dried blood cannot supply these organisms since it has also been
sterilized in drying. Activated sludge, however, when used
wet or air-dried,1 teems with proteolytic and nitrifying organisms,
thus possessing an advantage over commercial organic am-
moniates which the latter cannot reasonably be expected to
overcome quickly. If activated sludge were dried on a commer-
cial scale in the same manner as commercial ammoniates now
are, it would not possess th.s advantage. Furthermore, in
actual agricultural practice the sterile soil would not be used, so
that the nitrifying organisms in the soil would attack one or-
ganic ammoniate as well as the other.
Another fact developed in this respect lies in the so-called
availability, as determined by the empirical methods in use
in the New England States, the alkaline permanganate method,
and the method in use in the Southeastern States, namely, the
neutral permanganate method. While we do not believe that
these methods can in all cases determine the true availability
of organic nitrogen, the fact remains that thej are law in these
States anil must therefore be applied in determining the value
of any given form of organic nitrogen < >ur tests have shown re-
peatedly that the nitrogen in activated slmlyc falls below the
minimum limit of availability set by the authorities in these
States, thus classing it as an "inferior organic ammoniate,"
while the nitrogen in dried blood, tankage, bone, etc., is classed
as "highly available." These methods preclude the use of many
1 Nasmith and McKay, page 339, and presumably also Bartow and
Hatfield, This Journal. 8 (1916), 17.
organic ammoniates which are thus wasted. Dr. J. W. Turrea-
tine, of the I". S. Bureau of Soils, has been studying this prob-
lem for some time.
Please do not misunderstand our attitude in this matter. We
are vitally interested in the successful working out of the activated
sludge problem, since it presents for the first time in the his-
tory of sewage disposal a hope of successful recovery of the
sludge in a form commercially usable, thus repaying, at least in
part, the cost of sewage purification, while heretofore the dis-
posal of the sludge has been the feature on which all other pro-
cesses of sewage purification have failed. It has not only been
the expense of disposing of the sludge, but in many cases the
actual impossibility of finding a place where it might be dumped
without objection. The nitrogen content of activated sludge
is from two to three times as high as that of any other sludge
previously produced, thus placing it at once within the range
of commercial ammoniates which will stand expense of trans-
portation outside of the immediate locality in which they are
produced. We must not, however, permit experimental condi-
tions which will not obtain in actual practice to fool us as to the
actual monetary value of activated sludge. The facts so far
developed on this most interesting process have fully justified
all the energy, time and money expended without making any
unjustified assumptions as to the final value of the sludge.
Chemical Laboratory, Armour & Company PAUL Rud.S'ICK
Chicago. Illinois, March 4, 1918
REGULATIONS UNDER THE POTASH LEASING ACT
The Department of the Interior has issued the following:
Secretary of the Interior Lane has approved working instruc-
tions and regulations under the Potash Leasing Act of October 2,
1917, a matter which has been given the most careful considera-
tion, in view of the importance attached to this pioneer work
in the development of a great national asset
The act is liberal in its terms, authorizing the exploration for
and disposition of potash deposits generally in the public lands
of the I'nited States, under a system that provides for a pre-
liminary permit to the holder for the exclusive privilege of search-
ing for deposits of potash for a period of not exceeding two years.
ONE PEK.MIT LLMITED TO 2,560 ACRES
The acreage embraced within one permit is limited to 2,560
acres, and the Secretary, upon a satisfactory showing that valu-
able deposits of potash have been found within the permit, is
authorized to issue a patent to not exceed one-fourth of the
amount covered by the permit, the remaining lands in the permit
being subject to lease either by the permittee or others, after
advertisement, competitive bidding, or such other methods as
the Secretary may by general regulations adopt.
KI l LATIONS BROAD IN OUTLINE
To the end, therefore, that the liberal purposes of the act
may Inal the fullest scope of operation, the instructions and regu-
lations now approved are broad in outline, simple in form,
yet so directly addressed to the matter in hand that it is believed
all applicants under the law will find but little difficulty in pre-
senting their claims for consideration by the department.
Requests for copies of these instructions should be addressed
to the Commissioner of the General Land Office, Washington,
NOTES ON "FREE CARBON" OF TAR
Editor of the Journal of Industrial and Engineering Chemistry:
Although rather extensive investigations are under way con-
cerning the nature of the free carbon" of pitch and tar, the
work as yet is not in such form as to warrant publication. How-
ever, the conclusions of Monroe and Broderson1 as drawn from
' This Jouuial, 9 (1917). 1100.
II
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
their results, on the effect of solvents on certain bodies in coal
tar, should not be passed without comment. We, therefore,
take this opportunity to discuss the results of these investigators
in connection with their remarks concerning the article by Weiss1
on "free carbon."
Weiss found that both chloroform and carbon bisulfide, when
held in contact with coal tar over varying periods, formed in-
soluble compounds containing chlorine and sulfur, respectively.
Chlorine was found qualitatively and sulfur was determined
quantitatively by Weiss. Monroe and Broderson substantiated
the qualitative tests for chlorine by quantitative methods but
do not mention the fact that carbon bisulfide also precipitates
insoluble materials containing sulfur. Weiss also found that,
with benzene and toluene as solvents, the free carbon content
of tar increased with the time of contact and concluded that
this was also due to the reaction between the solvent and certain
tar bodies. Monroe and Broderson claim that this does not
happen in the case of benzol, but that the colloidal "free carbon"
is merely precipitated by the action of the solvent with no actual
chemical combination. Weiss noted2 that when a solution of
tar in toluol or in aniline was placed under the microscope in
the form of a hanging drop, a gradual increase of insoluble
matter took place with the toluol, but that the aniline solution
remained clear for more than 24 hours. For this reason, it
would appear that the toluene actually reacted chemically as
there is no reason to believe that this would break the colloidal
suspension any more easily than would aniline.
If we now consider the method and results, illustrated by graphs
by which Monroe and Broderson attempt to prove that benzene
as a solvent does not form insoluble compounds by chemical
reaction and that chloroform does give insoluble compounds by
chemical combination, we encounter one fallacy. They attempt
to prove the formation of compounds of higher molecular weight
through the reaction of the solvent on the tar, by a rise in the
boiling point of the solvent, but the compounds that are formed
and in which they are interested are insoluble. Insoluble
materials could have no effect on the boiling point of the solvent.
The horizontal graphs representing the boiling points of the
solvents, benzene and carbon bisulfide, could very well represent
the results of actual chemical combination between the tar and
the solvent, resulting in the formation of insoluble materials.
If chemical combination took place, both a portion of the tar
and of the solvent would be removed from the solution in the
insoluble form, and hence the line would still remain horizontal.
We do not know the molecular comparison between the amounts
of tar and solvent removed, but the actual formation of insoluble
compounds is rather small. Therefore, the probable variation
in the temperature, due to the removal of more solvent than tar
(or vice versa) entering the insoluble compound, could hardly be
determined by a Beckmann thermometer.
There seems to be but one explanation of the peculiar graph
for chloroform, the rise of which Monroe and Broderson explain
is due to the formation of insoluble "free carbon," that is, that
there may be a reaction between the chloroform and the coal
tar to form soluble bodies that would increase the boiling point
of the solvent. This is, however, merely speculative and not
of direct bearing on the claims in the paper.
Research Department Laboratory JOHN Morris WEISS
The Barrett Company, New York City Charles R. Downs
December 20, 1917
THE GROWTH OF THE INDUSTRIAL FELLOWSHIP
SYSTEM*
Twelve years ago, the late Robert Kennedy Duncan, while
attending the Sixth International Congress of Applied Chem-
istry in Rome, conceived the idea of a practical method of
1 Tms Journal, 6 (1914), 279.
1 Loc. cil.
1 Reprint of report issued by Mellon Institute of Industrial Research.
bringing the science of the University — the new knowledge — to
the service of industry. The idea called for the establishment,
in the University, of Industrial Fellowships by individuals,
companies or associations for the investigation of specific manu-
facturing problems involving the physical sciences.
The first Industrial Fellowship was founded in 1907 at the
University of Kansas, where Dr. Duncan was then professor
of industrial chemistry, by a company interested in the chem-
istry of laundering. In 19 10, Dr. Duncan was called to the
University of Pittsburgh to inaugurate the Industrial Fellow-
ship System in the Department of Industrial Research, now
known as the Mellon Institute of Industrial Research.
The first Industrial Fellowship at the University of Pitts-
burgh was founded in March 191 1, through a grant from a
baking company which desired to improve its product. In
the seven years which have elapsed, seventy-five distinct con-
cerns have endowed some one hundred eighty-nine one-year
Industrial Fellowships for the study of specific manufacturing
problems.
During the past year, the Mellon Institute, in common with
all of the other research institutions of the country, has suffered
a marked depletion in its staff. Twenty-one of its members,
including the Director and an Assistant Director, have entered
Government service in response to their country's call. The
Institute, in most cases, has been able to fill the vacancies on
the Industrial Fellowships. However, the shortage of research
men, of the type demanded by the Industrial Fellowship Sys-
tem, has forced the Institute to decline to accept, temporarily,
a number of very desirable research problems. It is gratifying
to report that, notwithstanding the unsettled condition of the
business world, an increasing number of industrialists are as-
signing problems on their processes and products to the Institute.
The following table shows the number of Industrial Fellow-
ships which have been founded in the Institute from March to
March of each year — 191 1 to 1918; the number of researchers
or Industrial Fellows, as they are called, who have been em-
ployed on these Fellowships; and the total amounts of money
contributed for their maintenance by industrial concerns:
Number of Number of Amounts
March to March Fellowships Fellows Contributed
1911-1912 11 24 $39,700
1912-1913 16 30 54,300
1913-1914 21 37 78.400
1914-1915 21 32 61,200
1915-1916 36 63 126,800
1916-1917 42 65 149,100
1917-1918 42 64 172,000
The total amount of money contributed by industrial firms
to the Institute for the seven years ending March i, 1918,
was $681,500. In addition to this sum, over $400,000 was
expended by these concerns in the construction of experimental
plants. During the seven years, the Institute itself expended
about $280,000 in taking care of the overhead expenses — salaries
of members of permanent staff and office force, maintenance
of building, apparatus, etc. — in connection with the opera-
tion of the Industrial Fellowships. Besides this amount,
the building and permanent equipment of the Institute, which
make it the most complete and modern industrial experiment
station in the country, represent an investment of about $350,000.
The money for the building, its equipment and the yearly allow-
ance for overhead expenses is the gift of Andrew William Mellon
and Richard Bcatty Mellon, citizens of Pittsburgh.
It required the cataclysm nf the C.reat War to bring men to
realize fully the part which applied science is playing and, more
particularly, will play in the life of nations. As men have
come to know that everything in modern warfare is controlled
in a large measure by science — no gun of large caliber is located
or fired without its aid — so they have come I" know that in
the making of things — in the economy IB »i maiiu-
4°-
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 5
facturing operations — science must have a place, an important
place too. With this idea in mind, institutions of learning and
industries in this country, hut more especially abroad, are
investigating and studying methods to bring about cooperation
between science and industry. The Mellon Institute is proud
that, while- very young, it has been a pioneer in the field. Its
principal claim to distinction, apart from its contributions to
specific industries, is based on the service it has been able to
render to other institutions in demonstrating the practicability
of a system which brings together science and industry for the
development of a future and more gracious civilization.
Mellon Institute of Industrial Research
University op Pittsburgh
March 1, 1918
AMERICAN DYESTUFF MANUFACTURERS' ASSOCIATION
The Board of Governors of the American Dyestuff Manu-
facturers' Association met on April 5 at the office of its counsel,
Benjamin M. Kayc, 149 Broadway, New York City, to elect
officers, execute the certificate of incorporation, and adopt the
constitution and by-laws.
According to the incorporation papers the objects of the As-
sociation are'
To promote the welfare and business interests of those en-
gaged in the dyestuff manufacturing industry in the United
States of America.
To promote and encourage the manufacture and use of
American dyes; to cooperate with Congress, the Tariff Com-
mission, the Federal Trade Commission, the Department of
Commerce and all other governmental agencies in order to secure
adequate protection against unfair competitive methods employed
by foreign producers.
To cooperate with the United States Bureau of Standards
and other similar bureaus and departments for the purpose of
establishing proper trade standards of dyestuffs in the United
States.
To collect and disseminate accurate information relating to
the manufacture, sale and use of dyes, chemicals and kindred
products in order that the statistics so gathered may be utilized
in the effort to establish the manufacture of dyestuffs as one of
the real industries of the United States.
In adopting its constitution, special consideration was given to
eligibility to membership, and the first section adopted reads:
All persons, firms or corporations engaged in the business of
manufacturing dyestufts or intermediates in the United States
shall be eligible for membership in the Association. No concerns
having affiliations with concerns doing business in those countries
now at war with the liiitnl States or its allies shall be eligible
to membership.
Officers were elected as follows:
President: Morris R. Poucher, of E. I. du Pont de Nemours
& Co., Wilmington, Del.
First Vice President: L. A. Ault, of Ault & Wiborg, Cincin-
nati, Ohio.
Second Vice President: Frank Hemingway, of Frank Hem-
ingway, Inc., New York City.
■ ■■' y: C. Cyril Bennett, Manager of tne "Color Trade
Journal," New York City.
Treasurer: Charles Jenkinson, of the National City Bank,
New York City.
Executive Board: President Poucher; August Mir/, of Heller
and Merz, Newark, N. J.; Robert C. Jeffcott, of the Calco
Chemical Co., New York City; J. Merritt Matthews, of the
Grasselli Chemical Co., New York City; Robert P. Dicks,
of the Dicks, David Co., Inc., New York City.
Within a short time the Association will issue propaganda in
orda to acquaint the American public with the enormous strides
made in the dyestuff industry in this country since the start of
the European war.
CHEMICALS DIVISION OF NATIONAL WAR SAVINGS
COMMITTEE ORGANIZED
A Chemicals Division of the National War Savings Com-
mittee appointed by the Secretary of the Treasury has been
organized with committee as follows:
Chairman: Ellwood Hendrick, Consulting Editor, "Metallurgical
and Chemical Engineering;" Vice Chairman: J. R. de la Torre Bueno,
Editor. "The General Chemical Bulletin;" Treasurer: Jerome Alexander,
National Gum and Mica Co.; Secretary: T. E. Casey, The BarTett Co.;
Charles F. Roth. Manager National Exposition of Chemical Industrie*;
Geo. W. Nott, Advertising Manager, "The Journal of Industrial and
Engineering Chemistry;" F. M. Turner, Technical Editor, "Chemical
Engineering Catalog;" Wm. H. Nichols, Jr., President. General Chemical
Co., T. M. Rianhard, Vice President, The Barrett Co.; J. B. F. Herreshoff,
Vice President, Nichols Copper Co.; Charles H. Herty, Editor, "The
Journal of Industrial and Engineering Chemistry," Franklin H. Warner,
Secretary and Treasurer, Warner Chemical Co.; H. I. Moody, Treasurer,
National Aniline and Chemical Co.; C. E. Sholes, Sales Manager, Grasselli
Chemical Co.; C. P. Tolman, Manufacturing Manager, National Lead Co.;
E. D. Kingsley, President Electro Bleaching Gas Co.; Charles F. Chandler,
Emeritus Professor of Chemistry, Columbia University; J. M. Matthewa,
Editor, "Color Trade Journal."
The committee in a letter sent to all manufacturers of chemi-
cals, dyestuffs, and chemical apparatus has requested each
manufacturer to organize his establishment to forward the sale
of Thrift Stamps among his employees. They ask that one or
more individuals connected with each company be made a
distributing agent, and suggest that each department of a large
company have its accredited agent. The committee being
advised of the appointments has a signed certificate bearing
the name of the appointee sent from the Secretary of the
Treasury. Each employee is privileged to purchase War Sav-
ings Stamps from the agent in his plant but because of the
value placed upon them, the Government will allow no more
than Siooo worth to be sold any one person.
The patriotic cooperation of all manufacturers with Uncle
Sam is asked to make it easy for employees to purchase these
Stamps. The committee makes many suggestions as to methods
of promoting thrift among employees, and the sale of stamps;
it must be remembered that an employee who has learned thrift
is always responsible. All who would cooperate with the
Chemicals Division are requested to communicate with Mr.
T. E. Casey, The Barrett Co., 17 Battery Place, New York City.
AMERICAN CERAMIC SOCIETY
Tlie Northern Ohio Section of the American Ceramic
Society met in Toledo, Saturday, April 6. The program was
preceded by a visit to the plant of the Buckeye Clay Pot Com-
pany where an experimental humidity dryer was of special
interest. At the afternoon session, Dr. A. F. Gorton, of the
Buckeye Company, gave a very interesting account of the result
of three months' Operation of the dryer working on heavy blocks.
A S. Walden, foreman of the Furnace Department, of the
National Carbon Company in Cleveland, presented a paper
treating of the points to be considered in the choice of refrac-
tories for various furnace conditions The material presented
was directly based on a large experience in the construction and
operation of furnaces of greatly varying types. The charter
granted to the Local Section by the Trustees at the recent meet-
ing of tin National Society in Indianapolis was presented by
Ex-President C. W. Parmelee, Department of Ceram
versity of Illinois. Prof. Parmelee's address of presentation
touched on the history and tradition of the American Ceramic
Society and the part the Local Sections are to take in the future
di yelopment of the organization. A business session provided
for a completion of the organization details of the section. Fol-
May, 1 918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
403
lowing the afternoon program the members dined together and
the meeting adjourned.
This Local Section draws from a very active field of ceramics
and a real live organization should develop from the present
preliminary efforts. The officers of the section are as follows:
Chairman: E. P. Poste, The Elyria Enameled Products
Company, Elyria, Ohio.
Secretary and Treasurer: Bryan A. Rice, The Elyria Enameled
Products Company, Elyria, Ohio.
Councilor: Robert D. Landrum, Harshaw Fuller Goodwin
Company, Cleveland, Ohio.
TECHNICAL ASSOCIATION OF PULP AND PAPER
INDUSTRY
The Third Annual Spring Meeting of the Technical Association
of the Pulp and Paper Industry will be held at Dayton, Ohio,
on Thursday and Friday, May 16 and 17, 1918. Headquarters
will be established at the Miami Hotel, Dayton, and the busi-
ness meetings will take place in Community Hall. On the
afternoon of the first day papers and discussions will be given
on the subject of Coal Conservation. The second day of meet-
ing, Friday, May 1 7, will be given up to visits to mills in Dayton
and vicinity.
All pulp and paper manufacturers should be represented at
this meeting by the technical men in their employment who are
members, as they will gain a great advantage by meeting other
technical workers for the discussion of new developments,
methods aud processes.
The Secretary, T.J. Keenan, 117 East 24th St., New York
City, will be glad to assist in making reservations for members
at the hotels. Details of the Program will be issued as soon
as the Local Committee has completed arrangements.
CALENDAR OF MEETINGS
American Society of Mechanical Engineers — Worcester, Mass.,
June 4 to 7, 191S.
American Institute of Chemical Engineers— Annual Summer
Meeting, Berlin, N. H, June 18 to 22, 1918.
American Society for Testing Materials— Atlantic City, N. J.,
June 25 to 28, 1918.
Technical Association of Pulp and Paper Industry — Third
Annual Spring Meeting, Dayton, Ohio, May 16 and 17, 1918.
SYNTHETIC MATERIALS— CORRECTION
In the note printed under the above title in This Journal, 10
(1918), 314, the following correction should be made:
Page 314, right-hand column, "Phenylmethyl" in the 6th line
from the top should read "Phenylethyl."
WASHINGTON LETTER
By Paul Wooton, Metropolitan Bank Building, Washington, D. C.
Steps are being taken by the purchasing agencies of the
Government to give advance notice of its requirements for drugs
and chemicals. Since the United States entered the war, large
government orders have been placed with little anticipation.
This has had the effect of unsettling the market and has been
objected to strenuously by other consumers. In numerous
cases the reserve of certain drugs and chemicals has been wiped
out entirely to fill an unexpectedly large order from the govern-
ment. When other buyers found stocks exhausted, a flurry
often resulted, causing prices to reach fictitious levels. Manu-
facturers, as well as consumers, have objected to this unnatural
condition. Had advance knowledge of government require-
ments been had, there would have been no difficulty in having
ample stocks to meet it and the needs of the regular demands
of commerce as well.
Charges made in connection with the application of the
California Trona Co., for patents covering certain lands in the
Searles Lake region of San Bernardino County, California, have
been disapproved by the Secretary of the Interior and the
patents will be granted. The charges that were made are,
substantially: that the claims do not contain a mineral deposit
of the form and character contemplated by the mining laws as
subject to entry; that all of the acts performed by the com-
pany on the properties were for the purpose of securing title in
the interest of non-resident aliens; that at the date of the with-
drawal of the lands, the company was not the bona fide owner
of the claims and that at the time of application for patent, the
company was not qualified to receive the patent because a large
majority of its stock was controlled by aliens.
In the decision, which was made after extensive hearings and
a full investigation, it was stated that the scientific information
at the disposal of the department shows the commercial value
<>f several substances Found on these claims, and that, chemically,
each and every one of them is a mineral. The rule laid down by
the department is that whatever is recognized by the standard
authorities as a mineral, whether metallic 01 mm -metallic, when
found in the public lands, comes within the purview of the mining
1 \icw ni these facts, the decision holds "that brine in
a lake from which potash is procured in valuable and commercial
quantities is subject to location and patent under the mining
laws."
The alien ownership feature was disposed of quickly by the
citation of a ruling in a previous case in which it was held thai
"a corporation organized under the laws of tin- United
of any state or territory thereof, may, under Sections 2319 and
2321 of the revised statute, occupy and purchase mining claims
from the government, irrespective of ownership of stock therein
by persons, corporations, or associations not citizens of the
United States."
Preparations for big troop movements to France have inter-
fered importantly with the plans of the Chemical Service Sec-
tion of the National Army and of Charles L. Parsons, the sec-
retary of the A. C. S., for securing the return of chemists to the
essential industries. In many cases, where troops were ready
to go to France, permission for transfers could not be secured,
as commanding officers did not want to interfere even slightly
with their organizations. Dr. Parsons has held a number of
conferences with officials in regard to the matter, which he be-
lieves is in a fair way to be straightened out.
By far the most drastic steps taken in the reduction of imports
to release ships are those of the War Industries Board in es-
tablishing partial and complete embargoes on many imports.
One list of articles, the importation of which is to be restricted,
already has been issued and others are in the making. Among
the articles on the first list are all acids; muriate of ammonia;
all coal-tar distillates, except synthetic indigo; all salts of soda,
except nitrate and cyanide of soda; graphite and pyrites. The
embargo is not complete on pyrites and graphite. It permits the
importation of 125,000 long tons, up to October 1. The imports
are to come in on a graduated scale as follows: April, 40,01111
tons; May, 30,000 tons; June, 20,000 tons; July, 15,0011 tuns;
August, 10,000 tons; September, 10,000 temv
A substantial cut in the imports of manganese ore from Brazil
is understood to have been decided upon by the authorities in
Washington. The exact figures have not been made public,
but it is understood that the imports of Brazilian ore for 1918
do not exceed 350,000 tons. In 1017 they exceeded 500,000 tons.
It is understood that there will be iki [imitation on the importa-
tion "f ammonia, antimony, arsenic, bismuth, kainite, mica.
tin, tungsten and vanadium. Imports will be restricted Or cut
off in most of the othei important minerals.
The Car Service Section of the Railroad Administration is on
the point of taking drastic action to compel the loading of cars
i.i iinn full capacity. The chemical industries havi
dcrs to some extent in this matter, it is repotted 1 111
Administration is keeping a record of ligh.1 loading, and serious
losses are likely i" I" caused shippers who fail t" follow instruc-
tions in the matter of loading.
404
THE JOURNAL OB INDUSTRIAL AND ENGINEERING i HE MISTRY Vol. 10. No. S
At the request of the War Industries Board, the Committee
on Furtili/.ers lias made a survey of stocks of nitrate of soda.
Fertilizer manufacturers who operate sulfuric acid plants have
been asked to keep on hand enough nitrates to insure operation
for ninety days.
All plants engaged in the manufacture of chemicals, ferro-
alloys, explosives, gas, insecticides, mineral and vegetable oils,
soap, tanning extracts and fertilizers are among the plants and
industries embodied in the War Industries Board's preference
list No. i. Those on this list are to receive preferential treat-
ment in the matter of fuel supply. In giving out its statement
in regard to this list, it was made clear that it is not an attempt
to classify any industry as non-essential. In determining what
industries or plants are entitled to be certified, the relative ur-
gency of the uses for which the product of the plant is utilized
and the per cent of the product of the plant which is utilized in
war work or in other work of exceptional or national importance,
will be considered.
Owing to the wide-spread interest among chemists in the an-
nouncement of the Federal Trade Commission with regard to
licenses under German dye and drug patents, the official state-
mi nt is reproduced herewith in its entirety:
After extensive experimenting with approximately 600 German owned
or controlled dye patents, the proper combinations of the patents for the
quantity production of the dyes have been determined, and the Federal
Trade Commission has granted 22 applications of the E. I. du Pont de
Nemours and Co., of Wilmington, Del., for licenses under these
patents to manufacture the dyes which have been unobtainable since 1914.
Ei^ht applications made by the National Aniline and Chemical Co., of
Buffalo, N. V., have been granted by the Commission also.
The licenses were not granted until careful research and investigation
by the Trading with the Enemy Division of the Federal Trade Commission
to determine the proper combinations of patents necessary to make par-
ticular dyes or groups of dyes. Examination of the patents disclosed the
fact that in many instances insufficient descriptions were given to enable
anyone to follow the correct formulas. In some cases where attempts to
combine the ingredients were made, explosions or failure from other cause*
resulted. In other cases the formulas worked without a hitch whea tried
in a laboratory, but were a failure when an effort was made to produce the
dyes in commercial quantities.
After the proper combinations of patents for the mercantile production
of dyes were established, further careful experimentation was necessary to
discover which patented formula or formulas it was necessary to follow
in order to introduce the dyes into fabrics It was not until these problems
were solved satisfactorily that the licenses were approved.
The licenses for American use of the enemy patents in nearly all cases
are for the entire life of the patent instead of only for the duration of the wax.
Additional licenses to American firms to manufacture drugs under I
enemy patents have been issued by the Federal Trade Commission, too.
Licenses have been issued to the Antoine Chiris Company, of New York,
to manufacture "barbital" (veronal); to the Calco Chemical Company
to manufacture "pro-caine" (novocain); and to the DJarsenol Chemical
Company, of Buffalo, to manufacture "arsphenamine" (salvarsan). An-
nouncement has already been made of former licenses to manufacture these
drugs under enemy-owned patents.
The first licenses for the manufacture under German patents of "neo-
arsphenaminc" (neo-salvarsan) have been issued by the Federal Trade
Commission to the Farbwerke Hoechst Company, of New York, the Taka-
mine Laboratory, Inc., of New York, the Diarsenol Chemical Company,
of Buffalo, and the Dermatological Research Laboratories, of Philadelphia.
In Kranting applications for licenses to manufacture "barbital," which
is regarded as one of the best and safest hypnotics and nerve calmatives,
it is provided that the old name "veronal" may be used on packages in an
explanatory sense. This drug has practically supplanted cocaine as a local
anaesthetic having the effectiveness but none of the dangerous habit-form-
ing qualities of cocaine. Before the first license was issued to make "pro-
caine" it had sold in the United States as high as $720 a pound, but now can
be obtained at less than SI00 a pound.
As in other licenses under enemy-owned or controlled patents, the con-
cerns to benefit by the licenses will pay the Alien Property Custodian 5
per cent of their gross receipts from the sales of the articles involved, or
5 per cent of a valuation determined by the Federal Trade Con
PERSONAL NOTL5
Mr W. S. Dean, a graduate in textile engineering of the North
Carolina State College of Agriculture and Engineering at Raleigh,
N. C, who for some time has been connected with the cotton
marketing division of the U. S. Department of Agriculture, has
resigned that position to take up work for the Board of Vocational
Education, under T. K. Browne, director of vocational education
in North Carolina.
Dr. J. C. Olsen, head of the department of chemistry at
Cooper Union, has accepted the position of professor of chemistry
and head of the department of chemistry at the Polytechnic
Institute of Brooklyn. A new chemical laboratory is to be
equipped and installed at the Polytechnic Institute and more
emphasis given to the course in chemical engineering, both day
and evening. Considerably more space is available for the work
in chemistry since the Institute has taken over the building
formerly used by the preparatory department, in which new
chemical laboratories will be built. This building has been
thoroughly overhauled and put in first class condition.
Mi R. C. Bergen, assistant editor of Metallurgical and Chemical
Engineering, has resigned his position to go into manufacturing
work. He has been with the journal since its change to a semi-
monthly publication in 1915 and was formerly with the Roessler
and Hasslacher Chemical Compan]
Dr. E. B. Spear, professor of chemistry of the Massachusetts
Institute of Technology, has been appointed consulting
chemist to the Bureau of Mines in connection with the gas war-
fare work.
Mr. Elwood P. Wenzelberger, formerly assistant chemist
for the Victor Talking Machine Co., has been trans-
ferred from Camp Dix to the 11. S. Army School of Military
Aeronautics at Princeton, N. J., where he is pursuing a course
of training for a commission in the aviation corps.
Prof. D. C Dyer, of the State Experiment Station, Newark,
Del., hi- been appointed by the chairman of the Delaware Sec-
tion, A. C S., as a committee of one to promote the use of garbage
for feeding purposes, in response to a requesl for cooperation
from the Garbage Utilization Division of the I'. S. Pood Ad-
ministration.
Dr. 1.. C, Jones, chief chemist of tin- Seme! Solvay Company
and Solvay Process Company, has ben elected a vice president
of the National Aniline and Chemical Compan; .
The Navy Department has designated the Stevens Institute
of Technology, Hoboken, X. J., as the headquarters for the new
United States Steam Engineering School for the training of engi-
neer officers for the U. S. Naval Auxiliary Reserve. This school
is the only one devoted to training engineer officers for steam-
engine service, and is a branch of the large training school now
located at Pelham Bay Park, N. Y. The education of engineer
officers at Stevens is directed by Prof. F. L. Pryor who has
been appointed by the Navy Department with the approval of
President Humphreys, civilian director.
Dr. Samuel A. Tucker, of Columbia University, Dr. H. R.
Moody, of the College of the City of New York, and Mr. J. M.
Moorehead, of Chicago, have been added to the personnel of
the chemical section of the War Industries Board.
From April 1 until June 15 the offices and laboratories of the
Pittsburgh Testing Laboratory will be located at the B. F.
Jones Law Building. 4th Avenue and Ross Street, Pittsburgh,
Pa. After June 15 they will be located at 612 to 620 Grant Street,
Pittsburgh.
Among the demonstrators in McGill University last year the
following are now doing work in connection with the war:
M J. Marshall is with the Shawinigan Electro-Metals Com-
pany, Shawinigan Falls, Que.; C. F. Hamill is at the New York
State College of Forestry, Syracuse, N. Y.; W. J. Geldard is
engaged on war work for the American Government; G. L.
Magoun is with the du Pont Powder Company, Wilmington,
Delaware.
Prof. Lawrence J. Henderson is at present engaged in the
Wolcott Gibbs Memorial Laboratory at Harvard L'niversity
ch on the physical chemistry of breadmaking and the
study of the use of substitutes in the making of bread. Assist-
ing Professor Henderson in this work are Lieutenant Cohn,
and Sergeants Cathgart and Wachmann.
Mr W. B. D Penniman, of the firm of Brown and Penniman
of Baltimore, has accepted the position of chemist on the staff of
the (J. S. Shipping Board.
Dr. Elbert C. Lathrop has resigned his position as biochemist
in the laboratory of soil fertility investigations, U. S. Depart-
ment of Agriculture, to accept a research position with the
Jackson laboratory of E- I du Pont de Nemours and Com-
i Wilmington, Del.
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Mr. Leighton M. Long, for the last two years with the Kawin
Company of Toronto, Canada, is now assistant chemical engineer
at the works of the Dominion Tar and Chemical Co., Sault
Ste. Marie, Ontario.
Mr. A. McGill, chief chemist, Department of Inland Revenue,
Canada, is in Pittsburgh, Pa., investigating questions relating
to gasoline.
Dr. E. P. Wightman, formerly a research chemist for Parke,
Davis and Co., Detroit, Mich., who enlisted in the 30th
Engineers Regiment, U. S. N. A., and was later transferred to
the Chemical Service Section, has been promoted to First Lieu-
tenant and has been sent to the overseas laboratories.
Word has been received of the promotion of First Lieutenant
Lawrence J. Fairhill, Ph.D., Harvard, 1018, to a Captaincy.
Second Lieutenant Lee I. Smith has been made a First Lieutenant,
and Private Alexander D. MacDonald has been commissioned
a Second Lieutenant in the Chemical Service Corps.
Mr. G. O. Richardson, 22 Maple Ave., Andover, Mass., has been
appointed Second Lieutenant, Chemical Service, National
Army.
Mr. P. E. Sprague has been granted leave of absence for the
period of the war from the position of Assistant Purchasing
Agent, The Glidden Varnish Co., Cleveland, Ohio, and
has enlisted as a private in the Chemical Service Section of the
National Army. He is stationed at the American University
in Washington and has been assigned to serve as chemical
engineer in the Mechanical Research Department, War Gas
Investigations.
Mr. Henry Mandle has resigned as chief of the technical
staff of Herman and Herman, Inc., New York City, and has
resumed his former practice as a consulting chemical engineer
with offices at 220 West 42 nd Street, New York. He is also
acting in the capacity of technical adviser for the National
Bronze and Chemical Works.
Mr. W. H. Beers, secretary of the Alabama Section of the
A. C. S.,has been appointed bacteriologist of the City of Birming-
ham, Ala., and will be located at the City Hall in that city. His
duties begin May 1st.
Mr. Leo Stein, president of Stein, Hall and Co., 61
Broadway, New York, died on March 31. He was born in
1866 at Chicago, 111., and had been engaged in the chemical
trade for thirty years. He was a graduate of Yale University
and became associated with his uncle, M. M. Hirsch in the firm
of Stein, Hirsch and Co. Mr. Hirsch recently retired and was
succeeded by Frank G. Hall.
The Powers-Weightman-Rosengarten Co., Philadelphia, cele-
brated its century mark as a producer of medicinal chemicals
the early part of April.
Messrs. Ostenberg and Christiansen, consulting chemical
engineers of San Jose, Cal., have both taken up war work.
Dr. Ostenberg has entered the Naval Flying Station at San
Diego, and Dr. Christiansen is a Lieutenant on the medical staff
of the navy.
Captain G. L. Norris, chief metallurgist of the equipment
division of the Signal Corps of the United States Army, will be
in command of the general laboratories that have been estab-
lished in Pittsburgh where all metals entering into the con-
struction of aircraft are to be scientifically tested. The labora-
tories, manned by a force of 200 picked chemists, engineers,
metallurgists and machinists, will occupy the best equipped
testing plant in the district, which has been taken over by the
Government for that purpose. Captain Norris will be assisted
by Dr. H. T. Beans and Prof. J. F. Macgregor on leave of
absence from Columbia University, as chief chemist and chief
of physical tests, respectively.
Mr. \'. \'. Kelsey, Industrial Agent for the Carolina, Clinch-
Geld and Ohio Railway, has severed his connection witli tin
ad to become resident manager for the American Wood
'lion Company at their plant now building at Kingsport,
Tenn., for the distillation of hardwood. He is retained by the
railway company in a consulting capacity.
Mr. Byron M. Hcndrix, of the department of physiological
listry of the medical school of the University of Pennsyl-
1. has been loaned by the University to the War Trade
Board where he is acting as trade expert in the chemical division
of the Bureau of Exports of the Board.
Mr. J. T. Janson of the Experimental Farm, 1 tttawa, Canada,
a member of the A. C. S. for the past four years, has been ;it tin
front in Franci ;ince July 1915. He is now a I, irnl 11. ,!,,,, 1
II i' been mentioned three times in dispatches, and in June
last was given the Distinguished Service Order and since then
has had a bar added to i1
Dr. Frederic Bonnet, Jr., professor of chemistry at Worcester
Polytechnic Institute, has resigned to accept the position of
chief chemist at the Perryville plant of the Atlas Powder Company.
Mr. F. K. Bezzenberger, who has been in charge of the Rad-
cliffe Laboratories for the past few years, has entered the Govern-
ment service, and is now stationed at Cleveland, Ohio.
Mr. John Diggs, State Water Chemist of Indiana, is a First
Lieutenant in the Sanitary Corps, and is to serve in France.
Messrs. George B. Walden and Earl Roberts, both with Eli
Lilly and Company, have enlisted in the Radio Division of the
Signal Corps.
' Mr. A. E. Roberts, of the department of chemistry, Yonkers
High School, Yonkers, N. Y., is now connected with the
research department of the Barrett Company at Philadelphia.
Mr. A. H. Putnam, formerly with the Warner-Klipstein Co.,
South Charleston, W. Va., is now assistant chief chemist,
Inspection Section, Metallurgical Group, Ordnance Department,
Washington, D. C.
Dr. Louis S. Munson, for eleven years associated with the
Ault and Wiborg Company of Cincinnati as a chemist, and in
recent years chief chemist, has resigned to take care of the
production department of the new dye plant being erected
by the du Pont Dye Works on the Delaware River, near Wil-
mington. The company is a subsidiary of the du Pont interests
engaged in the manufacture of explosives. Employees of the
Ault and Wiborg Company tendered Dr. Munson a dinner on
the occasion of his departure.
Mr. R. E- Christman, formerly engineer of tests for the War
Department at the plant of the Consolidated Car-Heating Com-
pany, has been appointed Supervising Engineer of Tests on metal-
lurgical and testing work at the various plants in the vicinity of
Detroit with headquarters at the American Car and Foundry
Co., Detroit.
Mr. William Wallace Mein, of New York City, has been ap-
pointed assistant to the Secretary of Agriculture in regard
to the licensing of the fertilizer industry as ordered by the Procla-
mation printed on page 323 of the April issue of This Journal.
The United States Civil Service Commission announces an
open competitive examination for assistant chemist in forest
products, salary ranging from $1200 to $1800 a year, for men
only. On account of the urgent needs of the service, applications
will be received until further notice. Applicants should at once
apply for Form 1312, stating the title of the examination desired,
to the Civil Service Commission, Washington, D. C.
Dr. C. L. Reese, of E. I. du Pont de Nemours and Co., has
been named Chairman of the Committee on Dyestuffs and Inter-
mediates of the Chemical Alliance.
Dr. Robert C. White has just resigned as laboratory manager
of the H. K. Mulford Company, after nearly fifteen years connec-
tion with that house. He has become associated with Joseph V.
Little and Thomas A. Burrows in the manufacture of pharma-
ceutical specialties. The new concern will be known as the Bur-
rows-Little-White Company and will have its principal laboratory
in Philadelphia.
Mr. Philip S. Barnes, formerly with the Avery Chemical
Company of Lowell, Mass., is now associated with the Sales De-
partment of the Pfaudler Company of Rochester, N. Y., as con-
sulting chemical engineer, with headquarters in the New York
office.
Dr. William P. Wood, assistant professor of chemical engineer-
ing at the University of Michigan, has resigned to join the Signal
Corps of the Army.
A fellowship in physiological chemistry has been established at
the University of Chicago by the Fleischmann Company of
Peekskill-on-Hudson, New York, for the purpose of investigating
some of the scientific questions which have arisen in the 0
of the manufacture of compressed yeast under present war con-
, litmus. The university has appointed the first fellow on this
foundation, who is now engaged in research upon the problems.
Dr. Ethel M Terry, of the department of chemistry of the
University of Chicago, has been appointed I" an assistant profes-
sorship.
Mr. William J. Gross, formerly with the Sherwin-Williams
apany at Chicago, is now chief chemist of the Nordyki
Mariniiu I'", Inc., of [ndianapolis, manufacturers of automobiles
ancl 0 rii, Nordyke and Marmon Company is do-
1 tensive war work for the Government.
M, 1 M. Goetchius has n li med as vice president and directoi
,,1 the Genera] Chemical Company in order to give his set
,1 He has be* n succeeded both as vice p
id diri ' t"i bj Mr. A. W. Hawkes.
406
THE JOl RNAL OF INDl si KIM. AND ENGINEERING ( // / WISTRY Vol. 10, No. 5
Captain J. K. Anderson, of tin- Geneva Experiment
and Lieutenant W A. Perlzweig, Henry R. Cates and Charles
K. I'rcv, are making a nutritional survey of the army camp';
situated in the southern states. The sur\. the work
at present conducted I >y the Surgeon General's OfEc< to detei
mine the character of the food supplied to the American soldiers.
Dr, \V B. Bentley, head of the department ol chemistry of
Ohio University, lias been commissi, .mil as .apt. mi by the War
I lepai -Intent, and is stationed at Watertown, Ma
the department of inorganic chemistry, of the Watertown
Arsenal.
Pro) Watson Bain, of the department of applied chemistry
in the I niversity of Toronto, has been granted leave ..1 absence
for the duration of the war. He is going to Washington, D. C,
where he will be on the staff of the Canadian Mission.
Dr. John W. Kimball, instructor in chemistry and physics
at the denial school of Western Reserve University, has been
calle-.l to Washington to undertake chemical work for the Army.
Dr. Kimball has been granted leave of absence from the university
and will leave immediately to take up his new work.
Dr. Francis C. Frary, research chemist of the Aluminum Com-
pany of America, has been commissioned as captain in the 1 ird-
nanee Reserve Corps and assigned to research work in the trench
wai face Tel ion, Engineering Bureau, office of the chief of ordnance,
Washington, D. C.
The .hath is announced of C. I. Istrati, professor of organic
chemistry and dean at the University of Bucharest and president
of the Roumanian Academy of Sciences.
Mr. F. I.. Locke has resigned as superintendent of the chemical
plant of the Chattanooga Chemical Company to join the tech-
nical stall" of the British American Chemical Co., Inc., of
New York City, to assist in the design, and later superintend
the operation of extensive additions now being made to their
plant.
Dr. A. D. Brokaw, assistant professor of mineralogy and chem-
ical geology at the University of Chicago, has been called to Wash-
ington to take charge of the oil production east of the Rocky
Mountains.
In I! II. King, associate professor of chemistry at the Kansas
ricultural School, has been advanced to the head of the
it the University of Chicago
completing the work for his Ph D
Mr. A, V. I ti I temist in charge of the Provincial
Board of Health of 1 mtario, has joined the overseas forces and is
now in England qualifying as an officer in the Royal Engineers!
He had formerly been attached to the Hydrological Corps with
the rank of Captain and served at the Toremtu Exhibition Camp
last winter.
Dr. John K. Bucher, professor of chemistry in Brown I'ni-
\. rsity, has been granted leave of absence for the second semester
of the- academic year, ill order to devote himself to experimenta-
tion in chemical n the industry. He will continue to
direct the work of certain advanced students in the University
laboratory, but will be relieved of all teaching during the remain-
der of the year. Dr. Robert F. Chambers, a Brown graduate,
will be acting head of the- department during the second semester.
Dr. E. V. McCollnm, professor of chemistry in the school of
hygiene and public health. Johns Hopkins University, gave the
Cutter lectures on preventive medicine and hygiene at the Har-
vard Medical School on March 19, 20 and 21.
Mr. Henry A. Gardner, until recently assistant director of the
Institute of Industrial Research, at Washington, D. C, has re-
ceived a commission as Senior Lieutenant in the Naval Flying
Corps. At present he is stationed in Washington.
Mr. William H. Barrett, president of Barrett and Barrett,
vinegar manufacturers of Chicago, Minneapolis and Bangor,
Maine, died recently in Jacksonville, Florida, at the age of sixty-
eight.
INDUSTRIAL NOTES
Yl.AK
1905
7K2.7.V)
837,017
11K Federal Trade Commission fur Licenses r.\r
the Enemy ACT'
rENTKE Assignee
Berlin, Germany E. Merck, Darmstadt, German
1913 1.075,171
11 ! I. .11 y\ vi
ron Wetsbach, Vienna, Treibacher Chemisette Werke
Gesellschaft, m. b, b . of Trei
1 1 u h Austria Hungary
Thick- and Georg Chemische Pabrik auf
mi 01 Berlin, Get ivorm. E. Schering) of Berlin,
Germany icid
Ostwald of Cologne Ball-mill
Germany
Enemy-Co
Patent
C-C-dialkylbarbituric
process of making ;
Pyrophoric alloy
En Patents Pcrsuant to the "Trading with
Applicants
nd Antoine Chiris Co., 18 Piatt St.,
New York
The Pfanstiehl Company, Inc.,
North Chicago, 111.
Albrecht
Wichn
many
The Martlcn, Orth and Hastings Corporation has obtained
control of the- Calco Chemical Company, a $7,000,000 corpora-
tion ..I New Jersej The- Calco Company was incorporated in
1916, an. I since- then has been engaged in manufacturing dyes,
intermediates and other chemicals.
The American Cellulose and Chemical Co., Ltd., capit di ed
at $25,000,000, has filed application for a chartei at Dover. Del..
and will deal in cellulose- and its products. The incorporators
are Henry J, Bigham of N.» York City, Frank C. Williams.
New Rochelle, N. V., and Oscar R. Houston of Great Neck Sta
tioti, N. Y.
An imp. 11 la nt private company has been registered in London.
England, under tin- title- of the- British Cellulose and Chemical
Manufacturing Parent Company with a capital of $17,500,000.
in. board ol directors includes Herbert McGowan of Nobel's
Explosives, Sii Trevoi Dawson, of Vickers, Ltd., which companj
it 1 rumored is about to merge with the British Decs, Ltd
The Edible Cocoanut Oil Corporation of Wilmington, Dela-
ware, has applied for a Delawan chartei to manufacture perfumes
and derivatives of coco a 1 1 1 1 1 ml h ha ...ipnai.
The incorporators are C I. Rimlinger, M M Clancy and F. A.
Armstrong
Chemical industry in Japan is growing rapidly. A numbei ol
new companies have- been organi ed to manufacture a variety
of substances including ammonium sulfate, potassium chloride,
potassium sulfate-, bleaching powder, nitric acid and dves. The-
manufacture of chlorate ol potash is an important industry
which has developed since the war. and it is reported that the
quantity shipped to this country from Yokohama during this
period exceeds [0,000 bands Another industry that has made
remarkable progress is the- extraction of vegetable wax, the out-
put of which amounts to about >s ;i • i pel J e 11
Chemicals for war purposes will be manufactured at Saltville.
Virginia, in a $250,000 plant which the War Department has de-
cided to build there for operation with the Mathieson Alkali
Works Preparations have begun for constructing the necessary
buildings.
The recent action of the President in fixing the price of alu-
minum calls attention to the rapid growth of this industry in the
United Slates The great increase in our production in this
the United States fai in the lead among the aluminum-
producing countries of the- world. In fact, about one-half of the
world's output of aluminum is now produced in the United
States Bauxite-, the mineral from which most of the world's
aluminum is produced, is found in many parts of this country,
though the- bulk of that now used in the industry is the product
state- of Arkansas
the Interioi Lane has designated Bartlesville,
Okla., as the location of the new experimental station of the
Bureau of Mines I'm the- investigation of problems relating to the
petroleum and natural gas industries. The station is one of
three new experimental stations for the- establishment of which
the sum of $75,000 was appropriated by the last Congn
two other si.iti.nis have been located at Minneapolis, Minn., for
tlu- study of iron and manganese problems, and at Columbus,
Ohio, for research connected with the ceramic and clayworking
industries
In the- Apiil issue of Tins Joi knai. we printed a report, taken
from Drug and Chemical Markets for March 1.?. that the Dow
Chemical Company's plants at Midland and Mount Pleasant.
Michigan, were t.. be- commandeered by the Government. Ac-
cording to the Oil, Paint mid /Vug Reporter for March 1 8,
and alse> for April is. the Dow Chemical Company says that
there is no foundation to the rumor.
May, 191 J
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
We learn from The Little Journal for April that Mr. C. F.
Eckart, a leading authority on sugar planting in Hawaii, has
developed a process in the raising of sugar cane in Hawaii which
reduces the cost of labor 50 to 70 per cent and increases the
yield 28 per cent. His process consists in laying yard-wide
strips of paper longitudinally over the rows, holding them in
place by covering the edges with cane field trash. The paper
must be strong enough to keep down the weeds but not strong
enough to kill the young cane. Five or six weeks after applying
the paper the weed seeds that could germinate have done so
and their sprouts are smothered, while the shoots of the sugar
cane, being stiff and sharp, have either come through the paper
or show their presence by little tent-like elevation in the paper
which can be slit with long knives by laborers passing between
the rows. A pretty problem in industrial research was pre-
sented to the Arthur D. Little, Inc., laboratories when the
question of making a paper from bagasse suitable for this
purpose was put to them. Many sorts of paper have been made
from bagasse but they have tended to be hard and tinny, whereas
there was required here a paper which would be strong enough
to withstand the Hawaiian rainfall and yet give way under
constant, gentle pressure. Also it had to be dark in color and
very, very cheap. This problem was solved and plans are being
made for a paper mill to take care of Mr. Eckart's plantation.
Some interesting pictures appear in The Little Journal com-
paring cane 4'A months after planting, one showing cane which
had received the Eckart treatment, another that which was
cultivated and hoed in the usual manner.
According to the Canadian Chemical Journal another recent
achievement of the American chemist is the perfecting of a process
for treating cotton cloth for the making of a suitable gas mask
for use in the second line trenches. A product has been found
which withstands the effect of cold and hard usage. The avia-
tion branch of the service presents many problems difficult to
overcome, among the chief of which is the numbing effect upon
the aviator of the cold, wind and rain at high altitudes. A
Canadian chemist has perfected an invention whereby the inside
of an outer garment can be kept at a comfortable temperature by
means of a network of fine wires connected with a small electric
generator in the machine. An American chemist has perfected
a process of treating cotton cloth for garments so as to render it
water-proof and unaffected by the low temperatures and high
winds experienced at high altitudes.
Prof. A. W. Grabau, of Columbia University, addressing the
New York Academy of Sciences recently at the American
Museum of Natural History, commented on the world-wide
need of potash, and said that "if Germany should lose Alsace
a potash supply for many years would be assured to the rest of
the world for a period long enough either to re-establish friendly
relations, or, if that may not be, to bridge over the space of time
which must elapse before the known non-German deposits can
be made available or new deposits found by careful and system-
atic search."
Professor Grabau was speaking on "The Salt and Potash
Deposits of Alsace-Lorraine and Their Significance in the Pres-
ent Conflict." An exhaustive study which he has made of this
subject shows that the potash deposits of Alsace consist of two
beds of chloride of potassium which lie in an intercalated rock
salt deposit nearly 800 feet thick. The total quantity of the im-
pure potash salt is estimated at 1,500,000,000 tons, equivalent to
300,000,000 tons of pure potash.
Professor Grabau said in part:
"The world needs potash. In spite of arduous search no great
potash deposits are known from accessible regions, and we must
turn to the more expensive utilization of potash brines and potash-
bearing minerals of refractory type. It is true that there are
potash deposits in northeastern Spain, but they have not been
in idi accessible, and it looks as if they would not be within reach
for many \ ears to come. There are potash salts in eastern Abys-
sinui and from them 20,000 tons a year have been obtained in
recent times. But these are over fifty miles from the coast, and
they must be transported on camel back across a country whose
bitants are at best none too friendly. If Germany should
lo e Alsace, a potash supply for many years would lie assured to
the rest of the world."
The War Trade Hoard announces "List No. 1 of re tricted
imports." which establishes a prohibition against tin1 bringing
into this country, under certain conditions, of 82 commoditii
falling into the' "less essential" category. Metals, foodstuffs,
luxuries and other products not necessary to the war are plaeed
under the ban, which !>eeame effective on April 15 and does not
apply to rail shipments from Canada or Mexico of goods origina-
ting in these countries.
The list includes the following items of interest in the drilK,
chemical and dyestuff trade:
Asbestos, blacking, candle pitch, palm and other vegetable stearine.
All acids, muriate of ammonia, alcohol, tar distillates, except synthetic
indigo, fusel oil or amylic alcohol, citrate of lime, all salts of soda except
nitrate of soda and cyanide of soda.
Sumac, ground or unground, chicory root, raw or roasted, clocks,
watches and parts thereof, cocoa and chocolate, prepared or manufactured.
Manufacturers of cotton, cryolite, except not to exceed 2,000 long tons
for the year 1918.
Explosives, except fulminates and gunpowder, manure salts, fluorspar.
All nuts except coconuts and products thereof. Gelatine and manu-
factures thereof, including all from Europe.
Sulfur oil or olive foots, grease, hay, honey, hops, infusorial and diato-
maceous earth and txipoli.
Mantels for gas burners.
Matches, friction and lucifer.
Nickel.
Oilcake.
Oilcloth and linoleum for floors.
All expressed vegetable oils from Europe only.
Lemon oil.
Non-mineral paints and varnishes.
Photographic goods
Plumbago or graphite (until July 1, 1918, thereafter not exceeding
5,000 long tons for remainder of 1918).
Pyrites (except not exceeding 125,000 long tons to October 1, 1918).
Rennets, artificial silk and manufactures thereof.
Soap.
Tar and pitch of wood.
Vinegar.
Manufactures of wool.
Manufactures of hair of camel, goat and alpaca.
Zinc.
The United States consuls have been instructed not to issue
consular invoices on and after April 15, 1918, for the articles
mentioned in the list without first being furnished with the
number of the import license or being given other evidence
of the issuance of such license. Shipping agencies are also
advised not to accept for shipment consignments of the articles
mentioned in the list without similar evidence of the issuance
of the import license. This applies only to the articles mentioned
in the list.
A synthetic indigo plant now being erected by the National
Aniline & Chemical Company, Inc., at Marcus Hook, Pa., is
intended to cover at least haif the requirements of the United
States. Much of the equipment is now on the ground and is in
course of erection. The buildings are now mainly completed.
A few months hence it should be possible to undertake contracts
for specific deliveries. The development of this important chem-
ical industrial problem has been coordinated under the direction
of Dr. E. S. Johnson of the Semet-Solvay Company, and Mr.
Robert M. Strong, Chief Works Engineer of the Marcus Hook
plant of the National Aniline & Chemical Company. When the
European War broke out and the supply of indigo (an essential
staple of the American textile colorist ) was threatened with elim-
ination, the General Chemical Company, The Barrett Manufac-
turing Company, and the Semet-Solvay Company, recognizing
the chemical catastrophe represented by the lack of mdtgo,
entered upon its cooperative development. Research men from
each organization were delegated to conduct the necessary experi-
mental investigations, and about eighteen months were consumed
before, in the matter of quality and yields, the product of the
great German plants had been equaled. A semi -commercial
operation is now producing small quantities of indigo, in connec-
tion with the extensive installation now under way at Marcus
Hook.
Recruits for poison gas offensive and defensive experimental
work are being organized at the Case School of Applied Science
in Cleveland. Interest in the work for the Government has been
aroused by William Green, representative of the gas investigation
department of the Tinted States Bureau of Mines. He says the
students whoenlist mil Ik placedinthe Chemical Service Section
Of the Army. There are now about 1 .so members m this service
and 7i< 1 are wanted.
Dr. S W. McCallie, state geologist of Georgia, reports the
oj .,,, important deposit of organic asphaltum con-
the organic matter from which certain gradi s of ( ■■ rm in
dyes are made. The deposit was first discovered in a Georgia
tnd 1'r McCallie savs it is sufficiently large ami easdj
,,,, ible io justify an immediate commercial <leveloi.ni.ui t..
,, .„ I and marl 1 I thl dyi I H has been believed that the only
deposit ol tins mineral in the United States was m Florida,
the lai. t discovery is considered more extensive than the
Florida deposit, in bettei position foi mining, and it has easier
to the market.
4oS
I III JOURNAL Of INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 5
The crushing of copra in New Orleans is becoming more
and more extensive. The Southport Oil Mills, Ltd., have just
taken over the large plant of the Orleans Cotton Oil Co., where
they are crushing copra imported from the South Sea Islands
through San Francisco. As a nucleus of a castor bean industry
in Louisiana, a 3000-acre tract which was once a famous sugar-
cane producing property, but idle for some time, is to be planted
in castor beans.
Experiments were recently made in Sydney, at the instance
of the Commonwealth Advisory Council of Science and In-
dustry, as to the possibility of producing alcohol at a low cost
from some natural products. A Sydney chemist has experi-
mented with the Zamia palm, or, as it is popularly known, the
Burrawong palm, which grows in great profusion along the Sea
Coast of Xew South Wales. It is stated that the yield of alcohol
from this plant is 45 gallons per ton of material.
Ault and Wiborg Company, Cincinnati, has increased its
capital stock from $2,000,000 to $10,000,000 and is to materially
enlarge its production of coal-tar dyes.
K. Arndt in the Vossische Zeitung for February 5, 1918,
states that alcohol is being produced from calcium
carbide. Acetylene is passed through acidified water, contain-
ing a mercury salt, whereby acetaldehyde is formed; the latter
is vaporized, mixed with hydrogen and the mixture passed over
a nickel catalyst, when alcohol results. Alternatively acetalde-
hyde is converted into acetic acid by passing the vapor, mixed
with oxygen, over a nickel catalyst. It is stated that a plant
is being built near Visp in Wallis, Switzerland, capable of an
annual production of 100,000,000 kg. alcohol by this process,
this being sufficient to cover the whole requirement of Switzer-
land.
Drug and Chemical Markets reports that a representative
of the German War Committee for Oils and Fats recently
addressed a meeting of the agriculturists and mill owners of the
district of Solingen (Prussia) on the subject of the extraction of
oil from the germ of grain. The speaker stated that although
only 40 per cent of the German mills have so far made the
necessary arrangements for the work, 1,321,000 gallons of oil
have been obtained from this source in nine months. The germ
contains 10 to 12 per cent of oil, which can be utilized for the
production of margarine. After the extraction of the oil, the
residue of the germ yields a valuable albuminous food. A still
greater advantage resulting from the removal of the germ,
said the speaker, is the impossibility of the flour obtained from
the grain becoming musty. The flour is in no way inferior
after the removal of the fatty substance; it bakes better and the
bread does not so easily turn moldy.
According'to Drug' and Chemical Markets, a color which has
notjbeen obtainable in the United States since the war, and was
formerly manufactured only in Germany, has made its appear-
ance on the American'market_and is now made in this country.
It is said that the American product cannot be differentiated
fromithe German color formerly imported. The offer of Rhod-
amine B, the dye referred to, came as a surprise to the dye and
textile trade and led to much speculation as to the source of the
supply. Some incredulous dealers, who did not believe it could
be.; made in) America, suggested that the product was imported
from'Germany by way of Russia and Japan to the Pacific Coast.
It is interesting to learn that the color is made by an expert who
formerly made Rhodamine B in Europe, but his name and
previous connections are kept secret for trade reasons.
Possibilities for increasing the supply of ferro-alloys were dis-
cussed in Washington on March 22 by makers of these products
with representatives of the War Industries and War Trade
Board. In the morning a group of chrome men met with Govern-
ment officials and made a complete canvass of the situation. The
aim of the conference was to devise measures of developing domes-
tic production and eliminating dependence to the present extent
on foreign sources. The manganese situation was discussed
during the afternoon and tungsten also was taken up. L. L.
Summers, head of the section on explosives and chemicals of the
War Industries Board, was a leading figure at the manganese
meeting, while that on chrome was in charge of Pope Yeatman
of the raw material division.
A $5,000,000 plant, including a by-product coke oven and two
blast furnaces, is to be erected for the St. Louis Coke and Chem-
ical Company on a 300-acre tract of land in Madison County,
Illinois. The location of the new plant was determined upon
because of its nearness to coal supply and to numerous metal-
consuming industries. An annual production of a million gallons
of toluol will be among the products of the new plant.
The Allied Industries Corporation is a new undertaking
launched for the purpose of permanently establishing American-
made goods in seventy markets in foreign countries, the plan
being to represent groups of manufacturers and sell their goods
under their own trade-marks on a selling commission basis regu-
lated by the amount of goods shipped and sold. The association
is affiliated with the French-American Constructive Corporation
which has secured business amounting to $140,000,000 for execu-
tion after the war. Included in the directorate of the new
corporation are Alfred I., William and Francis I. du Pont of Wil-
mington, Delaware. The markets named by the company in-
clude the principal countries and colonies in Asia, Africa, Aus-
tralia, eleven European countries, and South and Central America
and the West Indies.
GOVLRNMLNT PUBLICATIONS
By R. S. McBrjde, Bureau of Standards, Washington
NOTICE — Publications for which price is indicated can be
purchased from the Superintendent of Documents, Government
Printing Office, Washington, D. C. Other publications can
usually be supplied from the Bureau or Department from which
they originate. Commerce Reports are received by all large
libraries and may be consulted there, or single numbers can be
9ecured by application to the Bureau of Foreign and Domestic
Commerce, Department of Commerce, Washington. The regu-
lar subscription rate fur these Commerce Reports mailed daily is
$2.50 per year, payable in advance, to the Superintendent of
Documents.
CONGRESSIONAL COMMITTEES
Coal and Asphalt Deposits. Minutes of Senate Indian
Affairs Committee hearing on the House Resolution 195 for the
saU of coal and asphalt deposits on segregated mineral land in
Choctaw anil Chickasaw Nations, Okla 64 pp. Dated January
10-17, 1918. The report of the committee to the Senate on
Report 207. Dated January 18. 4 pp.
Fuel in the United States. House Report 246. Submitted
January 18. 2 pp. This is a Mines and Mining Committee
report to the House of Representatives on House Resolution
7235 which relates to the uniform selection and purchase of
fuel to be used in tlu United States
PRESIDENTIAL PROCLAMATION
License of Ammonia Industry. 2 pp. Presidential Proclama-
tion. Dated January 3. No. 1421.
SMITHSONIAN INSTITUTION
The Annual Report of the Board of Regents of the Smithsonian
Institution. A volume of over 607 pp. which includes the
following articles of chemical interest. The report is known as
Publication 2441). Price, cloth Si. 00.
(1) Ideals of Chemical Investigation. Theodore William
Richards.
(2) Molecular Structure and Life. Amk Pictet.
; The Earth, Its Figure, Dimensions, and Constitution of Its
Interior. T. C. CbambBRLTN, Harry Fielding Reid. John F.
Hay ford and Frank SCHLSSINGBR.
14"! Petroleum Resources of United States. Ralph Arnold.
(5) Outlook for Iron (with bibliography ). James Firman
KSMP.
^6) On Origin of Meteorites. Friedrich Berwerth.
1,7) Relation of Pure Science to Industrial Research. J. J.
Carty.
May, 1018 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
SUPERINTENDENT OF DOCUMENTS
Chemistry, Industrial Alcohol, and Preservatives. Pricelist
40, 9th Ed. 8 pp. This list covers the publications on these
and related subjects which are for sale by the office of the
Superintendent of Documents.
Mines, Explosives, Fuel, Gas, Gasoline and Petroleum.
Pricelist 58, 5th Ed. 21 pp. This list covers the publications
for sale by the Superintendent of Documents.
FEDERAL TRADE COMMISSION
Hide and Leather Situation. House Document 357 5 pp.
Issued January 24, 1918.
NATIONAL MUSEUM
Mineral Industries of United States: Coal, Resource and
Its Full Utilization. Chester G. Gilbert and J. E. Pogue.
Bulletin 102. 4 pp.
PUBLIC HEALTH SERVICE
Stream Pollution. Public Health Bulletin 87. A digest of
Judicial Decisions and a Compilation of Legislation Relating to
the Subject.
Investigation of the Pollution of Certain Tidal Waters of New
Jersey, New York, and Delaware, with Special Reference to
Bathing Beaches and Shellfish-Bearing Areas. H. S. Cum-
ming. Public Health Bulletin 86. Issued December 1917.
Disinfectants, Their Use and Application in Prevention of
Communicable Diseases. T. W. McClintic; revision by G.
W. McCoy, A. M. Stimson and H. E. Hasseltine. Public
Health Bulletin 42. 71 pp. Paper, 10 cents. Issued January
1918.
The Application of Ozone to the Purification of Swimming
Pools. W. A. ManhEIMER. Public Health Reports, 33. 7
pp. Issued March 1 .
Ozone when properly applied to the water of a swimming pool
effectively purines the water. When one part of ozone per
million parts of water is used, the result is sterile water. When
half part ozone per million parts of water is used, a bacterial
reduction of 99.8 per cent results, except when too great an
excess of air is introduced with the ozone.
A study of the cost of operation of the ozonator has shown
that a current consumption of 2 kw. per day with alternating
current and of 4 kw. per day with direct current, plus 1 cent a
day for calcium chloride, represents the total operating cost for a
60,000-gal. pool. This amounts to 11 to 15 cents a day for
alternating current (at 5 to 7 cents per kw.) and to 21 to 29
cents a day with direct current. The cost of refilling the pool is
at least $30. The use of the ozonator decreases the number of
times the pool must be emptied to such an extent that the cost
of the installation is soon paid for.
The application of ozone to the purification of swimming pools
is automatic in control, reliable in action, and inexpensive in
application. Accordingly, we recommend the consideration of
this chemical as a standard procedure in the sanitary control of
swimming pools.
GEOLOGICAL SURVEY
The Flaxville Gravel and Its Relation to Other Terrace Gravels
of the Northern Great Plains. A. J. Collier and W. T. Thom.
Professional Paper 108-J, from Shorter Contributions to General
Geology, 1917. 6 pp. Published January 26, 1918.
Ore Deposits of the Northwestern Part of the Garnet Range,
Montana. J. T. Pardee. Bulletin 660-F, from Contributions
to Economic Geology, 1917, Part 1. 81 pp. Published January
10, 1918.
The Dunkleberg Mining District, Granite County, Montana.
J. T. Pardee. Bulletin 660-G, from Contributions 10 Economic
Geology, 1917, Part 1. 7 pp. Published December 27, 1917.
Strontianite Deposits near Barstow, California. A. Knopf.
Bulletin 660-I, from Contributions to Economic Geology,
1917. Part 1. 24 pp. Published January 18, 1918.
Possibilities for Manganese Ore on Certain Undeveloped
Tracts in Shenandoah Valley, Virginia. D. F. Hewett, G. W.
Stose, F. J. Katz and H. D. Miser. Bulletin 660-J. Pre-
pared in cooperation with the Geological Survey of Virginia.
From Contributions to Economic Geology, 1917, Part 1. 26
pp. Published January 21, 1918.
Phosphatic Oil Shales near Dell and Dillon, Beaver Head
County, Montana. C. F. Bowen. Bulletin 661-I, from Con-
tributions to Economic Geology, 1917, Part 2. 6 pp. Pub-
lished January 12, 1918.
Lode and Placer Mining on Seward Peninsula, Alaska. J.
B. MertiE, Jr. Bulletin 662-I, from Mineral Resources of
Alaska, 1916-I. 32 pp.
Geologic Structure of the Northwestern Part of the Pawhuska
Quadrangle, Oklahoma. K. C. Heald. Bulletin 691-C, from
Contributions to Economic Geology, 1918, Part 2. 44 pp.
Published February 7, 1918.
Gold, Silver, Copper, Lead, and Zinc in Colorado in 1916.
Mines Report. C. W. Henderson. Separate from Mineral
Resources of the United States, 1916, Part I. 58 pp. Pub-
lished February 5.
Gold, Silver, Copper, Lead and Zinc in Utah in 1916. Mines
Report. V. C. Heikes. Separate from Mineral Resources of
the United States, 1916, Part I. 35 pp. Published January 24.
Gold, Silver, Copper, Lead and Zinc in Nevada in 1916.
Mines Report. V. C. Heikes. Separate from Mineral Re-
sources of the United States, 1916, Part I. 44 pp. Published
January 19.
Arsenic, Bismuth, Selenium and Tellurium in 1916. J. B.
UmplEby. Separate from Mineral Resources of the United
States, 1916, Part I. 5 pp. Published February 2.
The production of arsenic in the United States in 1916, as in
1915, exceeded that of any previous year, amounting to 5,986
short tons, valued at $555,187, an increase over 1915 of less than
9 per cent in quantity and of nearly 84 per cent in value.
Imports of white arsenic and arsenic sulfide, or orpiment, de-
creased from 3,183 short tons to 2,163 short tons, or 32 per cent.
Thus the total supply in 1916, as compared with 1915, fell from
8,681 short tons to 8,149 short tons.
Only two companies produced bismuth in 1916, the United
Metals Refining Co. and the American Smelting & Refining Co.,
from plants located, respectively, at Grasselli, Ind., and Omaha,
Neb. So far as known to the Geological Survey, ores from
Tintic, Utah, supplied most of the metal, although some was
also produced from flue dust shipped to Omaha by the Garfield,
Utah, copper smelter. Only one carload of bismuth ore is
known to have been shipped and this contained considerable
gold, silver, and copper.
As in recent years, details of production cannot be given,
although from data available it seems that the total output is
not very different from that in 19 15.
The New York price, as quoted in the Engineering and Mining
Journal, ranged in 1916 from $3.15 to $4 a pound, or from 15
.11I to $1.25 higher than during 1915.
The imports during the year were greater than in 19 15, al-
though lower than for several years previous thereto.
No new developments in the selenium industry came to the
attention of the Geological Survey during 1916. It should be
borne in mind, however, that this element has very exceptional
photo-electric properties and may at any time be made the basis
of some war or industrial invention which would greatly increase
the demand for it. Selenium is obtained as a by-product in the
refining of copper, and it is the opinion of copper metallurgists
4io
THE JOURNAL OF INDl si KIM. AND ENGINEERING I EEMISTRY Vol. 10. No. 5
that if market, conditions warranted, its production in this
country might be greatly increased.
The value of imports for consumption of selenium and
selenium rose from $59 in 1915 to $302 in 1916.
During 1916 the American Smelting & Refining Co. was the
only producer of selenium, as against two producers in 191 5.
Thi total output was somewhat greater, however, than in 1915.
Prices at the refinery averaged approximately Si. 35 a pound,
and on the New York market, according to the Engineering and
Mining Journal , prices ranged from $2.50 to 85 a pound, largely
depending on the quantity purchased.
No production of tellurium in 1916 was reported to the
Geological Survey.
Borax in 1916. C. G. Yale and H. S. Gale. Separate from
Mineral Resources of the United States, 1916, Part II. 3 pp.
Published January 7, 1918.
Tn 19 16 the production of crude borate material in the United
States was 103,523 short tons, valued at 82,409,459, compared
with 67,003 short tons, valued at 81,677,099 in 1915, and 62,400
short tons, valued at 81,464,400 in 1914. All the crude borate
material now used in this country is the mineral colemauite
(calcium borate), and the output in 1916 came from a few '.nines
in southern and southeastern California. The value of the
product given is the value of the ore at the point of shipment
estimated on a basis of Si per unit (per cent) of anhydrous boric
acid (boron trioxide, B2Oa) in the raw material. All the ore
shipped from California, however, was calcined or concentrated
before being put on the cars at the mines.
Price quotations given in the trade journals show a gradual
rise in the price of borax and boric acid, reaching about 7 or 8
cents a pound for borax and about 12 cents a pound for boric
arid toward the close of 1916. It is understood that contracts
for large quantities of borax were placed during the year at 53A
cents a pound and that contracts for 1917 delivery were at 63/<
cents a pound.
Sulfur, Pyrite, and Sulfuric Acid in 1916. P. S. Smith.
Separate from Mineral Resources of the United States, 1916,
Part II. 30 pp. Published January 23, 1918.
Some sulfur is imported by the United States, but usually it is
less than 10 per cent of the quantity consumed, and during 1916
the great expansion in consumption made the imports relatively
still less significant. More than 95 per cent of the sulfur im-
ported is crude, and although it is the least expensive of the
various forms of sulfur received, its value in 1916 was about
88 per cent of the combined value of all the sulfur imported in
that year.
In 1913 the United States exported 89,221 long tons of sulfur,
valued at 81.599,761; in 1914 the exports were 98.163 long
tons, valued at $1,807,324; in 1915 they declined greatl] and
Were only 37..U2 long tons, valued at 8724,079; in 1916, how
ever, the exports increased to 128,755 long tons, valued at
$2,505,857, or an increase of approximately 250 per cent in
both quantity and value. Prom these figures it will be seen that
in n,io the export 1 cceeded the imports by 106,520 long tons
101,073. The exports in 1916 wen about 45 per cent
jrreatei than the exports in 1913, which may be taken as fairly
representative of the normal conditions immediately before the
war The large quantity of sulfur exported was usui chiefly
for the manufacture of munitions and undoubtedly could be
transported more advantageously in the form of sulfur than as
explosives or sulfuric acid.
The demand in 191I1 for pyrite to meet the unusual con-
sumption "i iulfuric acid created bj the war increased notably
over the demand in 1915. Never before was so much pyrite
produced 01 imported by the I nited States, and prices increased
throughout the year. Even with the stimulus of an in
demand and good prices, however, the number of pyrite mines
in operation in the United States showed practically no increase.
Six new producers were operating in 1916, but their plants were
all small, several of them recovering the pyrite from coal, and
their total yield was only about 2.000 tons. On the other hand,
three mines that were in operation in 1915 and during that
year yielded over 7,000 tons of pyrite, were idle in 1916, and at
one of the former larger producers almost the entire year was
siient in repairing the damage from the caving of the mine
shaft, so that it produced much less than its normal output of
pyrite.
The increase in production is therefore to be attributed to the
greati 1 yield from the old mines rather than to the opening of
new deposits. This condition is believed to be due to the lack of
initiative in attempting to find suitable deposits rather than to
of undeveloped deposits ol commercial value. The
low cost of foreign pyrite, under normal conditions, has deterred
the pyrite users from seeking a domestic supply and from en-
couraging the expenditure of the money necessary to prospect
and develop properties that appear to promise success
The domestic production of pyrite in 1916 was 423.556 long
tons, valued at {1,965,702, an increase of about 30.000 long
tons in quantity and of about S290.000 in value, as compared
with the production in 1915. The consumption of pyrite ore
in 1 91 6 — that is, the domestic production plus imports —
amounted to about 1,670,000 long tons and was about 310,000
long tons greater than the consumption in 19 15. This increase
was largely attributable to the greater demand for sulfur in
industries connected with the war and was made possible mainly
because of increased imports.
Cement in 1916. E. F. Burchard. Separate from Mineral
Resources of the United States, 1916, Part II. 35 pp. Pub-
lished January 26, 1918.
The year 191 6 proved a busy period for the cement industry
in most parts of the United States. Labor troubles caused the
temporary suspension of operations at a few Portland cement
plants in the Mississippi Valley, but no plants were embarrassed
by lack of business In 1914 and 1915 there was a decrease in
the production of cement, consumers having exercised strict
111 its use. but the year 1916 showed a reaction, it
having opened with a demand unprecedented for a midwinter
season. Prices of Portland cement, which averaged only 86
cents a barrel for the entire year 19 15. began to rise toward the
end of that year and continued to do so until well toward the
close of 1916, so that the average price per barrel in bulk at the
mills for the year was $1,103, an increase of 24.3 cents, or 28.3
per cent. The increased prices, of course, did not mean an
equivalent net increase in returns to the manufacturers, because
the cost of fuel, explosives, machinery parts, bags, labor, and in
fad the costs of all the items that enter into the manufactured
product rose considerably during the year. The comparatively
high prices did not. however, check the demand for cement.
Many manufacturers sold all they could produce and others
drew heavily on stocks. The net decrease in stocks for the
country at large was more than j.ixxi.ooo barrels, or 27 1 per
cent, as compared with the quantity on hand at the close of
1915. Every commercial district but one showed a decrease in
stocks on hand
The total quantity of Portland, natural, and puzzolan cements
marketed or shipped from the mills in the United States in
1916 was 95,394,433 barrels, valued at S104.6S9.090. as com-
piled with 87,685,222 barrels, valued at S75.155.102 in 1915.
This represents an increase in quantity of 7,709.211 barrels.
or 8 8 per cent, and an increase in value of (
39 3 per cent.
Tin in 191b. A Knock. Separate from Mineral Resources
of the l nited States. 1916, Part I. 6pp. Published February 6,
The production of metallic tin of domestic origin in 1916 was
approximately 14" short tons .\s in recent years, this output
May. 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
was derived almost wholly from Alaska. The main part of the
Alaskan output was won by dredges operating in the York district,
in the western part of Seward Peninsula, and the remainder
was recovered incidentally to gold placer mining in the Hot
Springs district, in the sector between Yukon and Tanana rivers.
The bulk of the concentrate was shipped to Singapore to be
smelted, but a part was sent to the recently completed tin-
smelting plant at Perth Amboy, N. J.
The total importation of tin in 1916 was 74,619 short tons.
Tin recovered from drosses and waste metals amounted to 17.400
tons. The total supply of primary and secondary tin in the
United States exclusive of a small quantity reduced from
Alaskan concentrate, therefore amounted in 1916 to 92,019 tons.
The world's production of tin in 19 16 was roundly 136,000
short tons, or slightly less than it has been in the preceding two
years. The output of the various tin-producing regions is shown
in the accompanying table. The figures given are based in the
main on official reports, except those for Banca, Billiton, and
Nigeria, which are taken from "Mineral Industry."
World's Production of Tin, 1914—1916, in Short Tons
1914
Federated Malay States 54,92
British Protected Malay States. . . . 4,001
Bolivia 25,039
Banea
Billiton
China(!>)
Siam(c)
Nigeria
Australia
Cornwall
Union of South Africa
Other Countries
1914
1915
1916
54,927
52,378
49,134
4,000(o)
4,600
4,900
25,039
244IW
23,508
15,650
15,426
16,294
4.480
6,440
5.600
9.000
•1 (Kill
9,000
7,600
8,700
9,400
5.059
5.102
5,684
5,400
5,400
5,000
5,663
5,564
4.200(a)
2,200
2,260
2,100
1,500
1,000
1.500
140,518
140,279
136,320
(a) Estimate.
(b) Based on the estimate of the production of China for 1915 given
by V. K. Ting ("China's Mineral Resources," Far Eastern Rev., 13 (1917),
569.)
(c) Shipments to Straits Settlements.
Iron Ore, Pig Iron and Steel in 1916. E. F. Burchard.
Separate from Mineral Resources of the United States, 1916,
Part I. 58 pp. Published February 13. The iron ore, ex-
clusive of that containing 5 per cent or more of manganese,
mined in the United States in 1916 amounted to 75,167,672
gross tons, as compared with 55,526,490 gross tons mined in
1915, an increase of 19,641,182 gross tons, or 35 per cent. Bene-
ficiated ore, instead of crude ore mined, is included, if the ore is
treated in any way. The quantity of iron ore shipped from the
mines in the United States in 1916 amounted to 77,870,553
gross tons, valued at 8181,902,277, as compared with 55,493,100
gross tons, valued at S101.288.984, shipped in 1915. This repre-
sents an increase in quantity of 22,377,453 gross tons, or 40 per
cent, and in value of $80,613,293, or 80 per cent. The average
price of ore per ton for the whole country in 1916 was $2.34
as compared with Si. 83 in 1915. These quantities of ore, both
mined and shipped, include the iron ore used for fluxing other
metallic ores at smelters in the Western States, but the ship-
ments do not include the iron ore sold for the manufacture of
paint. The quantity of iron ore sold for the manufacture of
paint in 1916 amounted to 16,968 gross tons, valued at §45,256
67 per ton. In Arkansas one producer shipped 5 tons of
loadstone, averaging 70.5 per cent of metallic iron, which was
sold at a high price to manufacturing druggists. This ship-
ment is not included in the tabulated statistics of iron ore. The
ore reported as sold for fluxing other than in the manufacture of
pig iron amounted to 88,601 gross tons, valued at $288,089
in 1916 1 d with 17,213 gross tons, valued at $27,456
in 1915. The domestic iron ore actually sold for the manufac-
ture of pig iron amounted in 1916 to 77,781,952 gross tons,
valued 11.188 as compared with 55.475.887 gross
tons, valued at (101,261,528 in '
According to reporl t" the United States Geological Survey
by the manufacturers, the shipments of pig iron, exel
ferro-alloys, in 1916 amounted to 39,126,324 gross tons, valued
f. o. b. at the furnaces at $663,478,1 18, as compared with 30,384,-
486 tons, valued at $401,409,604 in 1915, an increase in quantity
of 8,741,838 tons, or 29 per cent, and in value of $262,068,514,
or 65 per cent. The average price per ton in 1916 was $16.96,
and in 1915 it was $13.21, an increase in 1916 of $3.75 a ton,
or 2S per cent. These values represent the approximate price
per ton f. o. b. at the furnaces; this approximate price eliminates
freight costs, selling commissions, and other items, which are
included in the market prices of certain grades of pig iron as
published in the trade journals.
The pig iron shipped includes the metal produced from foreign
as well as from domestic ore. The quantity and value of pig
iron derived from ore imported from Africa. Canada. Chile,
Cuba, Nova Scotia, Spain, and Sweden, although it constitutes
a very small percentage of the total production, is considerable,
as it is calculated that the shipments derived from foreign ore
in 1916 amounted to 764,850 gross tons, valued at $15,996,756,
as compared with 945,022 tons, valued at $13,011,950 in 1915.
In the manufacture in 1916 of 727,550 gross tons of pig iron,
1.295.5 18 gross tons of foreign iron ore were reported to have been
used, thus indicating an average pig-iron yield of 56. 16 per cent,
as compared with the quantity of imported ore. Domestic ore,
including 4,036,022 tons of cinder, scale, scrap, etc., and amount-
ing to 74.8°5.359 gross tons, was reported in 1916 as used in the
manufacture of 37,974,413 tons of pig iron, thus indicating a
yield of 50.76 per cent in pig iron from the domestic materials.
The statistics of production of the principal grades of pig iron
have been published by the American Iron and Steel Institute
for 1916, as follows:
Grade Gross Tons
Bessemer and low phosphorus 14,422,457
Basic (mineral fuel) 1 7,684,087
Forge pig iron 348,344
Foundry and ferrosilicon 5.553,644
Malleable 921,486
Spiegeleisen 194,002
Ferromanganese 221,532
White, mottled, direct castings, etc 89,245
Total 39,434,797
In the following table are given the statistics of the American
Iron and Steel Institute showing the production of pig iron,
according to the fuel used for 19 16. The charcoal figures
include small quantities of pig iron made with charcoal and
electricity. The total includes small quantities of ferro-alloys
made with electricity, coke and electricity, etc.
Pic Ikon Produced
Fuel I 5ED Gross Tons
Bituminous, chiedv coke 38,844,598
Anthracite and coke 217.788
Anthracite alone
Charcoal 372,41 1
Total 39,434,797
The following table gives an incomplete outline of the sales
of ferro-alloys in the United States in 1914, 1915 and 1916:
Quantity
LRXSTY <>F Gross
Alloy Tons
Domestic Manufacture Sold in 1914, 1915 and 1
1915 . . 1916
Quantity Quantity
Gross Gross
Tons Value Tons Valu
II $4,440,253 144,260 1,103 $30,123,493
76,625 1,586,1 v
77.182 1.621,830 128.263
5,273,088
Spiegele
Fetro-
■
denum
dium
■
tungsten) )
Totm.s ...255
or 1914 or 19] 5.
986 1,702,023 1,565 3,198. 1 2
3,524 8. 7 26,909
THE Jol R V.i/. Of IXDVSTRIAL AS I) ENGINEERING ( HEMISTRY Vol. 10, No. 5
Fbrro-Au.oys Imported for Consumption in the United States in
1914, 1915 AND 1916
. 1914 . . 1915 ■ - 1916 .
Quantity Quantity Quantity
Variety of Gross Gross Gross
Alloy Tons Value Tons Value Tons Value
Chrome or chrom-
ium and ferro-
chrome 200 $21,553 32 $1,662 10 $1,998
Ferrophosphorus. 26 1,136 12 617
Ferrosilicon 6,249 341,925 5,128 311,219 6,740 384,384
Molybdenum and
ferromolyb-
denum 0.10 59 203
Titanium and
ferrotitanium.. 18 8,356 100 8,126
Tungsten and
ferrotunKsUn . 195 222,447 7 9,588 38 157,711
Ferromanganese.. 82,997 3,619,607 55,263 3,333.699 90,928 9,240,528
Spieiieleisen 2.870 71,147 200 5,110
Totals 92.555.10 $4,286,230 60,642 $3,662,098 97,816 $9,792,747
BUREAU OF THE CENSUS
Census of Manufactures, 1914: Petroleum Refining. 13
pp. One of a series of bulletins being issued by the Bureau,
presenting statistics of industries concerning which inquiries
were made at the quinquennial census of manufactures in 1914.
Statistics are presented in three sections: Summary and analysis
giving general data compiled for industry; special statistics,
relating to materials, products, and methods of manufacture;
and State tables giving comparative summary, by States, for
1904, 1909 and 1914, and detailed statistics for industry, by
States. 1914.
BUREAU OF EDUCATION
Higher Technical Education in Foreign Countries, Standards
and Scope. A. Tolman Smith and W. S. JesiEN. Bulletin 11.
1917. 121 pp. Paper, 20 cents.
BUREAU OF LABOR STATISTICS
Trend of Accident Frequency Rates in Iron and Steel In-
dustry during the War Period, by Causes. L. \Y. Chaney.
Prom Monthly Review of Bureau of Labor Statistics. December
I9I7- 5 PP-
BUREAU OF MINES
Suggestions for the Safe Operation of Gasoline Engines in
Mines. R. H. KuDLICH and E. Higcins. Technical Paper
174 19 pp. Paper, 5 cents.
Blast-Furnace Breakouts, Explosions, and Slips, and Methods
of Prevention. F. II Wnxcox. Bulletin 130. 267 pp.
Paper, 30 cents.
The Mining Industry in the Territory of Alaska During the
Calendar Year 1916. S. S. Smith. Bulletin 153. S5 pp.
Paper. 15 cents.
Cost Accounting for Oil Producers. C. G. Smith Bulletin
158. 1 17 pp. Price, 15 cents.
Occupational Hazards at Blast-Furnace Plants and Accident
Prevention Based on Records of Accidents at Blast Furnaces in
Pennsylvania in 1915. F. II. WlLLCOX. Bulletin 140. 145
pp. Paper, 30 cents. This report was prepared under a
1 with tin- Pennsylvania Department of
! tboi •i"1 Ind
Firing Bituminous Coals in Large House-Heating Boilers.
S li Flagg. Technical Paper 180, 15 pp Paper1, 5 cents
Combustion of Coal and Design of Furnaces. II. Kkims
E. At'.rsTixi; and ]•' K. OvrTZ. Bulletin 135. 138
pp Paper, 20 cent The material presented consists mainly
mi of about 100 tests made in the special furnace
having nbustion space; tabulated ami plotted
results of tlu si tests, and the- discussion of these results with
deductions furnishing the basis for rational furnace
I with time knuls of coal, namely, P
hontas, Pittsburgh, and Illinois coal. The coals were burned
at five rates — 20, 30, 40, 50, and 60 lbs. per sq. ft. of grate
per hour. Several tests were made with each coal at each rate
of combustion, each test being run with a different percentage
of excess air.
The material is arranged in four parts : the first part con-
tains the description of the apparatus and the methods of con-
ducting the experiments; the second part gives the results of
the experiments, explains their meaning and points out their
practical application; the third part consists of discussions of.
miscellaneous observations; and the fourth part contains a
discussion of the process of combustion in the combustion space
and of the laws that govern it.
Determination of Unsaturated Hydrocarbons in Gasoline.
E. W. Dean and H. H. Hill. Technical Paper 181. 20 pp.
Paper, 5 cents. The experiments described herein have dealt
chiefly with the estimation of unsaturated constituents in mix-
tures which also contain paraffin or paraffin and aromatic hydro-
carbons. Allowance has been made for the presence of aromatics
in only the moderate proportion usual with petroleum products.
The problem of estimating aromatic constituents is not con-
sidered, as none of the experiments recently performed has shown
any method to be better than that described in a recent paper
by Rittman, Twomey and Egloff.1
Flotation of Chalcopyrite in Chalcopyrite-Pyrrhotite Ores o*
Southern Oregon. W. H. Coghill. Technical Paper 182-
7 pp. Paper, 5 cents "Gravitation methods of concentrating
the copper-bearing mineral cannot be applied, because the
gangue sulfides have practically the same density as chalcopyrite.
Magnetic separation de>es not seem practicable — assuming that
the gangue sulfides can be made to respond naturally or by a
preliminary treatment to an electromagnet — because fine grind-
ing is required to liberate the mineral grains. The methods of
concentration now in vogue are hand sorting and jigging which
eliminate some of the siliceous gangue. An inspection of the
smelter returns in the possession of mine operators gives the
impression that the average grade of ore shipped runs 10 per cent
copper.
"The experiments on separating the chalcopyrite from the
gangue by flotation have been carried through the preliminary
laboratory stage with flattering results."
New Views of the Combustion of the Volatile Matter in Coal.
S H Katz Technical Paper 183. 9 pp. Paper, 5 cents.
Accidents at Metallurgical Works in the United States During
the Calendar Year 1916. Compiled by A. H. Fay. Technical
Paper 201. it. pp. Paper. 5 cents.
Concentration Experiments with the Siliceous Red Hematite
of the Birmingham District, Alabama. J. T. Singewald, Jr.
Bulletin 110. 68 pp. Paper. 13 cents.
BUREAU OF ORDNANCE
Microscopic Examination of Steel. Reprint. 47 pp. Paper
15 cents.
BUREAU OF STANDARDS
Wave-Length Measurements in Spectra from 5600 A. to 9600 A.
W. F. Meggers. Scientific Paper 3 12. 25 pp. Paper, 10 cents.
1918.
Specific Heat of Liquid Ammonia. N. S. Osborne and
M. S Van Dusen Scientific Paper 313. 36 pp. Paper,
5 cents. Published December 13, 1917. "The results of the
determinations by the two independent methods have been
expressed by the following two empirical equations:
First method: a = 3.0931 — O.OO064 6 +
method: ir = 3.1800 — 0.000508 +
V133 — 0
10.35(1
V133 —6
(A)
(B)
1 \V. I\ Rittman. T. J. Twomey and Gustav Er1o<T. "The Estimation
of Aromatic Hydrocarbons in Cracked Petroleum Mixtures." Mrl. and
Chem EnS., IS (1915), 682-686.
,
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
413
where the positive value of the square root is to be used. * * *
The greatest difference between the mean results by both methods
and the results of either method as represented by empirical
equations is seen to be less than 1 part in 1000."
Latent Heat of Vaporization of Ammonia. N. S. Osborne
and M. S. Van DusEn. Scientific Paper 315. 34 pp. Paper,
10 cents. Published December 21, 1917. "As a final result
the latent heat of vaporization of ammonia, that is, the heat in
joules per gram required to convert saturated liquid into saturated
vapor at constant temperature is expressed in the range — 42
to 520 C. by the equation: L = 1 57 91 V 1 3 3 — 9 — 2.466
(133 — 0). If the latent heat of vaporization be expressed in
calories per gram, taking 1 calorie = 4.183 joules, the equation
becomes L = 32.968V 133 —8 — 0.5895 (133 — 6).
Gas Interferometer Calibration. J. D. Edwards. Scientific
Paper 316. 5 pp. Paper, 5 cents. Published December 8,
1917. "The method here proposed requires no special ap-
paratus and only a knowledge of the refractive indices of the
gases which are to be used. The calibration is accomplished by
filling both chambers of the interferometer with dry air free
from carbon dioxide, and determining the scale reading when the
pressure in one chamber is reduced by known amounts."
Wire Gauges. Anonymous. Circular 67. 5 pp. Paper,
5 cents. Published January 17, 1918.
Paint and Varnish. Anonymous. Circular 69. 82 pp-
Paper, 15 cents. Published November 17, 1917. "This pub-
lication is intended to give in a general way, without unnecessary
detail, such information as would be valuable to various people
who desire information upon this subject. While the composi-
tion and methods of manufacture of paint may not in every case
be essential, it is believed that a broad knowledge of these sub-
jects will, in general, lead to a more intelligent selection and
application of paints. On the other hand, little reference will be
made in this Circular to methods of analysis, which would be useful
only to persons engaged in the manufacture or testing of paints."
For varnishes, the raw materials, methods of manufacture and
of testing, and the procedure of application are described.
Similar information is given for paints but with most attention
to the nature, sources, and characteristics of the paint pigments.
Various whites, blacks, reds, yellows, browns, blues, greens,
and bronzes are discussed.
Materials for the Household. Anonymous. Circular 70.
254 pp. Paper, 25 cents. Published December 5, 1917.
"This circular describes the more common materials, other than
foods and drugs, used in the home. A previous circular in this
series described household measurements and a third circular
(now in preparation) treats of household safety. The present
circular relates to the quality and use of materials. While
written primarily for the household, it may incidentally interest
dealers in materials for the household, who should be in close
touch with its needs, and teachers of home economics who
are training future home makers in scientific home management.
"The purpose of the circular is practical: (1) To stimulate
the interest in household materials, (2) to explain the nature of
their desirable properties, (3) to aid in their intelligent selection,
and (4) to promote their effective use and preservation. A
better utilization of materials will aid the efficient administra-
tion of the home and promote the health and comfort of the
household. Home economics is of growing interest at this
time. The subject is of universal and permanent concern,
and win n its importance is realized it must become a factor of
primary importance to national well-being. The excellent
instruction in the subject now given in high schools and col-
leges begins a new era in home management."
The following is a list of the most important subjects dis-
cussed: Clay products, wood, metals, lime, cement, plasters
and stucco, paints, paint oils, and varnishes, bituminous roofing,
rubber, leather, textiles, paper, inks, adhesives, water, soap,
miscellaneous cleansing agents, bluing and starch, materials
for fireproofing cotton fabrics, polishes, disinfectants, preserva-
tives, fuels, illuminants and lubricants, and quantity in the
purchase and use of materials.
Table of Equivalents — Millimeters to Inches. Anonymous.
Supplement to Bureau of Standards Circular 47. 10 pp.
Paper, 5 cents. Published October 27, 191 7.
Properties of Portland Cement Having a High Magnesia
Content. P. H. Bates. Technologic Paper 102. 42 pp.
Paper, 15 cents. Published January 19, 1918. "It is not to
be thought that this investigation was intended to show the de-
sirability of increasing the amount of magnesia now allowed
by the standard specifications. Its primary purpose was to
determine what new constituents, if any, were produced in
clinker by increasing the magnesia content, also how this latter
increase affects the constituents already present, and, finally,
to correlate the quantitative changes in the amounts of the
various constituents with the changes which would be produced
in the general physical properties of the cement.
"Portland cement with a magnesia content of about 9.50
per cent may be burned in a rotary kiln without producing a
clinker materially different from one containing less than 4 per
cent. The clinkering temperature will be reduced somewhat,
however. With greater amounts of magnesia present the re-
sulting clinker is very vitreous and dusts more or less slowly,
the rapidity and amount of dusting increasing with the magnesia
content.
"The strengths developed, either by the neat cement or
1 : 3 sand mortar or 1 : 1V2 '■ 4-Vs gravel concrete, show that
cements containing as much as 7.5 per cent of magnesia are
satisfactory. It would be impossible to predict from the strength
tests at the end of one and one-half years which were the
cements containing low magnesia or magnesia up to 7.5 per cent.
With higher amounts the strengths developed decreased with
increased magnesia, but even with the high-magnesia cements
there is a noticeable increase of strength with age."
Typical Case of the Deterioration of Muntz Metal (60 : 40
Brass) by Selective Corrosion. H. S. Rawdon. Technologic
Paper 103, 28 pp. Paper, 10 cents. Published December 15,
191 7. "One very common type of deterioration of metal of
this composition, particularly when exposed to some electrolyte
(e. g., sea water), is selective corrosion or 'dezincification,'
the term 'selective corrosion' being used to signify a corrosive
attack of certain of the microstructural constituents of the alloy
rather than a general uniform action upon the metal as a whole.
Though this type of deterioration of brass has been known for
years and numerous references on this subject have appeared
in the technical literature, the description of the various forms
in which it may occur and of the changes produced in the metal
by which it may be detected are very meager. The numerous
samples illustrative of this type of metal failure submitted to
this Bureau for examination, together with the inquiries re-
ceived on this subject, suggested the utility of a description of
typical cases of metal affected by this type of nonferrous cor-
rosion as an aid in the detection and identification of similar
cases of this type of deterioration of metals. A study of the
various forms in which this type of corrosion may occur, together
with the resulting structural changes within the metal, also aids
in defining the conditions which are most favorable for such
deterioration to occur."
Safety for the Household. Circular 75- 127 PP- Paper,
15 cents. This is a popularized description of hazards com-
monly occurring in the home from fire, electricity, lightning, gas,
chemicals, etc.; suggested precautions and rules for emergencies
are given.
4U
////■; JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 5
COMMERCE REPORTS, FEBRUARY, 1918
Exports of pulp and paper from Canada have increased from
about $8,000,000 in 1910 to $43,000,000 in 191 7, and are ex-
pected to 000,000 in 1918. (P. 419)
Hardened whale fat lias been u ed in margarine in Denmark
for three years, and is now being introduced into Norway.
1 1 19
Salt is produced by solar evaporation at Aden under particu-
larly favorable conditions, owing to the low rainfall and hu-
midity. (P. 456J
New deposits of manganese ore being developed in Brazil
contain over 300,000 tons of ore with 45 to 50 per cent manganese.
(P. 522)
Production of lignite in Italy shows a marked inert a 1 P
55°)
The annual mineral output of the Rio JintO district in Spain
has increased to 6,000,000 tons, principally of copper-iron
ores. The ore is roasted in McDougal furnaces, and then smelted
to blister copper, of which the output is 15,000 to 20,000 tons.
Only a small part of the sulfur is recovered as sulfuric acid of
which nearly [4,000 tons were made in 1914. Antimony
graphite and manganese ores are also obtained in this district.
(Pp. 568-573)
The reported securing of 257 dye recipes from Germany is
treated lightly in England, since it is recognized that much more
than a knowledge of "recipes" is necessary for a successful dye
industry Progress in the British dye industry has been very'
great, but the problem of providing adequate plant facilities
and material and labor has not yet been solved. 1 Pp. 580-2)
The zinc industry of Japan has made great progress since
1914, so that Japan is now exporting large quantities of zinc,
instead of importing. (P. 600)
Exports of tungsten ore and antimony from China show marked
increases. (P. 602)
Salt is obtained in India from rock salt mines, brine lakes,
and sea water. The latter method is not very successful, owing
to the high humidity. (P. 638)
Tungsten deposits in Hongkong include several outcrops
with as much as 18 per cent. (P. 663)
Plans are being made to increase the quinine output of India,
especially by the cultivation of cinchona plants of high quinine
i 'P. 726)
Both total output and output per acre of sugar beets in Canada
show a marked increase. (P. 729)
An enormous increase has been made in Germany in the out-
put of vegetable drying plants, especially dried potatoes,
and turnips.
Special Supplements Issubd in February
Italy — 8a
Hritish Indi
1 s 1 „
1 -78o
STAi 1 ] ' TH LTNITB1 CAT1
Japan (P \6 Bokdi 11 1 1 Terns. I , u.\ Sup. 80
!
aese ore
ilicon
Perrotun
.11,. dust
It i.lintn ore
Palermo
M.innitr
Olive "il (soap stock)
Sumac
I Ml.
\lo\ilr
Tartar
Rubbi 1
1 Hive ■•
Hid,
Rl
Hides
I root
led rubbei
Artificial silk
0 yarn
British
Indigo
Republic ( ,
i',-.
Boni 1 1 Hi.
Divi-divi Fustic
Hides
Fustic
l SYLON Sup. .SI,;
M, oil
lit oil
Papain
Graphite
COMMERCE REPORTS. MARCH, I918
Efforts are being mad' to arrange for increased exports of
graphite from Madagascar to the United States. (P. 788)
1 of soya-bean oil from Manchuria to the United States
in ) 1 ,| from about 45,000,000 pounds in 1916 to nearly 200,-
pounds in 191 7. (P. 809)
tory lor the manufacture of caffeine from tea is being
erected in Formosa. P
Early in the war, the British government bought up the avail-
able supply of natural indigo, viz., 267 tons, which has since been
old, thui preventing a shortage. 'P. 853)
A substitute for absorbent cotton for surgical dressings is
being made in Sweden from wood pulp. (P. 8t
gas for motor traction is increasing greatly in England,
where it is predicted that its use will become permanent, using
later, however, compressed gas instead of as now gas at nearly
atmospheric pressure in flexible holders. (P. 946)
One British private firm of dyestuff manufacturers is produc-
dyes than all other British companies combined, in-
cluding the government-controlled British Dyes, Ltd. < P. 1000)
Investigation by the Bureau of Standards upon anti-freezing
solutions for automobile radiators led to the conclusion that
1 1 calcium chloride solutions should be used with caution if at
all, on account of their corrosive action; 12) kerosene or similar
oils should not be used on account of their inflammability, high
boiling point, and effect on rubber; (3) mixtures of alcohol and
glycerine, though satisfactory, are precluded by the need for
glycerine for munitions; and (4) aqueous solutions of wood
alcohol ot denatured alcohol form the most desirable anti-freezing
solutions. (P. ma.'
A new oil seed of a species of strephonema found in Belgian
Congo yields about 40 per cent of a soft, yellow fat, probably
edible. The residual meal contains appreciable tannin and is
hence not suitable Ol ..nil food. P. 1092)
Efforts are being made in South Africa to develop the manu-
facture of potash from sea-weed, of a variety known as "sea-
bamboo," which is lower in potash content than American sea-
weed I ' 1 1 ' 1 7
Although there are a number of manganese properties in Eastern
Cuba, only a few can be operated at a profit. Production is,
however, increasing. (P. 1146I
Large amounts of orchid liquor, obtained from the lichen
' the United States from the
Cape Verde Islands. p. 1193)
The British Government has contracted for the entire copper
output of Australia up to June 30, 191S, estimated at from
15,000 to 20,000 tons. (P. 1 197)
Special Supplbmbnts Issued in March
France
Cuba
French V/esI Indie!
Argentina — 38a
Statistics op Exports
Rubbei
opal Tin
d imar
elotong
Cult. 1 percha
Gutta si.ik
Hulls
Mangrove bark
Rubbei
Tin
Hongkon
1 i — 60<J
French East Africa — 70a
Portuguese Hist Africa
the United States
Argbhtin8 —Sup. 38a
wax
Platinum
HONGR ING Sup. 52o
Chemicals
Peanut oil
links
Ipecac
Manga n
Rubbei
Tallow
Potassium carbon.
Hides
Sut;.ir
Asphalt
Alcohol
Ani!
oil
Suear
Tin
Australia
link's
» temeridium
Eucalyptus .
Beesv -i\
Graphite
Hides
Glycerine
Ipecac
Tartar
Copper
Glue stock
Grease
Guano
Hicks
Leather
Linseed
Mica
Castor oil
PetitgraiD oil
Stearin
Tungsten ore
Quebracho
Rubber
Tallow
Zinc
May, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
415
NLW PUBLICATIONS
By Iksns DeMatty. Librarian. Mellon
Alcohol: Practical Handbook on the Distillation of Alcohol from Farm
Products and Denaturing. F. B. Wright. 271 pp. Price, $1.50.
Spon & Chamberlain, New York.
Analysis: A Manual of Qualitative Chemical Analysis. J. R. Morton.
12mo. 189 pp. Price, SI .25. Sir Isaac Pitman & Sons, New York.
Artificial Dyestuffs, Their Nature, Manufacture and Uses. A. R. Ramsey
and H, C. Weston. 8vo. 212 pp. Price, $1.60. E. P. Dutton & Co.,
New York.
Carbon and Its Allies. R. M. Craven. 8vo. 489 pp. Price, 15s.
Charles Griffin & Co., London
Chemical Industry in France: L'Avenir de Tindustrie chimique en France.
A. Kling. 8vo. Chaix, Paris.
Chemical Physiology: Directions for a Practical Course in Chemical
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Longmans. Green & Co., New York.
Chemistry: Cours experimental de chimie. M. Grandmontagne. 8vo.
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Chemistry: The Laboratory Study of Chemistry. H. R. Smith and H. M.
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Chemistry: Treatise on Applied Analytical Chemistry. V. Villavecchia.
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Coal: Chemistry of Coal. Myles Brown. 8vo. 75 pp. Price, Is. 6d.
Thomas Wall & Sons, London.
Coal Distillation, Gasification and By-Products. J. E. Christopher. 8vo.
90 pp. Price, 2s. 6d. Science and Art of Mining, London.
Coal Gas Residuals. F. H. Wagner. 2nd Ed. 8vo. 214 pp. Price.
J2.50. McGraw-Hill Book Co.. New York.
Coal Tar: The Treasure of Coal Tar. Alex. Findlay. 8vo. 151 pp.
Price. 4s. 6d. G. Allen & Unwin, London,
Coal Tar Distillation. A. R. Warner. 8vo. 314 pp. Price, $3.50.
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Colliery Sinking. James Keen. 8vo. 48 pp. Price, Is. Thomas Wall
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Dyeing and Cleaning. F. J. Farrell. 4th Ed. 8vo. 263 pp. Price,
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Economic Geology: The Principles of Economic Geology. W. H.
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Electrodynamic Wave Theory of Physical Forces. T. J. J. See. 4to.
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Engineering: Applied Mechanics. H. Aughtie. 8vo. 227 pp. Price,
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Engineering: Elements of Sanitary Engineering. Mansfield Merri-
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Flour Milling: A Theoretical and Practical Handbook. P. A Kosmin.
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Geologic Handbook of the Miami Mining District. E. S. Perry. 30 pp.
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Powdered Coal as Fuel. C. F. Herington. 8vo. 211 pp. Price, $3.00
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Proteins: The Physical Chemistry of the Proteins. T. B. Robertson
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Rubber: A Wonder Book of Rubber. B P. Goodrich Rl
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Soil Physics and Management. J G. Mosier and A. F. Gostafson. 8vo.
442 pp. Price, $2.00. J. B. Lippincott Co., Philadelphia.
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Waste in Modern Boiler Rooms, Finding and Stopping. G. H. Gibson
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Vol 22 (1918), No. 2, pp. 128-149.
Alcohol from Sulfite-Pulp Waste Liquor. Ellwood Hendrick. Metal-
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Alundum Manufacture and Use. M. A. Williamson. The Metal In-
dustry, Vol 16 (1918), No. 3, pp. 128-129.
Ammonia: Recovering Ammonia at Tar-Distilling Plants. C. R. Wood-
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Black Dyes. C. S. Wehrly. Color Trade Journal. Vol. 2 (1918), No. 3,
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Burning Slack Containing Excessive Moisture. J. F. McCall. Power,
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Caffeine: About Caffeine-Free Coffee. C. W. Trigg. The Tea and
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Chrome Production and Distribution. S. H. Dolbear. Engineering and
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Coal: Combustion Characteristics of Coals. J. G. Worker. The Electric
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Fatty Acids: Determination of Fatty Acids in Butter Fat. E. 1:
and J. P. Bdcklby, Jr Journal of Agricultural Research, Vol. 12
(1918), No. 11. pp, 719
Fuel: Methods for More Efficiently Utilizing Our Fuel Resources. Kskil
Hekc;. Genei 1 ol -'1 1 1918), No I, pp !16
Fuel Resources of Canada with Reference to the Pulp and Paper Industry.
11 1- Haanei. Pulp and Paper Magazine, Vol. 16 (1918), No. 1(1. pp.
Gas: Making Substitutions for Natural Gas. I Dbns The Blast
6 191! No 1 pp 1 56 158.
Nitric Acid and Copper Ore d Chemical
Vol 18 ( 1918), Xo o pi
Nitric and Mixed Acids. W E. Hlrkhard. The General Chemical
Bulletin. Vol 4 I 1918), ' pp '4-226.
Nitro Dyes. J. M Matthews. Color Trade Journal. Vol 2 (1918), No.
4,
Oil Shale of Colorado. R I. Chase Mining and Scienlifit Press, Vol.
116 (1918), Xo. I '•. pp t 1 ^ I -If
Ore and Coal Bridges. II D Iambs 1 to Bleetrii Journal, Vol is
Xo 1. pp 1 10-114.
Pyrometry and Its Several Limitations.
MARKET REPORT-APRIL, 1918
WHOLESALE PRICES PRr.VAII.ING IN THE NEW YORK MARKET ON APRIL l6, I918
Aqua
Arses
INORGANIC CHEMICALS
Acetate of Lime 100 Lbs.
. lump 100 Lbs.
iron free) Lb.
m Carbonate, domestic Lb.
in Chloride, white I,b
nonia, 26°, drums Lb.
hite Lb.
Barium Chloride Ton
Barium Nitrate Lb.
Barytcs, prime white, foreign Ton
Bleaching Powder, 35 per cent 100 Lbs
Blue Vitriol Lb.
Borax, crystals, in bags Lb.
Boric Acid, powdered crystals Lb.
Brimstone, crude, domestic Long Ton
Bromine, technical, bulk Lb.
Calcium Chloride, lump, 70 to 75% fused Ton
Caustic rioda, 76 per cent 100 Lbs.
Chalk, licht precipitated Lb.
China Clay, imported Ton
Feldspar Ton
Fuller's Earth, foreign, powdered Ton
Fuller's Earth, domestic Ton
Glauber's Salt, in bbls 100 Lbs.
Green Vitriol, bulk 100 Lbs.
Hydrochloric Acid, commercial, 20° Lb.
Iodine, resublimed Lb.
Lead Acetate, white crystals Lb.
Lead Nitrate Lb.
Litharge, American Lb.
Lithium Carbonate Lb.
Magnesium Carbonate, U. S. P 1.1,
Ma^nesite. "Calcined" Ton
Nitric Acid, 40° Lb.
Nitric Acid. 42° Lb.
Phosphoric Acid, 48/50% Lb.
Phosphorus, yellow Lb.
Plaster of Paris Bbl.
Potassium Bichromate, casks Lb.
Potassium Bromide, granular Lb.
Carbonate, calcined, 80 @ 85%.. -Lb.
Chlorate, crystals, spot Lb.
C yanide, bulk, 98-99 per cent Lb.
Hydroxide, 88 @ 92% Lb.
Iodide, bulk
Nitrate Lb.
Permanganate, bulk . Lb.
, flask 75 Lbs.
Red Lead, American, dry Lb.
Salt Cake, glass makers' Ton
Silver Nitrate Oz.
Soapstone, in bags Ton
Soda Ash, 58%, in bags 100 Lbs.
Potassiun
Potassiun
Potassiun
Potassiun
Potassiun
Potassiun
Potassiun
Quicksilv
nominal
4.00
@
4.50
3 'A
@
3'/i
nominal
18
@
19
25
<a
26
16V.
@
17
65.00
@
85.00
9'A
@
11
40.00
@
45.00
2.25
®
2.50
9
@
9'/.
7 V.
@
8'A
!3>/i
@
15
nominal
75
@
85
27.50
@
30.00
5.00
@
5.25
4V.
@
5
18.00
<a
30.00
8.00
@
15.00
nominal
20.00
@
30.00
1.75
@
3.00
1.15
@
1.25
2Vi
@
2 'A
4.25
@
4.30
1.50
2.00
nominal
83>A @
4.00
123.00
10.00
2.55
125
00
10'/,
25
00
63
12
50
2
65
Sodium Acetate 1.1,
Sodium Bicarhonate, domestic 100 Lbs.
Sodium Bichromate Lb.
Sodium Chlorate 1,1,
Sodium Cyanide Lb.
Sodium Fluoride, commercial Lb.
Sodium Hyposulfitc 1 00 Lbs.
Sodium Nitrate. 95 per cent, spot 100 Lbs.
Sodium Silicate, liquid, 40° Be 100 Lbs.
Sodium Sul6de. 60%, fused in bbls Lb.
Sodium Bisulfite, powdered Lb.
Strontium Nitrate
Sulfur, flowers, sublimed 100 Lbs.
Sulfur, roll
Sulfuric Acid, chamber 66° B6 Ton
Sulfuric Acid, oleum (fuming) . .Ton
Talc, American white .Ton
Terra Alba, American. No. I 100 Lbs.
Tin Bichloride, 50° Lb.
Tin Oxide Lb.
White Lead, American, dry., Lb.
Zinc Carbonate Lb.
Zinc Chloride, commercial .Lb.
Zinc Oxide, American process XX I.h.
ORGANIC CHEMICALS
Acetanilid, C. P., in bbls Lb.
Acetic Acid, 56 per cent, in bbls Lb.
Acetic Acid, glacial, 99'/i%, in carboys Lb.
Acetone, drums Lb.
Alcohol, dennturcd, 1 80 proof Gal.
nomina
2.25
@
2.50
nomina
5 'A
@
6
22
@
28
4.05
@
4.50
3.70
@
4. 10
37.50
&
40.00
65.00
®
75.00
15.00
@
17 '/.
18.00
23>/.
@
24
nominal
nominal
nominal
Alcohol, sugar cane, 188 proof Gal.
Alcohol, wood, 95 per cent, refined Gal.
Amyl Acetate Gal.
Aniline Oil, drums extra Lb.
Benzoic Acid, ex-toluol Lb.
Benzol, pure Gal.
Camphor, refined in bulk, bbls Lb.
Carbolic Acid, U. S. P., crystals, drums Lb.
Carbon Bisulfide Lb.
Carbon Tetrachloride, drums, 1 00 gals . Lb.
Chloroform Lb.
Citric Acid, domestic, crystals Lb.
Creosote, beeebwood Lb.
Cresol, U. S. P Lb.
Dextrine, corn (carloads, bags) Lb.
Dextrine, imported potato Lb.
Ether, U. S. P. 1900 Lb.
Formaldehyde, 40 per cent Lb.
Glycerine, dynamite, drums included Lb.
Oxalic Acid, in casks Lb.
Pyrogallic Acid, resublimed, bulk Lb.
Salicylic Acid, U. S. P Lb.
Starch, cassava Lb.
Starch, corn (carloads, bags) pearl 100 Lbs.
Starch, potato, Japanese Lb.
Starch, rice Lb.
Starch, sago flour Lb.
Starch, wheat Lb.
Tannic Acid, commercial Lb.
Tartaric Acid, crystals Lb.
OILS, WAXES, ETC.
Beeswax, pure, white Lb.
Black Mineral Oil, 29 gravity Gal.
Castor Oil, No. 3 Lb.
Ceresin. yellow Lb.
Corn Oil, crude 100 Lbs.
Cottonseed Oil, crude, f . o. b. mill Lb.
Cottonseed Oil, p. s. y 100 Lbs.
Menhaden Oil, crude (southern) Gal.
Neat's-foot Oil, 20° Gal.
Paraffin, crude. 118 to 120 m. p Lb.
Paraffin Oil, high viscosity Gal.
Rosin. *F" Grade. 280 lbs Bbl.
Rosin Oil, first run Gal.
Shellac, T. N Lb.
Spermaceti, cake Lb.
Sperm Oil. bleached winter, 38° Gal.
Spindle Oil. No. 200 Gal.
Stearic Acid, double-pressed Lb.
Tallow, acidlcss Gal.
Tar Oil. distilled Gal.
Turpentine, spirits of Gal.
METALS
Aluminum. No. 1, ingots Lb.
Antimony, ordinary Lb.
Bismuth, N. Y Lb.
Copper, electrolytic Lb.
Copper, lake Lb.
Lead. N. V Lb.
Nickel, electrolytic Lb.
Platinum, refined, soft Or.
Silver Oz.
Tin. Straits Lb.
Tungsten (WOi) Per Unit
Zinc N. V Lb.
FERTILIZER MATERIALS
Ammonium Sulfate 100 Lbs.
Blood, dried, f. o. b. Chicago Unit
Bone. 3 and SO, ground, raw Ton
Calcium Cyanamid Unit of Ammonia
Calcium Nitrate, Norwegian 100 Lbs.
Castor Meal I'nit
Pish Scrap, domestic, dried, f. o b. work-
Phosphate, acid, 16 per cent Ton
Phosphate rock, f. o. b. mine. Ton
Florid, land pebble, 68 per cent Ton
Tennessee, 78-SO per cent Ton
Potassium "muriate," basis 80 per cent Ton
Pyrites, furnace size, imported Unit
Tankage, high-grade, f. o. b. Chicago I'nit
2.00 1
20
8'/.
3.15
®
3.25
90
@
1.00
6.30
0
6.45
io'A
@
11
8'A @
15
e
18
18.70
e
18.75
17V:
e
—
20.40
(a.
20.50
1.00
e
1.02
3.15
0
3.20
10
e
10"/,
12'A @
12' ,
3.50 @
3.65
23'A @
—
23'/: @
—
7 @
7 'A
55 @
56
nominal
93«A @
94
nominal
20.00 @
26.00
7>A @
8
6.70 @ 6.75
35.00 @ 40.00
nominal
nominal
16.00 @ 17.00
nominal
3.25 @ 3. SO
5.50 @ 6.00
310.00 @ 335.00
nominal
6.50
rne Journal of Industrial
and Engineering Ghemistry
Published by THE AMERIGAN GMEAIGAL SOCIETY
AT BASTON, PA.
Volume X
JUNE I, 1918
No. 6
Editor: CHARLES H. HERTY
Assistant Editor: Grace MacLeod
Advertising Manager: G. W. Nott
ADVISORY BOARD
H. E. Barnard, H. K. Benson, F. K. Cameron, B. C. Hesse, A. D. Little, A. V. H. Mory
Published monthly. Subsc:
! per single copy to American Che
Entered as Second-clasi
iption price to non-members of the American Chemical Society, $6.00 yearly; single copy, 60 cents
nical Society members. 50 cents Foreign postage, seventy-five cents, Canada, Cuba and Mexico excepted
Matter December 19, 1908, at the Post-Office at Easton, Pa., under the Act of March 3, 1879
All communications should be sent to The Journal of Industrial and Engineering Chemistry.
Telephone: Vanderbilt 1930 35 East 41st Street, New York City
Subscriptions and claims ior lost copies should be referred to Charles L. Parsons, Box 505, Washington, D. C.
ESCHENBACH PRINTING COMPANY, EASTON, Pa.
TABLE OF CONTENTS
Editorials:
America in Safe Hands 418
Washington Notes 418
An Inglorious Rout 419
Prophecy and Fulfilment 419
The Great Gamble 419
Typical German Pronouncements 420c
Research and the Tar Baby 420^
Societe de Chimie Industrielle:
Conditions of the French Chemical Industries during
1916. F. J. LeMaistre 42 1
The Great Effort of the French Industries. Marcel
Knecht 423
Original Papers:
The Quantitative Estimation of Anthraquinone. Harry
F. Lewis 425
Critical Elaboration of Quantitative Precipitation
Methods. H. Heidenhain 426
Improved Methods for the Estimation of Sodium and
Potassium. S. N. Rhue 429
A Comparative Study of the Thermal Decomposition of
Coal and of Some of the Products of Its Carboniza-
tion. M. C. Whitaker and John Richard Suydam,
Jr 43i
The Influence of Cold Shock in the Sterilization of
Canned Foods. L. D. Bushnell 432
Detection of Added Color in Butter or Oleomargarine.
Herbert A. Lubs 436
An Accurate Loss-on-Ignition Method for the De-
termination of Organic Matter in Soils. J. B. Rather. 439
The Agricultural Availability of Raw Ground Phos-
phate Rock. William H. Waggaman and C. R.
Wagner 44-'
1 pun the Action of Tetrazodi-o-Tolylmethane Chloride
upon Naphthol and Naphthylamine Sulfo Acids.
James H. Stebbins, Jr 44.S
Method of Calculating Comparative Strength and
Efficiency of High Explosives from Their Composition
and Apparent Densities. Charles E. Waller 448
Para Cymene. I — Nitration. Mononitrocymene,
l-CHi, 2-NOj, 4-CH(CH,),. C. E. Andrews 453
Effect of Acetylene on < Ixidation of Ammonia to Nitric
Acid. Guy B. Taylor and Julian II. Capps 457
Laboratory and Plant:
A Rocking Electric Brass Furnace. II. W. Gillett and
A E Rhoads
A Summary "i thi Proposal !"i the Utilization of Niter
Cake. John Johnston ... 468
Chemical Tests f 01 thi Detection of Rancidity. Robert
II. Kerr 47 >
Notes on the Color Designation "f Oil Varnishes,
F. A. Wertz 475
Addresses:
Planning a Research Laboratory for an Industry. C.
E. K. Mees 476
The Ammonia Program for 1918. Charles W. Merrill. 480
American Chemists Welcomed by the Cercle de la
Chimie 482
Willard Gibbs Medal Award:
Introductory Address. L. M. Tolman 483
Medal Address. Chemistry in the Petroleum Industry.
William M. Burton 484
Current Industrial News:
A New Copper Area; Electric Zinc Furnace; Electrical
Energy from the Volterra "Sofnoni;" Utilization of
Fish Oil; Australian Gelatine, Glue and Size; Pure
Cyanamide; Indigo Crop of India; Gypsum Deposit
in a Boiler ; Reactions of Acetylene ; Magnesites ; Water
Lubrication of Gas Exhausters; Utilization of Waste
Sulfite Lye; Coal Saving; British Board of Trade. . . . 487
Scientdjic Societies:
Annual Meeting of the Chemists' Club; American Elec-
trochemical Society; Sixth National Textile Exposi-
tion; New York Section, American Chemical Society;
North Carolina Academy of Science and North
Carolina Section of the American Chemical Society;
National Fertilizer Association; Alabama Technical
Association and the Alabama Section of the Amer-
ican Chemical Society; American Leather Chemists'
Association; American Institute of Chemical Engi-
neers; Research as an Aid to Industrial Efficiency;
Calendar of Meetings; Annual Meeting of the Amer-
ican Chemical Society 489
Notes and Correspondence:
Women's National League for the Conservation of
Platinum; Searles Lake Open to Lease Application;
A Letter from France; The Association of British
Chemical Manufacturers; Conservation of Alcohol,
Glycerin, and Sugar as Used in Medicines; High-
Grade Technical Men and Skilled Operatives Wanted
for United States Army Ordnance 494
Washington Letter 496
Ohituaries 498
Personal Notes 499
Im.i stkiai. Notes 501
Government Publications 503
Hook Reviews 504
blication9 soj
Market Report 506
4i8
TTIE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 6
EDITORIALS
AMERICA LN SAFE HANDS
As Chairman of the Committee: of the American
Chemical Society advisory to the United States
Bureau of Mines it was our fortunate privilege, through
the courteous invitation of Director Van. H. Manning,
to be present at the opening conference between
tlu leaders of the various lines of work at the Bureau
of Mines Experiment Station located at American Uni-
versity and the National Committee advisory to that
Experiment Station. In the afternoon an inspection
was made of the entire Experiment Station plant,
where field demonstrations were given of the various
products there evolved.
Utmost secrecy was enjoined as to every feature
of the day's program, but permission has been given
to speak editorially of the impressions gathered on
that most memorable day. Permission was sought
because it was desired to share with the chemists
of the country some of the inspiration, confidence, and
enthusiasm gained.
These feelings were begot primarily by the sight of
the men gathered around the conference table. With-
out attempting a complete enumeration we would
mention the presence of Director Manning, the follow-
ing members of the Advisory Committee: Doctors
Nichols, Venable, Talbot, Franklin, Hoskins and Parsons
(Dr. T. W. Richards joined the group the following day),
and representative leaders of the Experiment Station
work, among whom were Burrell, Bancroft, Norris,
W. K. Lewis, Cottrell, Hulett, Jennings, Kohler,Richter,
Reid, Frazier, Fieldner, Cheney, Henderson, Rowland,
Winternitz, Underhill, Hunt, Marshall. The Chemical
Service was represented by Lieutenant Colonel Bogert,
and there were present distinguished members of the
War and Navy Departments.
A glance o\er this group of mor6 than fifty men
thrilled us with the thought of how great an asset
America possesses in her chemists, men who with
characteristic American agility have changed their
whole train of thought from the accustomed subjects
, of research to those pressing problems of modern
warfare upon whose prompt and efficient solution
i so much the success of our righting forces.
That this thought transference has already borne
much fruit, despite the brief period of activity, was
shown at the Experiment Station grounds, where
every phase of the work was under full headway.
In these days of difficulty in procuring material and
equipment it was amazing to sec how rapidly thi
has grown since its inception by a few foresighted men
in the Bureau of Mines, immediately upon our entrance
war. Financed during the early months solely
from the funds of that Bureau, its resources ha
been greatly increa appropriations from the
War and Navy Departments. In Spite of the necessity
on there was evidenced no slightest
n itaking accui icy of the most i
research.
Tht field demonstrations constituted an eye-opener
to all of the uninitiated, and yet as we look back,
that which impressed us most was the fine esprit de
corps which has been developed, the harmonious
cooperation of all divisions of the work and the com-
plete sinking of self in the spirit of service to the cause
in which we are enlisted.
Some day when these buildings are dismantled and
when the men return to their peaceful pursuit of
science, the full story of this work must be written and
published to the world. It will prove one of the most
striking narratives of these stirring days and con-
stitute one of the most glorious tributes to the genius
of the American chemist.
WASHINGTON NOTES
A three-day sojourn in Washington furnished so
many topics for editorial discussion that limited space
necessitates brevity. Hence the following condensed
notes:
i — A Spring Meeting of the American Chemical
Society was unnecessary. Go to Washington any
old day — you couldn't tell the difference.
2 — The colors of the Society, cobalt-blue and golden
yellow, have changed their function from the decora-
tive feature of banquet menu cards to the more ap-
propriate r61e of the distinctive hat-cord now worn
by the enlisted men of the Chemical Service Section
under due authorization from the Secretary of War.
Stand by the colors!
3 — Lieutenant Colonel Bogert, head of the Chemical
Service Section in this country, is no longer with the
National Research Council or the War Industries
Board, but is quartered in Unit F, Corridor 5, Floor 3,
•;th and B Streets, X. W., Washington, D. C.
4 — The authorized quota for the Chemical Service
Section has been increased to a total personnel of
something over 1300.
5- — Organization is sufficiently -perfected and the
needs of the situation are so clearly understood that
the assignment of all chemists in the present draft to
chemical work is assured. The stock of perforated
filters for such assignment has fortunately been ex-
hausted.
6 — There is an error somewhere. Major G. F. Tyler,
of the office of Assistant Secretary of War Crowell
thai it was the conviction of the War Department
that chemists in camps must be transferred to chemical
work because of the scarcity of chemists. In answer
to our suggestion that there were still some three
hundred chemists in camps he stated that the records
had been carefully gone over and that not more than
fourteen or fifteen remained. A return visit to
tary Parsons' office confirmed the three hundred idea,
gained originally from the careful records which the
Secretary has kept since the census of sixteen thousand
chemists was compiled. l.cr Messrs. Major
and Secretary and compare notes. Perhaps it would
simplify matters if the Major would adopt the method
of the chemist and rcfilter the solution
June, 191S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
419
7 — Serious thought is being given to the matter of
the training of chemical reserves. With so many
professors engaged upon war research and no instruc-
tors exempted in the draft because of the character
of their work, the possibility of such reserves is very
slight. Yet in various other ways we are preparing
for a long war.
8 — The Mineral and Ore Control Bill, already passed
by the House and now before the Senate, embodies two
important principles: the release of shipping for trans-
port of men and supplies to France, and the furtherance
of national self-containedness. Why not extend its
scope to products other than minerals?
9 — With the passage of this bill in sight, the Railroad
Administration, in the interest of economy, discharges
the industrial agents, among them the very men who
last September at the Chemical Exposition brought
the undeveloped mineral resources of the South to the
attention of the country and particularly of the
chemists who best understood the rational methods for
their development. Think again, Mr. McAdoo. An
automobile would be an inefficient means of progress
were it not provided with reverse gear as well as for-
ward gears.
10 — We heard that the "Garabed" had too much
juice turned on and the machine broke down, necessita-
ting extensive repairs before its exhibition to the com-
mittee of eminent scientists. Meanwhile the matter
of winning the war continues to be prosecuted vigorously
by the usual methods, which, though perhaps to be
rendered obsolete by the use of "Garabed," never-
theless impart at the present time a greater feeling of
confidence.
AN INGLORIOUS ROUT
Among the many difficulties the new American
dyestuff industry has had to overcome, none has been
more nagging, more malicious, and less founded on
fact than the prejudice engendered by the oft-heard
phrase "American dyes are not fast." That this prop-
aganda has been quietly and subtly promoted by
those who wished to preserve for post-bellum days
the American market for German dyestuffs has been
understood by those who knew the facts. But the
propagandists capitalized our national weakness for
the "imported" brand, and the one-time prevalent
belief that the Germans possessed certain magical
secrets which enabled them alone to make dyes worthy
of confidence. Our good people of the trade fostered
their designs by placarding their goods with such
statements as "The color of these goods dannot be
guaranteed."
It was the old story of "giving a good dog a bad
name," and against this propaganda counterstate-
ments have proved of little avail. However, the
poisonous slander received its effective antidote during
the recent Textile Exposition in New York City, in
the clear, legitimate, and efficient demonstration by
the National Aniline and Chemical Co., Inc., of the
relative qualities of American and German dyi
rative exhibits were made of fabrics dyed with
foreign and domestic products, and subsequently sub-
jected to similar conditions approximating those of
daily use. In this contest the American products
fully held their own. To meet the possible criticism
that the tests may not have been genuine, a dyestuff
laboratory was installed, and there, upon request,
comparative experiments were carried out before the
eyes of the skeptical. Here, too, the results sub-
stantiated all that the most ardent advocate of the
American industry had claimed. Xow the press is
doing its part in publishing these facts to the world.
Another German drive has been stopped, and as the
exhibit and laboratory travel to various cities it is safe
to predict that the drive will be turned into an in-
glorious rout.
PROPHECY AND FULFILMENT
We received a letter recently from a former member
of the chemistry staff of the Medical School of the
University of Minnesota. The heading reads "Some-
where in France, March 24, 1918." and the concluding
paragraph follows:
As the Regimental Gas Officer I find plenty to do and also
find my chemical training and experience most valuable assets
both when at the front and when in training. While tn repos
I conduct a Gas School for the Officers and N. C. O's. * * My
lecture room is the rear room of a French cafe; our campus,
the great outdoors of untilled fields; our laboratories, the battle-
field and gas-shelled areas; and our source of demonstration
material is No Man's Land where the only cost of material is
the nerve to go after and the energy necessary to carry away
what is found and desired. * * *
Sincerely,
(Signed) Robert A. Hall,
Lt. Inft., N. A.,
Regimental Gas Officer,
18th Infantry, A. E. F.
The following excerpt from "General Orders No. 15,"
dated one week later than the above letter, gives a
prophetic coloring to the reference to the "source of
demonstration material."
Headquarters First Division
American Expeditionary Forces
France, March 31, 19 18
General Orders No. 15
The Division Commander cites the gallant conduct of the
following officers and men:
» * * * 2nd Lieut. Robert A. Hall, N. A., iSth Infantry,
"voluntarily went into No Man's Land on two occasions: once
to bring back the body of an American soldier, again to secure
equipment left by the enemy."
By command of Major General Ballard,
(Signed) H. K. Loughry,
Major, F. A., N. A.,
Division Adjutant.
[Seal]
■■Official:
First Division American Expeditionary Fo
Here's to Dr. Hall! And here's to his comrades in
the Service! Keep up the good work.
THE GREAT GAMBLE
"Of course, the first duty, tin duty that we must keep in
tin foreground of our thought until it is accomplished, is to
win the war. I havi ",l 'hat we
I live million men ready. Why limit it to five million?"
The New York limes, May 10, [918
Thus spol.i lent of the United Si
the great Red Cross meeting in New York City on the
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, \o. 6
evening of May 18, 19 18. Our answer to the Presi-
dent's question is that, should a Limitation of the size
of our armed forces evei 1 ry, it will not
be due to lack of determination on the part 1
American people to win the war, nor to unwillingness
to sacrifice their lives, nor to any disposition to with-
hold the smallest fraction of the Nation's wealth; but
a limitation may be forced upon us by inability to
manufacture sufficient ammunition, and this matter
depends directly upon our output of sulfuric and
nitric acids, and the extent of manufacture of these
two fundamental war necessities is indissolubly bound
Up in the matter of our available supplies of platinum.
But, it may be argued, platinum was commandeered
on March 1,1918. So it was; and on May 15 the press
throughout the country carried the announcement that
platinum had again been commandeered. Why this
duplication of commandeering orders? The answer
is simple. In the preparation of the original order
someone blundered in two regards — first, in failing
to include iridium within the scope of the order;
second, in assuming that manufacturing jewelers would
comply with the spirit and intent of the order and
hold hands off, which some did not, as set forth
by excerpts from the jewelers' own publications in
the May issue of Tins Journal, in an editorial entitled
"Platinum Scraps." Those charged with building a
dam across the platinum stream to store up its waters
extended the dam two-thirds of its needed length
(the importers and refiners) whereupon through the
remaining open space (the manufacturing jewelers)
platinum flowed into the already green fields of non-
essential adornment of the nouveau ricke, while the
builders of the dam rested contentedly upon their labors,
oblivious to the possibility of a drought and to the
important r61e of this rare metal in the winning of
the war.
A VISIT TO MR. CONNER
On Tuesday, May 14, we called at the offices of the
War Industries Board in Washington and received a
copy of the latest commandeering order from Mr. C.
II. Conner, in charge of platinum for that Board.
Iridium and palladium were included in the order but,
mirabile dictu, the dam had not yet reached the opposite
shore, for while jewelers were this time spei
mentioned, neverth at of the stocks
thus commandeered was released for commercial
usage, on condition that the holders waive any liability
of the Government for the remaining seventy-five
Siime bargain that! And the dam had been
purposely buill shorl o'i completion, for, in reply to our
remonstrances, Mr. Conner asserted Ins conviction
that the present measure would furnish adequate
supplies for ammunition manu mgh President
Wilson asks why the number of men to be equipped
should be limited to five million, and though the esti-
mated sufficiency of the sevei er cent to be
held was determined in advance of the inventory of
pi ere sent out along
wiili the commandeering order), [n support of the
wisdom and justice of the new order Mr. Conner gave
all of the stock arguments of the jewelers: Theirs
is a great industry which should not be suddenly shut
off from its supplies fas if the jewelers were dependent
largely upon platinum for a livelihood); ten thousand
skilled workmen and their families would be deprived
of a living wage (as if there was not work, and crying
for every able-bodied man in America);
it may be possible still to get some platinum from
Russia in exchange for food and clothing (as if con-
ditions in Russia could be depended upon for anything) ;
and we will get some from Colombia (as if German
money and plotting could never possibly cripple our
supplies from that source). Holding such views it was
only natural that Mr. Conner should take strong
exception to the patriotic and unceasingly vigorous
campaign being conducted by the Women's National
League for the Conservation of Platinum, under the
able and fearless leadership of its chairman. Mrs.
Ellwood B. Spear, of Cambridge, Mass. Thus is
begun the great gamble, under official authorization,
between the paltry profits of the jewelers and the
limitation of the number of men in our army — unless
some of the future drafts fight without ammunition
and without supporting artillery, depending for their
offense and defense upon the bayonet alone.
IME AUTHORITATIVE STATEMENTS
Feeling that we might possibly be unduly ap-
prehensive, at the. same time clearly mindful that
there had already been several other woeful mis-
calculations in Washington by those clothed with
direct authority, we sought the views of those in best
position in other Government circles to give authorita-
tive statements. Such statements were promptly
furnished and are reproduced here, fully confirming
our apprehension.
Department of the Interior
United States Geological Sirvev
Washington
May 16, 1918
Office of the Director
Dr. Charles H. Herty, Editor,
Journal of Industrial 6k Engineering Chemistry,
35 Kast 41st St., New York, X. V.
My dear Dr. Herty:
The facts of serious shortage in platinum supply are beyond
question The largest source, Russia, cut off, our domestic
production only a fraction of 1 per cent of our needs, and our
military requirements increasing .it .1 rate tli.it no one can fore-
see, the remedy, and the only remedy is to out out non-
i uses one hundred per cent, not at some future date,
hul now. and of these non-essential uses jewelry is first and
greatest.
Willi! meaning is there in a national thrift campaign when
any luxury-maker is allowed to make and sell his wares, the
material of which is absolutely needed in the processes of manu-
facture of munitions needed by our Army in France? What
K.s patriotic use can lie made of excess profits than buying
platinum lings and platinum cigarette eases and platinum mesh
\ Hoover is needed to conserve platinum lest our
nnluais program halt simply because our acid works cannot
iil.tt their demands,
of course, Mr. Editor, 1 endorse your protest against a half-
waj "i .1 seventy-five per cent or even a ninety-nine per cent
restriction of non essential use of platinum. No American with
■ pen to the fatts ^.tn i\" less than stand behind you.
Yours \ei \ cordially,
ni .1 GEO. otis Smith.
Director
June, iqiS THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Department of the Interior
Bureau of Mines
Washington
May 16, 1918
Office of the Director
Dr. Chas. H. Herty,
Editor, Journal of Industrial & Engineering Chemistry,
New York City
Dear Dr. Herty:
Replying to your request for my opinion regarding the Country's
need of platinum and the use to which, in my opinion, platinum
should be put, I have no hesitancy in stating that in my belief
the present high price of platinum is due to the artificial value
which it has been given for use in jewelry, an entirely unessential
use even in time of peace and one which in my opinion should
be discouraged at all times, especially in time of war when the
metal is so greatly needed for the production of munitions and
other essential materials.
I believe that the use of platinum in jewelry is due to an
entirely false conception, as there are other white metals equally
valuable for the setting of gems and the production of jewelry
which would be used for that purpose to-day, except for the
fact that they are not so costly as platinum. When the price
of platinum was less than that of gold, there was practically
no demand for it in jewelry, with the possible exception of a
slight use as a setting for gems. Over fifty per cent of the
Country's supply of platinum is now used annually for jewelry.
No metal is more easily imitated than platinum and there is
much white metal now on the market which cannot be told
from platinum by the uninitiated.
I have stated to others that it is inconceivable to me that any
woman would wear a lead-colored ring or bracelet or adorn
herself with lead-colored jewelry except that its artificially
produced high price has been made to give it a false value in her
eyes. With the platinum of Russia now under German control
and barely enough platinum in sight for this year's needs,
with no prospect of increased American supplies, I certainly
cannot consider the purchase of platinum in jewelry patriotic
now, and it appears to me, since it is worn almost solely on
account of its high price, to be in doubtful taste at any time.
Very truly yours,
(Signed) Van. H. Manning
Director
Department of the Interior
United States Geological Survey
Washington
May 15, 1918
Division of Mineral Resources
Dr. Charles H. Herty, Editor,
The Journal of Industrial & Engineering Chemistry,
35 East 41st St., New York, N. Y.
Dear Dr. Herty:
In reply to your letter of May 14:
It is my impression, based on such information as is available
to the U. S. Geological Survey, that the platinum situation is
not better at present but is far worse than it was six months ago.
At that time a shortage of platinum metals for war purposes was
indicated. Many plans made at that time have been enlarged
and still further extensions of the war program are indicated
by Secretary Baker's statements to Congress.
In view of these facts, it seems most unwise to permit the
use of these metals in non-essentials, such as jewelry. To
permit the continued utilization of 25 per cent of the stocks
held by manufacturing jewelers at the present time appears
to me to be the height of folly, siuce our stocks arc low, de-
mands for war purposes increasing with each addition to our
anny, and our source of new materials strictly limited.
Yours very truly,
(Signed) J. M. Hill
Geologist in Charge, Platinum Statistics
As a further contribution to the literature of this
subject there are added excerpts from an able editorial
in the Scientific American, May 18, 1918.
"We have within the past two months received a quantity
of circular mail from an association of manufacturing jewelers,
the general content of which has been a consistent minimizing
of the platinum shortage and a persistent decrying of the sug-
gestion that while the war lasts jewelry of this metal is out of
order. We have taken the trouble to look into the facts so
far as we are able to do so; and as a result we arise to brand this
propaganda as a most vicious one, conceived and carried out
from motives wholly selfish and unworthy of American business
men. * * * In doubtful taste at any time, surely now, when
our basic war needs for platinum are to be met only with the
greatest difficulty, the purchasing of jewelry made from this
unattractive metal cannot be considered as anything other than
the height of unpatriotism. It is surpassed, in its class, by
but one act — that of deliberately, and for the sake of profit,
urging those ignorant of the true state of affairs to buy such
jewelry."
THE JEWELERS POINT OF VIEW
In striking contrast to the above official letters from
Directors Smith and Manning and Mr. Hill is the
interview attributed to Mr. William E. Eisenhower
of the firm of J. E. Caldwell and Company and printed
in the Philadelphia Public Ledger of May 16. 19 iS.
According to the Ledger, Mr. Eisenhower said:
"About six weeks ago the Government requested us to submit
a report of the amount of platinum owned and what percentage
we could reserve in case of a shortage later. Out of the reserve
stock the Government requisitioned 25 per cent, which was a
very small proportion of the whole and which never may be
needed. This 25 per cent of the total reserve stock, however, is
enough to fill nil war needs five years, even under a much larger
war program than outlined now." (Italics are ours.)
We know nothing of the 25 per cent requisition
referred to, but the statement is absurd in itself, as
evidenced by the latest commandeering order requiring
the holding of 75 per cent subject to the call of the
Government, and if based upon supposedly official
statistics, then Mr. Eisenhower has access to some
mysterious source of information, for we have never
yet found anyone connected with the munitions
program who was willing even to admit that any such
information existed. How could it exist, with the
war program constantly expanding? The effort to
create the impression that war needs of platinum for
five years are provided for in the present reserves is
so seditious in character that it deserves the serious
consideration of Government officials.
The jewelers, however, do not have to depend
solely upon interviews in the daily papers Eor their
propaganda. Some magazines (whether knowingly or
not, we cannot say) are lending their aid. For instance
Vogue, May 1, 1 9 1 8 , pp. 74 and 75, contains these
items:
"There has been designed anothei en 1 ement ring that is
meant especially I'm the war bride-to-be, a ring which is patriotic
without being conspicuous about it; when it is worn, one would
never think, by merely looking at its light and graceful platinum
setting, that if the ring were slipped off and held up [01 1 rutin)
one WOUld see that tin 1 . are, ..11 each Side, WTOUgW shields
bi irirj tai and stripes, and that the two small ilia in. mils mi
ritliii side of the large one twinkle in stai shaped settings.
A wedding ring is designed to go with this engagement ring
.in engraved all around its platinum circle with stais *
in.. .. din jewel that belongs to hei oi the uniformed fiance
is the servici pis Of course, service pins, whether thej art ol
enamel on gold or precious stones set in platinum, are all alike
in .1. , .ii .i red border, a white center, and a blue star in the
middle; but when thi ■ I b diamonds and sapphire,
set iii platinum, they are very beautiful."
420b
THE JOURNAL 01 INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. to, No. 6
'" Wliii an impudent parading of our old friend
"the slacker wedding ring" under guise!
What a hollow mockery is thus sought lo he imposed
upon the young womanhood of America and
who are prepared to offer their lives as a sacrifice for
democracy! Why should these lives be needlessly-
jeopardized? And for what? From the aesthetic
standpoint, such platinum can be replaced by "'white
metal." No words from Director Manning are needed
to confirm this statement. Let the jewelers add their
own testimony on this point.
"A resolution recommending the discontinuance of the use of
white gold in place of platinum in the manufacture of jewelry
embodying precious stones was passed yesterday at a meeting
of jewelry manufacturers and retailers at the Hotel Biltmore
The meeting, which grew out of the commandeering of platinum,
iridium and palladium by the Government for war uses, was
called by the Jewelers' Vigilance Committee, and was attended
by representative retail jewelers from Chicago, Cincinnati,
St. Louis, Pittsburgh, Boston and this city. A second resolu-
tion passed recommended the inclusion in the karat designation
stamped on articles such as watch chains, cigarette cases, etc.,
of the letter 'w' or the words 'white' or 'white gold' in cases
where they are made of this metal instead of platinum. The
purpose is to protect the public from the selling, by unscrupulous
dealers, of articles of white gold as platinum. While this metal
resembles platinum more or less in appearance, it does not
resemble platinum so far as 'workability,' value, and wearing
qualities are concerned." — The New York Times, May 16, 1918.
The eye cannot tell the difference; the letter "w" or
the words "white" or "white gold" must be stamped
on the article to protect the young soldier from imposi-
tion in the purchase of a "patriotic" engagement ring!
SIDE-LIGHTS
Interesting side-lights are thrown upon this whole
platinum situation from another source. Again we
prefer to let the story be told in the words of the
jewelers themselves and of the publication devoted
to the interests of the jewelry trade. On page 55 of
The Jewelers' Circular, April 10, 19 18, an account is
given of the annual meeting of the Jewelers' Vigilance
Committee. This account contains the report of
Chairman Harry Larter, three paragraphs of which
are herewith reproduced:
"While the platinum matter, in so far as its connection with the
Government is concerned, is now out of the hands of this
platinum committee, the Jewelers' Vigilance Committee is still
interested in the adverse propaganda, started afresh with new
vigor because of the acute situation now existing throughout
the world in regard to this precious metal.
"The commodity tax, in which jewelry is a factor, developed
in Congress just about a year ago in the War Revenue Bill,
which, as you know, has since become a law. Again, our com-
mittee called a mass meeting, and at it another powerful, rep-
resentative committee was appointed, headed by the former
very able and efficient chairman, Mr. Rothschild, and ever
since then, committees large and small in number — sometimes
only the chairman -have been in Washington and in constant
telephonic or telegraphic touch with the Internal Revenue
Commissioner's Department.
... * « Yvinje other things have been accomplished and plans
for the future discussed, because of existing conditions, they
have been temporarily postponed. All of the above work has,
naturally, imposed a huge expense, and through the energetic
and persevering \\ ■ 0 k of the chairman of the finance committee
has been met by contributions of large and small amounts bj
the generosity of ovei .100 persons and linns connected with
our industry. We still have left a nucleus for .1 fighting fund
which can and will be used in the interest of every branch of
the jewelry trade."
Following this report the account of the meeting
(.again page 55) gives some interesting statistics.
"An idea dI some of the work done by the committee during
the year was given in the report of Secretary Dickinson, which
showed that during the year there have been 6l meetings of
tin- directors and committees, divided as follows: Directors,
!; 1 1 .nil imiltee, 14; platinum committee, 16; legislative
committee. _> , tax committee, 12. *
"There have been sent out 17,072 letters, circulars, announce-
ment, etc., through the mail, and 445 telegrams, the shortest
of which was 42 words and the longest consisting of 708 words,
this latter having been sent to 1 1 firms.
"There had been 18 trips made by committees on various
matters, [4 to Washington, two to Albany, one to Scarsdale
and one to Boston. In all 115 members of the Jewelers' Vigilance
Committee, and delegates from the trade at large making the
triiis."
How some of these activities impressed a dis-
tinguished member of Congress is best set forth by the
following letter from the Hon. Henry T. Rainey of
Illinois to Mrs. Ell wood B. Spear, which is reproduced
here by the consent of Mrs. Spear and Congressman
Rainey:
House "i Representatives U. S.
Washington, D. C.
May 9, 1918
Mks. ELLWOOD B. Speak,
Chairman, Woman's Xat'l League
for Conservation of Platinum,
-'7 Walker St., Cambridge, Mass.
Dear Madam:
I am in receipt of an editorial which was released May 1,
1918, in Industrial and Engineering Chemistry, with ref-
erence to the conservation of platinum.
I am quite familiar with the subject. I am a member of the
committee which draws war tax measures, and on the Floor
of the House I made a speech in favor of amending the bill so
as to tax platinum used in the manufacture of jewelry .'50
per cent. The matter is serious indeed, and your organization
is rendering a splendid war service. I know of no profiteers
in the United States who have more justly earned all criticism
and condemnation that can be phrased against them than the
jewelers who organized a lobby and sent it here to Washington
and maintained it here for a considerable period of time in order
to enable them to continue their profitable business in the use
of platinum for jewelry. They came here and infested the
Capitol building, and stood around the committee rooms,
pledging themselves to conserve platinum, and pointing with
pride to the fact that they had passed a resolution discouraging
the use of platinum in jewelry, and also produced on every
occasion the statement of Secretary of Commerce Redfield,
commending their action as wise and patriotic. There was
absolutely nothing in their position. The platinum supply
could not be conserved in that way and the promises and pledges
they made at that time they have failed to keep, and I knew
they would not keep their promises or even attempt to keep
them.
They pointed to the fact that platinum came from Russia
and that Russia was at war with Germany, and that we could
get all the platinum we wanted while Germany could get none.
The arguments some of us used in our interviews with the mem-
bers of their lobby, calling attention to the unstable conditions
in Russia, and the possibility that Germany might soon control
Russia, had not the slightest effect upon them.
flu organization which maintained a lobby here in Wash-
ington ought to be held up to the contempt of patriotic citizens
of the United States Although I am a Democratic member
of the committee which prepares the revenue bills, I did the
unusual thing from a standpoint of a Democratic supporter
of the measures which come from the committee, and joined
with Representative Longworth in his attempt to amend the
bill, which failed on account of the efforts of the jewelers' lobby.
Ma\ 1 call attention to ni\ speech made on May 2 1 , 1017,
wlu.ii you can lmd as of mat date on page 2862 of the Con-
gressional Record, which you can of course find in your library.
Very truly yours,
■^Signed) Henry T. Rainey
June, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Further comment is unnecessary, except that we
recommend the reading of this section of this editorial
to Congressman Nicholas Longworth, who sought
about a year ago to build a one hundred per cent dam
across the platinum stream by placing a prohibitive
tax upon platinum jewelry, which patriotic effort, how-
ever, was defeated.
THE JEWELERS AGAIN
What the jewelers' publication would have to say
regarding the most recent commandeering order, was
a matter of interest to us. In The Jewelers' Circular
of May 15, 1918, we found what we sought. On page
102 it is stated
"In speaking of this platinum order, the Jewelers' War Service
Committee, which has been in close touch with Mr. Conner
in the preparation of all details in connection therewith, made
a full statement through its secretary, in explanation of the way
the order will work out." (Italics are ours.)
and on the following page (103) the "Statement by the
Jewelers' War Service Committee, Regarding the
Government's Most Recent Order, Commandeering
Platinum, Iridium and Palladium" contains this
illuminating paragraph:
"The order has been sent from Washington to approximately
1,000 manufacturing and retail jewelers and refiners. Our
committee has been in constant touch with the officials, ad-
vising them as to the necessary steps, and the manner and form
in which they should be taken. It was our function to assist
the government and to protect the interest of our trade in even-
way possible. The committee, therefore, urged that the order
be drawn up in a different and simpler manner than that which
the trade has just received, but it was impossible to do this on
account of the legal restrictions placed upon the officials issuing
the order. The representatives of the Government were very
solicitous of the welfare of the jewelry trade, and we are pleased
to state that every question was given careful and courteous
consideration. However, the objects to be attained could not
be reached in any other way. The result was that all platinum,
iridium, and palladium in the hands of those receiving the order,
no matter in what form, has been commandeered; but releases
or waivers of delivery to the Government have been arranged
in order not to disturb the industry unnecessarily." (Italics are
ours.)
One final quotation from the same issue (page 105,
editorial page) gives the jewelers' view-point:
"The men and women in the factories and workshops who
to-day are making large wages for the first time in their lives,
can obtain the necessaries of life by working half time and if
their purchases are confined to the necessaries of life they will
work only half time. What they are striving for — the in-
centive that makes them work the full day and even overtime
is the opportunity to buy the luxuries of life which are for the
lir>t time within their reach.
"Take from these people the opportunity to buy jewelry, to
dress well, to go to the theatres or indulge in luxurious cat 11m
or living and you take away the real reason that 90 per cent of
them are willing to start in their work early and go home late.
They '1" not want money as money; they want the money for
what it will buy. It is the luxury that they have craved for
years and one they could not get, that they demand now as a
compensation for their work."
In the name of the factory and workshop men and
women who have just bought so widely Third Liberty
Loan !'>" every thought now is 1o help win
this war, and whose effective labor is to day SO
responsible for the speeding up of the great national
tie, we protest against any such
' ■ upon the motives which lead them to their
daily toil.
PATRIOTIC SERVICE BY WOMEN
Fortunately there is a strong popular movement,
growing stronger each day, which will eventually
offset such sordid activities; the full story of Mrs.
Spear's untiring and patriotic personal activities must
some day be told; Mrs. Alfred S. Weill's letter, mailed
to ten thousand women of Pennsylvania, and reprinted
on page 494 of this issue, constitutes another phase of
this movement; so too the war pledge cards for platinum
conservation will have their decided effect, and finally
the stirring words of the wife of the Governor of
Massachusetts, Mrs. Samuel McCall, will surely find
a ready response in the hearts of all American women.
We quote from an interview reported in the
Boston American of May 4, 1918.
"The giving up of little things like jewels — luxuries — and
things that have no value as necessities, does not entail a great
sacrifice.
'And even if it did, the women of America would not hesitate.
They have given their sons, their fathers and their husbands.
They have given all that they value most, the people that make
life for them. Are they going to hang back when it is a question
of mere bauble?
"The women of the country aren't lacking in the spirit that
has to go behind a country in war times. They can give without
a murmur, and jewelry is a small concern when it is considered
in connection with life.
"It seems to me that any woman who orders any jewelry in
platinum settings at a time like this either cannot understand
or feel deeply the love of country. And if she has any of the
material on hand she ought to be entirely willing to surrender
it — such a small thing to do, when others are giving their lives."
That interview must have taken place at the base of
the Bunker Hill monument.
FURTHER LOSS POSSIBLE
In conclusion, attention is called to paragraph 5
of the letter signed by Mr. Conner and sent out by
him along with the commandeering order to ap-
proximately one thousand jewelers. The paragraph is
as follows:
"The undersigned will consider applications, on forms which
will be supplied upon request, for further releases of platinum,
iridium and palladium."
Is there to be still further dissipation of our limited
supplies of these vitally important metals?
Finish thai dam !
TYPICAL GERMAN PRONOUNCEMENTS
A correspondent has forwarded by mail to this
office a newspaper clipping containing a dispatch
from Amsterdam, dated April 18. The article an-
nounces the conferring of the Bunsen medal upon
Professor Haber, head of the Chemical Research
Institute of Berlin, for his lecture on "The Relation
of the Exact Sciences to Militarism."
Professor Haber is quoted as having said in the
course of his lecture, "Gas attacks arose on both sides
out of the requirements of the situation." Why did
he not follow more closely the example of German
ini and say, "Gas attacks were inaugurated
by our enemies while we were defending in Belgium
the invasion of the Fatherland," despite th<
memories of the British in connection with tha
wave of chlorine at Ypres? When international
42od
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 6
amenities are again the order of the day it may be
well to take under careful consideration the q
of readmission to good fellowship in the world-body of
chemists of those German chemists who wi
sponsible for the plans which started the armies of the
world upon this frightful medium of attack.
Again Professor Haber is quoted as having said,
"The reason why the use of gas is disliked by our
enemies is that the use of protections against gas
attack calls for a special measure of discipline and
intelligence in the common soldier."
How typical of the German mind!
RESEARCH AND THE TAR BABY
There is one product on the market which is too
cheap, and this through the natural working of the
law of supply and demand. That is a rather startling
statement in these days when prices of all commodities
are soaring. Still more startln: iat statement
become when it is revealed that this product is com-
posed solely of organic compounds, for these seem to be
adapted particularly to spectacular price elevation.
Nevertheless, the statement is true, for in a recent
number of the Weekly Naval Stores Review the editor
remarks (and market quotations seem to sustain his
contention) that "spirits of turpentine is the only cheap
raw product in the world to-day, rosins being the next
cheapest."
The explanation of this anomalous situation is easily
found in war conditions which have largely decreased
building operations, made difficult the securing of
shipping space, and shut off from the producers of
naval stores the hitherto extensive markets of Ger-
many and Austria, particularly the former. Certain
increased uses of these products for war pur])"
not compensate in any measure for these unfa
influences and the net result is financial distress for the
producer.
Three remedies have been suggested. The first,
most natural, and usually applied in industry, was the
curtailment of production; but with an industry so
loosely organized as this one, success in such an effort
cannot always be safely predicted. The second was
a proposal by i orri pondent of the Review to "divide
the territory into zones and have an agent for each
• hose duty it would be to visit each still and ship
the turpentine for the operator." If we were over-
producing, it would be the duty of this zone agent
"to dump tin surplus spirits on the ground." The
i han the gutter is good,
in view of the extra-urban character of the industry,
but we cannot refrain from a surmise as to what would
happen ult of the physical
activities of the individual operators, about the time
the aforesaid dumping process began. Such a test of
the value of the anti-dumping clause enacted by the
last Congress would scarcely be fail its un-
d character. The third remedy was si'
a1 nference las i between representatives
of the producers and officials of the Bureau of Chemis-
i ry . when th< Goven i ists were in
find new uses for turpentine. This would be a step
in the right direction. That Bureau exists to serve
the people; but herein lies a real difficulty — there are
so many people interested in so many different
lines of industry that no particular industry ought to
expect everything in the way of salvation from this
source, especially in view of the restricted appropria-
tions available to the Chief of the Bureau and his
able associates.
Xone of these measures adequately meets the situa-
tion. May we, therefore, venture to call the attention
of our friends in the naval stores industry to a develop-
ment of the past few years in many lines of industry,
namely, the creation of well-equipped and well-manned
industrial research laboratories, in which by scientific
procedure, seemingly slow at the outset, real industrial
progress is being made through improvements in
methods of manufacture, resulting in increased yields
and more efficient plant operation in general, through
the discovery of new possibilities of raw material
and through the development of new uses for the
manufactured products. Millions of dollars have been
invested in these laboratories and the end is not yet.
No surer safeguard of the industrial future of this coun-
try exists.
If, however, it be argued that the output of the
plant of any naval stores operator is too small to justify
large expenditures for research, we would urge careful
consideration of the movement in many industries
toward cooperation in such endeavor. A typical
case is that of the research laboratory of the National
Canners' Association in Washington. Proving no
severe tax upon any individual concern, this laboratory
has solved a multitude of problems, has had at its
disposal material from all sections for test and study,
and through the tact of its Director has brought all
elements of the canning industry into more harmonious
relationship. Following this example, the oil men
of the West have united in a cooperative research lab-
oratory at the University of Oklahoma, and still more
recently the leather trade has determined upon a similar
cooperative effort and its research laboratory is now be-
ing equipped in New York City. The growth of the
idea has been rapid and its roots have struck deep
into the industrial life of the Nation. Its latest mani-
festation is the appointment of Dr. John Johnston
tary of the National Research Council with the
understanding that his energies are to be directed largely
to the development of cooperative industrial research.
an opportunity for fine service by a man preeminently
qualified for the undertaking.
If the turpentine operators are soon to gather in
annual assemblage, may we suggest that Dr. Johnston
be invited to address the convention on the subject
which he has so deeply at heart, along which line will
be found the real and permanent cure for low prices
and the future advance of the naval stores industry.
thing we know: the turpentine operators are
somewhat slow in taking hold of a new idea but when
they do. they take hold hard. There was genuine
foundation for Uncle Remus' story about the tar
June, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
50CILTL DL CHIMIL INDU5TRILLLL
On April 24, 1918, the first meeting of the recently
formed New York Section of the Societe de Chimie
Industrielle was held at the Chemists Club, New
York City, Dr. L. H. Baekeland, president of the
Section, presiding. The deep interest felt in the
relations between France and America were clearly
reflected in the spirit and enthusiasm of the large and
representative assemblage. Dr. Wm. H. Nichols,
president of the American Chemical Society, ad-
dressed the meeting, welcoming the new association
to its place among the chemical societies of America.
Prof. George A. Hulett, a member of the first
special War Commission sent to France and England
from this country, spoke on "Some of the Chemical
War Problems," and was followed by Mr. Frederick
J. LeMaistre and Mr. Marcel Knecht whose addresses
appear below. — Editor.
CONDITIONS OF THE FRENCH CHEMICAL INDUSTRIES
DURING 1 91 6
By F. J. LeMaistre
Member of the American Industrial Commission to France
I have been requested by Dr. Baekeland to present
to you this evening a few remarks on the "Conditions
of the French Chemical Industries during 1916." I
presume the only justification I have for appearing
before the Societe this evening is that I have had the
good fortune of making a visit to France during war
times, an experience which I shall not soon forget,
and it is my sincere hope that I shall never be in-
sensible to the responsibilities which go with such
privileges.
The American Industrial Commission to France,
of which I was a member, has issued a very full report
of its findings entitled "Franco-American Trade,"
a volume of over 250 pages. The twelve Commis-
sioners were all representatives of important industrial
and technical associations; the speaker was the official
representative of the American Chemical Society
and The Franklin Institute. It is extremely interest-
ing to look back upon the efforts of this group of men,
representatives from a country which was then neutral.
A repetition of this visit under present conditions with
America on the side of the Allies would, undoubtedly,
be of added interest.
It must be remembered that my remarks this eve-
ning are not of present conditions, but of conditions as
we found them in the fall of 1916. Some supple-
mentary material has been added, and consists of
information general in character, which for various
reasons it was thought inexpedient to publish at that
time. I have also been assisted in selecting material
for this paper by statements made to me personally
by Professor Grignard and Lieutenant Engel on the
occasion of 1heir visit to this country some months
ago.
With the latitude Dr. Baekeland has kindly gj
I have gone somewhat afield of the topic sele<
my address, and for convenience my remarks are
grouped in two general divisions:
1 — Subjects of interest, in France, to the American
chemical industry.
2 — Subjects of interest, in America, to the French
chemical industry.
Before proper consideration can be given to these
two subjects, we must presuppose that a state of mind
exists regarding the meaning of the word "reciproc-
ity," as no true progress can be made by the in-
dustries in these two countries without a full knowl-
edge of what this term implies, and in this connec-
tion I think Mr. Frank Hemingway's statement, made
at the St. Louis Meeting of the American Institute of
Chemical Engineers, is pertinent, that "frequently
wrong-minded public action is based on ill-informed
public opinion." True reciprocity cannot be had
without a knowledge of the facts in the case.
It is important to remember that on such a hurried
trip as this — 45 days' travel through France — no
complete survey can b.e made of any one industry
under normal conditions, let alone during war time,
and this was our experience even though the Com-
mission was granted very many unusual privileges
by the French Government. I am giving you to-night,
therefore, but a few impressions made during a hurried
trip under expert guidance. We, of course, heard
much from people in authority, and had many
privileges not granted the ordinary traveler, such
as discussions with Chambers of Commerce, economic
associations, special Government commissions, and
business organizations.
SUBJECTS OF INTEREST, IN FRANCE, TO THE AMERICAN
CHEMICAL INDUSTRY
Any group of American chemical manufacturers
seeking trade with France should have a thorough
knowledge of the French language, and this is further-
more imperative if we are to be of any permanent
help to this country in their period of reconstruction.
It was the terse expression of opinion of the foremost
American business men in France that "the export of
American men should follow the export of American
goods," and that these men should be representative
and better qualified than those ordinarily assigned to
such du 1
Knowledge of France and its people is also essential.
Adventures have been undertaken and money lost,
due to the lack of appreciation on the part of American
concerns of the characteristics of the French people.
The French are essentially artistic, are naturally
opposed to production in quantity, which th
It must not be overlooked that on i
of their love of home, they often lack a knowli
ill. possibilities of their own country. The banking
system and the thrift of the French people should be
common ;e to all those se< in tins
country.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 6
The number of French technical schools is sur-
prisingly small. One of the foremost educationalists
advised us that there is a great need at the present
time, by the French nation, for higher education.
In 1914, the total number of students in Government
universities was approximately 42,000 and of these
about 15 per cent represented the foreign element.
The above number of students could be grouped as
follows:
Per cent
U« 38
Medicine 20
Science 18
Arts, etc 24
In this connection, it is of interest to note that
on a basis of unit population, Switzerland has 300
chemists, Germany 250, while France has only 7.
It is commonly accepted that, pending the develop-
ment of more technical schools in France, the young
men will be forced to obtain their technical education
elsewhere, and the United States has been preferred.
It has been thought that the intercourse of the French
and British soldiers has afforded the Frenchmen an
opportunity to learn the English language, so that on
this account such a step will be entirely practical.
It is, therefore, our duty to prepare now for such a
contingency. It seems to me that we should see to it
that the rank and file of the French people know what
educational facilities we have to offer.
As in our country, there has not been in France
sufficient intercourse between the college professor
and the technologist. I personally had a subject up
for consideration with one of the prominent college
professors in France, and failed to obtain an inter-
view with the professor, as he sent back the report
through his commercial representative that he was
busy on other subjects and could not arrange to visit
Paris for two or three weeks, and that on no account
could he or his assistants take time to consider the
commercial application of this work.
I think it is of interest to all American chemists to
know of the work done by the Commercial Attache"
of the American Embassy. An inspection of the list
of subject matters passing through this office clearly
shows how often are the attempts to embark on
absolutely worthless projects. These ventures usually
represent a serious money loss both at home and
abroad.
My own experience permits me to endorse heartily
the efforts of Lieutenant Engel and his confreres to
have a French chemical publication of special interest
to the technologists, as a gulf at present separates the
college professors from those in direct charge of
chemical plants. Lacking this intercourse, antiquated
methods of manufacture are followed in certain
branches of the chemical industry, which it is hard to
believe can still be in use.
It is of interest for the American chemist to know
that the French chemists are generally at a loss to
account for our lethargy and slowness in adopting the
metric system in America. It is to be hoped that
one of the beneficial effects of the war will be the more
active study of this problem by the authorities in
Washington. We surely ought to look for some
accomplishment shortly.
SUBJECTS OF INTEREST, IN AMERICA, TO THE FRENCH
CHEMICAL INDUSTRY
Much profit would be obtained by the annual visit
of a group of men interested in the French chemical
industry to this country, probably at the time of the
annual chemical exhibition in New York. This
character of legitimate advertisement is much needed
and, in my opinion, would fill a very direct need. I
consider that such a delegation should be made up of
representatives from the industrial sections of France.
It is the duty of the French chemist visiting this
country to acquaint himself with the many important
associations interested in foreign trade. Such per-
manent exhibits as the Commercial Museum in Phila-
delphia and similar institutions should be visited.
It seems to me that much progress could be made by
a study of standardization of chemical equipment in
America, as well as in France. The manufacturers
of both countries should seek counsel together. There
is no real reason why prices of this class of equipment
should maintain at the present high level, when in
many cases the selection of three sizes — large, medium,
and small — and the manufacture of these in quantities
would satisfy all demands. The French chemical
industry, however, is greatly influenced by the general
tendency of the French people to have variety rather
than quantity.
In the future development of the chemical industry
in France, liberal use will, undoubtedly, be made of
woman labor, as very gratifying results have been
obtained in this direction during the past three years.
Those best qualified to judge are emphatic in their
statements that a return to old conditions cannot be
made if competition is to be met and the quality of
German goods equaled.
Raw materials from America is a subject which has
received very active study by many companies
throughout France. Much work still remains to be
done before specifications are clearly understood by
both parties. In many cases misunderstandings arise,
due to poor translation. The present facilities for the
translation of technical French in this country are
wholly inadequate. Could not our universities
profitably take over this work?
It was the consensus of opinion of all the Com-
missioners that the French people were more favorably
disposed than ever before to American products. In
certain factories making munitions of war, as high as
60 per cent of the mechanical equipment came from
America. This surely affords a wonderful opportunity
for follow-up trade.
It was our general observation that an arduous task
will devolve upon the French manufacturer upon the
return to normal conditions. Under stress of war-
time manufacture, chemical control is not always
June, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
possible of attainment. It is generally conceded
that the maximum efficiency can be secured only by
the entire regrouping of many industrial sections,
as a number of the chemical plants are illogically
located. The majority of the more active chemical
manufacturers fully appreciate the importance of in-
creasing efficiency, but hesitate in branching out on
new methods of manufacture on account of the
enormous expenditures such a change involves. It
is believed that the necessary encouragement from this
side would enable them in future to compete with the
efficiency of the German chemical manufacturers.
It would, no doubt, be of interest to give a few
specific statements which may indicate the view-point
taken by some members of the affiliated chemical
industries of France.
perfumes — The French manufacturers were warned
by some of their own trade specialists of the inroads
that might be made by the synthetic perfume manu-
facturers of Germany. They did not take heed, how-
ever, maintaining that these artificial compounds
could not approach the true perfumes of France.
They have, however, recently decided to embark on
the artificial perfume industry and to develop this
trade in a logical way.
petroleum — It was also acknowledged by a number
of manufacturers that many changes will be needed
in the factories now refining crude petroleums. They
acknowledge that this industry before the war was
conducted on altogether too small a scale to be profit-
able.
celluloid — This old established industry of France
was inactive during our visit, owing to the fact that
most of these factories have been commandeered by
the War Department for the manufacture of nitro-
cellulose. The love of the French for the artistic is
well illustrated in this case. The French manu-
facturers in recent years have purchased large quanti-
ties of sheet celluloid from Germany and have manu-
factured this stock material into miscellaneous artistic
articles.
electrochemical industry — This industry ap-
pears to receive very active study by both chemists
and engineers. Extensive programs have been out-
lined and are now in process of development which will
undoubtedly bring about many economies which were
not formerly enjoyed by the French manufacturers.
We heard of a number of cases where the Field Com-
manders were requested to release men from the front
who were specialists along this line. These men were
assigned to three to four months' study of this
special problem.
kkcovery of sulfuric acid — We had the pleasure
of meeting Mr. Kessler of the company by this name.
He informed us that since the war began they had
sold, up to November 1916, some 300 Kessler ap-
paratus of varying sizes, and that their apparatus
alone installed in France was equivalent to a daily
capacity of 4,000 metric tons of sulfuric acid, 66°
Be\
dyes — The manufacture of dyes was receiving in
1016 the same attention in France as elsewhere. It is
unfortunate that many are rushing into this industry
wholly ignorant of the difficulties of this line of manu-
facture. It seemed to the Commission that the
tendency in France was towards Government super-
vision and ownership of the dye industry.
pharmaceutical chemicals — Few pharmaceuticals
were manufactured in France prior to the war. Plans
are now on foot to return to this manufacture, which,
due to the special trade agreements with Germany,
had entirely passed into their hands.
denatured alcohol — The laws regarding denatured
alcohol and its uses are being gradually revised.
The same problem exists in France as we find in this
country. On several occasions the writer had an
opportunity to recommend a liberal extension of
privileges for the use of this valuable solvent. As
in many other cases, the Germans have been the
leaders in this direction. There is no real reason why
much of the Government red tape now required should
not be eliminated.
It is of interest to note that, in 1913, 70 per cent
of the denatured alcohol sold in France was used for
heating and lighting, the balance representing that
consumed in the manufacture of ether and explosives.
It is also of commercial interest to note that some
of the leading French economists have recommended
to the Government fixing the price of denatured
alcohol for a period of five years.
I cannot close my remarks this evening in a more
fitting way than to voice the impression of all the
Commissioners that the present industrial effort of
France commanded our fullest admiration and to
quote the following from our official report:
There is a striking resemblance between many of the social,
industrial and commercial problems of the two sister republics,
and there is evident a tendency to solve them on similar lines.
Nothing could be more profitable than a joint comparative study
of them.
THE GREAT EFFORT OF THE FRENCH INDUSTRIES
By Marcel Knecbt
Member of the French High Commission to this Country
France has been invaded; France has suffered
terribly. But France is in no way bled to death as
the propaganda of the German emperor has tried to
make you believe.
The French army — and I give you these, not my
figures, but the official figures given recently to your
War Secretary, Mr. Baker, by the French Commissioner,
Mr. Andre" Tardieu — the French army at the begin-
ing of the war sent 1,500,000 fighters, and you know
with what heroism those soldiers have been fighting,
and you know how many of those have been wounded
and disabled. Yet, still, through the energy of our
soldiers, through the energy especially and the great
spirit and sacrifice of the mothers of France who have
sent all their sons to the front, we now have a fighting
force of 2,600,000 men ready to keep up the conflict.
424
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 6
Do you know the loans which the French people
have given to their government? Do you know this
little nation of 30,000,000 people at the beginning
of the war, which has been so terribly reduced since
the north and east parts of France were invaded, do
you know the amount of money loaned by the people of
France, by the peasants and by the workmen of
France — for we have 20,000,000 peasants in France —
we have loaned to our Government since the beginning
of the war $18,000,000,000.
Do you know — and it is always M. Tardieu who
speaks — do you know how many shells for guns of 75
millimeters we could shoot every day in August of
1014? The French light artillery, the field artillery —
for we hardly had any big artillery, the French light
artillery could shoot 15,000 shells every day; and now,
with the wonderful effort of our business men of the
Chambers and Associations of Commerce — and I insist
on that fact to prove to you that you have in France
brothers in business who are quite worthy of your
admiration and sympathy — for the men of industry
in France before the war were considered too old-
fashioned, were considered small business men in a
country where we had lost 60 per cent of our iron ore,
and 60 per cent of our coal mines, and 50 per cent of
all the best mechanics of France who were taken
prisoners from the invaded districts — now, we can
give to the French army 250,000 shells of 75 milli-
meters every day.
And at the beginning of the war we had only 300
big guns against those huge guns of Germany which
had been destroying so many cities in Belgium and in
France — we had only 300 guns and a very small
quantity of shells, and now we have 6,000 huge guns
from the best factories of France, and we also have
100,000 big shells every day to shoot in those big
guns.
France lost the best of her industries, of her mines,
of her heart in the beginning of the war. You know,
perhaps, that in the east of France, in my district,
there were enormous mineral resources, but some years
before the war those resources were very little known,
even in France; for France was too much interested
in literature and in her theatres; and though we had
fine people, though we had people who were working
hard, we did not interest ourselves enough in industry
and in business.
You did not know it at all. And there is only one
nation who knew better than we knew, and knew
exactly what was in France, in the east of France,
what was going on in France, and that was Germany.
It is in Lorraine that your boys will show that they
are brave soldiers of America. If Germany had not
taken, in 1871, ami, also recently in 191.1, the two
parts of Lorraine, Germany could never have de-
1 France or any other nation in Europe.
And I will prove to you why.
In 1913 the annexed pari of Lorraine, whi
under German domination, produced 21,000,000 tons
of the best iron ore ever known. And the French
part, which had no1 been taken by Germany in 1871,
the part which has been occupied, nearly all of it,
since 1914 — produced in 1914, 19,000,000 tons of
iron ore. Then you can understand how, in 187 1,
Germany was able, with those 21,000,000 tons of
Lorraine iron ore to make her big guns and shells, and
prepare for this war.
In the same year, 19 13, the whole German territory,
excepting the annexed Lorraine part, produced only
6,000,000 tons of iron ore. If Germany had not
taken in 1871 those 20,000,000 tons she had in 1913,
and if she had not occupied in 19 14 this wonderful
district to the north of Nancy, where we produced
19,000,000 tons, Germany could not have declared
war on the world because she would have had only
6,000,000 tons of iron ore, and with this it is im-
possible to go into a war where steel is the one great
strength.
Then, if you know of the wonderful richness of the
Lorraine district which was French before 1871, the
annexed part and the French part, you know that we
produced in 1914, 48,000,000 tons of iron ore, and in
your Lake Superior district in the same year there
was a production of 52,000,000 tons. That is a very
slight difference, and you can understand how this
district of Lorraine, by the blood of your sons and by
the richness of its soil, compares to the Lake Superior
district, is extremely important for you Americans,
because it means many things for the future.
Another figure which is also instructive is the figure
that in Lorraine, in the annexed part, in the French
part, and in the Luxemburg part, there are resources
of iron ore which will exist when there will be no more
iron ore left in the Lake Superior district. We have
resources amounting to 5.000,000,000 tons of iron ore
in those two little spots on the map of Europe.
And another great factor is this, that if we leave in
the hands of German militarism, German autocracy,
not only annexed Lorraine — if we leave in the hands
of German militarism those 19,000,000 tons of
iron ore, and the 2,000,000,000 tons in reserve which
there are in the district of French Lorraine, invaded
only since 1914, the business men of Germany can see
that they not only want to keep annexed Lorraine,
but they want to occupy the districts which they took
in 1914.
If we leave 19,000,000 and 21,000,000 tons of
iron ore, and this 6,000,000 tons, and all their re-
sources to German autocracy and militarism, even if
peace comes, we will see. in the next ten years, in the
next fifteen years, a new, big war; because when a
nation with a militaristic spirit and an autocratic
spirit has in her possession the best of the iron ore of
Europe, equal to your iron ore in America, then she
must make war again.
At the conclusion of the speaking, moving pictures,
by the Ministry of War of France, were ex-
hibited, showing:
1 — A great munitions works.
2 — A war port.
3 — The armies of the Marne, Verdun, and the
So mine.
June, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
42S
ORIGINAL PAPERS
THE QUANTITATIVE ESTIMATION OF ANTHRA-
QUINONE
By Harry F. Lewis
Received April 29, 1918
In the analysis of anthracene by the method of
Luck,1 an impure anthraquinone is formed. Various
methods for the purification of this anthraquinone
have been proposed. The most popular common
modification is the one which goes by the name of
the "Hochst Test,"2 which prescribes a solution of
the product in pure fuming sulfuric acid and the re-
sultant separation of a pure crystalline anthraquinone
by dilution with water. This is a long process and
with certain types of anthracene it may be very in-
accurate. Basset3 suggests boiling the impure anthra-
quinone, obtained according to Luck's method, for
some time with a solution of mixed chromic and nitric
acids, for the reason that the pure anthraquinone does
not lose weight by this treatment, while that obtained
from commercial anthracene may lose from i to 2
per cent.
If it is desired to accurately determine the amount
of anthraquinone present in samples contaminated
with either large amounts of anthracene or phenan-
thraquinone, the above methods leave much to be
desired.
Quantitative determination of anthraquinone based
upon the formation of the oxime by the methods de-
scribed by Goldschmidt,4 Schunck and Marchlewski5 and
Musenheimer6 have not been found practical for the
reason that the manipulation is long and difficult and
the yield of oxime could not be made quantitative.
A method for the estimation and purification of
anthraquinone has been developed based upon the
susceptibility of the carbonyl radicals to reducing
agents.
Grabe and Liebermann7 described the preparation of
a compound, which they call oxanthranol or anthra-
hydroquinone, formed by the reduction of anthra-
quinone by an alkaline suspension of zinc dust. This
compound is quite soluble in hot alkaline solution but
in that solution is easily reoxidized to anthraquinone.
They recommend the use of 2 parts of zinc dust and
•30 parts of a 50 per cent sodium hydroxide solution
to 1 part of anthraquinone. The anthraquinone is
suspended in a small amount of 50 per cent alcohol
and the hot alkaline solution and zinc dust added.
This mixture is heated for half an hour and filtered.
On the filter paper arc found the unchanged portion of
the anthraquinone and the zinc dust; the oxanthranol
in the filtrate may be oxidized with air, and the anthra-
quinone formed filtered and weighed.
Following out the above directions, a dark green, alka-
line solution is obtained instead of the cherry-red
1 Z. anal. Chtm., 12 (1873), 34; 13 (1874), 25.
' Ibid., 16 (1877), 61.
• Chtm. New;, 73 (1896), 178.
• Ber., 16 (1883), 2179. i
> Ibid.. 27 (1894), 2125.
• Ann., 323 (1902), 207.
'Ibid., 160 (1871), 126.
solution described by Grabe and Liebermann. The
red color is formed on dilution, so it seems possible
that a typographical error in regard to the concen-
tration of alkali employed was made in the original
paper. When the concentration of the sodium hy-
droxide solution is about 5 per cent or less it has been
found that the reduction and subsequent reformation
of anthraquinone can be made quantitative.
Johann Walter1 has made use of this process for
the separation of anthraquinone from anthracene and
phenanthraquinone. He gives no detailed description
of the method.
The following procedure, if carefully followed, has
been found to give very accurate results. In addition
to the factor of increased accuracy this method has
the added advantage of a substantial saving of time.
One part of anthraquinone is wet with a small -
quantity of alcohol, mixed with 2 parts of zinc dust,
and about 50 parts of a hot 5 per cent sodium hydroxide
solution added. The mixture is heated just below the
boiling point for 5 min., and then rapidly filtered by
suction, and washed once with water. The filter
paper with the residue is heated with another equal
portion of the sodium hydroxide solution and rapidly
filtered into the same flask. A third heating with
alkali is sufficient to effect the solution of any residue
of anthraquinone that may remain unreduced. The
combined nitrates are cooled and reoxidized by shaking
in the presence of air. A practical procedure is to
shake the suction flask under a stream of cold water
until the red color disappears. The resulting anthra-
quinone is filtered upon a weighed Gooch crucible,
washed with water, dried at 110° and weighed.
The following precautions must be observed:
If the mixture is boiled for too long a period, there
is some formation of the next reduction step, the c6m-
pound called by Liebermann and Gimel,2 anthranol,
which contains one less oxygen atom than does the
oxanthranol and does not reoxidize to anthraquinone
by the action of air. The presence of this compound
is easily shown by any yellow color in the' fiftr'ate1 From
the final reoxidation.
There is danger that all the anthraquinone may not
go into solution through the reduction. This is readily
determined. If the residue on the third filter paper
imparts no red color to the liquid when boiled again
with hot alkaline solution, the reduction is complete.
A green color showing in the reoxidized anthraquinone
indicates the presence of a reduced compound of phen-
anthraquinone, the structure of which has not been
determined. Phenanthraquinone in the original sub-
stance causes high results, but when present in amounts
less than 10 per cent the error is not sufficient to vitiate
the practical value of the method.
It is necessary that the hot solution of the reduced
anthraquinone be filtered rapidly in order to prevent
reoxidation on the filter.
■ D. R. P. No. 168,291 (1904).
' Ber., 20 (1887), 1854.
426
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 6
It has been found that certain grades of asbestos
are affected by alkali and it is necessary that the as-
bestos, before use, should be freed from alkali-soluble
constituents.
For analytical purposes a very good sample of an-
thraquinone was obtained from a so-called chemically
pure commercial sample by recrystallizing several
limes from hot toluene. This commercial sample
was analyzed by the above method and gave the fol-
lowing result:
Anthraquinone taken 0.2000 g.
Anthraquinone recovered 0. 1992 g.
Loss 0.008 g. = 0.40 per cent
After purification the sample was analyzed as follows:
Table I — Analysis op Pure Anthraquinone
Sample Zinc Dust Sodium Hydroiide Recovered Per
Gram Gram Co of 5% Soln. Alcohol Gram cent
0 2000 0 4 15 To 0.2003 100.15
0.3002 0.6 20 wet 0.2997 99.83
0 2003 0 4 15 sample 0.2007 100.19
This method of purification and estimation seems
to be especially adapted to supplant the "Hochst
Test" in the estimation of anthracene because of its
greater speed and accuracy. It may also be used' with
excellent results in estimating the purity of anthra-
quinone which is contaminated with anthracene and
less than 10 per cent of phenanthraquinone.
The examples given in Table II illustrate the degree
of accuracy to be expected when no special precautions
are taken. Some of these analyses were completed
in less than 2 hours.
Table II — Analyses of Mixture?
Composition of Mixtures
Anthra- Antfara- Phenanthra- Anthraquinone
quinone cene quinone Recovered Per
Gram Gram Gram Gram cent
0.1803 0.0297 0.0000 0.1805 100.09
0.1982 0.2000 (10000 0.1975 99.65
0.1782 0 0000 0 0228 0.1805 101.28
0.2018 0 0747 0.0000 0.2020 100.10
0.2005 0.1342 0.0098 0.2000 99.75
0 2004 0 0000 0 0100 0.1999 99.75
A single analysis may be easily completed in i'/s
hrs., exclusive of the drying of the final product to
constant weight. If analyses must be completed in
a short time the drying of the sample may be hastened
by washing with alcohol and ether. The sacrifice
in accuracy may be as little as i per cent.
A modification of this method is being worked out
to increase the accuracy in the presence of large amounts
of phenanthraquinone.
Color Investigation Laboratory
Bureau of Chemistry
Washington, D. C.
CRITICAL ELABORATION OF QUANTITATIVE PRECIPI-
TATION METHODS
EXEMPLIFIED BY A METHOD FOR THE DETERMINATION OF
PHOSPHORIC ACID
By H. Heidsnhaxn
Received December 12. 1917
Of the numerous quantitative precipitation methods
comparatively few have had the benefit of a thorough
critical investigation. With most of them their authors
have been satisfied when "good results" had been ob-
tained. Such, however, are by no means proof of
the correctness of a method. A compensation of
errors must always be considered a possibility. As
long as there exists any doubt in this respect, the
scientific analyst will not be satisfied. On the con-
trary, he will desire to learn how a method will work
under various conditions, i. e., what influence the
quantity of substance employed, concentration of
solution, temperature, presence of certain substances,
etc., may have on the result.
The task of examining a method as to its reliability
has been put up to me repeatedly. While at first
such work was lined out by me just for the particular
case on hand. I later found that certain methods em-
ployed in my researches were applicable in a great
number of cases. I might say that in a measure I
have found a scheme for this class of work.
It is the purpose of this article to develop this scheme.
However, before taking up my subject proper, I think
it advisable to show how in one case of my experience
the scheme has been successfully applied, as by so
doing it will be easier for me to make myself clear
later on.
A PRACTICAL CASE
The method of determining phosphoric acid by pre-
cipitating the same by molybdic acid solution and
transforming the molybdic precipitate into magnesium
ammonium phosphate is generally known. This trans-
formation was necessary as long as we did not under-
stand how to produce the molybdic precipitate in con-
stant form. This, however, has finally been accom-
plished. Several articles on this subject have been
published, but it was the thorough researches by
Hundeshagen, Zeilschrift fiir analytische Chemie, 1889,
which chiefly aroused my interest. Hundeshagen
proved in convincing manner that the precipitate con-
tains, for every 3 equivalents of phosphoric acid,
24 equivalents of molybdic acid and 3 equivalents of
ammonium, if produced under certain conditions,
and that the precipitate could be determined by ti-
tration with standard alkali solution, using phenol-
phthalein as indicator. Testing Hundeshagen's method
I could confirm his findings, but I noticed that the
end reaction at titration was lacking in sharpness.
Hundeshagen used a solution of ammonium nitrate
as wash liquor, an appreciable amount of which re
mains in the filter and precipitate. This, as well as
the ammonium in chemical combination with the
phosphoric and molybdic acids, evidently is to be
blamed for the uncertainty at titration, as ammonium
salts cannot be titrated with exactness with phenol-
phthalein as indicator. On the other hand, this indi-
cator seems indispensable to bring phosphoric acid to
a definite stage of neutralization. There was, however,
a way out of this dilemma. After the precipitate had
been washed with ammonium nitrate solution, this
salt could be removed by washing with alcohol and
the ammonium in the precipitate could be gotten rid
of by supersaturation and evaporation with the stand-
ard alkali solution, and determination of the excess
of alkali by boiling with an excess of standard acid
solution and titrating back with standard alkali solution.
Thus the end-reaction was made sufficiently sharp and
the results obtained were very satisfactory, but the
method had become rather cumbersome.
'
June, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY 427
As stated, the trouble was caused by the presence III — As to the completeness of the precipitation of
of ammonium. If in its stead a fixed alkali could be phosphoric acid by the solution of potassium molyb-
used, all difficulties, it seemed, were overcome. The date in nitric acid by standing without stirring.
thought suggested itself, to precipitate the phosphoric IV— As to the effect of stirring on the completeness
acid in the form of potassium phosphomolybdate, of precipitation.
which likewise is a compound of very little solubility. v » . ., • a , . , . , .,
, , .j. • , . v — As t0 tne influence of nitrate of potash on the
Hundeshagen mentions the potassium compound in „~»;^t.ii„
, ... precipitation,
his article and states that its composition is analogous . ...
,, , 1 ,, . « . . ., . .. . VI — As to the influence of nitric acid on the ore-
to that of the ammonium compound, but that it is . . ».*«*.«« uiuu. <».m ^n mc h.c
more soluble than the latter. My own experiments
confirmed this. At the same time, the results I ob- VII— As to the influence of different substances as
tained were so good that I thought it worth while to chlorides, sulfates and tartrates on the precipitation.
follow the matter up, i. e., to subject the contemplated The results of these investigations are given in the
method to my scheme of criticism. following tables. Table VIII shows a few determina-
One of the first observations made was that the wash- tions of phosphoric acid in a chemically pure mono-
ing of the precipitate could not be declared finished potassium phosphate.
by any test employed, be it a test for acidity or for T ,„ . c
v J r j 1 j Table I — Solubility of Potassium Phosphomolybdate in Solutions
molybdic acid. The wash liquor used at first was a °' potassium nitrate
solution of 10 per cent potassium nitrate in water. The After Disestion with Potassium Phosphomolybdate
filtrate remained acid even after prolonged washing. KNOa in Neutralized by spending
Tirt. j.u L-_ a 11 j n t_ 1 Expt. 100 cc. AT/50 KOH to PsOi
When the washing finally was stopped after such large no. Grams Cc. Mg.
quantities of wash liquor had been used that un- ' }° 2.1 0.130
doubtedly all free acid had been removed, the results 3 20 2.1 0.130
were too low. Obviously the solubility of the pre- _ _ _
J • c Table II — Solubility op Potassium Phosphomolybdate in Solutions
Clpltate was the cause of this loss. Following famous of Potassium Nitrate Acidified by Nitric Acid
precedents I might have declared the washing finished 10cc Neu. PotasA[uem pfesphTmoiybdate
after a "certain" amount of wash liquor had been used. <rSnu"on c£Nmned traiized '° «• s°lu''°n Corre-
^ KNOa in HNO3 by Neutralized by spondmg to
Such arbitrary methods, however, I never approved Expt. 100 cc. Corresponding N/50 koh avso koh p2o.
J . ' rr No. Grams to a Cc. Cc Mg.
of. I tried washing until constant acidity of the fil- 1 10 i/iooA'som. 5 5.1 0.006
trate was attained, assuming that the acidity of the \ ;;;; 5o i/250 n loin! 2 f.l oiois
filtrate must gradually diminish until all free acid had 4 10 i/soo 2V soin! 1 lis oio49
been removed, and that when the acidity of the filtrate Tablb hi—Precipitation of Phosphoric Acid by Potassium Molyb-
was caused only by the solubility of the precipitate, DATE Solution A*TBR 16 HRS- standing without stirring
constant acidity would prevail. This principle was pfo"?mpToyed -'0.6174 mg. | constant
a gOOd One, Only I found that when Constant acidity folium' moiybdate solution'-tarying
was attained, already losses had been sustained which Solution of Titration
, , 11 i_ j- j j, t^ 11 j Potassium of Precipitate PiO&
could not very well be disregarded. It then occurred expt. Moiybdate by N/50 koh Lost
to me to give the wash liquor from the beginning a N(0' pC p°0 0*?4
certain acidity by addition of nitric acid, thus rendering 2 1.0 0.0 0.6174
. . J , , ,, ^, . , , 3 2.5 7.15 0.176
the precipitate less soluble. 1 his move was successful. 4 5.0 7.60 0.148
T f , ., . . . , .. , . 5 10.0 7.65 0.145
I found that in a 10 per cent solution of potassium & 20.0 7.35 0.164
nitrate with SO much free nitric acid as Corresponds > This solution was prepared analogous to the usual ammonium molyb-
to a 1/100 normal acid, the solubility of the precipitate date ^"tio" lt contained 5 per cent Moo..
Was but 1/20 of that in the neutral Solution. The Tablb iV— Precipitation of Phosphoric Acid by Potassium Molyb-
losses were now so small that the results were not DATB Solution after 5 Min. storing and 45 Mm. standing
affected any more to any serious extent. The small See Table in for description of solution
... „ e .. .. • ., /,,1 . Solution Titration
quantity of tree acid remaining in the filter and pre- Potassium of Precipitate PtO»
cipitate could be determined with satisfactory accuracy E^T- Moiybdate by avso koh Lost
and a corresponding correction applied. While in 1 2.5 0.3 0.599
K , , T 2 5.0 9.65 0:014
my first experiments the results were too low, I now 3 10.0 9.9 0 006
obtained figures a trifle too high, presumably caused 5;;;; " Jo!o s!io 0 117
by some molybdic acid which had been carried down _ „ . _
* , » Table V — Influence of Potassium Nitrate on the Precipitation
by the precipitate. of Phosphoric Acid as Potassium Phosphomolybdate
From these preliminary experiments I had learned P20" "mpToyed -c'o.6i74 mg. ^ Constant
to handle the method. However, in order to become Potalslurn aulltt- 'varying " '° "' ^
clear concerning all phases of the method I had to fTprecMtate p.o
proceed systematically. I made a series of experi- Expt knOj by avso koh Lost
J J r No Grams Cc Mg
ments- • 1 5 0.0 0.6174
I — As to the solubility of the precipitate in a neutral *•■•■ ]',' *|5 ?> mI
solution of potassium nitrate. 4.'.'.'.'.'. 20 9.3 o.o«
II— As to the solubility of the precipitate in an acidi- ^j™ 9olution wa3 stirred for 5 mi... and allowed to stand 2V, to .
fied Solution Of potassium nitrate. the others were also stirred for 5 min. but allowed to stand only 1 hour.
428 I 111. JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 6
Table VI — Influence of Free Nitric Acid on Tin: Precipitation of i_ u • 1 a -e j r i
phosphoric Acid as potassium phusp.iomui.vbdat.' error, however, may be avoided if, instead of large
7 l0? cc„ , ) quantities, small quantities are employed, for in small
tnployed = 0.6174 mg. I .... ,
■■iiiiii nitrate - 20 g. ( constant quantities the absolute amount of the impurities is
Potassium molvbdatc soln. — 10 ,, , , , , .. , ,
Nitrii very small and may, therefore, be disregarded.
Titration In experiments to study the solubility of precipitates
Expt. by N/ Lost we must keep apart (a) the influence of the solution
No.(a) Cc. Mg.
i o 9.3 0.043 from which the precipitate is separated, (b) the influ-
3.'.'. '.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'. 20 o!o o'o?74 ence of the wash liquor.
(o) These solutions were stirred for 5 min. and allowed to stand 1 hr. (a) For the determination of the former the method
Table vii-Influence op Different Substamcbs oh tub i'recp.ta- is the same as with an ordinary determination, only
tion op phosphoric Acid as pot IMOI.YBDATB the quantity employed is to be taken so small that
Volume = 100 cc. \ ,., ' * , .. , ..
FiOi employed = 0.6174 mg. ( Constant while a considerable portion remains in solution, still
Potassium moiybdate soil. = io cc. f a decided precipitation is taking place so that the effect
Titration of of supersaturation has not to be taken into account.
Precipitate PiOi ...
Expt. Additions o koh Lost According to circumstances, either the part remaining
No. 1 g. of Each Cc. Mg. , ° ., . . .. . 7?
, EC] g 9S 0 065 ln solution or the precipitated part is determined.
\ khc.'ii.o. o'o° o'oi74 Sometimes both parts may successfully be determined
* CaCOa dissolved in hno. 9.25 0.046 which, of course, will give the most satisfaction. It is
Table VIII— Determinations op Phosphoric Acid as Potassium hardly necessary to mention that solutions employed
PHOSPHOBOlLVBDATa IN MONOPOTASSIUM PHOSPHATE' for these ^^% ^ lQ contajn aU gubstanCeS in the
EHtPOi PiOi PiOi Time of . .
Expt. Employed Found Calculated Difference Standing Same proportion as in a practical analysis.
No. Gram Per cent Per cent Per cent Hours T, , - , . . . J . . n r .
, 0 , 52.14 52.20 —0.06 ■/» purpose of determining the influence of the
2 2/} I2?2 52-22 _2'2«: '/,'■ single substances of the solution, it is commendable to
3 0.1 52.14 52.20 — 0.06 Va
■* o.i 52.23 52.20 +0.03 'i* make series of tests in which, at a time, one substance
5 0.05 52.17 52.20 — 0.03 2'/i . .
6 0.05 52.35 52.20 +0.15 3'/. is varied while the others remain constant and to pre-
i The sample of KH.PO, and 7 g. KNO, was dissolved in 30 ee. water. sent the results in the form of tables. The study of
Then 4C ice. potassium moiybdate solution was added i. The precipitate the influence of temperature and concentration does
was washed with a 1/100 normal nitric acid solution containing 10 g. JCNOi r
in 100 cc. until 10 cc. of the nitrate were neutralized by 5.1 cc. -V/50 KOH not need any explanation
solution. (Compare Table II, Expt. I.) .,._,",.. . ...
(o) The determination of the solubility of a pre-
RcTurning to my subject proper — it seems to me cipitate in the wash liquor seldom presents any difficulty
that the accuracy of a precipitation method depends if we have plain water or another volatile liquid. All
upon two circumstances — first, upon the degree of that need be done is to digest a small quantity of the
solubility of the precipitate; second, upon its purity. washed precipitate for a sufficiently long time to ensure
If we fail to find satisfactory conditions in these two saturation and to determine the dissolved part by
respects we consider the method as worthless or em- weighing after evaporation or by titration, etc. If
ploy it only conditionally. However, we must alwTays solutions of salts are used as wash liquors the determina-
keep in mind that ideal conditions can never be ful- tion by evaporation and weighing the residue is out
filled. All precipitation methods, therefore, are more of the question. There remain, however, all other
or less defective. methods of determination.
If we wish to try a method as to its accuracy, it is It is hardly necessary to mention that the methods
not sufficient to submit a certain quantity of a substance for the determination of such small quantities as we
to a prescribed process and accept the result as final have to do with in this class of investigations must
criticism, because the two sources of error mentioned be adapted to the conditions. Filters, funnels, evapo-
may influence the result in such a manner that one rating dishes, etc., must be taken proportionately small
compensates the other. In order to avoid the danger and standard solutions proportionately dilute, or the
of such deception, either source of error must be in- unavoidable errors from weighing and measuring may
vestiiv itely and the amount of either error invalidate the results.
mUS' " X"1 Until theSC> nre kn0WD "U1 INVESTIGATIONS AS TO THE PURITY OF PRECIPITATES
it be possible to pass judgment upon the worth of a
method. Tne Parity of a precipitate may be impaired by two
different causes — first, by incorrect stoichiometric
INVESTIGATIONS AS TO THE SOLUBIL] CIPITATES M„„Ar;(;„„. ,„„„j k,. ( : „ u„t-„~^*.
composition; second, by toreign substances.
As mentioned above, precipitates are afflicted with In contradistinction to the experiments on solu-
the evil of impurity. If, in order to determine the bility for which small quantities are employed, the
solubility of a precipitate, we would digest a large examination as to purity requires large quantities,
quantity of it with a liquid or a solution, it is not at because impurities or deviations from the theoretical
all impossible that the parts of the main substance composition are permissible only to a small extent in
and the impurities going into solution stand to each precipitates which are adapted for quantitative de-
other in a ratio different from that in which they were terminal
originally present. In such a case, no matter whether A general scheme of procedure for these researches
the part going into solution or that remaining undis- cannot very well be given, as the variety of cases is
solved be determined, the results are misleading. This too great. All thai ma] be said in a general way is
June, 191S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
429
that the precipitates must be subjected to analysis
just as if they were original substances for an analysis.
If it is found that the composition of a precipitate
comes up to expectation fairly well, it might be suffi-
cient to establish a factor by which the results are to be
multiplied. However, if this is not the case we must
endeavor to improve the purity of the precipitate.
In general, precipitates are the purer, the more dilute
the solutions from which they have separated. Still,
too great hopes in this respect should not be enter-
tained, for the ratio of the precipitate to the substances
in solution remains the same on dilution, and it is the
influence of these substances which, in many cases,
prevent the pure separation of the precipitates. The
purpose is better accomplished if precipitation is re-
peated after the bulk of the first solution has been
removed. Especially is this to be recommended if
the precipitation had to take place in highly concen-
trated solution.
If removal of the impurities is impossible, nothing
else remains to be done but to make determinations
with varying quantities in order to arrive at an esti-
mation of the amount of impurities, taking into ac-
count any losses caused by the solubility of the pre-
cipitate. If at the same time the possibility of incorrect
stoichiometric composition prevails, such results, of
course, allow more than one explanation.
From the aforesaid it is clear than two radically
different methods of procedure are necessary to criti-
cize precipitation methods. The completeness of
precipitation and the losses on account of solubility
must be studied on small quantities. As a matter of
fact, a few milligrams of the substance are sufficient
in most cases. Simultaneously we learn from this
part of the critical work on a method the limit of its
applicability for the determination of small quantities.
In order to characterize these conditions I would like
to introduce the term "micro-analytical." On the
other hand, examinations as to purity and correct
composition, likewise the final tests with the view to
practical application, must be made with large quanti-
ties. For these reasons I would like to call this part
of the criticism of the method "macro-analytical."
For another reason also it would be well to make
such distinction. The micro-analytical errors are
always absolute losses. Accordingly their corrections
will consist in additions. But the macro-analytical
errors have the form of proportions and must, there-
fore, find their corrections in multiplications or di-
visions. The general algebraic formula for the correc-
tion of a result will be thus:
Q X M1 X M- + m' + m-
in which Q represents the actual quantity of a pre-
cipitate, M1 and M2 the factors for the macro-analytical
corrections and m1 and m2 the losses caused by solu-
bility.
While methods requiring corrections have not been
considered the best, there is no reason why one should
hesitate to use a method after it has undei
thorough critical treatment; in other words, after the
errors have been scientifically determiii'
contrary, results corrected on a scientific basis deserve
more confidence than such as are obtained by methods
which are believed to be reliable, but which never have
been criticized in a methodical manner.
25 Ogden Street
Indiana
IMPROVED METHODS FOR THE ESTIMATION OF
SODIUM AND POTASSIUM
By S. N. Rede
Received September 19, 1917
■ A method for the estimation of sodium, involving
considerable modification of the procedure of the
Association of Official Agricultural Chemists, was pub-
lished from this department by Forbes, Beegle and
Mensching in Bulletin 255 of this Institution, under
the date of January 1913. Since the time of this
publication we have made extensive use of this im-
proved method and have devised further improvements,
which it is our purpose to record. The general prin-
ciples of the method as now used are the same as
stated in the earlier publication referred to above,
but changes of detail have been devised which shorten
the process and remove certain sources of possible error,
at the same time calling for much less use of platinum.
Incidentally, improvement has been effected in the
method for the estimation of potassium.
For the quantitative test of the new procedures a
salt solution was prepared in such manner as to con-
tain the same kinds and proportionate amounts of
the mineral elements as are present in wheat bran.
Nitrogen, also, was added to this solution, in the form
of ammonium sulfate. The elements and the com-
pounds in which they were present were as follows:
Sodium CiHiONa
Potassium CzHtOK
Calcium CaHPO.^HiO
Magnesium Mgj(POf)i.4H20
Sulfur H2SO. and (NHi):SO.
Chlorine HC1
Phosphorus Salts of Ca and Mg
Nitrogen ." (NH«);SO.
The sodium and potassium ethylates were prepared
from the pure metals by dissolving in absolute alco-
hol and standardizing by titration against benzoic
acid. Calculated from the weights of the metals (in
air), 10 cc. of the solution should have contained
0.01045 g. Na and 0.03926 g. K. The titration
against benzoic acid indicated the presence of 0.01037
g. Na and 0.03757 g. K (0.03202 g. sodium sulfate
and 0.08373 g- potassium sulfate) in the same volume
of solution. The latter weights were used as the basis
for judgment as to the correctness of analytical
methods.
MODIFICATION OF THE METHOD FOR SODIUM
In the use of the method for sodium, as published in
Ohio Agricultural Experiment Station, Bulletin 255,
we have found much advantage in the principle of
the second of the optional methods of ashing. The
first method proposed for destroying the organic
matter, by nitric-sulfuric acid digestion, necessitates
the subsequent burning off of much sulfuric acid, in
which process there is great likelihood of loss through
spattering and overheating. In our later work,
THE JOURNAL 01 INDUSTRIAL AND ENGINEERING i HEMISTRY Vol. 10. Xo. 6
therefore, the principle of the second optional method
of ashing (in which the little sulfuric acid used is en-
tirely driven off) has been followed, and the ashing
is now conducted in porcelain, instead of platinum.
After the precipitation of the phosphorus, in the
solution of the ash, as magnesium ammonium phos-
thc published method specified the evapora-
tion of the filtrate and the burning off of ammonium
salts in a platinum dish. In the later work, the am-
monium salts are destroyed by digestion with nitric
and hydrochloric acids, these acids being finally driven
off, first by evaporation and then by baking on the
hot plate.
The details of our later method for the estimation
of sodium are as follows:
Weigh the sample into a porcelain dish, cover with 25 per
cent sulfuric acid, reduce to dryness on the steam bath, and
char completely on the hot plate.1 After all foaming has ceased,
ash over an open flame. If necessary, to complete the ashing,
leach with hot water, and reburn the residue. Digest the ash
and teachings in HC1 and water on the steam bath for one hour,
and filter into a 400 cc. beaker, washing the residue on the filter
paper with hot water, or, in case the same solution is to be used
for both sodium and potassium estimations, filter into a volu-
metric flask.
Add enough ammonia to the solution to render it almost
neutral,' and enough magnesia mixture to precipitate the phos-
phorus as magnesium ammonium phosphate. After 15 min-
utes add 5 to 10 cc. of concentrated ammonia, and allow to
stand over night. Kilter, and wash out sodium and potassium
sulfates with 2.5 per cent ammonia. Now add 20 cc. of
concentrated HNOj and a little HC1, and evaporate to dry-
ness on the hot plate. Continue heating for 1 or 2
hrs. to drive off all excess acid. Dissolve the residue of
sulfates with hot water and transfer to a 250 cc. beaker.
Boil, and add a saturated solution of freshly prepared Ba(OH)2
to the complete precipitation of the magnesium. Filter, and
wash with hot water, testing the filtrate for complete pre-
cipitation of magnesium. (If the filtrate is milky it is an
indication of incomplete precipitation of magnesium. ) After
all the magnesium is filtered out make the solution ammoniaeal,
boil, and add enough ammonium carbonate and ammonium
oxalate (saturated solutions) to completely precipitate the
barium and calcium. Allow to stand at least 2 hrs.; filter,
wash with hot water, add 5 cc. ammonium sulfate solution
(75 8- (NH4)2S04 per liter) and evaporate to dryness. Dis-
solve the residue in hot water and transfer directly to un-
weighed platinum dishes. Evaporate to dryness on the steam
bath and heat carefully over a free flame to dull redness. Dis-
solve residue in hot water and filter into weighed platinum
dishes. Evaporate to dryness on the steam bath and heat to
constant weight over the open flame. The residue weighed
consists of the sodium and potassium sulfates. Calculate the
amount of potassium found to the sulfate, and subtract from
the weight of combined sulfates to obtain the amount of sodium
sulfate.
Milium \iii.\ D] 1111 Ml I 1 1 • > 1 > FOB POTASSIUM
Potassium was estimated by the official Lindo-
rin burning ..I the sample in a porcelain dish with H.So, dots not
in error by removing potassium 01 sodium compound! from the
di ii 1 1 determine this i»imi 10 g ol chemically pur, sugar und 25 cc.
d in ne« and in old porcelain dishes, and
potassium and sodium were determined bj ibeat ;
I unpublished «ork in this i.,
shown ill ii nd aluminum il present should be precipitated
and removed at this point. — (E. B, Forbes)
Gladding procedure, modified as to the method of
ashing, and also for preliminary precipitation of cal-
cium and iron, where such treatment is necessary.
The details of the method as used are as follows:
Prepare and digest the ash in the same manner as specified
for sodium above Make the solution ammoniaeal; boil and fil-
ter, washing well with hot water. Heat the ammoniaeal filtrate
to boiling and add sufficient ammonium oxalate (saturated solu-
tion) to completely precipitate the calcium. Allow to stand
overnight. Filter, and wash with 2 . 5 per cent ammonia. Add
20 cc. of concentrated HNOj and a little HC1; evaporate to
dryness and bake on the hot plate for 1 or 2 hrs. to drive
off excess nitric acid. Take up the residue with hot water
and a few drops of HC1; filter into a 150 cc. beaker. Add enough
H2PtCU solution for the complete precipitation of potassium.
Evaporate the solution on the steam bath almost to dryness,
cool and add a few cc. of 80 per cent alcohol. Filter through a
small sugar tube, and transfer the precipitate to the tube by
means of a rubber-tipped rod and 80 per cent alcohol. Wash
the precipitate and asbestos free from H2PtCl« with 80 per cent
alcohol. Wash the precipitate about five times with 5 to 10
cc. of NH,C1 solution (100 g. NH4C1 in 500 cc. H20 saturated
with K2PtCl«) or until all white or light orange material is dis-
solved. Then wash the precipitate and pad free from XH,C1
with 80 per cent alcohol and drive off the alcohol in a hot-air
oven. Wash the K2PtCl6, with hot water, from the sugar tube
into a weighed platinum dish ; evaporate to dryness on the steam
bath, and heat to constant weight in a hot-air oven at 105 ° C,
weighing as K2PtCle.
ANALYTICAL RESULTS OBTAINED BY MODIFIED METHODS
Estimation of sodium in the test solution, by the
improved method, gave results as stated below:
Gram
Combined sulfates found in 10 cc. solution 0.1131
0.1135
0.1139
0.1141
0.1 143
0.1153
0.1169
0.1173
Average 0.1148
Actually Present 0. 1 1575
This method was found much superior to the usual
procedure, both as to ease of operation and agreement
of results. The amount of sodium found was 99 per
cent of the amount present.
Sodium Estimations on Foodstuffs — Dry Basis
Combined Potassium Sodium
Com* sulfates sulfates sulfates
SAM- Wt. of bined per gram per gram per gram
ftB sample sulfates sample sample sample Per cent
No. Foodstuff Grams Gram Gram Gram Gram sodium
1 Corn meal.. 10 0 0838
2 Corn meal . .. 10 0 0870
3 Corn meal 10 0.0850
Average. .. 0.0853 0.00853 0.66770 0. 00083 0.2269
1 Corn silage S 0.0824
silage 5 0.0820
Corn ail 1 [e 5 O.osos
Average .. 0 0817 0.01634 0.01463 0.00171 0 0554
ed oil
meal O.Ofi
2 Linseed oil
meal
Linseed oil
meal • 0.08IC
A.VTSRAOB. 02747 0 02617 O.o6i30 0 .04:1
it bran. 3 0.0S60
2 Wheal bran ) 0 0846
> Wheal in. in . 11 0808
l-VBKACB 0.083S 0.02793 0 02791 0.00002 00007
1 Alf:,H.i I 0 is;-!
2 Alfalfa ... 3 0. I860
3 Alfalfa 0.I86O
Average. 0 1851 0.06170 0.05549 0.66021 0 2011
June, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Estimation of potassium in the test solution, by
the improved method, gave results as stated below:
: chloride) found i
Average 0 . 228 1
Actually Present 0 . 2336
Results obtained by the usual method were high,
and the agreement was not satisfactory, probably
because of incomplete washing out of the calcium
and magnesium sulfates with ammonium chloride
solution. The improved method of ashing converts
the calcium and magnesium into the chlorides which
are easily washed out with ammonium chloride solu-
tion. The agreement of results by the improved
method is satisfactory, and the amount of potassium
found was 98 per cent of the amount present.
Potassium Estimations on Foodstuffs — Air- Dry Basis
Potassium
platii
Fooost
Corn meal.
Wt. of
sample
Grams
Corn silage
Corn silage
Corn silage
Average
Linseed oil meal.
Linseed oil meal .
Linseed oil meal .
Average
Potassium
platinie
chloride
Gram
0.1083
0.1163
0.1065
0.1074
0.0937
0.0913
0.0897
0.0916
0.1083
0. 1115
0.1087
0.1095
chloride
per gram
sample
Gram
Potassiurt
sulfate
per gram
sample
Gram
0.02148 0.00770 0.3455
0.04080 0.01463 0.6562
0.07300 0.02617 1.1741
Wheat bran
Wheat bran
Wheat bran
Average 1 and 3 .
Alfalfa
Alfalfa
Alfalfa
Average
0.1147
Dish broke during ignition
0.1189
0.1168 0.07786 0.02791
0.1561
0 . [ 539
0.1545
0.1548
0.15480 0.05549
Department of Nutrition
Ohio Agricultural Experiment Station
Wooster, Ohio
A COMPARATIVE STUDY OF THE THERMAL DECOMPO-
SITION OF COAL AND OF SOME OF THE
PRODUCTS OF ITS CARBONIZATION1
By M. C. Whitaker and John Richard Suydam, Jr.
The work of Whitaker and Rittman,2 Egloff,3 Alexan-
der,4 Leslie,5 Zanetti,6 and others has shown that it is
possible to control the thermal decomposition of hydro-
carbons in such a way as to give the maximum yields
of certain products of decomposition, such as con-
stituents of gases, aromatic hydrocarbons, etc.
. The purpose of this investigation was to determine
if different hydrocarbons and other organic compounds
1 Abstract of dissertation submitted in partial fulfillment of the require-
ments for the Ph.D. degree, Columbia University. New York City, 1917.
! Tims Journal. 6 (1914), 383. 472.
1 Mrl. and Chtm. Eng... 7 (1915), 16, 17. /. Phys. Chem., 1916, This
roUKMAL, 7 (1915), 481, 578, 1019.
' This Journal. 7 (1915), 484.
* Ibid., 8 (1916), 593, 684.
'Ibid.. 8 (1916), 674, 777.
did not give results that were peculiar to their ultimate
composition and chemical structure. It was hoped
in this way to throw further light on the chemical
structure of the substances in coal, by comparing the
results obtained from organic compounds with those
obtained from coal when treated in the same way.
The experiments were carried out in a vertical,
electrically heated, iron tube furnace, 4 in. in diameter
and a little more than 6 ft. long.
The substances examined were powdered coal, gas-
oline, kerosene, gas oil, benzene and naphthalene. The
coal used was a Pennsylvania gas coal of the following
composition:
Moisture Volatile Matte r Fixed Carbon Ash
Proximate, percent 0.9 34.1 59.2 5.8
Carbon Hydrogen Nitrogen
Ultimate, percent 80.2 5.7 1.6
In the experiments in which powdered coal was used,
it was fed in by a worm conveyor from a hopper at the
+ = Kerosene
x = Gasolene
o = Gas Oil
o = Coal
£l = Benzol
a = Napthalene
Temperature ~ Degrees Centigrade
top of the furnace. The powder dropped through the
heated furnace, some of it sticking to the walls, and
the coke was collected below. The gas formed was
led off from the bottom of the furnace to a gasometer.
Experiments were carried out studying the effect
of temperature, rate of feed, and size of coal particles
on the production and composition of the gas. The
results are summarized in the table on page 432.
The quantity of tar produced was too small for exam-
ination.
In the work on the thermal decomposition of the
other substances examined, the liquid was fed into the
THE JOURNAL OF INDUSTRIAL AND ENGINEERING I II I UISTRY Vol. 10, Xo. 6
Temp.
°C.
650
0
750
875
875
650
750
800
800
800
Feed
Lbs. per Hr.
0.38
0.38
0.38
0.38
0.38
0.38
0.78
0.78
0.38
0.38
0.38
Size of
Coal Mesh
20-60
20-60
20-60
20-60
20-60
20-60
20-60
20-60
40-50
30-40
20-30
Cu. Ft. Gas
Per Lb. Coal
2.82
2.79
3.92
3.96
'..14
6.26
.V40
4.90
4.60
4.30
CO
15.2
12.1
12.3
12.0
15.7
16.5
12.0
12.4
■ Analysis of Gas-
H, C„H(2„ + 2) °»
5.6
2.7
2.8
2.0
30.2
28.6
35.3
34.8
52.3
53.6
31.1
36.8
45.2
44.4
42.7
47.2
43.0
41.0
26.0
0.7
0.2
0.4
0.3
0.2
0.5
0.5
0.4
0.2
0.2
5.6
7.3
2.6
0.6
4.6
5.3
top of the furnace from a sight feed pressure oiler and
vaporized from a length of chain hung in the upper
part of the furnace. Curves showing the composition
of the gas produced by the cracking of these liquids
and by carbonizing coal by the above method at various
temperatures and equal rates of feed of volatile matter
are contained in Fig. I.
CONCLUSIONS
The paraffin hydrocarbons when cracked by the
method herein described give gases which at the same
temperature have practically the same composition.
The aromatic hydrocarbons without side chains
gave a totally different form of gas curves. They do
not begin to decompose at such low temperatures as
the paraffins do and when they do break down they
apparently yield only hydrogen and methane.
After eliminating the nitrogen- and the oxygen-
containing constituents of the coal gas produced, this
gas is similar to that produced from paraffin oils and
not at all similar to the gas produced from the aromatic
bodies examined.
The above results indicate that coal is made up in
general of straight chain compounds. The best evi-
dence of this that has been put forward to date is the
fact that "low temperature" coal tar consists practically
entirely of straight chain oils.
Chemical BnoxnBBRXNO Laboratory
Columbia University
Ni;w York City
THE INFLUENCE OF COLD SHOCK IN THE
STERILIZATION OF CANNED FOODS
By L. D. Busiinbll
Received March 29, 1918
INTRO] •
The inllmi! after healing, is a
importance in the canning
industry. Its value in the blanching of foods was
first mentioned by Benson1 who reports in part as
follows:
When a food product has been blanched in boiling hot water
or live strain, remove quickly from tins and plunge immediately
into cold water. The influence of tins method upon bacteria,
1 "11"" Pi nit mci Vegetable
cms. Northern and
, 1915. p I
spores, and molds is very effectual; when this is followed by a
single period of sterilization, we contend that the success of
canning is just as sure as though three periods on three successive
days were used.
Bitting and Bitting,1 in discussing the influence of
cooling, make the following statement:
The primary effect is to make a better appearing product,
but secondly it appears to be a factor in insuring the sterility
of some products.
only possible influence that this procedure could
have, would be that of shock to the bacterial cell.
This might possibly devitalize the cell in such a way
that it would be more easily destroyed by a subsequent
heating, or, perhaps, perish slowly, or not be able to
grow, under such rather unfavorable conditions as
exist in sealed containers. Of course, this initial period
of heating during blanching will destroy many organisms
in the vegetative stage, but a glance at Table X will
show that the organisms in the spore stage are the only
ones which are of importance in canning.
If the shock of cold is of value in sterilization it
should be more widely known than it is at present, as
it could be used in many lines of investigation other
than that of food canning.
The question of blanching and cold dipping is of
particular importance in the canning of foods, as in
this case the cooling can be made much more rapid
than is possible after the material is packed in jar?.
For this reason we conducted quite extensive experi-
ments upon this problem during our preliminary work
upon canned vegetables in the summer of 191 7. The
process consists of a short period of heating in boiling
water or steam, followed by rapid cooling. The
product is later subjected to the sterilizing process.
This procedure is of much practical importance in
improving the physical condition of the product and
in causing shrinkage before the material is added to
the jars. The experiments were conducted to estab-
lish its value as an aid to sterilization.
In much of this preliminary work we used large
test tubes and half-pint bottles with large mouths.
Some of these were plugged with cotton, while others
were sealed with rubber stoppers. This was not from
an idea of economy in cost of material so much as an
economy in laboratory space and time, as rubber
stoppers usually cost more than jars. Several dozen
test tubes, however, occupy no more space in the
steamer than would be occupied by one dozen pint
jars. Also, heat penetrates them much more rapidly
were able in this way to save at least half an
hour on each experiment. The results which we ob-
tained were comparable in every way to results which
we obtained by the use of jars.
The tubes are somewhat more difficult to seal,
but if tluy are completely filled before heating begins
and are sealed at once by a sterile solid glass rod as
soon as the heating period is completed, practically
no troul rienced by the stoppers being blown
out on second heating. Better results are obtained
by using stoppers with one hole and plugging this with
1 "Bacteriological Examination of Canned Foods." Research Labora-
u hits' AssocittlOD, Bull. 14 il9l7), 7.
June, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
a sterile glass rod, than by fitting the tubes with solid
stoppers. The rods should fit very firmly, otherwise
they may be drawn into the tube or leak air on cooling.
The stoppers should be pushed well into the tube
before the heating begins.
In all the vegetables the time allowed for heat to
penetrate in test tubes was 5 min.; in bottles, 15 min. ;
in pint jars, 30 min. This time was always allowed
to elapse before sterilization was supposed to have
begun.
EXPERIMENTAL
experiment i — The method of heating for a short
time followed by a plunge into cold water was tried
on several kinds of culture media containing varying
numbers of spores of both aerobic and anaerobic bac-
teria. The tubes were subjected to a short heating
in the steamer, followed by plunging them into cold
water, and by a second and longer heating. This
method failed in every case to shorten the time neces-
sary to sterilize, either in the streaming steam or in the
autoclave.
experiment 2 — The same procedure was followed as
in Experiment 1, except that the tests were made in
duplicate; half of the tubes were cooled rapidly in ice
water and half allowed to cool slowly to this tempera-
ture. The time required was from 15 to 30 min.
In no case was the reduction in number more marked
in the tubes cooled rapidly than in those cooled slowly.
experiment 3 — Several pure cultures obtained from
spoiled canned goods were used in this experiment.
The cultures were grown in broth for several days
and equal amounts placed in test tubes as near the
same thickness of wall and the same diameter as could
be obtained. These were then placed in streaming
steam for 10 min. Half of the tubes were plunged
into ice water and the remaining half allowed to cool
slowly to the same temperature. These tubes were
then all placed in the steamer and steamed for 30
min. and plates made. Table I shows the results
obtained.
Table 1
Original Cooled Rapidly Cooled Slowly
No. Per Cc. Per Cc. Per Cc.
1 38,000,000 2,600,000 2,500,000
2 1,000,000 0 100
3 90,000,000 14,000,000 11,000,000
4 40,000,000 7,000,000 600,000
5 70,000 200,000 200,000
6 268,000,000 4,300,000 1,300,000
7 1,580,000,000 60 0
8 600,000,000 20 0
This table shows that the shock of cold did not
influence the thermal death-point of pure cultures,
as all the above data, except, perhaps, No. 4, are
easily within the limits of experimental error.
experiment 4 — In this experiment we tried the
influence of cold shock upon the time necessary to
sterilize peas. The peas were treated in every way
as in ordinary canning and blanched for different
periods of time. In order to avoid contamination
in handling and to insure rapid cooling in the ice
water, the peas were placed in test tubes of medium
size, covered with water, and the tubes plugged with
cotton. The tubes were heated in streaming steam
for different periods of time. Xo time was allowed
for penetrating, which was found later to be about
5 min. The time of spoilage was noted by the ap-
pearance of clouding of the liquid surrounding the
peas and by presence of growth on the surface. We
have always noted these signs when spoilage appeared
in containers sealed with cotton only.
Table II
Cooled Rapidly Cooled Slowly
Blanched Heated Time of Spoilage Time of Spoilage
Mm. Min. Hrs. Hrs
5 60 72 120
10 60 72 120
20 60 72 120
5 90 72 120
10 90 72 120
20 90 72 120
In this case there is no evidence that the length
of blanching time or the rapidity of cooling influenced
in any way the ease with which the spores were subse-
quently killed by heat. In fact, those cooled more
slowly seem to be least easily destroyed if the time
of spoilage is an indication. We may account for
this on the basis of germination of the spores during
the slow process of cooling, as this usually requires
several minutes (see Table IV).
experiment s — Table III shows the influence of
cold shock followed by intermittent heating. In
this case green beans were used and the conditions of
the experiment were similar to those in Experiment 4,
except that blanching was continued for 15 min.
in the steamer.
Table III
Time between Last Heating and Spoilage
Heated Cooled Rapidly Cooled Slowly
15 min. twice 1 day Spoiled after 48 hrs. Spoiled after 60 hrs.
30 min. twice 1 day Spoiled after 60 hrs. Spoiled after 60 hrs.
60 min. twice 1 day Good after 10 days Good after 10 days
90 min. twice 1 day Good after 10 days Good after 10 days
This experiment also shows that spores are not
devitalized by cold shock and that blanching for
rather long periods followed by cold dipping does not
aid in sterilization.
experiment 6 — This experiment was devised to
test the possibility of spore germination between the
time of blanching and heating. Fresh peas were
used. The conditions of the experiment are as in
Experiment 5, except that the blanching was for
5 min.
Table IV
10 m
5 60 Sp. 48 hrs. Sp. 48 hrs. Sp. 4S hrs. Sp. 48 hrs.
5 60 Sp. 48 hrs. Sp. 48 hrs. Sp. 120 hrs 5p .48 hrs
5 180 Sp. 48 hrs. Sp. 72 hrs. Sp. 96 hrs. Good 7 days
Sp. = Spoilage.
Table IV shows that the incubation period has but
little influence upon the ease of sterilization. In the
column showing incubation for 80 min. and heating
for 180 min., the product did not spoil. This might
have been due to the fact that the spores had all changed
to the vegetative stage, but this is not likely, because
heating for 60 min. will easily kill all in the vegetative
stage and this, together with that heated 120 min.,
spoiled. This would seem to indicate that the incu-
bation period, due to slow cooling, will not
why, in some cases, the organisms cooled slowly are
more easily killed, or at least grow more slowly, than
those cooled more rapidly. In several instance
ever, we have observed spoilage to take place more
434
THE JOURNAL OF INDl si RIAL A V D ENGINEERING CHEMISTRY Vol. 10. No. 6
rapidly, and in some cases more spoilage follows
blanching than when no blanching is practiced.
EXPERIMENT 7 — This, together with some of the
following experiments, was conducted to determine
the necessity of complete sterilization to insure the
keeping of canned foods. We believe that it is usually
considered necessary to sterilize completely to avoid
spoilage unless some substance is added to alter the
physical or chemical nature of the product. We
have repeatedly received inquiries concerning this
point at the laboratory. Also, many conflicting re-
ports have reached us as to the time necessary to
process to insure keeping, certain people losing the
entire pack, while others, under very similar conditions
and methods of treatment, lose very little.
Tadi.k V
Heated Cooled Rapidly
Min Cotton Seal Rubber Seal
60 Sp. 48 hrs. Good 5 days(.u)
120 Sp. 96 hrs. Good 5 days
180 Sp. 72 hrs. Sp.
{a) We have found that a product which
will usually keep indefinitely. We have som
which are still good after 6 raos,
(M Rubber stopper became loosened and Leake
In some of our work we have been surprised to note
the ease with which certain foods, supposed to be very
difficult to sterilize, would keep indefinitely if properly
sealed. Also to find that most organisms isolated
from the product after prolonged heating were aerobic
in nature.
To determine this point we devised the method of
sealing one set of tubes with rubber and a duplicate
set with cotton plugs.1
In this experiment small beets were used. They
were first dipped in boiling water and the skins re-
moved. They were then blanched for 10 min. in
streaming steam. Upon removal from the steamer
they were divided into two lots. One lot was dipped
immediately into cold water and the second cooled
very slowly to the same temperature. These were
then packed in large, wide mouth bottles and processed
as indicated below. No exceptional precautions were
taken to prevent contamination. In this case 15 g.
of salt were added to each 1000 cc. of liquid used.
Table V shows the results of this experiment. Spoil-
age was determined by the appearance of the material
after standing at 350 C. for the time mentioned.
1 Slowly
Table VI
Cotton Seal Rubber Seal
Heated
Cooled Rapidly
Sp 4S hrs. Good 5 days
Min
■lavs Good 5 days
Sp 60 h» Good 5 days
60
Sp. 48 hrs. Good 5 days
rill keep lor 5 days at 35° C.
120
Sp 60 hrs. Good 5 days
180
Good 5 days Good 5 days
Heated 10 Pe
1 day ...... Sp 4S hrs
1 day Sp. is hrs
1 day Good 10 days
2 days Sp IS bra
2 days Sp is hr,
2 days Sp 48 hrs.
2 days Sp 60 hrs
< days Sp 48 hrs
3 days. Good 10 days
3 days Sp mi \u-
. Good 10 days
Table
Blanched 5 Minutes
t S.ilt .' 0 Per cent Salt 4
Sp 48 hrs.
Sp 4S hrs.
Sp 48 hrs.
Sp 48 hrs.
Sp 48 hrs.
Sp. 60 hrs
Good 10 days
Sp (8 hrs.
- hrs.
0 ,lays
Good 10 days
EXPERIMENT 8 — This is an experiment similar to
Experiment 7 except that vinegar was used in place
of salt, 15 cc. of vinegar being added to each 1000 cc.
of water used. (Five cc. of the vinegar required
i V 20 NaOH to neutralize to phenolphthalein.)
Table VI shows the results obtained. The results are
similar to those in Experiment 7.
EXPERIMENT 9 — The following experiment was de-
vised to see if blanching increased the ease of steriliza-
tion over a similar product packed without blanching.
In this experiment fresh green beans were used.
These were snapped into small pieces and divided
into two lots. One lot was placed directly into large,
clean test tubes which had been autoclaved shortly
before use A second lot was blanched in a steamer
Sp. 48 hrs. Good 5 days
Sp. 72 hrs. Good 5 days
Sp. 96 hrs. Go, I
for 5 min., dipped into cold water, and placed in similar
tubes. All were then covered with salt solution of
various strengths, plugged with cotton, and processed
as indicated in Table VII.
In filling the tube with blanched beans a sterile
funnel and forceps were used so that they did not
come into contact with the hands of the operator. They
were, however, cooled in running water from the
tap. Table VII shows results obtained.
These results show that blanching does not increase
ease of sterilization and that salt, except in amounts
too large to be permissible, has no influence upon
the keeping quality.
experiment 10 — In this experiment an attempt was
made to show the influence of blanching upon sweet
corn. The corn was of excellent quality and freshly
picked. Test tubes were used throughout the ex-
periment. The corn, after blanching for 5 min.
in steam, was cut from the cob with a sterile knife
and poured into large, sterile glass bottles, at the end
of the blanching period. The unblanched corn was
treated in a similar manner except that no preliminary
heating was applied. Tables VIII and IX show the
VII
0 Per cent Salt
Sp 48 hrs
Sp. 48 hrs
Good 1 0 days
Sp 48 hrs.
Sp 48 hrs.
Sp. 60 hrs.
Good 10 days
Sp »8 hrs
Good 10 days
Good 1 0 days
Good 10 days
1 0 Per cent !
Sp. 72 1
Sp. 72 1
Good 10 1
Sp 48 1
Sp. 48 hrs
Good 10 days
Sp 72 hrs.
Sp 72 hrs
Good 10 days
Sp 4S hrs.
Sp 48 hrs.
Sp 4s hrs
Good 10 days
Sp 4 days
Sp 4 days
Good 10 days
Good 10 days
Good
Good
Good
cent Salt
72 hrs
10 days
10 days
48 hrs
48 hrs
10 days
10 days
48 hrs.
10 days
10 days
10 days
This experiment shows that no improvement in
quality is to be expected from blanching
and cold dipping. Exclusion of air, however, does
have a very marked influence upon keeping quality.
This point will be discussed more in detail later.
ir,- two reasons, ror using cotton plugs in this work The first
is ih it spoilage takes place very rapidly, if it takes place at all; the second
is that cottoo acl ■ 1 bacterisJ filter ami .it the same tunc alios
influence of heating upon the keeping quality of corn
treated by various methods. The plus sign indi-
cates spoilage. The minus sign indicates that the
product was good after 10 days in the warm room.
These resul' it there is no influence due to
blanching, very little due to small amounts of salt,
very little due to small amounts of acid, and a great
lue to larger amounts of :o sealing.
June, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
435
Table VIII — Corn Blanched 5 Minutes
Sealed with Sealed with
Cotton Stopper Rubber'Stopper
Table IX — Corn Not Blanched
Sealed with Sealed with
Cotton Stopper Rubber Stopper
Heated & _J
min. 1 day + + -
* 5
+ +
i. 1 day. . .
1. 1 day
1. 2 days + +
1. 2 days + +
1. 2 days — —
1. 2 days — —
1. 3 days + — —
1, 3 days — — — — — —
:. twice 1 day -f — + -f — —
;. twice I day + -f -j- — — —
1. twice I day + — — + — —
1, twice 1 day — + — — — —
. twice 2 days — — — — — —
. twice 2 days — — — — — —
. twice 2 days — — — — — —
. twice 2 days — — — — — —
. twice 3 days — — — — -f- —
. twice 3 days — — — — — —
. twice 3 days — — — — — —
. twice 3 days — — — — — —
+ — — + —
It is interesting to note the influence of heating
twice a day upon the keeping quality. We devised
this method for the sterilization of culture media.
Occasionally we resort to this method in the summer
time when the temperature of the laboratory remains
nearly that of the incubator for the entire 24 hrs.
Several Jtypes of spore-forming aerobes not only change
from the spore to the vegetative stage, but change again
into the spore stage in 24 hrs. These types grow but
very little at low temperature and do not show in the
media for several days if the room is cold. Thus
the incubation of the product with two applications
of heat each 24 hrs. usually aids greatly in the steriliza-
tion. These types also grow but little in the absence
of free oxygen and are the types which we have ob-
tained most commonly from spoiled vegetables in cotton-
sealed tubes. This method may be of considerable
value in canning of vegetables but we have not done
enough work to advocate its use.
experiment ii — This experiment shows something
of the influence of heating upon the reduction in
numbers of bacteria in sweet corn. To determine
these numbers the tubes were shaken for several min-
utes before the sample was taken. The kernels were
usually reduced to a pulp by the shaking process so
the results may be considered fairly representative
Table X
Per cent
Per Cc.
Destroyed
4000
30
99.25
15
99.62
10
99.75
7
99.82
6
99 . 85
4
99.90
1
99.97
I
99.97
120
150
170
180
of the numbers present. Every test will give slightly
different numbers. We have in some cases found more
and in some less, but this is a fair illustration for a
good quality of corn. In this case the material was
in a jar sealed only with cotton. The temperature
surrounding the jar was 080 C. (boiling point of water
at this altitude).
Heated
60 min. 1 day .
1 day.
120
180
d d &
— — +
1 day
15 min. 2 days.
30 min. 2 days.
60 rain. 2 days.
90 min. 2 days.
15 min. 3 days.
30 rain. 3 days.
60 min. 3 days.
90 min. 3 days.
15 min. twice 1 day —
30 min. twice 1 day —
60 min. twice 1 day. —
90 min. twice 1 day —
15 min. twice 2 days —
30 rain, twice 2 days —
60 min. twice 2 days —
90 min. twice 2 days —
1 5 min. twice 3 days —
30 min. twice 3 days —
60 min. twice 3 days —
90 min twice 3 days —
— — 0 —
Table X shows that over 99 per cent of the organisms
are killed in 5 min. at this temperature, but that
0.03 per cent survived even after 3 hrs. This is
probably enough to cause spoilage in a container
sealed with cotton, but not in one sealed with rubber.
experiment 12 — This experiment shows the in-
fluence of heating upon the thermal death-point of
organisms found on sweet corn treated in various ways.
Table XI tends to show that the total number
of bacteria which may be cultivated from a product
after a short heating is very small. The few remaining,
however, may bring about spoilage if they develop.
This apparently is not always the case, as too few
are present to establish the initial growth which seems
to be necessary. In comparing the relationship of
Table XI
Number of Bacteria per Cc.
1.0 2.0 3.0 0.05 0.1 0.3
Per Per Per Per Per Per
cent cent cent cent cent cent
Heated Water Salt Salt Salt Acid Acid Acid
20.000 20,000 20,000 20,000 20,000 20,000 20,000
Before heating
60 min
34
38
27
24
32
24
18
120 min
180 min 4 2 1 0 3 1 0
15 min. twice 1 day 50 44 32 28 32 28 21
30 min. twice 1 day 20 19 10 12 14 10 8
60 min. twice 1 day 8 6 2 6 2 10
bacterial counts to the keeping quality of the product
it is often found that certain containers may show a
few organisms upon culture media and yet show no
signs of spoilage, especially if acid is present or the
tube has been properly sealed to exclude air. It is
very difficult to make comparisons between two lots
of this kind of material as the organisms are so unevenly
distributed throughout the mass; for this reason aver-
ages of several trials should be used in compiling
tables.
Many tests in this laboratory have led to the belief
that keeping is not due, in a great many cases, to
absolute sterilization. We have had jars of vegetables
that are easily spoiled by bacteria, which have kept
under conditions of incomplete sterilization. Others
that hud been heated for a long time and plugged
carefully with cotton have spoiled in a few days.
lave kept some of the sealed jars for io mo.
436
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 6
with no signs of deterioration, either in flavor, odor,
or appearance, and have been able to cultivate both
aerobes and anaerobes from them after that time.
r-processing in favor of sealing as a preserving
agent should not be advocated, but we feel sure that
many products have been placed on the market which
were under-processed and have not spoiled. We
hope to determine this point later.
Table XII shows a comparison between numbers
of bacteria destroyed by sterilization and the keeping
quality. This table is a compilation from Tables
IX and XL The two tables were not made on the
same date or from the same lots of corn. We have,
however, made several tests of this sort with similar
results. Unfortunately no counts were obtained from
sealed tubes, but they probably would differ but
very little from those sealed with cotton.
Table XII
Number of Bacteria per Cc.
1.0
2.0
0.05
0.1
0.3
Per
Per
Per
Per
Per
cent
cent
cent
cent
cent
Salt
Salt
Acid
Acid
Acid
90 rnin. twi
1 day
1 day
1 day
. twice 1 day.
twice 1 day.
twice 1 day.
twice 1 day..
1 day +
1 day +
... —
1 day... —
1 day... —
ce 1 day.. . —
1 day... —
Sealed with Cotton
Sealed with Rubber
n. 1 day + __ — — —
:1. 1 day —
n. 1 (lay — — — — — —
q. twice 1 day... — — — — — —
n. twice 1 day... — — — — — —
n. twice 1 day... — — — — — —
90 min. twice 1 day... — — — — — —
These results show that in several cases spoilage
did not occur even when there were, no doubt, a few
organisms present. This is shown particularly in the
case in which acid is used. The influence of sealing
is also very marked. Even in cases in which con-
siderable spoilage occurred in cotton-sealed tubes no
spoilage appeared in tubes properly sealed with rubber.
experiment 13 — This experiment was devised to
show influence of rubber alone upon the keeping quality.
Tabus XIII
0
!'. 1 l'i :
cent cent
Water Salt Salt
ubber stoppers, the hole being plunged
2.0 0.05 0.1 0.2
Per Per Per Per
cent cent cent cent
Salt Acid Acid Acid
th cotton
II, ii. .1
with onc-holi
is mil, 1 daj +
A0 11,111 I day + + + — — — —
60 min. 1 day — — — — — — —
il with one-hole rubber stopper and glass rod
15 min. 1 day -f- — + — — — —
30 min. 1 day — — — — — — —
60 min. 1 day — — — — — — —
Plugged with cotton only
15 min. 1 day + + + + + — —
30 min. I . I ■ . ... + + — — — — —
60 min. 1 day + — — — — — —
d such marked results 1 1
itiK tubes wiiH rubber as compared to sealing with
cotton it was coi that the rubber
! might contain some substance toxic to the
used in parked iii large mouth
bottles anil treated as indicated in Table XIII. The
plus sign means spoilage. The minus sign means good
after 10 days.
We may conclude from Experiment 13 that it was
not the influence of the rubber alone that could account
for the preserving action in rubber-sealed containers.
Table XIII serves again to emphasize the great value
of sealing and the use of acid in the canning industry.
CONCLUSIONS
1 — Blanching is of no value in reducing the time
necessary to properly process canned foods.
2 — Small amounts of salt are of little value in pre-
venting the growth of bacteria in canned foods.
3 — Small amounts of organic acid (acetic acid) have
a distinctly retarding action upon the growth of bac-
teria in canned vegetables. The use of small amounts
should be advocated in all cases in which it will not
injure the texture, flavor, or appearance of the product.
4 — In many cases an unsterile product will keep
indefinitely if properly sealed. This, however, is
not true in all cases and sealing should not be expected
to take the place of proper processing because of the
danger of loss due to spore-forming anaerobes.
Department op Bacteriology
Kansas State Agricultural College
Manhattan. Kansas
DETECTION OF ADDED COLOR IN BUTTER OR OLEO-
MARGARINE
By Herbert A. Lubs
Received December 12. 1917
I OBSERVATIONS ON SOME QUALITATIVE TESTS FOR
THE DETECTION" OF ADDED ( KS IN FATS
A study of the various methods described for the
detection of added colors in butter and butter substi-
tutes reveals a number of misleading statements which
might lead a more or less inexperienced analyst to
false conclusions. For example, certain tests described
in the literature lead to the false conclusion that some
aniline colors are vegetable colors, and vice versa.
Furthermore, certain azo colors cannot be detected
by methods which are supposed to reveal their presence.
Some of the tests described in the literature for the
on of added color are perfectly satisfactory
when certain compounds are present, but fail to reveal
the presence of added color when other dyes are used,
and for this reason some changes must be made in the
procedure. These modifications will be discussed
under the tests in question. The analyst should make
a combination of tests with the modifications subse-
quently recommended to obtain reliable results.
low's test — According to Low,1 if a fat contain-
ing an azo color is shaken with a mixture of four parts
of glacial acetic acid and one part of concentrated
sulfuric acid the acid layer will settle out with a wine-
red color. It is quite true that in some cases a wine-
red color is obtained, but in other cases a yellow,
brown, or even a blue color is imparted to the acid
i the presence of various azo colors. For
i J. Am Cktn M • . S89.
June, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
437
instance, Yellow O B, Yellow A B,1 Sudan I, Sudan II,
Butter Yellow, Aniline Yellow, and some other dyes
will give reddish colorations to the acid layer, while
with Sudan G and Aniline-azo-phenol a yellowish
brown color is obtained. Sudan III imparts a bluish
tinge to the acid layer. Although turmeric is not often
used for the coloration of butter, its presence has been
occasionally detected, and in this test will impart a
brilliant violet-red coloration to the acid layer. How-
ever, if turmeric is present it will be detected upon ex-
tracting the fat with aqueous alkali and' identifying
by the usual methods.2
When the test is made as originally described by Low,
the separation of the two layers is very slow and in-
distinct and, particularly in the case of oleomargarine,
the color due to the reaction of the fat practically
obscures the color due to the presence of an azo dye.
A decided improvement on the method of Low consists
in first diluting the fat, about 20 g., with an equal volume
of petroleum ether, and shaking in a separatory funnel
with 10 cc. of the acid mixture, consisting of one volume
of concentrated sulfuric acid and 10 volumes of glacial
acetic acid (99.5 per cent). In this way a more rapid
and clean-cut separation of the two layers is effected
and there is less decomposition of the constituents of
the fat. Pure butter fat will impart no color to the
acid layer, except upon very long standing. Some
specimens of oleomargarine after standing for a short
time will impart a brownish coloration to the acid
layer, the intensity of which increases upon standing.
If an azo color be present the coloration of the acid
layer is very distinct and appears immediately.
doolittle's test3 — A small portion of the fat is
dissolved in ether, the solution divided into two equal
parts and one portion is shaken with dilute alkali
and the other with dilute hydrochloric acid. If the
aqueous alkaline layer is colored yellow, it is stated
that a vegetable color is present; and if the acid layer
is colored pink, the presence of a coal-tar color is
assumed.
Since this test was developed the list of coal-tar,
oil-soluble colors has been considerably augmented
and some of these colors will give reactions by the above
method which might lead to false conclusions. For
instance, Aniline-azo-phenol and Sudan G will impart
a yellow color to the alkaline layer and furthermore,
many oil-soluble azo colors do not give a pink colora-
tion with dilute hydrochloric acid. In order to de-
termine the limitations of this method solutions of ten
different oil-soluble azo colors in butter were prepared.
Two imparted a pink color to the acid layer when dilute
acid was used; with the remainder the acid layer was
colorless. When concentrated hydrochloric acid was
used, eight imparted color to the acid layer. Six of the
eight gave a red coloration, and two, a yellow colora-
tion. In making Doolittle's test it is advisable to
use 10 to 20 g. of fat and in the acid extraction to
substitute concentrated for dilute hydrochloric acid.
1 These arc the trade names for o-toIuene-azo-j3-n:iphthylamine and
benzene azo-0-n:iphthylamine For butter coloring a mixture of the two
is usual 1',
> Allen'* "Cos oil AnaJyns," 6 (1911), 415.
• U. S. Dept of Agr.. Bureau of Chemistry. Bull. 65 (1902). 152
geissler's test1 — Geissler states that if a few drops
of clarified fat are mixed with a small amount of fuller's
earth, a pink to red coloration will be produced in the
presence of various azo dyes. Several azo colors will
give this test quite satisfactorily, but the majority will
not and hence this test cannot be relied upon as a
general method for the detection of azo colors.
PROCEDURE RECOMMENDED FOR PRELIMINARY EXAMINA-
TION OF FAT FOR THE DETECTION OF
ADDED COLOR
Dissolve about 20 g. of the fat in 50 cc. of petroleum
ether, and 20 g. in 50 cc. of ethyl ether. Shake out
the ethyl ether solution in a small separatory funnel
with dilute sodium hydroxide solution. If the aqueous
solution is colored yellow a vegetable color is indicated
and the alkaline extract must be tested for such colors.
Add 10 cc. of a mixture of one volume of sulfuric acid
and 10 volumes of glacial acetic acid to the petroleum
ether solution and shake vigorously. The acid layer
will settle out in a few minutes with a decided colora-
tion if an azo dye is present. In this test annatto,
if present in sufficient concentration, will impart a
momentary green color which changes over to brown.
Turmeric imparts a fairly permanent violet-red colora-
tion similar to that given by certain azo dyes, but its
presence will be detected in the alkaline extract. The
azo colors impart a yellow, brown, red or blue color to
the acid layer.
AN IMPROVED METHOD FOR THE DETECTION OF ANNATTO
Perhaps the most extensively used vegetable color
for butter at the present time is annatto. Its pres-
ence can be readily determined by a slight modifica-
tion of described tests. If the aqueous alkaline ex-
tract from about 20 g. of fat dissolved in 50 cc. of ether
is passed through a filter paper several times, the
excess of alkali washed off, the red coloration produced
by a solution of stannous chloride is very readily ob-
tained. It is advisable to add a small amount of hydro-
chloric acid to the stannous chloride solution.
In applying the Massachusetts State Board of Health .
method2 to fats which contain very small amounts of
annatto, about 30 g. of fat should be warmed with 60
cc. of 2 per cent sodium hydroxide and filtered through
a funnel surrounded by warm water. The aqueous
filtrate is returned through the filter paper repeatedly
for 3 or 4 hours. After washing the fat and alkali
from the paper the test for annatto is made in the usual
way. The paper need not be dried.
II THE SEPARATION OF THE AZO COLORS FROM FATS
AND THE IDENTIFICATION OF YELLOW O B
AND YELLOW A B
In a bulletin3 recently issued from this Bureau,
■.son has sumrrj 1 various m
previously used for the separation of azo dyi
and described several new methods
which he developed. For the Sudan dy< pari icularly,
he suggests extraction with a mixi
and sulfuric acids and states that I d is not
I J. Am. Chem. Soc. 20 (1898). 110.
: Bureau of Chemistry. Bull 107 1912), rev . 126
• lh„l . 448 i
43»
THE JOURNAL Of INDl SI RIAL AND ENGINEERING < BEMISTRY Vol. 10, .No. 6
able to such colors as o-toluene-azo-/3-naphthyl-
amine, since they are destroyed by treatment with
strong acids. This statement is not quite correct,
as will be shown below.
A solution of Yellow O B, one part in 12,500, was
made as follows: 2 cc. of 0.4 per cent alcohol solution
of 0 B were diluted to 100 cc. with a mixture of 90
cc. glacial acetic acid, 10 cc. concentrated sulfuric acid
and 10 cc. of water. The spectrophotometric curve
of this solution was read immediately in a Hiifner
type spectrophotometer.1 Since the extinction co-
efficients are proportional to the weight of light-ab-
sorbing material per unit of volume, by determining
these extinction coefficients after certain definite times
had elapsed, it was possible to calculate the percentage
decomposition of the dye. The loss expressed as per
cent is plotted against time and it will be seen from the
curve that even after 5 hrs. have elapsed, a time surely
sufficient for any analyst to have completed this step
of the procedure, there is still 85 per cent of the original
dye undecomposed, while after half an hour, the time
usually required, the loss is only 2 per cent. The
points on the curve are each the average of seven ob-
servations at different wave lengths on the absorption
spectrum of the dye solutions.
. so
§ so
^--^
Fig. I — Curvb Showing the Percentage Decomposition of Ybllow
(1 Bin Acid Solution with Time
A concentration of one part in 50.000 of Sudan I,
under the same conditions, showed absolutely no de-
composition during the same time interval, namely
75 hrs. The specific action on Yellow 0 B is possibly
a direct result of the presence of the free amino group
in the dye molecule.
In the same bulletin2 it is stated that o-toluene-
azo-0-naphthylamine (Yellow 0 B) and its benzene
analog can be slowly extracted from the gasoline solu-
tion of the fat by 4- to 6-normal hydrochloric acid.
This is true if the dye is present in relatively large
amount, but it the quantity of dye in the fat is about
one part or less in 50.000, practically no extraction of
Yellow O B can be effected. Very rarely would an
amount of dye greater than this be used.
The phenol method of extraction3 is, as
"somewhat inconvenient" and particularly so if one
attempts to work with a pound or so of the fat.
Though the method suggested in this paper is of
general application in the separation of azo dyes from
fats in a fairly pure state, yet very often it is more con-
' The spectrophotometric determinations were made by A. B. Clark
1.1 this laboratory, to whom the writer wishes to acknowledge his indebted-
ness.
: Bureau ol Chemistry, Bull. 448 (I'M 7), 7.
Ibid . 107 (1917).
venient to use a different method. For example, if
a dye is easily removed by dilute acid or alkali from the
fat such a procedure would be more convenient. The
proper procedure to be used should be decided by the
judgment of the analyst from a few preliminary tests
on small amounts of the fat. It might be suggested
at this point that if it is found preferable to extract
with dilute acid or alkali, dilution of the fat with ethyl
ether is more preferable than dilution with gasoline
having a low boiling point, since a more satisfactory
extraction can be secured when the former solvent is
used.
Table I — Colors op the Acid and Alkaline Extracts prom Buttbr
Solutions op Various Oil-Soluble Dyes
Butter solutions containing 1 part of dye in 50,000 of fat were pre-
pared. Before extiaction with hydrochloric acid or alkali these solutions
were diluted with an equal volume of ethyl ether; before extraction with the
sulfurie-aeetic acid mixture the solution? were diluted with petroleum
ether. The colors of the acid or alkaline extract are listed in the following
table. In the case of butter the shades are permanent for a fairly long
period, but with oleomargarine the change of shade is comparatively more
rapid.
lVol. 1 Vol.
Cone HCI H.SO.
4 Vols 1 Per cent 10 Vols.
live HiO Cone. HCI NaOH Acetic Acid
Aniline-azo-phenol.. . No color Yellow Yellow Yellow-brown
Sudan G No color Yellow-brown Yellow-brown Yellow-brown
Aniline Yellow Red color Brownish red
o - Toluene - azo - 0
napht h y 1 a m i n e
(Yellow- OB) No color Red Red
Benzene-azo-0-naph-
thylamine (Yellow
A B) No color Red Red
Sudan I No color Very faint red Cherry -red
Sudan II No color Very faint red Violet-red
Sudan III No color No color No color Blue
Butter Yellow Red Red
Amino-azo-a-naph-
thalene No color Violet Violet
It is not the purpose of this paper to present a system-
atic scheme for the separation and identification of
all of the possible oil-soluble colors, but to present a
method for the separation from fats of some oil-soluble
azo colors not easily removed by dilute acids or alkalies,
and principally to enable the analyst to determine
whether the dye present is Yellow A B or Yellow O B,
either singly or in combination, or some other azo dye.
Table II — A List of Some Oil-Soluble Colors (a)
Common Name Components Schulu No. (i>)
Yellow A B Aniline + 0-naphthylamine
Yellow OB r.-Toluidine + fl-naphthylamine
Aniline Yellow Aniline -f aniline
Butter Yellow Aniline -f- dimethylaniline
Spirit Yellow R o-Toluidine + o-toluidine 68
Benzene-azo-phenol Aniline -f- phenol
Sudan I Aniline ■+■ 0-naphthol 36
Sudan II Xvlidine + 0-naphthol 76
Sudan III Amido-azo-beozene + 0-naphthol 23
Sudan G Aniline + resorcin 35
Benzene-azo- o-naphthvlamine Aniline + o-naphthvlamine
Amino-azo-a-naphthalene . . a-Naphthylamine + o-naphthyl-
0-Naphthalene-azo- a-naphthol 0-Naphthylamine + a-naphthol
Benzene-azo- a-naphthol Aniline -f- a-naphthol
Sudan Brown a Naphthvlamine + a-naphthol 105
Carminaph Garnet a-Naphthylamine + S-naphthol 106
(a) Probably the most used are Butter Yellow. Aniline Yellow. Yellow
A B and O B and the Sudans.
(6) Farbtnstofftabcllcn, Schulu. 1914.
The writer has effected quite satisfactory separations
and identifications of Yellow A B and Yellow O B
from butter and oleomargarine containing the dye in
the proportion of one part in 100.000 by means of the
pi i icedure described.
P»d< 1 HIRE FOR THE SEPARATION FROM FATS AND THE
ID! NTIFICATI0N OF YELLOW A B AND YELLOW O B
If the preliminary tests have shown the presence of
azo colors the analyst must iirst examine the fat for the
presence or absence of certain azo colors. For this
purpose about 40 g. of the melted fat are dissolved in
June, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
about 100 cc. of ethyl ether and the solution divided
into two portions. One portion is extracted with 12
per cent hydrochloric acid and the other with
5 per cent sodium hydroxide. If the acid extract
is colored, the presence of any of the following dyes
is indicated: Aniline Yellow, Amino-azo-a-naphtha-
lene, Benzene - azo - a - naphthylamine, and Butter
Yellow.
The coloration of the alkaline extract would indi-
cate "Sudan G, Aniline-azo-phenol or /3-Naphthalene-
azo-a-naphthol.1 If the absence of dyes which can
be extracted by dilute acid or alkali has been shown,
proceed in the following manner:
Melt one or two pounds of fat2 (it is usually de-
sirable to use an amount of fat containing about 10
i mg. of dye) on a water bath; allow the water and solids
to settle; pour off the liquid fat and dilute with an equal
volume of petroleum ether. Filter through a Btichner
funnel or large folded niters. Place the nitrate in a
separatory funnel and extract with a mixture composed
of 10 cc. of concentrated sulfuric acid, 90 cc. of glacial
acetic acid (99.5 per cent) and 10 cc. of water. Use
about 100 cc. of the acid mixture for 200 cc. of petroleum
! ether solution of the fat. If Yellow A B or Yellow O B
: are present the acid layer will separate with a wine-red
coloration.3 Separate the acid layer, and for each 100
cc. of acid mixture originally used add 10 cc. of water
and 10 cc. of concentrated hydrochloric acid; add about
100 cc. of ether and shake; if the ether layer does not
separate out add more ether and shake again; separate
the aqueous layer and repeat extraction with one-half
the amount of ether originally used. Beside the fatty
material, Sudan I, II and III and Carminaph Garnet
are removed by the ether. Yellow O B and Yellow
A B remain in the acid solution. The acid layer is
then diluted with water, about two volumes, and care-
fully neutralized with strong alkali, cooling during the
process. The solution is then extracted with ethyl
ether, the ether solution washed first with water and
then with an excess of dilute alkali, drawn off, and
evaporated to dryness. Care must be taken that all
of the acid is removed from the ether solution before
evaporation to dryness. The residue consists of Yellow
O B or Yellow A B, or a mixture of both. Further
confirmation of the identity of these two dyes can be
obtained in several ways.
CONFIRMATORY TESTS FOR THE IDENTIFICATION OF
YELLOW O B AND YELLOW A B
The residue obtained from the sulfuric-acetic acid
extraction is then dissolved in several cc. of alcohol,
transferred to a test tube and reduced with hydro-
chloric acid and zinc dust. It is to be emphasized
that the volume of alcohol and hydrochloric acid used
should be as small as possible. This reduction mixture
1 For a systematic scheme for separating and identifying many of the
Oil-soluble colors see Mathewson, Bureau of Chemistry, Bull. 137 (1910),
54, or Aliens "Commercial Organic Analysis," 5 (1911), 666; see also
Bureau of Chemistry, Bull. 448 (1917).
* One experienced in the method can satisfactorily separate and identify
2 mz. of dye in 200 g. of fat. As a rule it is more satisfactory to use larger
amounts of fat. Of course, the amount of dye used is variable Only
occasionally will 2 lbs. of butter contain more than 10 mg. of dye.
* By noting the color of the acid layer, often a very good idea of the
nature of the dve present can be obtained. See Table I.
is then diluted with a few cc. of water, made alkaline
with sodium hydroxide solution, cooled and quickly
extracted with ether. The ether solution after filtra-
tion through a small, dry filter paper into a small
separatory funnel is then treated with a few drops of
a 0.5 per cent ferric chloride solution and shaken
vigorously. If Yellow A B or Yellow O B is present
a brilliant green coloration of the ether will be evident.
Upon adding several cc. of water and again shaking,
the green layer settles out beneath the ether. This
color reaction depends upon the effect of ferric chloride
upon 1-2-diaminonaphthalene, but is not specific
for this compound, since it will be given by a number
of diaminobenzenes and diaminonaphthalenes. Though
the ethereal solution of the reduction products of
Sudan III will give a reaction with ferric chloride
identical with that obtained from Yellow A B or
Yellow O B, as previously pointed out, the presence
of Sudan III is indicated by the very characteristic
blue color of the acetic-sulfuric acid extract, and fur-
thermore this dye would have been previously elim-
inated. 'It is because of the lack of specificity of the
ferric chloride reaction that a preliminary exclusion
of a large number of dyes must be effected as described.
In order to obtain a further check on the identity
of the isolated dye a portion should be used in making
a dyeing test. The colors of many oil-soluble dyes on
silk and the reactions of the dyed fiber are tabulated
by Mathewson.1 Yellow 0 B and Yellow A B dye
silk a yellowish brown. The dried dyed fiber gives
a violet coloration with concentrated sulfuric acid and
a red coloration with concentrated hydrochloric acid.
Color Investigation Laboratory
Bureau op Chemistry
Washington. D. C
AN ACCURATE LOSS-ON-IGNITION METHOD FOR THE
DETERMINATION OF ORGANIC MATTER IN SOILS2
By J. B. Rather
Received December 10, 1917
The loss-on-ignition method for the determination
of organic matter in soils gives highly erroneous results
which are due, as is well known, to hydrated mineral
constituents of the soil, carbonates and unoxidized
minerals. The organic carbon method for the deter-
mination of organic matter requires the determination
of total and inorganic carbon and an arbitrary
factor for the calculation of the carbon to organic
matter. Since the carbon content of that portion of
the organic matter which has been separated from the
soil may vary from 44 to 64 per cent3 many workers
content themselves with reporting organic carbon.
It is evident that if the hydrated, unoxidized, and
carbonaceous minerals were removed from the field
of action the loss-on-ignition method would be superior
I BurcMU of Chemistry, Bull. 448 (1917), 45.
• Abstracted by the author from Bull 140, Arkansas Experiment
Station, to irhicfa publication tin- reader is referred for additional details
and further data The material under the heading "Application of the
Method to Abnormal Soils" does not appear in the publication referred to.
This article was read in pari before the Association of Official Agricultural
Chemists, Washington. I). C , November, 1917.
i See Frepsjand Haunter. Texas Experiment Station, Pull. 119.
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 6
Percent
10
Sample
No.
a
\s
i
L2429
S J
ts
L
t )
k /,
4
2430
a
N
: —
2372
o y
"-■ — - — i
i
2400
?365
i 9
i J
i :i !f *
0 2. 4
DIGE5TI0N5
8 10
12
F:c. 1 — Effect ok Acid Reagent on Loss of Ignition
to the organic carbon method. The attempt is made
to do this in the method to be described.
AN ACCURATE LOSS-0N-IGNITI0N METHOD FOR THE DE-
TERMINATION OF THE ORGANIC MATTER IN SOILS
The proposed method depends on the fact that the
minerals in the soil which interfere with the accuracy
of the loss-on-ignition method can be removed by
digesting in the warm with a weak mixture of hydro-
fluoric and hydrochloric acids without decomposing
or dissolving more than a very small amount of organic
matter.
After a large number of preliminary experiments to
determine the optimum conditions of concentration,
temperature, length of digestion, ratio of soil to reagent,
fineness of division of sample, etc., the following method
was adopted:
reagents — Acid-washed and ignited asbestos; 2.5
per cent hydrochloric acid; 2.5 per cent hydrofluoric
acid in ceresine- or paraffin-lined bottle.
procedure — Weigh out 1 g. sample, prepared as in
the' Official Method of the A. O. A. C, into a platinum
dish and add 50 cc. water. Digest for 5 min. on a
boiling water bath or at 85° C. Allow to settle 2 or
3 min. if necessary and decant through a Gooch made
with a thin felt of asbestos, using suction. To the resi-
due in the dish add a second 50 cc. of water and digest
and decant as before. Transfer1 extract to beakers and
boil down to a small volume. Measure into a glass
cylinder 10 cc. of 2.5 per cent HC1, 10 cc. of 2.5 per cent
HF, and 30 cc. of water. Mix and add to soil the residue
in dish. Digest and decant as with the water extract.
Repeat, and then transfer contents of crucible, including
the asbestos, to the platinum dish, using 30 cc. water.
Add 10 cc. each of the acids and digest and decant as
before, making a new felt in the Gooch. Then digest
and decant three times more with the acid mixture
mentioned above, making a total of 6 digestions with
the acid reagent. Transfer residue in dish to crucible
with water and wash with water. Now transfer con-
tents of crucible to a smaller dish, add the concentrated
t with lolls coataiaini ovei make two digestions with
20 cc. 2.5 per cent HCI sad ;it oc. w.ii. r. ' under con-
ditions described for water extraction.
Percent
5
Sample
No.
2429
)'
4
3
2.
L2430
>
1
12372
0 I
»
2400
i23G5
1
0 I 2. 3 4 5 0,
Dl6t5TI0N5
Flo. 2— Effect op Treatment on Organic Carbon in Soils
water extract obtained above, evaporate to dryness
on the water bath, dry to constant weight, ignite and
weigh. The loss in weight represents organic matter.
The acid reagent does not have any appreciable effect
on the glass and porcelain vessels necessary in the above
operation, nor is the use of a hood necessary. It is
possible that fused silica dishes can be used in the
digestion. In order to avoid slow filtration it is nec-
essary that the decantation be made carefully after
settling for 2 or 3 min., if necessary. In the table
which follows, the above procedure is designated
Method A.
The proof of the accuracy of the method rests on the
fact that after a certain number of digestions with the
acid reagent the loss on ignition does not decrease-
further (Fig. 1), while at the same time the loss of*
organic carbon is not appreciable (Fig. 2). The fact
that the loss on ignition reaches a minimum is evidence
that there is no progressive decomposition of the organic-
matter, and the fact that the organic carbon decreases
only slightly when considered in connection with the
above facts is evidence that the loss on ignition ob-
Percent
100
Somple
No.
SO^
t2365
L,
GO
' J
L_ ,
£442
1
40
■ _J
>
2434
20
»
[2372
0
(2400
0 2 4 6
DIGESTIONS
10 12.
l'i. 3 RasiDtn aftkk Ignition wrra Different Trevtmknts with
Reagent
June, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY 441
tained is due to organic matter. The fact that the tically the same. With the soils under discussion
mineral residue continues to decrease (Fig. 3) after the Method B gives on the whole equally as satisfactory
loss on ignition reaches a minimum is evidence that the results and is much shorter than Method A.
mineral matter remaining in the soil is not hydrated. There are some soils, however, to which these methods
The number of digestions actually necessary varies are not applicable without modification; such soils,
from 2 with sands to 6 with heavy clays. which contain abnormally large amounts of acid-soluble
Since the amount of water-soluble organic matter organic matter, will be discussed below,
was small the following method was also used: The loss-on-ignition method gives results which bear
procedure — Treat 1 g. of the soil as described in no relation whatever to the organic carbon content of
Method A above, but omit the water extraction. Dry, the soil. In comparing this method with the proposed
weigh, ignite and weigh in the Gooch crucible (Method method it can be seen that the former method gives
B). Coors crucibles have been found satisfactory for much higher results in every case. The difference is
this purpose. 1000 per cent in the case of No. 2400, even after correc-
Method B adds about one hour to the time required tion for carbonates in the loss-on-ignition determina-
for the ordinary loss-on-ignition determination when tion. The average difference between the loss-on-
the soils are run in sets of six. Method A adds about ignition method and the proposed method is 2.95 in
3 hrs. per cent of soil and 1 53 in per cent of organic matter.
Detailed studies of the action of the acid reagent on
•i • i ,v 1 c 4.U -i APPLICATION OF THE METHOD TO ABNORMAL SOILS
some sou minerals, on the mineral matter of the soil,
and its effect on the loss on ignition and the organic With soils containing a large amount of acid-soluble
carbon of the soil were made, on which studies the organic matter the above method will give low results,
proof of the accuracy of the method rests, will be pub- and it becomes necessary to modify it so as to recover
lished in Bulletin 140, Arkansas Experiment Station. the acid-soluble material without including hydrated
or easily decomposed inorganic compounds.
RESULTS OBTAINED WITH THE METHOD ON SOILS OF ^, A- c ,■ , ■ . , • rp U1 T •. , ,■/. ,
1 he modification, designated in 1 able I as Modified
DIFFERENT TYPES A , ,, , . • , „
Method A, is as follows:
In Table I are given the results of determinations by Proceed as in Method A, using 2 per cent ammonium
the method proposed, together with those by other carbonate solution instead of water in the preliminary
methods. These results are selected from a larger extraction. Moderate the heat if effervescence be-
number given in the publication referred to. The dis- comes vigorous before the end of the five-minute
cussion relates to the whole of the data. digestion. Two digestions with this reagent will be
Table I — Percentage op Organic Matter in Soils by Different Methods
Organic Matter Calc. From Diff. bet.
Organic Carbon Modified Results by
Organic Basis Basis Basis (C) Loss on Method Method Mettiod Method A
Number Soil Type Carbon 44% 64% 58% Ignition BAA and (C)
2365 Norfolk sand 0.16 0.36 0.25 0.28 0.78 0.34 0.34 .. 0.04
2446 Orangeburg fine sandy loam 0.37 0.84 0.56 0.64 2.57 0.66 0.62 .. 0.02
2447 Orangeburg fine sandy loam, ss 0.20 0.45 0.31 0.34 1.13 0.37 0.35 .. 0.01
2449 BerryVille stony loam 0.94 2.14 1.47 1.62 2.62 1.41 1.54 .. 0.08
2450 Berryville stony loam, ss 0.44 1.00 0.69 0.76 2.22 0.73 0.84 .. 0.08
2373 Brewer silt loam 1.24 2.82 1.94 2.16 3.77 2.21 2.13 0.03
2400 Brackett silt loam. ss(o) 0.23 0.52 0.36 0.40 6.17 .. 0.60 .. 0.20
2429 Huntington silt loam 4.91 11.16 7.67 8.47 12.77 8.12 8.10 .. 0.37
2435 Huntington silt loam, ss 2.64 6.00 4.12 4.55 8.59 4.54 4.53 .. 0.02
2372 Brewer clay 1.80 4.09 2.81 3.10 7.61 3.13 3.14 .. 0.04
2430 Sharkey clay 2.62 5.95 4.09 4.52 9.25 4.46 4.52 .. 0.00
2434 Houston black clay 1.30 2.95 2.03 2.24 5.78 2.19 2.37 .. 0.13
2409 Alfalfa hay .. 81.73 77.20
2431 Calcareous peat, Minnesota 30.07 .. .. .. 53.70 .. .. 51.60
2461 Acid peat, Minnesota .. .. .. 85.40 .. .. 83.37
2507 Caribou loam, Maine(d) 3.88 8.82 6.06 6.69 9.35 .. .. 6.45 0.24
2510 Apple stems (sawdust) .. 92.23 .. 88.77
(a) About 86 per cent calcium carbonate.
(6) About 25 per cent organic matter soluble in warm, dilute acid.
In every case the amount of organic matter found by sufficient with mineral soils. Proceed from this point
the proposed method falls within the limits shown pos- as directed in Method A, but evaporate the ammonium
sible by the organic carbon method. Method A gives carbonate extract completely to dryness before corn-
results averaging somewhat higher than and in many bining with the residue from the acid digestion,
cases very close to those obtained by calculations based The ammonium carbonate volatilizes on evaporating
on the conventional assumption that the carbon con- the solution. There is a small retention of ammonia
tent of the organic matter is 58 per cent. Variations in chemical combination with the organic matter but
are from +0.37 to — 0.37 and average +0.02 per cent. this amount is quite small and may be disregarded.
These variations are to be expected in view of the well- Results with this method are given at the bottom of
known variation in the carbon content of soil organic Table I.
matter. Alfalfa hay and sawdust from appi
Results by Method B, in which the soluble organic as examples of undecomposed plant residues which
matter is disregarded, are quite close to those by may occur in the soil. With the former, assuming that
Method A. The maximum deviation is 0.18 per cent all the volatile matter is organic, the re. 04.46
in favor of Method A, the minimum deviation is zero, per cent, and with the latter 96.25 per cent. An acid
and the two methods give results which average prac- and a calcareous peat are taken as examples of partially
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. 6
decomposed organic matter. With the former the
recovery was 97.62 per cent and with the latter, after
allowing for the 1.80 per cent of inorganic carbon di-
oxide in the sample, the recovery was 99.44 per cent.
The sample of Caribou loam is an example of a soil
with an abnormally large amount of acid-soluble or-
ganic matter. The ammonium carbonate modifica-
tion gave 33 per cent higher results on this soil than
Method A, recovering 1.60 per cent of the acid-soluble
organic matter, which is 25 per cent of the organic
matter of the soil.
It is believed by the writer that the method and its
modifications here proposed will indicate the organic
matter content of the soil to within 3 per cent in per
cent of organic matter and within the limit of experi-
mental error with the average mineral soil.
The question of the carbon content of soil organic
matter will be studied further.
The writer is indebted to Dr. G. S. Fraps, Dr. E. C.
Shorey, and Mr. De F. Hungerford for some samples
of soils, and to Mr. R. H. Ridgell for assistance in the
analytical work.
SUMMARY
The minerals in the soil which interfere with the
accuracy of the loss-on-ignition method for the de-
termination of organic matter can be removed by di-
gesting in the warm with a weak acid solution con-
taining hydrofluoric and hydrochloric acids without
dissolving more than a small amount of organic matter.
This fact has been made the basis of a method for the
determination of organic matter in soils which is much
superior to the loss-on-ignition method and is believed
to be superior to the organic carbon method.
Arkansas Agricultural Experiment Station
Faybttevillk, Arkansas
THE AGRICULTURAL AVAILABILITY OF RAW GROUND
PHOSPHATE ROCK1
By William H. Waggaman and C. R. Wagner
Received April 16, 1918
INTRODUCTION
The present shortage and high price of soluble phos-
phate is one of the most serious problems which con-
fronts the agricultural interests of this country. The
fact that the munitions industry calls for immense
tonnages of sulfuric acid which are normally used in
the manufacture of superphosphates makes it appear
unlikely that the price of this latter material will de-
crease or its tonnage be much increased in the near
future. While at least 200 patents2 have been issued
dealing with methods of producing soluble and avail-
able phosphates, without the use of sulfuric acid, either
these have been proved commercially impracticable
or their adoption would involve too much time to
prove of immediate value. There is, therefore, a very
urgent demand for a phosphatic fertilizer which will
meet in part, at least, the present emergency, and raw
ground rock phosphate is the only material which can
1 This article is a summary of an exhaustive investigation of the sub-
led made by the Bureau o! Soils Thi Investigation iriU
appear in a later publication.
< V. S. Department of Agriculture. Butt. 314
be produced in sufficient quantities to make up this
serious shortage.
The value of raw ground rock phosphate as a fer-
tilizer has been a much-discussed question for over
fifty years. Some agronomists and agricultural chem-
ists have reported satisfactory results from its use
both in pot and field experiments. Others have de-
cided that while the material is beneficial to a number
of crops when applied under certain conditions, it is
so inferior to acid phosphate that it is unwise under
normal conditions to depend upon it as a source of
phosphoric acid, when one can obtain more soluble
superphosphates. Still others have concluded that
raw ground phosphate is entirely unprofitable on most
of the soil in their particular States under their present
crop systems.
In spite of the many adverse opinions regarding its
value, however, the use of finely ground, raw rock
phosphate has continued to increase until now the
annual consumption is over 65,000 tons involving an
expenditure of over $500,000.
THE NATURE OF MINERAL PHOSPHATES
It is not within the scope of this paper to discuss
in detail the nature and origin of phosphate deposits,
but the main constituent of most of the amorphous
phosphate rock is tricalcium phosphate, a compound
which is relatively insoluble in water and quite resistant
to weathering influences. In fact the formation of
phosphate deposits may be said to be largely due to
the slight solubility of this latter compound.1
A quick response from applications of such material,
therefore, is hardly to be expected unless it is subjected
to some treatment by which its solubility is consider-
ably increased, or is applied to the soil under such con-
ditions that it will yield its phosphoric acid to the soil
waters approximately as fast as it is taken up by grow-
ing crops.
In order to render the phosphoric acid in phosphate
rock soluble and facilitate its distribution in the soil,
it was proposed to treat the material with sulfuric
acid. This method was first practiced on bones and
bone products about 100 years ago and since then the
use of acidulated phosphates has grown rapidly until
now the vast bulk of the phosphate rock entering into
the fertilizer industry is treated with sulfuric acid and
manufactured into superphosphate.
It must be admitted, however, that most of the phos-
phoric acid contained in practically all productive
soils is in the form of relatively insoluble phosphates
of lime, iron and alumina, yet many of these soils con-
tinue to yield large crops without the addition of any
soluble phosphates and frequently give no response
to such applications.1
The question is, therefore, will raw rock phosphate
increase the yield of crops when applied under proper
conditions and if so, is the increase obtained commen-
surate with the cost of thi
1 Eliot Blackwelder, "The Geologic Role of Phosphorus." Scientific
American, Supplement No 2197, Feb 9,1917.
1 The fact is particularly well exemplified in the "Blue Grass" regions
of Kentucky and in the "Central Basin " Tennessee, where the soils are
very high in phosphoric acid.
June, 101S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
EFFECT OF FINE GRINDING AND ORGANIC FERMENTATION
ON THE SOLUBILITY AND AVAILABILITY OF
PHOSPHATE ROCK
No one questions the fact that fineness of division
facilitates the solubility of mineral matter. Relatively-
insoluble substances, such as tricalcium phosphate,
when in the precipitated conditions dissolve quite
appreciably in water as well as in certain conventional
solvents, such as ammonium citrate and 2 per cent
citric acid.
It has also been repeatedly demonstrated both in
laboratory and greenhouse experiments that the solu-
bility of raw rock phosphate is considerably increased
by fine grinding.1 Not only is the distribution of the
rock in the field much facilitated in this way, but an
enormous surface of the mineral is thus exposed to
the solvent action of the soil waters.
In the early experiments conducted with this material
strict attention was probably not given to this im-
portant factor and it is very likely that a great deal
of work with raw rock phosphate resulted adversely
on this account. Several companies offer raw phos-
phate rock for sale guaranteeing 90 per cent to pass a
sieve of 200 meshes to the linear inch. While tests
performed in this laboratory seem to show that it is
hardly feasible to put rock of this degree of fineness
on the market at a low price, it is entirely possible to
grind the material so that 00 per cent would pass a 100-
mesh sieve, and material of this degree of fineness
should prove quite effective. Because raw ground
rock phosphate has in many cases proved more effec-
tive on soils rich in organic matter or when applied in
connection with stable manure, it has been suggested
that certain organic acids in the soil exert a solvent
influence on the rock similar to the effect produced by
sulfuric acid. The existence of organic acids in the
soil in quantities sufficient to appreciably effect the
solubility of phosphate rock is doubtful, but soils of
high organic content are always rich in carbon dioxide
and bacteria, both of which have an important influence
on the solubility and alteration of soil minerals,2 and
hence it is reasonable to expect an increase in the solu-
bility of the phosphate contained therein over that
of soils of low organic content.
Other things being favorable, therefore, it appears
that soils low in phosphoric acid and rich in organic
matter should respond readily to additions of raw
rock phosphate provided that the material is very
finely ground, applied liberally, and is well distributed
by thorough cultivation.
WORK OF THE EXPERIMENT STATIONS
The experiment station literature contains the re-
sults of 232 field experiments and 23 pot experiments
' J. A. Voelcker, J. Roy. Agr. Soc, 4 (1868), 176-196; W. H. Jordon.
N. Y. Exp. Sta. (Geneva), Hull. 3S8 (1913); W. L. Burlison, J. Agr. Res., 6
(1916), 507-8.
• C. P. Williams. Chcm. News. 24 (1871), 306; T. Schloesing, Compl.
rend.. 131 (1900), 149; P. Kossowitch, liiedermann's Zcnlr., 31 (1902),
44-49; E. Truog, Wis. Exp. Sta., Research Bull. 20 (1912); Sackett,
Patten and Brown, Mich. Exp. Sta., Bull. (Special) 43 (1908); Totting-
nam and Hoffman, Wis. Exp. Sta., Research Bull. 29 (1913), 213-312;
C. A. Mooers, This JOURNAL, 6 ( 1914), 487-8; Fred and Start, Wis. Exp.
Sta., Bull. 36 (1915), 35-66; Hopkins and Whiting. Ill Exp. Sta . Butt.
5»0 (1916), 395-406.
conducted with raw rock phosphate, yet unless the
relative merits of these experiments are very carefully
weighed they cause the reader much confusion and
lead to the conclusion that raw rock phosphate is of
very questionable agricultural value.
It is now a generally accepted fact, however, that
field experiments must be conducted for a period of
several years before the results can be seriously con-
sidered, so after a careful study of the work recorded
by the stations, the writers decided to give detailed
consideration only to those field experiments which
were conducted for 5 years or longer. This method of
treatment has eliminated 195 field experiments, of
which number, 144 were conducted for 1 year only,
21 for 2 years, 19 for 3 years and 11 for 4 years. The
remaining 37 experiments (conducted for 5 years or
longer) were then given detailed study, careful at-
tention being paid (as far as possible) to the following
important factors which influence the results of field
work: (1) Uniformity of experiment field. (2) Topog-
raphy and drainage conditions. (3) Chemical and
physical composition of the soil. (4) Previous treat-
ment of the field. (5) Climatic conditions. (6)
Injuries from disease, insects, and animals. (7) Kinds
of crops grown and selection of seed. (8) Rate of
application and uniform distribution of phosphates.
(9) Methods of comparing raw rock with other phos-
phates. (10) Effect of other fertilizers. (11) Number
and distribution of plots. (12) Duration of experiment.
In most cases many of these factors were not re-
corded in the descriptions of the experiments, and since
the work was conducted under such a variety of con-
ditions and with so many objects in view it could not
be reduced to a common basis for the sake of com-
parison.
The details of these experiments will be discussed
in a subsequent publication, but a summary of the
results obtained is given below in Table I. It must
be borne in mind, however, that the classifications made
are necessarily somewhat arbitrary since it is impossible
to summarize the results of field work in such a way as
to give each experiment its proper weight.
Out of the 37 tests given in Table I, 22 were carried
on with a view to comparing the relative merits of
raw rock and acid phosphate. The conditions under
which such a comparison was attempted varied greatly,
but it may be said that in a general way, 13 of these
experiments or 59.1 per cent gave crop yields as favor-
able to raw rock as to the more soluble form of phos-
phoric acid. Of the 9 experiments in which raw rock-
did not compare favorably with acid phosphate, 2
were conducted on fields unresponsive to phosphate
treatments and 2 gave results which could be classed
as either favorable or unfavorable, depending on the
method of interpretation employed.
Of the 15 experiments in which no comparison be-
tween raw ground rock and acid phosphate was at-
tempted, 11. or 73.3 per cent, gave results strongly
indicating beneficial effects from the applications of the
former material, and 2 of the remaining 4 experiments
wen conducted on fields showing little or no response
to phosphate fcreal ment.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 6
ii i i Summary of Resuvts op Field Experiments with Raw Rock Conducted by the State Stations over Periods op prom 5 to 20 Years
Kxperiments com- Experiments making no
paring raw rock comparison of raw rock
with acid phosphate with acid phosphate
Experiments where
aw rock applications
were relatively light
Experiments where Experin
raw rock applica- rock wa:
tions were liberal tion wit
Apparent
cumulative
: matter effect
of Ex-
peri-
No. No. No.
unfav- favor- unfav-
orable Total able orable
Di i
Fla
Ga
Ill
.. 12
1
1(a)
9
7
2(a)
4
4
8
6
2(a) 11
9
2(e)
8
3(a)
i
Ind
2
1(a)
.'
1(a) 2
1
1(a)
2
Ky
1
1
1
1
1
i
La
.. 3
3
2
2
2
1
.. 2
2
1
2
2
i
1
M.I
.. 2
2
2
2
i
i
1
.. 2
1(6)
1
1
1
2
.. 2
2
1
2
2
2
Mo
4
4
2
2
4
2
2
2
2
4
N. J
.. 0
N. V
.. 0
N. C
.. 0
.. 4
2
1(6)
2
2
3
2
1(6)
3
1
3
Pa
1
1
1
i
R. I
1
I
1
i
S. C
.. 0
.. 0
Va
.. 1(a)
1(a)
1(a)
1(a)
1(a)
Ka)
W. Va...
Wis
Total . . .
.. 37
22
13
9
5
11
4
21
15
6
6
13
3 23
18
5
17
7
13
(a) Soil not responsive to phosphate treatment.
(6) Figures for this experiment are favorable according to (
i method of computation and unfavorable according to another.
In 21 experiments the applications of raw rock were
relatively light (250 lbs. or less per acre), yet 15 of
these experiments, or 71.4 per cent, showed distinctly
favorable increases in yields on the fields treated with
this material.
In 16 experiments where the raw rock applications
were more liberal, 13, or 81.3 per cent, resulted favor-
ably to raw rock phosphate, and the remaining 3 ex-
periments were conducted on soils showing little or no
response to phosphate treatment.
Raw rock phosphate was applied in connection with
organic matter in 23 experiments. Out of this number,
iS, or 78.3 per cent, gave distinctly favorable results,
and of the 5 remaining experiments 3 were conducted
on fields unresponsive to other forms of phosphoric
acid.
In regard to the cumulative effect of raw ground
phosphate rock it may be said that in 17 instances
(46 per cent of the entire number of experiments)
there was evidence of greater availability after raw
rock had been applied for a number of years. In 13
out of the remaining 20 experiments the data are not
sufficient to give evidence on this point, and in 4 out
of the 7 cases where no cumulative effect was shown
the soils were not responsive to phosphate treatments.
CONCLUSIONS
After carefully weighing the results of all laboratory,
field and greenhouse experiments with raw rock phos-
phate the writers feel that the following general con-
clusions are justified:
1 — Field experiments conducted for only one or
two years, where the various fertilizer treatments are
not replicated or where no index is given to the rela-
tive natural fertility of the various plots employed,
have little or no meaning.
2 — Liberal and even medium quantities of raw rock
phosphate to most soils produce an increase in the
yields of many crops the first year of its application.
3 — The effectiveness of raw rock phosphate depends
largely on its thorough distribution in the soil, this
distribution being brought about by liberal applica-
tions of very finely divided material and thorough
cultivation.
4 — The presence of decaying organic matter in the
soil increases the effectiveness of raw ground rock phos-
phate, due probably both to greater bacterial activity
and the higher content of carbon dioxide in such soils.
5 — As a corollary of 3 and 4, the effectiveness of
raw rock phosphate is usually increased after remain-
ing in the soil for a year or more.
6 — Most crops respond more quickly to applications
of acid phosphate than to bone, basic slag, or raw rock
phosphate. Therefore, where the early stimulation
and quick maturity of the crop are the main considera-
tion, acid phosphate is probably the best form of phos-
phoric acid to apply.
7 — Field experiments in which raw rock and acid
phosphate are compared on the basis of equal applica-
tions of the two materials or on equal applications of
phosphoric acid in the two forms result often in favor
of acid phosphate (particularly when such experi-
ments are conducted for a short period), since in order
to get the maximum benefit from the natural phosphates
they must be applied at a rate far exceeding that at
which acid phosphate proves effective.
8 — The question whether increases in yield can ordi-
narily be produced more economically by applica-
tions of the soluble or relatively insoluble phosphates
must be considered in a measure a separate problem for
each farmer, since it depends on a number of factors
of which the most important are the nature of the soil,
the crop system employed, the price of the various
phosphates in each particular locality, and the length
of the growing season.
Bureau of Soils
Department op Aoriculturb
Wasiiinoton, D. C.
June, 1918 THE' JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
445
UPON THE ACTION OF TETRAZODI-o-TOLYLMETHANE
CHLORIDE UPON NAPHTHOL AND NAPH-
THYLAMINE SULFO ACIDS
[first paper]
By James H. Stebbins, Jr.
Received December 17, 1917
Prior to 1885, cotton fiber had to be put through
a preparatory treatment before it could be dyed with
artificial coloring matters. In 18S4, P. Bottiger1
discovered and patented a new dyestuff, which a year
later was introduced into commerce by the "Actien-
gesellschaft fur Anilinfabrikation" under the name of
Congo. This new product was the first of a series
which had the property of dyeing the cotton fiber
direct, without prior mordanting.
Congo is produced by the action of 1 molecule of
tetrazobenzidine chloride (tetrazodiphenyl chloride)
upon 2 molecules of sodium naphthionate.1
G. Schultz2 has shown that benzidine is a dipara-
— NH., hence
aminodiphenyl, NH2
the constitution of ^ongo is:
>— SOsNa
-SOsNa
When o-nitrotoluene is subjected to alkaline reduc-
tion it forms hydrazotoluene, which, on treatment
with acids, is transformed into di-^-aminoditolyl,
or tolidine having the constitution:3
CH3
CH,
This product like benzidine is capable of forming a
tetrazo compound on treatment with nitrous acid,
which in turn may be coupled with two molecules of
sodium naphthionate to form the red substantive dye
known as Benzopurpurin 4B. The property of Congo
of fixing itself directly to the cotton fiber is evidently
due to the presence of the diphenyl residue in its mole-
cule, since other coloring matters derived from benzi-
dine and its homologues possess the same character-
istics.
The homologous bases of the aniline series may be
divided into two classes, according to their behavior
with formaldehyde:4
1 — Those in which an unsubstituted carbon atom
(i. e., hydrogen-bearing carbon atom) stands in the
para position to the amino group. Among the tech-
nically most important bases of this class are aniline,
1 D. R. P. No. 28,753. Feb. 27, 1884.
• Ann., 1T« (1874), 227.
■ Ber., 17 (1884), 467.
• D. R. P. No. 87,615, Sept. 1895; Friedljndir, 4, 65.
-NH2; o-toluidine, H— <^ ^> — NH2; and
CH3
CH3
/"-xylidine, H-
>— NH2.
2 — Those which contain a substituted carbon atom
'in the para position to the amino group.
The technically most important bases of this class
are ^-toluidine, CH;
w?-xylidine, CH3
NH;, and asymmetrical
NH..
The bases of this second class unite with formalde-
hyde with much greater difficulty, under the same con-
ditions, than those of Class i. Furthermore, bases
of Class 2 in admixture with bases of Class i will not
unite at all with formaldehyde as long as bases of Class
i are present. This peculiarity permits a complete
quantitative separation of such bases.
Availing myself of this reaction, 200 g. technical
o-toluidine (about 2 moles) were dissolved in the calcu-
lated amount of HC1 of sp. gr. 1.10 or 71.9 cc, diluted
with 400 cc. H20, and 75 g. of 40 per cent formaldehyde
added. The mixture was now heated on the water
bath to 70— 76 ° C. for 4 hrs. and then made alkaline
with NaOH solution. A copious, whitish, crystalline
precipitate is thus thrown down and the latter steam-
distilled until no more toluidine passed over. The
crystalline mass thus obtained was collected upon a
filter, dried and then recrystallized from alcohol,
from which, on rapid cooling, it is obtained in the shape
of small octahedra, among which are many twin crys-
tals. On slow cooling, it crystallizes in rhombic prisms,
also showing much twinning. Melting point, 1490 C.
The product is, therefore, diparaaminodi-o-tolyl-
methane,
CHS CH3
obtained by the condensation of 2 molecules of 0-
toluidine with 1 molecule of formaldehyde.
As this product partakes somewhat of the structure
.i dine and toluidine, but differing from the latter
compounds in having the two benzene rings coupled
to a methane rest, it was of interest to ascertain whether
.di-o-tolylmethane, like benzidine and tolidine,
zotized and coupled with phenols, amines
and their sulfo acids to form substantive dyes, or
whether its difference in structure would materially
affect the nature of the dyestuffs derived therefrom.
To answer these questions, the following experiments
were made.
446
THE JOURNAL OF INDUSTRIAL AND ENGINEERING < HEMISTRY Vol. 10, No. 6
EXPERIMENTAL
TETRAZODI-0-TOLYLMETHANE CHLORIDE A few quali-
tative tests showed that nitrous acid combines with
diaminodi-o-tolylmethane in HC1 solution to form a
diazo compound, but the question which naturally
arose was whether only one, or both of the amino groups
in the above-named product were diazotized. This
question was easily settled by titrating a known quan-
tity of the diamino base with sodium nitrite solution,
using iodide of starch paper as an indicator.
Base taken 1 00 g.
Dissolved in 3 cc. HCI (sp. gr. 1.2) diluted with 200
cc. HiO. Cooled with ice and titrated with
NaNOi solution.
1 cc. NaNOi soln. = 0.0047 HNOi
Required for titration 85.4 cc. NaNC" soln.
HNO, used 0.4003 g.
Calculated 0.4159 g.
It will be seen that the above figures agree very closely
with the theory for di-para-aminodi-o-tolylmethane
and consequently the product formed on treating the
above compound in hydrochloric acid solution with
nitrous acid must be a tetrazo-di-o-tolylmethane
chloride,
CH, CHj
N=N.
CI
DI-0-TOLYLMETHANE - 4 - HYDROXYAZO-I-N APHTHOL-4-
SULFO acid — According to the usual manner of coupling
tetrazo compounds with amines, phenols and their
sulfo acids,1 it was expected that i molecule of tetrazo-
di-o-tolylmethane chloride and 2 molecules of 1,4-
naphtholsulfo acid would interact to form
(4) yOH(i)
CH,(CH,).N=N.C,oH6<'
I ^SOjHU)
CH,
(4) /SO,Hu)
C,H,(CH,).N=N.C,oH/
X)H(i)
However, subsequent examination of the product
obtained showed this not to be the case.
0.01 mole diaminodi-o-tolylmethane, or 2.26 g.,
were dissolved in 0.04 mole HCI, or 3.1 1 cc. HCI of
sp. gr. 1.2, diluted with 200 cc. water. This solution
was now cooled with ice and tetrazotized by slowly
stirring in 0.02 mole NaNO,, or 1.38 g. dissolved in 50 cc.
H2O. The above solution was now allowed to stand
until the complete absorption of the HN02 had taken
place as shown by iodide of starch paper, and then
slowly stirred into a solution of 0.0 1 mole of 1,4-
naphtholsulfo acid, or 2.24 g., made alkaline with 0.02
mole Na2C03, or 2.12 g. My motive in using only one-
half the theoretical quantity of 1,4-naphtholsulfo
acid was to note whether as in the case of tetrazodi-
phenylchloride2 an intermediary compound of the
following formula would be formed:
' BOttlger, D. R. P. No. 28,753; Witt, Ber., 19, 1719; C. Schulti.
2d Edition, p. 302; Ibid., 257.
1 Bucherer, p. 362.
OH
SO.H
On mixing the tetrazo solution with the 1,4-naph-
tholsodiumsulfonate solution a copious blood-red pre-
cipitate is formed. The latter was allowed to stand
over night and the next morning was collected upon
a filter and washed. The filtrate, on being tested with
an alkaline solution of /3-naphthol, was found to be
free from tetrazo compound. The red precipitate
formed is insoluble in water and when boiled with
the latter gives off nitrogen, which would suggest the
presence of an intermediary compound of the foregoing
composition. It was then rinsed into a beaker and
treated with an additional 0.0 1 mole 1,4-naphtholsulfo
acid, or 2.24 g., and made alkaline with 0.01 mole of
NajC03, or 1.06 g., and the mixture allowed to stand,
with occasional stirring, for 24 hrs.
No apparent change having taken place, the red
precipitate was collected upon a filter, thoroughly
washed and dried.
The product thus obtained is but little soluble in
hot or cold water, but is soluble in dilute caustic soda
solution. The filtrate from the above red precipitate
on being tested with diazosulfanilic acid showed the
presence of considerable uncombined 1,4-naphthoI-
monosulfo acid, showing that the second molecule of
sulfo acid had not combined with the red product.
Thinking that possibly better results might be ob-
tained by treating the tetrazo compound at once with
the two moles of 1,4-naphtholsulfo acid, the experiment
was twice more repeated, using 4.48 g. sulfo acid in-
stead of 2.24. The final result, however, was the
same.
Believing prolonged digestion of the red product
(which was considered to be an intermediary product)
with an extra molecule of naphtholsulfo acid might
bring about a union of the two, a mixture of the two
was digested at 37.5 ° for 24 hrs. A more soluble
product was obtained, but the additional molecule of
sulfo acid remained uncombined. Therefore, we must
infer that an intermediate compound of the formula
(4) /OH(i)
C,H,(CH,).N =N— C.oH/
XSOs(4)
CH,
I (4)
CHHCH,).N=N
a
June. 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
447
has been formed, which on standing or upon heat-
ing loses nitrogen and is gradually transformed into
a product of the following composition:
(4) X)H(i)
C,Hi(CHj)N =N— CioH/
I XS03(4)
CH,
I (4)
C6H,(CH8)OH
This reasoning has been fully borne out in the course of
our experiments. In further evidence of the fore-
going, a nitrogen estimation of the free dyestuff acid,
prepared as follows, was made:
The acid soda salt of di-o-tolylmethane-4-hydroxy-
azo-i-naphthol-4-sulfo acid, obtained by boiling the
insoluble red precipitate with the calculated amount
of sodium hydroxide, was filtered and the filtrate
treated with an excess of concentrated HC1. The
red precipitate of the free acid thrown down was col-
lected upon a filter, washed with cold water till free
from HC1 and NaCl, air-dried upon a porous plate and
then finally dried at 130-1350 C.
All attempts to obtain the free acid in a crystalline
form failed and, therefore, the product obtained as
just described had to be used for analysis.
The nitrogen was estimated by the Kjeldahl method
and gave the following result:
Free acid taken 0. 1018 gram
N found 5 . 92 per cent
(4) /OH(l)
Theory for C.Hi(CHi)N - N — CioH^ 6.04 per cent
| NSOiH(4)
CHi
I (4)
C.Hi(CH«)OH
Barium in the barium salt was estimated as follows:
The salt was prepared by dissolving the acid soda
salt in boiling water and treating with an excess of
barium chloride. This threw down the barium salt as
a red precipitate. The latter was collected upon a
filter, washed with boiling water till free from BaCl2,
air-dried, and then finally dried at 100° C. The
product thus obtained is by no means pure, but is the
best that could be obtained under the circumstances.
Barium 9alt taken 0.1 592 gram
BaS04 weighed 0 . 0366 gram
Equivalent to barium 13.19 percent
(2) (4)
/OH(l)
NSO.(4)
CeHs(CHj)N - N -
|
Ba
CHj
1 (2) (4)
CiHj(CH>)OH
2
Hence the free acid must be constituted as previously
stated and consequently the acid soda salt must have
the following constitution:
(4) X)H(i)
C,H3(CH,)— N =N— C,oH/
| XSO»Na(4)
CHj
I (4)
C«H3(CH,)OH
It is further shown that in following the technique
previously described, one molecule of tetrazodi-o-
tolylmethane chloride unites with only one molecule of
i ,4-naphtholsulfo acid to form the intermediate product,
(4) /OH(i)
C,H3(CH3)— N =N— C,oHt<f
I XSOaH(4)
CH2
I (4)
C,H3(CH3)— N=N
I
CI
which latter compound is gradually transformed by
substitution of OH for N into
(4) /OH
C6H3(CH,)— N = N— C10H/
XS03H.
CH2
I (4)
C«H,(CHs)OH
Up to very recently it was found to be impossible
to combine i molecule of tetrazodi-o-tolylmethane
chloride with more than i molecule of 1,4-naphtholsulfo
acid, but lately upon taking the subject up again and
slightly modifying the technique, I have been able to
combine 1 molecule of the tetrazo compound with two
molecules of 1,4-naphtholsulfo acid with the greatest
ease. Briefly described, the new technique is as follows:
2.26 g. diaminodi-o-tolylmethane are dissolved in
4.5 cc. HC1 of 1. 1 9 sp. gr. diluted with 100 cc. H20.
The solution is then cooled with ice and tetrazotized
by gradually stirring in 1.38 g. NaN02 dissolved in
25 cc. H20.
The tetrazo solution is then gradually stirred into a
solution of 4.48 g. 1,4-naphtholsulfo acid (0.02 mole)
dissolved in 50 cc. water and 50 cc. alcohol (denatured
will do). A heavy carmine precipitate with bluish
tinge is at once formed. This is allowed to stand over
night and the next morning is filtered under suction
and dried. The product thus obtained is the acid soda
salt of1
(4) /OHO)
C«H3(CH3)— N =N— CoH/
I XSO>Na(4)
CH2
(4) /SO,Na(4)
C6H3(CH3)— N =N— C10H6<(
XOH(i)
It appears as a dark red powder, is easily soluble in
water, and dyes wool, in a bath containing sulfuric acid
and sodium sulfate, a fine, scarlet color, which is fairly
fast to light (4 weeks' exposure) and to washing and
fulling. Contrary to expectations, however, it has
but little affinity for cotton. Why the mere addition
of a little alcohol to the reaction mixture should bring
about a union of 1 molecule of tetrazo compound
with 2 molecules of sulfo acid is hard to explain.
DI-0-TOLYLMETHANEAZO-2-NAPHTHOL-3,6-DISULFO ACID,
azo-2-naphthol-3,6-disulfo acid— On mixing an
1 That the 2 molecules of 1 ,4-naphtholsulfo acid had combined with
the 1 molecule of tetrazo compound was easily proved by treating a drop
of the reaction mixture upon filter paper with a drop of diazosulfanilic acid.
As no coloration was observed, it is evident that all the sulfo acid had com-
bined with the tetrazo solution.
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 6
aqueous solution of i mole tetrazodi-o-tolylmethane
chloride with an aqueous NajCOs solution of 2 moles
2,3,6-naphtholdisulfo acid, an intense scarlet-red pre-
cipitate is obtained, and on testing the outer watery
edge of a drop of this solution upon filter paper with
a drop of diazosulfanilic acid, no red coloration is ob-
tained. From this it is evident that the 2 moles of
2,3,6-naphtholdisulfo acid have combined with the
1 mole of tetrazo compound.
On heating the solution to boiling, all the red pre-
cipitate dissolves, and separates again, on cooling,
in a semi-crystalline form. It was collected upon a
filter at the pump and finally dried upon a porous plate.
When dry, the acid soda salt of the new product ap-
pears in the shape of a dark red powder with beetle-
green luster. It is easily soluble in hot or cold water
with a scarlet color and has the following constitution:
(4) /OH (2)
CsHatCHa)— N =N— C10H^SO3Na(3)
I ^SOsNaCe)
CH2
I (4) /SO,Na(6)
C6H,(CH3)— N = N— CioH4^-S03Na(3)
X>H(2)
It likewise is a strong wool dye and dyes the latter,
in a bath acidulated with sulfuric acid, a bright scarlet
shade, somewhat resembling that obtained with the
previous product.
It will, therefore, be seen that we here have a cer-
tain deviation from the results obtained with 1,4-
naphtholmonosulfo acid, for, whereas only 1 molecule of
the latter will unite with 1 molecule of tetrazodi-o-
tolylmethane chloride when operating under normal
conditions, i. e., in aqueous solution, in the present
case the tetrazo compound unites easily in an all-
aqueous solution with 2 molecules of the disulfo acid.
Why these two naphtholsulfo acids should act so
differently I am hardly prepared to say, but if I may
venture an opinion, I would attribute it to the different
positions of the sulfo groups in the naphthalene rings.
In coupling diazo salts with phenols or amines of
the naphthalene series, if a hydroxyl group or amino
group is in the alpha-position, combination takes place
in the 4-position. If this is occupied, or if the positions
3 or s are occupied by sulfonic groups, union takes
place in the 2-position.
Now in the case of the product from 1 molecule of
tetrazo compound and 1 molecule of 1,4-naphtholsulfo
acid the 4-position of the naphtholsulfo acid is occu-
pied by a sulfo group, thereby forcing the tetrazo com-
pound to couple in the 2-position and it has been shown
that it took quite a little coaxing to cause the tetrazo
compound to unite with an extra molecule of 1,4-
naphtholsulfo acid under these conditions. On the
other hand, in the case of the last-named dye from 1
molecule of tetrazodi-o-tolylmethane chloride and 2
molecules of 2,3,6-naphtholdisulfo acid, the 4-position,
of the disulfo acid being unoccupied, the tetrazo com-
pound was enabled to couple directly in the 4-position,
and as we may infer that the 4-position is the one of least
resistance, this may possibly account for the greater
ease of union between the 1 molecule of tetrazodi-o-
tolylmethane chloride and 2 molecules of 2.3,6-naph-
tholdisulfo acid.
If, as is supposed, the presence of the diphenyl
residue in the molecule is necessary for the production
of substantive cotton dyes, then it is possible that
the presence of the methane rest uniting the two
benzene rings in tetrazodi-o-tolylmethane may be the
reason why the dyes obtained from this product are
wool dyes and have practically no affinity for cotton.
This is only a surmise on my part which at present
I am unable to back up by further proof.
27 East 22nd Street
New York City
METHOD OF CALCULATING COMPARATIVE STRENGTH
AND EFFICIENCY OF HIGH EXPLOSIVES FROM THEIR
COMPOSITION AND APPARENT DENSITIES
By Charles E. Waller
Received April 2, 1918
INTRODUCTION
A number of laboratory tests have been devised for
obtaining comparative or definite values as to "strength"
of explosives, of which may be mentioned the Trauzl
test, ballistic pendulum, mortar tests, pressure gauges,
etc., in each of which it is the practice to note the effect
of a certain unit weight of an explosive and compare
some with results of an equal of another explosive.
These results, however, do not always conform with
those obtained in the field, for the reason that "strength"
of explosives is there often judged by the effect of a
certain bulk of explosive, i. e., the volume of the charge
chamber, in which explosives are compared in the field,
is practically a constant, whether it is a bore hole or
a war head. The importance of loading density of
explosives for military purpose has been considered
by the U. S. Ordnance Department, which even in-
cludes the same in their specifications.
It would therefore seem more rational to compare
explosives in the laboratory by volume; for instance,
instead of using the customary charge of io g. in the
Trauzl test, a charge equivalent to the weight of io
cc. at its apparent (or loading) density should be used.
All ballistic tests in the laboratory require careful
and elaborate execution, and the method of calculating
"strength" and efficiency as outlined in this paper is
suggested as a means of obtaining values which have
been proved to conform with carefully made laboratory
tests.
The word efficiency, as applied to explosives, is
generally used to express the amount of useful work
that is done with a certain weight or "bulk" of an ex-
plosive; in coal-mining, for instance, it means the
amount of lump coal that is obtained from a certain
amount of explosive, while in tunnel work it means
the progress that can be made, etc. In this article,
however, the word efficiency denotes the maximum
available energy stored up in a unit "bulk" of an explosive,
and which, according to definition below, is propor-
tional to the volume which the gaseous products of
explosion of a unit "bulk" — say i cc. — would occupy
at t° and atmospheric pressure.
June, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
449
The method used in calculating 1° is practically the
same as outlined in the literature on this subject,1 but
in constructing the chemical equations representing
the explosion, special rules have been outlined and
followed, and the object of calculating t" is here only
to obtain a value, theoretically correct, from which
the gas volume at t° may be found.
In the method used for calculating the gas volume
at 1° of explosives containing nitrostarch with a speci-
fied nitrogen content, it will be noted that the chemical
formula given to such nitrostarch contains fractional
numbers of atoms, which, although irregular from a
chemical standpoint, is mathematically correct and
facilitates the calculations.
DEFINITIONS
The strength of high explosives may be considered
as a function of the maximum pressure of the gaseous
products, obtained by detonating unit weights (1
gram) of the explosives under exactly equal conditions.
The efficiency of high explosives may be con-
sidered as a function of the maximum pressure of the
gaseous products, obtained by detonating unit volumes
(1 cc.) of the explosives at the apparent densities at
which they are intended to be used under exactly equal
conditions. '
According to a well-known physical law the pressure
of gases confined in a closed vessel is proportional to
their temperature (t°), and also to the volume that the
same gases would occupy at t° under atmospheric
pressure. The above definitions may therefore be
substituted by the following:
The strength of high explosives is proportional to
the volume which the gaseous products of explosion of
a unit weight (1 gram) of the explosives to be compared
would occupy at t° and atmospheric pressure.
The efficiency of high explosives is proportional
to the volume which the gaseous products of explosion
of a unit volume (1 cc.) of the explosives to be com-
pared would occupy at t° under atmospheric pressure.
temperature of explosion (t°)
No means have been found to directly measure the
temperature of explosion, but by knowing the products
of explosion as they exist at t", their heat of formation
as well as their mean specific heat between 0° and t°
and, furthermore, the heat of formation of the ingre-
dients of the explosive, a correct value for t° may be
calculated by the well-known formula:
Q
a + bt
(1)
in which Q = calorific power of the explosive (in gram-
calories), obtained by subtracting the sum of molec-
rular heats of formation of the ingredients of the ex-
kplosive from the heats of formation of the products of
explosion; a = specific heat at o° C. of the products
of explosion; and b = increment of specific heat for 1°
C. of these products.
By solving t" in above equation we obtain:
o = — a + V46Q + o2
26
1 Bureau of^Mincs, Bull. 16.
M
GAS VOLUME AT 0° C.
Assuming that i gram-molecule of a gas occupies
22.4 liters at o° C. and 760 mm. pressure, the gas
volume at o° C. per gram of explosive is found from
the following formula:
M X 22-4
Vo = ~"~~r~ (3)
in which M = number of gram-molecules formed from
g grams of explosive.
GAS VOLUME AT t° PER GRAM OF EXPLOSIVE
The gas volume at t° and 760 mm. is found from
equation:
V, = Vo (1 + 0.003665 t) (4)
GAS VOLUME AT t° PER CC. OF EXPLOSIVE
The gas volume at 1° per cc, which has been defined
as a function of comparative efficiency, is obtained by
multiplying the gas volume at t° per gram by the ap-
parent density of the explosive, or
\,i = d XV, (5)
HEAT OF FORMATION
Berthelot and Thomsen have made extensive re-
search on determining the heat of formation of a number
of substances which may enter as ingredients in ex-
plosives or may be formed on explosion, and although
their results vary somewhat, the difference is so small
that practically the same results as to gas volume at
1° are obtained whether following a table by one or by
the other of above authorities. The following table
gives the heat of formation of substances which have
entered into calculations in this paper:
Mol. Heat
Molecular of Formation
Substance Formula Weight Calories
Ammonium nitrate NH.NOa 80 88.0
Barium nitrate Ba(NOi)s 261 228.4
Barium carbonate BaCOj 197 285.6
Sodium nitrate NaNOj 85 111.25
Sodium carbonate NaiCOj 106 272.6
Sodium sulfate Na:SOi 142 328.6
Nitroglycerine CiHt(NTOi)i 227 98.9
Nitrostarch C.Hio_x(NOi)IOs_x 162 + 45* 225.9—15*
Trinitrotoluene C.HjCNOjIiCHj 227 29.0
Picric acid "CeHs(NOs)iOH 229 50.9
Vaseline C»Rio 338 270.2
Wood pulp CiiHmOio 382 463.4
Water vapor HsO 18 58.1
Carbon dioxide COi 44 94.3
Carbon monoxide CO 28 26.1
The following table gives the molecular specific heat
at t° of the following substances, which have entered
into calculations below:
Substancb Mol. Sp. Heat at (°
1 mol. COi 6.26 + 0.0037 I
1 mol. HiO 5.61 + 0.0033 (
1 mol. Ni 4.80 + 0.0006 <
1 mol. Oi 4.80 + 0.0006 1
1 mol. CO 4.80 + 0.0006 t
Carbon (C) 6.40 + 0.00128 <
NaiCOj 26.00 ■+■ 0.0052 I
NaiSOi 33.00 + 0.0066 I
BaCOi 21.00 4- 0.0042 /
BaSO. 28.00 + 0.0056 (
CaCOj 20.00 + 0.0040 I
CHEMICAL REACTIONS OF EXPLOSION AND PRODUCTS
EXISTING AT /"
In collecting and analyzing the products of explosion
(as, for instance, in a Bichel pressure gauge) a num-
ber of products are often found, which our knowledge
of chemistry tells us could not exist at t°, but which
must be the results of secondary reactions taking place
4 50
THE JOURNAL OF INDUSTRIAL
on cooling. Of such products may be mentioned car-
bonates and bi-carbonates of alkaline metals, methane,
etc.
In order to obtain a theoretically correct value for
t° it is clear that only such products as exist at 1°
should be considered, and only such reactions as have
taken place before and up to the moment that t" has
been reached should enter into the calculations of
strength and efficiency of explosives.
Assuming, for instance, that N'aN03 enters as an
ingredient in an explosive containing a sufficient amount
of C and H (in some combination or other) to form
with the oxygen C02 and H20, this salt may be de-
composed according to one or the other of the following
reactions:
(a) 2NaN03 + H2 + 2C = Na20 + 2CO. -f
H20 + N2 (6)
(6) 2NaN03 + H2 + 2C = Na2C03 + C02 +
H20 + N2 (7)
(<-) 2NaN03 + H2 + 2C = 2NaHC03 + N2 (8)
Assuming that the explosion takes place according
to one or the other of these equations and calculating
t° for each, we obtain
(a) / = 1772° C.
(b) t = 266o°C.
(c) t = 3i6i°C.
Reaction (c) not only seems improbable, but the
results of various ballistic tests of explosives containing
a high percentage of NaN03 indicate that the explosion
does not take place according to this reaction. In
our calculations as to strength and efficiency of high
explosives we have, therefore, to choose between reac-
tions (a) and (b), and to find what influence one or the
other of these reactions has on the gas volume at /°.
Let us assume an explosive consisting of
Nitrostarch (with 12.75 per cent N) 58.4 per cent
NaNOi (pure) 41 .6 per cent
According to (a) the explosion may be represented
by the following equation:
C,2H,6(N03)606 + 4.6NaN03 =
2.3Na20 + i2C02 + 7-5H20 4- 4-8N2
and according to (o):
C12H1S(N03)606 + 4.6NaNOj =
2.3Na2C03 + o.7C02 + 7oH20 + 4-8N2
Calculating t° and gas volume at t° according to these
two reactions, the following values are obtained:
According to According to
(«) (6)
0.59 1. 0.524 1.
1000 cal. 1 192 cal.
2490° C. 2836° C.
5.987 1. 5.9759 1.
Gas volume at 1° per g
A number of calculations of 1° and gas volume at /°
have been made for explosives containing NaN03,
according to one or the other of the above reactions,
and it has been found that although different values
are obtained for gas volume at oc. calorific power, and
/°, the gas volume at 1° per gram of explosive is prac-
tieally the same, whether following reaction (a) or reaction
(b). The same holds true with explosives containing
sulfur as an ingredient.
AND ENGINEERING CHEMISTRY Vol. 10, No. 6
When an explosive or explosive mixture contains a
deficiency of oxygen for oxidizing the C and H to CO,
and H20, free hydrogen is often found in the products,
resulting from the well-known reaction CO + H20 =
C02 -f H2. Should there still remain some CO in
the gases, this may under certain conditions react
with the H2 according to the equation CO + 3H; =
CH« + H20, but as this reaction can take place only
at a comparatively low temperature, it must be con-
sidered as a secondary reaction and not be taken into
account in calculating the strength and efficiency of
explosives.
DETAILS OF CALCULATIONS
Calculations as to strength and efficiency of high
explosives involve the following steps:
1 — Construction of the equation representing the
explosion.
2 — Finding the gas volume at 0° C. and 760 mm.
per gram of explosive.
3 — Calculating the calorific power (Q).
4 — Calculating 1°.
5 — Calculating the gas volume at t° and 760 mm.
per gram of explosive.
6 — Calculating the gas volume at t" and 760 mm.
per cc. of explosive.
I. CONSTRUCTING THE EQUATION REPRESENTING THE
explosion — When a number of calculations have to
be made on explosives containing one and the same
explosive base, the following method has been found
to greatly facilitate the work:
The equation is commenced by one molecule of the
explosive base, and from its molecular weight the total
number of gram-molecules which should enter into the
equation is found by dividing the percentage of ex-
plosive base into 100 times the molecular weight of
same. The number of gram-molecules of each in-
gredient which should enter into the equation is then
found by proportion, and the number of molecules of
the ingredient in question is again found by dividing
the number of gram-molecules by the molecular weight
of same.
Example:
Assuming an explosive having following composition:
Per cent
Nitroglycerine 40
Sodium nitrate 43
Wood pulp 15
CaCOi 1
Moisture 1
100
Nitroglycerine iC3H5(N03)s) has a molecular weight
of 227 and the total number of gram-molecules which
, 227 X 100
should enter into the equation is therefore ,
40
or 567.5 gram-molecules.
Sodium nitrate (NaNOjl has a molecular weight of
85, and according to our formula the number of gram-
molecules of NaNOa should be 0.43 X 567.5 = 244.03,
244.03
and the number of Na\'Os molecules — - — , or 2.87
NaNOj.
Wood pulp, CuHjjOio, has a molecular weight of 362
and the number of molecules of this substance which
June, igi8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
45i
should enter the equation is therefore
o-i5 X 5675
362
or 0.235 ClsH22Oio.
CaC03 (ioo), of which 1 per cent enters into the com-
position of the explosive, should enter into the equation
as
o.oi X 5675 , ■ n n„
, or 0.05675 mol. CaC(J3.
100
In similar manner the moisture (H20 = 18) should
enter as
0.01 X 567.5
— , or 0.315 mol. H>0.
18
After thus having constructed one side of the equa-
tion, the order of proceeding is as follows:
(1) The Na in NaN03 combines to form Na2C03 so
2.87
that — '- - — 1.435 mol. Na-C03 are obtained. It may
2
be mentioned that in presence of sulfur the Na first
combines to form Na2S04 while any remaining Na com-
bines to Na2C03, providing there is sufficient oxygen
present.
(2) All H atoms combine with O to form H20; the
total number of H atoms in above terms being 10.8,
we obtain 5.4 mols. H2Ot
(3) The remaining carbon combines with oxygen to
form C02, providing there is a sufficient amount of
oxygen (as in this case), while any remaining oxygen
remains free.
By analyzing our results up to this point we find:
in I mol. C>Hi(NOi)i 3 C atoms
in 0.235 mol. CuHmOio 3.525 C atoms
Total C atoms 6 . 525
But we have used
in 1.435 mol. NaiCOi 1 +35 C atoms
Remaining C atoms 5 . 090
In the above terms there is a total of 20.275 O atoms
But we have used 9 . 705 O atoms
Remaining O atoms 10 . 570
or sufficient to form, with the remaining C atoms, 5.09
mol. CO2, which leaves 0.39 O atom, equivalent to
0.195 o2.
The probable dissociation of the small amount of
CaCOa entering into the reaction is not considered to
influence the results to any appreciable extent, and this
ingredient is therefore assumed to remain unaltered
as 0.0567 mol. CaC03.
By adding up the N atoms we find 5.87, which is
equivalent to 2.935 Nj.
The complete equation representing the explosion
of the above high explosive is therefore as follows:
C3H5(NQ3)3 + 2.87NaN03 + o.23sC15H22Ol0 +
227 243-95 85.07
o.o567CaCO, + 0.3155H2O = i.435Na,C03 + 5.4H2O
S-67 567
\+ 5.09CO2 + 2.935N2 + o.i95<32 + 0.O567CaC03.
2. FINDING THE GAS VOLUME AT 0° C. AND 760 MM.
Per gram — By comparing the specific gravity of gases
with their molecular weights it has been definitely
established that the volume of any gas molecule is a
constant at o° C. and 760 mm. barometric pressure
and in the following calculations 1 gas volume is assumed
to occupy 22.4 liters at o° C. and 760 mm. As our
object in finding the gas volume at o° is only to obtain
a theoretical value from which we may calculate the
gas volume at t° , i. e., when H20 is gaseous, we must
assume H20 as a gas — even at 0° C. and 760 mm. —
and include same in our calculations.
By summing up the gas molecules formed in the above
reaction we find: 5.4 mol. H20 + 5.09 mol. C02 -+-
2.935 mol. N2 + 0.195 mol. 02, or a total of 13.620
gas molecules from a total of 567.5 g., or 0.53773
liters per gram.
3. calculating the calorific power — The calorific
power (Q) is found in the usual way by subtracting the
sum of the heats of formation of the different ingredients
of the explosive which undergo a change in the explo-
sion, from the total heat disengaged on formation of
the various products of explosion. By applying to
our equation the values found in the above table of
heats of formation, we obtain:
Heat disengaged on formation of
1.435 mol. NaiCOj = 1.435 X 272.6
5.4 mol. HzO = 5.4 X 58.1
5.09 mol. CO* = 5.09 94.3
13.62 gas mol. = 13.62 X 0.545
Heat of formation of
1 mol. CiHs(NOi)» = 1 X 98.9
2.87 mol. NaNOi =2.87 X 111.25
0.235 mol. CuHmOio = 0.235 X 463.4
0.315 mol. HiO = 0.315 X 69.0
391.18cal.
313.74 cal.
479.99 cal.
7.42 cal.
98.90 cal.
319.29 cal.
108.91 cal.
21.74 cal. Total
643490
CaloriEc power (Q) = 643490 cal.
1 134 calories per gram of explosive.
567-5
4. calculation of t° — According to the formula
Q
given above, the temperature of explosion, t = — , ,
in which we have found Q = 643490 cal.
A value for a + bt is obtained from the table given
for specific heats as follows:
1.435 mol. NaiCOi
5.4 mol. HjO
5.09 mol. COi
3.13 mol. (Ni + Oj)
0 0567 mol. CaCOj
1.435 (26 4- 0.0052 I)
5.4 ( 5.61 4- 0.0033 I)
5.09 ( 6.26 4- 0.0037 0
3.13 ( 4.8 4- 0.0006 I)
0.0567 (20 4- 0.0040 <)
37.310 4- 0.007462 (
30.294 4- 0.017820 (
31.863 4- 0.018833 1
15.024 4- 0.001878 (
1.134 4- 0.000227 I
4- bt =115.625 4- 0.046220
— 115.625 + V4 X .04622 X 643490 + 115.62 5 2
2 X 0.04622
t° = 2670. 70 C.
5. CALCULATING THE GAS VOLUME AT t" PER GRAM
of explosive — The gas volume at t° per gram of ex-
plosive is found from Equation 4 to be
Vi = 0.53773 (1 + 0.003665 X 2670.7) =
5.8007 liters per gram.
6. gas volume at t° per cc. : V dt = d X V< — As
the density of this explosive has been found to be
approximately 1.22, the gas volume per cc. at 1° and
760 mm. is
1.22 X 5.8007 = 7.0768 liters.
Example of calculating the strength and efficiency
of an explosive containing nitrostarch as base:
Nitrostarch is a name applied to nitration products
of starch, consisting of a mixture of starch-nitrates.
The formation of a starch-nitrate from starch and HN03
takes place according to the following equation:
452
I III-. JOl RNAL Of INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. Xo. 6
(I 5HI0O6)n + (IHNO,)„ =
(C,Hio_*(NO,)*06_*), + (XH20)„
It will be seen that for each NOa group there is one
HO group eliminated and therefore there is a certain
relationship between the per cent of nitrogen and the
number of X03 groups (AT), which is readily found to
be
X = (9)
1400 — 45N
and
kt 1400X .
N = , v iol
162 + 45X
Assuming an explosive of the following composition:
Per cent
Nitrostarch with 13.05 per cent N 25
Ammonium nitrate 35
Sodium nitrate 33
Sulfur 3
C harcoal 2
CaCO. 1
Vaseline 1
100
According to Equation 9 the number of X03 groups
(X) in nitrostarch, containing 13.05 per cent nitrogen is
162 X 13.05
, or 2.6 X03 groups.
1400 — 45 X 13.05
The chemical formula for above nitrostarch may
therefore be assumed to be C6H7.4(X03)2.602.4 = 279
gram-molecules, which according to our formula should
be 25 per cent of the total gram-molecules entering
279
into the equation, 1. e., = 1108.
0.25
By following the method described above, we obtain
the following terms to represent our formula:
C6H7.<(N03)2.602.4 + 4-85NH4N03 + 4-3NaN03 +
1.04S + 1.85C + 0.033C24H50 + o.nCaC03
As sulfur enters into this composition, this is first set
down as Xa2S04. i. e., 1.04 Na2S04, while the remaining
Na is next combined to form Na2C03, i. c,
4.3—2 X j. 04 = ixi Na;C03 By following the
2
methods used in the former example, the complete
equation is as follows:
C6H7.J(N03)2.602.4 + 4-8sNH4NO„ + 4-'3NaNO, +
1.04S + 1.85C + o.033C24H5o + o.nCaC03 = 1.04
Na2SO< + i.nNajCO, + i4.225H20 + 7-S32C02 +
0.3855O0 + 8.3N, + o.nCaC03.
There are 30.44 gas molecules from 11 10 grams of
30.44 X 22.4 0 _
explosive, or - — = 0.6143 hter at o C.
1 1 10
and 760 mm. per gram.
In order to calculate the calorific power of this ex-
plosive, the heat of formation of a starch-nitrate, cor-
■ • 1 ing to above formula must be known. Berthe-
5 the heat of formation of a starch-nitrate as
follows:
225.9 — l5 u- n which 225.0 is the heat of formation
of starch (C6Hio06) and a represents the number of
N03 groups which have taken the place of HO groups.
The heat of formation of the above starch-nitrate is
then i
225.9 — '5 X 2.6 = 1S6.9 cal. for 270 grams.
By carrying out the calculations as in the former ex-
ample we obtain the following values:
Calorific power = 1288016 cal. or 1170 cal. per gram.
t" = 26670 C.
Gas volume at t" per gram = 6.634 liters.
This explosive may readily be packed to a density of
1.2, so that the gas volume at t° per cc. is 1.2 X 6.634 =
7.9608 liters, and its efficiency should therefore be
higher than that of the explosive cited above.
Both of the above explosives have contained a suf-
ficient amount of oxygen to oxidize all the carbon to
C02. In calculating t°, etc., of explosives containing
a deficiency of oxygen, a slightly modified method 1
must be used in completing the equation representing
the explosion, and the following example is given to
illustrate same.
Assuming the explosive to have the following com-
position:
Per cent
Nitrostarch with 12.75 per cent N
This explosive may be expressed in the following
chemical terms:
C6H,.5(X03)2.502.5 + Ba(XO:), + o.o4C24H50
274.5 261 13.5
Summing up we find these terms contain
9.5 H atoms 1.0 Ba atoms
6.96 C atoms 16.0 O atoms
4.5 N atoms
Ba(,X03)2 may be assumed to split up in BaO +
X2 + 2-502. of which the BaO immediately combines
with C02 to form BaC03.
9.5 H with 4.75 0 forms 4.75 mol. H20.
4.5 N atoms are equivalent to 2.25 mol. Ni.
There remain now 16 — 7.75 = 8.25 O atoms and
(6.96 — 1) = 5.96 C.
As the remaining C and O atoms are assumed tol I
combine to form C02 and CO, the number of COi I
molecules are found by subtracting 5.95 from 8.25, oml
2.30 C02; and the number of CO molecules is againU
obtained by subtracting 2.30 from 5.96. i. e., 3.66 CQBf
molecules. The complete equation representing thJl
explosion of above explosive is therefore:
C,Ht.5(N0,)2.60..s + Ba(XOs). + o.04C2,Hso =J I
BaC03 + 4-75H20 + 2.25X5 + 2.30CO2 + 3.66CO |
By now following the described methods for cal
lating calorific power. t°, etc., the following values
obtained:
Gas volume at 0° C. and 760 mm. = 0.5288 liter per
gram.
Calorific power = 816 calories per gram.
I" = 25S20 C.
Gas volume at /° and 760 mm. = 5.5259 liters per gram.
Assuming that the CO formed reacts with H20 to
form C02 + II... what results would this have on the
gas volume at /°?
The equation would thus be:
- Ba NO,)i + o.o4Cj,05l> =
BaC03 + 1.0SH.O + 2.25NJ + 5-96CO; + 3.66H1
The follow-:: re then obt..
Gas volume at oc and 760 mm. = 0.52SS liter per gram.
June, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY 453-,
Calorific power = 855 cal. per gram. has been developed on a laboratory scale. A de-
t" = 2592° C. scription of this procedure together with a certain
Gas volume at (° = 5.552 liters per gram, or practically amount of closely related considerations forms the
the same as in the reaction above. subject matter of this paper.
When sulfur is present in explosives containing a
deficiency of oxygen, a part of it combines to form a Review of previous nitration methods
sulfide (H2S, Na2S, etc.) while the remaining sulfur is In 1856, J. Barlow1 attempted to nitrate cymene
oxidized and combines with the metal to form Na2S04, by dropping the cold hydrocarbon into strong nitric
etc. No definite rule can be made as to what part acid cooled with ice and salt. He obtained by steam
combines one way or the other, the proportions prob- distillation of the product a large quantity of an oil
ably having some relation to the oxygen deficiency. lighter than water. By reduction he obtained only a
The following table gives the calculated l° and gas small quantity of material soluble in hydrochloric acid,
volume at t" per gram of some of the most common The greater portion consisted of a light oil which,
explosives: boiled at 1 75 ° and was undoubtedly unchanged.
Gas volume nvrnprip
Explosive t° at 1° per gram *• J< mcuc.
Nitroglycerine...... 3158° c. 8.8328 liters Landolph2 about twenty years later stated that
Trinitrotoluene (TNT) 2217° C. 6.764 liters ... . , ., . . , , . , .
Picric acid 2599° c. 8.7270iiters nitric acid (density 1.5) cooled with ice and salt did
Tetranitromethyl-amline ("Tetryl") 3126° C. 9.81 liters „. . ,. ... TT .....
Tetranitro-aniiine (TNA) 3238° c. 10.55 liters not react at all with cymene. He used nitric acid
Nitrostarch with 12.75 per cent nitrogen. .. . 2205.7° C. 8.168 liters Manci + ir T .\ ~+ Tr° +^ ^«° „~A G~'„\ 1 4-1
Nitrostarch with 13 per cent nitrogen 2277° c. 8.28 liters (density i. 4) at 1 5 to 20 and finished the reaction
Nitrostarch with 13.47 percent nitrogen. . . . 2415.4° C. 8.4937 liters a£ 4.0° tO ?0°
Mixture of **■ 0 ■
?s:73 perclnf Ammonium nitrate 2310° c. 8.2622liters Fittica3 in the same year nitrated cymenes from
66 plr cent Irnmonium nitrate. .'. 2195° C. 8.3493 liters Vari°US SOUrCeS according tO the method of Landolph
44.77 per cent tnt „,--.„ <, ,,,*,•. and obtained products which were volatile with steam
55.23 per cent Ammonium nitrate 2122° C. 8.3315 liters .
58.6 per cent tnt and which he called nitrocymene. A year later he4
41 .4 per cent Ammonium nitrate 2146° C. 7.974 liters , r ,, ,. . , . .
92 per cent Nitroglycerine , gave the following directions for nitration: 20 g.
8 per cent Nitrocellulose (12 per cent N) 3208° C. 9.0424 liters , . . . - .. . ', ,,
cymene were dropped into 150 to 200 g. of nitric acid
That certain relations exist between "strength" of (density 1.4) heated to 400. After the addition of a
explosives and their calculated gas volume at t" per few drops of cymene, the mixture was cooled until the
gram as calculated by this method, has been proved, vigorous reaction had ceased. He steam-distilled
for instance, by results of Trauzl tests. Although the the nitration product and then redistilled this in
latter are subject to some errors, due partly to impuri- vacuo. He stated that his analysis showed contamina-
ties in the lead and partly to execution of the test, an tion with cymene.
approximate idea as to the number of cc. expansion Widman and Bladin° repeated the work of Landolph
that will be effected by 10 g. of a brisant explosive is and pittica and found that the nitrocymene which
obtained by multiplying the calculated gas volume at they had obtained contained only very little nitro-
/ per gram by 37.58. cymene. It consisted principally of a mixture of
Applying this factor to some of the explosives listed cymene and ^tolylmethylketone. They attempted to
above we obtain: Calculated Found nitrate by dropping cymene into a mixture of sulfuric
Explosive Cc. Cc. acid and the calculated amount of nitric acid cooled
TNTgyCCrme^ '.'. 253 235 by a freezing mixture. By steam distillation they
"Tetryr'd 368 375 found that a large part of the cymene had been un-
Jna-- •••■-■■■ ■ ••■• 395 415 attacked and that another part had been nitrated to
Nitrostarch (12.75 per cent N) 306 305 _ r
,.,,,,. derivatives higher than the mono. Soderbaum and
This method of calculating strength and efficiency ,T.., » , ■ . . .. . „.-, , ..
6 5 -^ Widman6 admitted that Widman s earlier attempt was
of high explosives is often useful to the explosives & ^^ They then reported a method which had
chemist in making up a formula for an explosive to be been fmmd satisfactory for the nitration of certain
used for a certain class of work or to take the place of compounds which were easily oxidized. The calcu-
another explosive. A study must at the same time ]ated amount of ^^ add mixed with Qne and Qne
be made of the apparent densities of various ingredients ha,f timeg .^ weight of sulfuHc add wag slowly ad,K.(1
as well as of the effect of the latter on 'the apparent .. „ , , -,i. . t., + .„+...„
t to the cymene cooled with water. the temperature
density of the explosive. was WM between 2Q° and 2-° at first but was finally
Allen-town, Pennsylvania . -
allowed to rise to 40 . In addition to the nitro-
PARA CYMENE. I— NITRATION. MONONITROCYMENE, cymene, they obtained by steam distillation large
1-CH3, 2-NO:, 4-CH(CH3jo' amounts of unattacked cymene and p-tolylmethyl-
Hy c. E. Andrews ketone. By fractional steam distillation they ob-
Received May 9, 1918 taincd a .sample which gave a fairly gciod analysis for
Although many methods for the preparation of nitrocymene.
mononitrocymene from />-cymene have appeared in 1 Ann., 98 (1856), 245.
the literature, it is evident from the reports themselves 6 (1873), 937.
and also from the present work that the yields were , ^ ' 172 ('|87'4) 303
very low in every case. A method giving good yields <■ iter , 19 (1886), 583.
1 Published by permission of the Secretary of Agriculture. * Ibid., 21 (1888), 2126
454
THE JOURNAL OF INDUS! KIM. AND ENGINEERING CHEMISTRY Vol. 10, No. 6
G. Sumnov1 discarded Fittica's method of nitration
as unsatisfactory. He mixed glacial acetic acid solu-
tions of cymene and nitric acid and kept the tempera-
ture down by continuous cooling with ice.
METHOD OF PREPARATION
nitration— One-half mole of />-cymene was added
to an equal weight of sulfuric acid (density 1.84) with
stirring and the temperature kept at 0° or below by
means of a bath of ice and salt. This required about
15 min. A well-cooled mixture of 50 g. of nitric acid,
density 1.42 (no per cent of theoretical amount re-
quired), and 105 g. of sulfuric acid (density 1.84) was
then added drop by drop to the sulfuric acid solution
of the hydrocarbon, keeping the temperature at o°
or below and stirring the mixture efficiently. It re-
quired about s hrs. for this operation on account of
the large amount of heat produced. The reaction
proceeded very smoothly without the evolution of
oxides of nitrogen and at the end the mixture became
reddish brown in color and about as viscous as thick
molasses. After all of the mixed acids had been
added, the reaction was allowed to proceed for from
15 to 30 min.
purification of the nitration products — The
mixture was then poured into an equal volume of cold
water and the oily nitration product allowed to collect
on top of the dilute acids. The two layers were
separated and the oily one washed with cold water
in which it sank. It was washed further with dilute
sodium hydroxide solution to remove the last trace of
acids, and finally with more cold water. In this manner
a dark reddish brown product was obtained which
weighed about 85 g. after drying with calcium chloride.
distillation— This oily product was then either
distilled with steam or in reduced pressure. When
distilled with steam, about 8 g. of an oil came over at
first which was lighter than water. After this the
greater portion, about 65 g., came over as a light
yellow oil heavier than water and having a strongly
aromatic odor. There remained in the distilling flask
a brown viscous mass (about 10 to 12 g.) which became
quite hard on cooling.
When distilled in an atmosphere of 3 to 5 mm.
pressure the first product came over at about 9s0 and
continued distilling until the temperature reached
about 120°. The greater portion boiled at 1 1 5 to
1160. When the temperature reached 1200, the rise
was very rapid and therefore the distillation was
stopped. A residue remained in the flask similar
to the one above. The product obtained by distilla-
tion in vacuo was not so pure as by the steam distilla-
tion since the former product contained the low-boil-
ing fraction which was difficult to remove by fractiona-
tion.
light oil from steam distillation — O. Widman
and J. 0. Bladin2 in investigating methods of nitra-
ting cymene proposed by Fittica2 and Landolph2
found that their product contained only very little
mononitrocymene, but consisted almost entirely of
unchanged cymene and />-tolylmethylketone. It was
■ Chem. Zcnlr . 1887, 752, Zurn. russfc. fit. ckim.. 19, I, 118-22.
1 hoc. cit.
therefore thought that this light oil might contain
some of this ketone together with cymene and nitro-
cymene. In order to free the oil from nitrocymene,
it was reduced with tin and hydrochloric acid and
steam-distilled from acid solution. Four grams of a color-
less oil were obtained, all of which distilled near 175°,
showing it to be essentially cymene. The reduction
mixture was then made alkaline with sodium hy-
droxide and again steam-distilled, which gave 3 g.
of an oil which formed a crystalline solid in con-
centrated hydrochloric acid with the liberation of
heat, and entirely dissolved on dilution. This was un-
doubtedly an amine corresponding to the nitrocymene
present. Therefore, the original 8 g. of light oil con-
sisted of 4 g. of cymene and 4 g. of nitrocymene
(equivalent to 3 g. of aminocymene). Working with
this small amount of material it was impossible to
recognize any ^-tolylmethylketone.
tarry residue — Landolph,1 Fittica,1 and Gerich-
ten2 have reported a solid mononitrocymene which
they obtained from the tarry distillation residue by
recrystallizing it from alcohol. In a later paper
Gerichten3 shows that the so-called solid nitrocymene
was soluble in potassium hydroxide and from this
solution p-toluic acid precipitated on acidification.
A. F. Holleman4 stated that this product had the
formula C9H8NO2 and therefore was not nitrocymene,
and that it was changed by sodium hydroxide and
sulfuric acid to />-toluic acid. The tar obtained in
these experiments showed the following characteristics:
It gave a very strong test for nitrogen but the sub-
stance obtained from this tar by two recrystalliza-
tions from alcohol solution was nitrogen-free. This
recrystallized substance, as well as the original tar,
was insoluble in boiling alkali of any concentration.
The class of compounds indicated by these peculiar
properties is not plain, and since it is evidently not a
higher nitration product of cymene, it was thought
not to be important enough to demand further in-
vestigation at this time.
heavy oil from distillation — It was evident that
this oil might contain the same compounds as the light
oil mentioned above. It might also contain a mixture
of the two isomeric mononitrocymenes. This de-
creased the possibility of purification by distillation.
Fractionation at ordinary pressures was prohibited
on account of the decomposition which took place.
Under a pressure of 3 to 5 mm. practically all of it
distilled at 100 to 1200, which gave a very narrow
limit for fractionation. A fraction was obtained,
however, boiling at 115 to n6° and 6 to 7 mm.
pressure, which was taken for analysis.
Found, 7.75 and 7.9 per cent nitrogen
Calc. for CuHuNOi, 7.82 per cent nitrogen
From these results it was evident that this oil was very
nearly pure mononitrocymene. This fraction con-
stituted practically the total yield. In this condition
it appeared as a li s^ H t yellow oil heavier than water
with a strong, not unpleasant, aromatic odor.
1 hoc. cit.
< Btr., 10 (1877). 1251.
> Ibid., 11 (1878), 1092.
« Chem. Zenlr.. 1886. 722; Rec. (rot. ekim., 5. 184-86.
June, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Previous investigators have described their nitro-
cymene as possessing these same physical charac-
teristics although no analyses have been reported
which agree so well with the theoretical. Soder-
baum and Widman1 gave 7.49 per cent as the result
of the nitrogen analysis. Fittica1 reported 68.38 per
cent carbon and 7.94 per cent hydrogen as the result
of the analysis of the product he obtained. The
theoretical hydrogen is 7.26 per cent and the carbon
67.03 per cent. The question of the presence of
the two isomers will be taken up later.
INVESTIGATION OF THE POSSIBLE PRESENCE OF THE
TWO ISOMERIC MONONITROCYMENES
reduction — As far as could be determined there
were no reports in the literature concerning the ex-
istence of two isomers of mononitrocymene except
the liquid and the solid isomers reported by Landolph1
and Fittica.1 It has been proven, however, that the
' solid variety was not nitrocymene.1 The liquid com-
pound has been proven to have the constitution
CH3(i)C6H3N02(2)CH(CH3)2(4) by oxidation to o-nitro-
^-oxyisopropyl benzoic acid.2 Although it has been
reduced to the corresponding amine, no derivatives
have been reported which would characterize it as a
particular one of the isomers.3 Lloyd4 has reported
the physical characteristics of several derivatives of
the amines prepared from carvacrol and thymol.
Wallocb6 prepared the derivatives of an amine ob-
tained from carvoxime. Goldschmidt6 reported the
characteristics of an amine obtained from isocarv-
oxime. Widman7 reported on an amine from cuminol.
As the constitution of all these was definitely estab-
lished it was decided to convert the nitro compound
into an amine and compare its derivatives with those
reported above. Accordingly, the whole portion (65
g.) of the heavy oil obtained from the steam distilla-
tion was reduced with tin and hydrochloric acid.
After the reduction was complete, there was no oil
visible which was insoluble in hydrochloric acid.
Upon distillation, however, about 3 g. of a light oil
came over. By making the solution alkaline with
sodium hydroxide and steam-distilling again, about
54 g. of a colorless oil came over which floated on
top of the water. The reduction was also carried out
with iron and hydrochloric acid in the same way that
nitrobenzene is reduced to aniline commercially.
The results were the same in both cases except that the
separation of the products is not affected by distilla-
tion from acid and alkaline solution, as is the case
when an excess of acid is used in the reduction with
tin. This was carried out separately with the same
results as above.
light oil from distillation of acid solution —
By collecting the light oil from several distillations,
enough material was obtained to carry out a fractiona-
tion. About two-thirds of the whole boiled near 175°
(cymene) and the remainder boiled between 2100
' Loc. cil.
' Soderbaum and Widman. Loc. cil.
• Harlow. Loc. cil.. Soderbaum and Widman, Loc. cil.
'Bar., SO (1887), 1262.
• Ann., 279 (1894), .168.
• Btr., 26 (1893), 2086.
' Ibid., 16 (1882), 166.
and 2220. This latter fraction had a pleasant odor,
and from its boiling point was thought to be p-to\y\-
methylketone. By further fractionation the greater
portion of it boiled from 218 to 2210. The boiling
point of />-tolylmethylketone has been reported over
quite a large range. Michaelis1 gave 217 °, Claus2
2200, and Widman and Bladin3 222.5 to 2240. The
dibrom derivative was made according to Michaelis,
and was found to melt at 99.5°, while Michaelis
reported ioo° and Widman and Bladin gave 990
as its melting point. The oxime was prepared
according to R. Meyer4 and melted exactly at 88°
as reported by Meyer and also by Widman and Bladin.
Analysis of the oxime showed the following per-
centages of nitrogen:
Found, 9.13 and 9.17 per cent nitrogen
Calc. for C1H11ON, 9.40 per cent nitrogen
From these results it seemed very probable that the
fraction of light oil boiling between 2100 and 2220
was principally ^-tolylmethylketone. The actual
amount of ketone produced during any one nitration
was about 1 g., which corresponded to a yield of 1.5
per cent. In many of the earlier reported nitrations
of cymene large amounts of ketone had been pro-
duced.6 This ketone together with the small amount
of cymene constituted the impurity in the nitro-
cymene as obtained after distillation.
OIL FROM DISTILLATION OF ALKALINE SOLUTION
Lloyd3 gave 241 to 242 ° as the boiling point of the
amine (1 -methyl, 2-amino, 4-isopropyl) obtained from
carvacrol, and 2300 for the one from thymol (i-methyl,
3-amino, 4-isopropyl). Walloch3 gave 240 to 241 °
for the 1,2,4-amine. Semmler6 gave 118 to 1210
at 13 mm. pressure for the same one. Barlow3 gave
2500, but did not attempt to say which amine it was.
When the oil from the alkaline distillation was frac-
tionated, it began to boil at 230 ° and then the tem-
perature rose rapidly to 238°. Between 23 5 ° and
238 ° almost all of it distilled. Nitrogen analyses
were made on this fraction which constituted almost
all of the yield.
Found, 9.44 and 9.47 per cent nitrogen
Calc. for CwHhNHj, 9.39 per cent nitrogen
These results showed that the total 54 g. of oil was
very pure aminocymene and therefore represented
a yield of 80 per cent, calculated on the cymene used.
As high as 85 per cent was obtained but the
lower yield was the most common. The yield of the
nitro compound was therefore at least equal to this.
Experiments showed the reduction to be practically
quantitative. Both the hydrochloride and the sulfate
were prepared and appeared as bright, lustrous plates.
The hydrochloride melted at 207° as given by Walloch3
and Goldschmidt3 for the 1,2,4-amine. The acetyl
derivative was prepared by boiling one mole of the
amine with two moles of glacial acetic acid under a
reflux condenser for 8 to 10 hrs. On cooling, the
mixture solidified to a white mass which was re-
■ Bcr., 16 (1882), 185.
'Ibid., 19 (1886), 234.
» Loc. cil.
' Ann.. 219 (1883), 234.
' Widman and Bladin, Loc. cil.
• Bcr., 26 (1892), 3352.
456
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 6
crystallized several times from dilute alcohol. Pure
white crystals were obtained which melted at 71 °.
Goldschmidt reported 71° as the melting point of the
acetyl compound of the 1,2,4-amine and Walloch
gave 72° for the same compound. Goldschmidt
pointed out that the melting point of 115° reported
by Lloyd1 was an error. Lloyd gave the melting
point of the corresponding 1,3,4-compound as 112.50.
In order to determine whether or not the boiling range
230 to 2380, which was between that of the two
amines, as reported, indicated the presence of both
isomers, the acetyl compound of the lowest fraction
and of the highest fraction were prepared separately.
Both compounds melted sharply at 710, which would
not have been the case if both isomers had been
present. The benzoyl compound was also prepared
by the Schotten-Baumann reaction and found to melt
at 96. 50, while it was reported at 102° by Lloyd.1
Analysis showed that the compound was very pure
and since Lloyd gave no analysis, it was assumed that
his melting point was incorrect.
Found. 5.36 and 5.43 per cent nitrogen
Calc. for CitIIibON, 5.53 per cent nitrogen
The melting point of the corresponding isomeric com-
pound could not be found in the literature. Since
all of the derivatives melted very sharply and from
the fact that the acetyl compounds from the two
fractions farthest apart melted at the same tempera-
ture, there seemed very little chance for the presence
■ 'I two isomers. The melting points also agreed very
well with those reported for the 1,2,4-isomer which
pointed to the fact that this was the isomer formed.
IDENTIFICATION OF THE MATERIAL SOLUBLE IN
sodium hydroxide — The sodium hydroxide solution
obtained as described in the purification of the nitra-
tion product was investigated in order to determine
the amount and character of the acids formed by any
oxidation of the side chains of the />-cymene. It was
boiled with decolorizing charcoal and filtered, the
Bltrate concentrated to a small volume and then
made acid with hydrochloric acid. By this method
no precipitation took place nor could any acid be ex-
tracted with ether when the alkaline solution from a
single nitration was -used. By employing the com-
bined solutions from several nitrations a small amount
of an acid was obtained which gave, after two crystal-
lizations from boiling water, very light yellow crystals
melting at 1 79 ° and giving a very slight test for
nitrogen. By again decolorizing and recrystallizing,
these crystals became colorless, soluble in alkali, and
gave no test for nitrogen. Melting point, 1800. The
compound is />-toluic acid. No statement has been
found in the literature indicating that the products
of nitration have been investigated in this way. The
small amount of acid formed showed that the oxida-
tion in this direction was almost negligible.
DISCI ssion 01 u 1 1 HODS
Although 1111 yields were given in any of the
. "i miration reported in the literature,
it was evident that very little nitrocymene was
obtained. In repeating the work of Soderbaum and
Widman,1 it was found that very low yields were
given when the reaction was carried out from 20 to
2 50, but when it was kept down to zero, there was a
marked increase. When nitric acid (density 1.42 to
1.5) was used alone at the temperature recommended
by Landolph1 and Fittica1 '20 to 500) low yields
were also obtained and there was almost no reaction
at 0°. Hence the presence of sulfuric acid and a
low reaction temperature became important conditions.
The solution of the hydrocarbon in a suitable solvent
previous to nitration proved to be a very important
factor. Petroleum ether, glacial acetic acid, and
concentrated sulfuric acid gave increasingly good
results as solvents, in the order named. No mention
of such a procedure could be found in the literature.
Although Sumnov1 nitrated in a solution of acetic
acid, his yields were low, as shown by a series of ex-
periments in which glacial acetic acid was substituted
for concentrated sulfuric acid. Acetic anhydride in
varying amounts was also added to the acetic acid to
take the place of the sulfuric acid, but in every case
there was practically no nitration. Some of the
earlier investigators2 let the cymene drop into the
nitrating acid but it was found that by reversing this
order, that is, by letting the acid drop into the cymene,
much better results were obtained. A slight excess
(no per cent of the theory) of nitric acid (density
1.42) mixed with about twice its weight of sulfuric
acid (density 1.84) formed the best nitrating mixture.
Practically no time was required to complete the
reaction after the acids had all been added. All of
the previous investigators neglected to observe at
least one of these important factors and consequently
did not obtain good yields of mononitrocymene.
In most cases several factors were not taken into
consideration, which accounted for the very poor
yields in those particular cases.
It is to be noted that one of the possible substitution
products is produced and the other is not formed in
any appreciable amount. The directing groups in-
volving this phenomenon are the methyl and the
isopropyl. The same nitro compound was produced
under all of the widely varying conditions used in the
course of the investigation, so it appeared that the
other isomer could not be prepared by direct nitra-
tion.
SI MMARY
i — A method for the nitration of p-cymene is de-
scribed which has given yields of mononitrocymene
(i-CHj, 2-NO,, 4-CH(CH,)j) as high as S5 per cent.
Wry small amounts of />-toluic acid and />-tolyl-
methylketone have been shown to be produced during
nitration.
3 — The nitrocymene has been reduced to the corre-
sponding amine. This reaction has been made to give
theoretical yields.
4 The amine, and hence the nitro compound, has
been shown to consist of only the 1 .2.4-isomer.
Color Investigation Laboratory
Buusaq ov CavaastT
D. C.
I
: Landolph. /.■>. , i: FittM
Ibid Widman and Bladin. Ibid.
June, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
457
EFFECT OF ACETYLENE ON OXIDATION OF AMMONIA
TO NITRIC ACID1
By Guy B. Taylor and Julian H. Capps
Received May 13, 1918
In experiments on the oxidation of ammonia to
nitric acid carried out in the laboratories of the Bureau
of Mines, some attention has been given to the question
of the effect of such impurities as normally occur in
ammonia gas derived from commercial sources. It
has been found that high-grade ammonia liquor de-
rived from carbonization of coal contains no deleterious
impurity whatever and that conversion efficiencies of
95 per cent are easily obtained with platinum as
catalyzer.
An important source of ammonia is calcium
cyanamide. Since this material is manufactured from
carbide, small amounts of which remain in the finished
product, the ammonia gas derived from it almost
always contains acetylene. The object of the experi-
ments described in this paper has been to determine the
effect of acetylene in the ammonia gas upon catalytic
oxidation with platinum.
EXPERIMENTAL
The oxidizer or converter consisted of two rectangu-
lar aluminum boxes, 6 by 3 by 12 in., bolted together
^L.
dJTTHl CD O O ILU /111)
UD-pU-Ur-piiij
with a platinum gauze between (Fig. I). The gauze
was crimped into two pieces of aluminum sheet at
either end and held between "Janos" gaskets. Heavy
1 Published by permission of Director of U. S. Bureau of Mines.
cables connected the aluminum electrodes to a low-
voltage transformer which furnished the current for
heating the gauze. Ammonia mixed with air was ad-
mitted at the top and the reaction products issued at
the bottom. A perforated aluminum plate was fixed
5 in. above the gauze to serve as a baffle for securing
uniform distribution of the gas flow through the gauze.
The mica window shown in the figure afforded an un-
obstructed view of the entire gauze surface.
The ammoriia-air mixture was obtained by bubbling
air through two metal drums in series containing pure
ammonia liquor of such strength as to secure a suitable
concentration of ammonia in the mixture. The feed
mixture then passed into an empty 50-gal. drum to
prevent pressure fluctuations and then through 10
ft. of rubber hose to the top of the converter. The
arrangement of the rest of the apparatus has been
previously described.1
Acetylene, with its accompanying impurities, was
generated in a Kipp apparatus from high-grade calcium
carbide and water, washed through water, and care-
fully measured. It was passed into the ammonia-air
mixture in the rubber hose line connecting the ammonia
saturator to the converter, about 8 ft. from the latter.
The acetylene-bearing gas came into contact with iron
only through a T-connection and short nipple.
The composition of the gas entering the oxidizers
was calculated from the rates of flow of the acetylene
and of the air through the ammonia vaporizer, together
with analysis of the ammonia-air mixture for ammonia.
The acetylene present in the gas could thus be de-
termined more accurately than by analysis at the small
concentrations employed.
The gauze used in these experiments was made of
pure platinum wire 0.003 in. diameter, 80 wires to the
linear inch. Platinum is never fully active when first
placed in the converter but is "activated" by the
reaction itself so that the conversion efficiency2 rises
with use, increasing from day to day until the maximum
efficiency is reached. Gauzes vary widely in the time
required to reach their full activity. The particular
gauze used in these experiments reached its full
activity unusually quickly. In Table I are presented
results showing the performance of this gauze with
pure ammonia. The converter was operated several
hours continuously each day over the 5-day period.
Table I — Tests op Pure Platinum Gauze from Baker * Co., 80 Mesh,
0.003 In. Wire, Using Pure Ammonia
NHi
Cu. ft. ■ in air
Test of air mixture Yield
Date No. per hr. Amperes Per cent Per cent
Pph 6 341 175 160 9.10 92.4
££' 6 i 342 180 135 9.58 93.2
Peb 7 343 170 160 8.40 93.5
rrth 8 344 170 150 8.78 M '•
££• I : 345 170 150 8.73 96.0
Feb' 8 "::::: 346 170 130 9. so 94.6
V?' 8 347 170 130 9.80 94.4
l± I i 348 180 160 7.48 95.0
tvh 9 349 180 160 7.49 94.0
£!h" 11 350 175 150 8.50 94.8
Feb-:!!::::::::::: If? m iso 8.55 94.3
Average yield 9*.6 per cent, excluding Nos. 341 and 342.
Ammonia escaping oxidation, 0.3 per cent.
The result of the addition of acetylene is shown in
detail .n Table II. The poisoning effeel at com
■ Taylor Cappi and Coolidge, Tll.s JOURNAL, 10 (1918), 270.
• The vacuum bottle method was need in determining efficiencies,
see Taylor and Davis, This Journal, 9 (1917), 1106.
45»
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. ic. No. 6
Table II-
— Effbci
S OF
AcBTYLEN
■ on Yield,
170Cu. Ft Aih pbs
Intak
i Gas
NHi
CiH,
Yield
1 1 1
Am]
- Per
Per
Per
Map of
Date
Ti
No.
erea
cent
cent
cent
Gauze
March
2
S68
165
7.50
0.0
96.0
March
.'
169
165
7.50
0.0
96
5
March
4
io'
Ml
150
8.0
0.0
Clear
March
4
10
30
150
8.0
1.12
March
4
10
32
150
8.0
1.33
■-,. <■ Map A
Fig
II
March
■1
10
}8
150
8.0
1.54
See Map H
Pig
II
March
4
10
53
ISO
8.0
0.53
March
4
11
20
150
7.9
0.21
See Map C
Fig
II
March
4
11
45
ISO
7.8
0.13
March
4
12
10
150
7.7
0.13
Clear
March
4
12
22
370
155
7.7
0.13
7i
X
Clear
March
4
12
.'7
371
155
7.7
0.13
75
i'
Clear
March
4
1
00
155
7.7
0.04
Clear
March
4
2
00
155
7.6
0.04
Clear
March
4
2
20
155
7.5
0.0
Clear
March
4
2
23
155
7.5
0.21
See Map D
Fig
II
March
4
2
45
155
7.5
0.13
Clear
March
4
2
50
372
150
7.5
0.0
90
4
Clear
March
4
2
55
373
150
7.5
0.0
92
5
Clear
i
Map A
MapC
MapJJ
FigJL
Ammonia
Escap-
Intake Gas
ing Oxi
NHj CiH.
Yield
dation
Test
Am
Per Per
Per
Per
Date
Ti
No.
teres
cent cent
cent
cent
Remarks
March 5
10
30
... 0
Start
March 5
1
00
374
140
9.35 0
92.6
0.7'
March 5
1
05
375
140
9.35 0
92.5
0.7
March 5
3
35
376
150
8.92 0
92.2
0.6
March 5
3
38
377
150
8.92 0
92.5
0.6
Shut down 3 : 4
March 6
9
10
... 0
Start
March 6
10
40
378
150
8.80 0
94.2
0.6
March 6
10
43
379
150
8.80 0
95.0
0.6
March 6
2
53
380
150
9.06 0
93.5
0.6
March 6
2
56
381
150
9.07 0
94.0
0.6
Shut down 3 p.m
March 7
9
10
... 0
Start
March 7
11
05
382
io5
7.40 0
95.9
March 7
11
08
383
165
7.43 0
95.0
March 7
1
40
7.0 0.12
March 7
2
30
385
160
6.70 0.09
69.0
2.5
March 7
3
19
386
165
6.40 0.16
46.5
5.4(0)
Shut down 3 : 2.
March 8
10
40
... 0
Start
March 8
11
25
387
160
7.79 0
9K4
March 8
11
45
... 0.04
March 8
12
15
388
150
8.05 0.05
92.8
0.5
March 8
1
10
389
150
8.05 0.04
85.6
1.5
March 8
3
OS
390
150
7.52 0.05
87.3
1.1
March 8
3
12
... 0
March 8
3
19
39 i
150
7.54 0
91 '. i
6!7
March 9
9
05
... 0
Start
March 9
9
57
392
150
8.18 0
9i!6
6.7
March 9
10
00
393
ISO
8.21 0
92.0
0.7
March 9
1
55
394
125
9.42 0
89.7
0.8
Shutdown 4 : \i
March 9
1
58
395
125
9.38 0
89.4
0.8
P.M.
March 11
9
30
... 0
Start
March 1 1
11
00
396
160
7.15 0
92! 3
0.6
March 11
2
50
397
140
9.32 0
93.6
0.5
March 1 1
2
53
398
140
9.32 0
93.4
0.5
Shut down 4 : M
March 1 2
11
00
... 0
Start
March 12
11
43
399
i io
10.75 0
90.6
6.7
March 12
11
46
OKI
llo
10.75 0
89.6
0.7
March 12
.'
■is
■101
120
9.50 0
91.7
0.5
March 12
_'
«
40.'
120
8.70 0
93.8
0.5
March 1.'
4
15
403
130
10.35 0
92.4
0.6
March 12
4
20
404
130
10.50 0
92.6
0.6
Shut down 4 2.
March 13
9
10
... 0
Start
Marco 13
10
22
... 0.03
March 13
10
30
10
i25
10 IS II m
93^6
6.6
March 13
11
00
10..
125
~, .in o in
90.0
0.6
11
V
407
1 Si
9.40 0.03
89.4
0.9
M u .lil.
.'
25
408
150
8.37 0.03
88.4
1.2
March 13
2
45
109
1 io
8.37 0.03
86.6
1.2
March 13
3
37
410
146
8.40 0.025
87.3
March 11
9
10
... 0
Start
March ii
9
15
... 0.08
March 1-1
10
08
4ii
140
8.72 0.10
68^3
2l2
March 11
10
15
412
1 io
8.73 0.10
68.7
2.4
March 14
11
;.(
413
140
8.14 0.09
77.5
March L4
1
08
414
150
; 'i.' o io
63.0
2^9
March 14
1
16
... 0.02
March 14
1
33
■lis
iso
8 07 o 02
8i!4
i'.o
March 14
2
43
4K.
145
8.70 0.02
87.0
1.0
March 14
2
45
117
145
8.75 0.02
88.7
0.8
0
cu.
. ail An
increase <>( ve
in ii v i.l this ord
CBUSeS ., .1
sen
mull
ii. on en i *■
mmon
11 of lesi.
th. in .' per cent.
tions above 0.2 per cent in the mixture is immediately
optically apparent on the gauze. Black inactive areas
appeared which are shown by maps of the gauze.
If the electric current is shut off, when running on
pure ammonia, the gauze remains dull red from the
heat of reaction. Under the same conditions with
0.1 per cent acetylene black areas immediately ap-
peared tending to spread over the entire gauze. These
areas are difficult to clear up and it is our opinion that
oxidizing ammonia from sources which may even
occasionally contain acetylene, would give unlimited
trouble from development of black spots, which could
not be cleared up readily without electric heating.
No black area appeared after March 4. The tests
showed that the yield was a function of the concentra-
tion of acetylene and that when the acetylene was
shut off the yield immediately rose to within 3 or 4
per cent of its original value, but required many hours
running on pure ammonia to restore it completely.
A gauze that has been rendered active by oxidizing
pure ammonia has a distinctive gray appearance to
the naked eye. Under the microscope the wires
appear to be covered with platinum sponge. Examina-
tion of the gauze at the conclusion of the tests on
March 4 showed an entirely different appearance.
It had a speckled crystalline appearance to the naked
eye and the wires appeared rough but shiny under the
microscope. Re-activation with pure ammonia re-
turned the gauze to its original gray. At the con-
clusion of the experiments on March 14, the gauze
was less different from the gray than the previous
examination had showed.
REMOVAL OF ACETYLENE FROM AMMONIA
These results show so conclusively the poisoning
action of acetylene or its accompanying impurities
that some method for its removal seems imperative
if cyanamide ammonia is to be successfully oxidized
with high efficiency.
Several methods for accomplishing this result suggest
themselves. Removal by scrubbing the gas with
ammoniacal cuprous solutions might be managed.
Cuprous acetylide was found to be readily precipitated
from ammonia gas by bubbling it through ammoniacal
copper nitrate solution containing metallic copper.
Such a process involves complicated procedure for
recovery of copper. Scrubbing with organic solvents
appears to be impracticable on account of their
volatility.
A thoroughly practical method is to convert the
ammonia into liquor by dissolving it in water. Water
dissolves its own volume of acetylene. Its solubility
in strong ammonia liquor as shown by our experi-
ments is of the same order. On this basis one liter
of liquor containing 300 g. XH3 would hold in solution
440 liters of ammonia gas and only 10 cc. acetylene
if saturated with ammonia gas containing 1 per cent
acetylene.
Such a liquor when vaporized with air to form a 10
per cent ammonia mixture should yield a gas for the
oxidizer containing about 0.0002 per cent acetylene
June, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
459
or 1 part by volume in 500,000. Acetylene at this
concentration would probably not poison platinum.
The calculation made above is based on Henry's
law. Since the acetylene is only 1 per cent of the
ammonia, its partial pressure is 0.01 atmosphere and
it follows therefore that 1 liter of liquor will dissolve
at equilibrium one liter of acetylene at 0.01 atmos-
phere, or 10 cc. at normal pressure. In dissolving
ammonia-acetylene in water, the former is absorbed
quite rapidly, thereby increasing the partial pressure
of the acetylene so that the concentration of acetylene
in solution is at first quite high. The gas must be
passed in some time after all absorption of ammonia
has ceased in order that equilibrium may be estab-
lished and the acetylene concentration in the liquor
reach its minimum value.
Laboratory experiments show conclusively that the
deductions arrived at by application of Henry's law
are correct. Ammonia gas containing 1 to 2 per cent
acetylene was passed into water until the ammonia
reached a concentration of 28 per cent. The acetylene
in solution was then determined by precipitation as
Ag2C2 with standard silver nitrate, and found to be
130 cc. C2H2 per liter. The ammonia-acetylene
mixture was then continued through the solution
until it passed freely and no more ammonia was being
absorbed. The liquor now contained 10 cc. C2H2 per
liter.
The application of this scheme industrially should
offer no difficulties. Ammonia absorption apparatus
is simple. Two or more absorbers would have to be
employed since equilibrium conditions must be estab-
lished by blowing the gas freely through the first
absorber after the liquor is saturated. The tempera-
ture of the absorber could be adjusted so that the
strength of the liquor would not be too high after
cooling, to avoid loss of NH3. This temperature in
winter would probably be in the neighborhood of
350 C. and warmer in summer. The heat of solution
makes such an adjustment easy.
Should it be desirable to make a liquor absolutely
free from acetylene, pure ammonia gas could be blown
through the absorber at the end of the operation.
About s per cent of this very pure liquor could be
reserved as a source of pure gas to treat the next
batch. An ammonia liquor free from all non-reacting
foreign gases may be prepared in this way.
SUMMARY
I — As little as 0.02 per cent acetylene in the ammonia-
air mixture has a distinctly deleterious effect. The
.yield drops from about 95 per cent to 89 per cent or
less.
II — The effect of 0.1 per cent acetylene, or its
accompanying impurities, is disastrous. The yield
may drop as low as 65 per cent.
Ill — A small quantity of acetylene will render the
platinum so inactive that the yield on pure ammonia
will be reduced 2 to 4 per cent for several hours. This
means that the ammonia used for manufacture of
nitric acid should be free from acetylene at all times.
IV — Operation of oxidizers working on the principle
of a self-sustaining reaction without electric heating
or preheating, and utilizing sources of ammonia that
contain acetylene, is probably impracticable.
V — Ammonia gas may be freed from acetylene and
other non-reacting gases by dissolving it in water to
make a strong ammonia liquor. Such procedure in-
volves no difficulty industrially, nor any considerable
expense in operating a commercial oxidizing plant.
ACKNOWLEDGMENT
The experiments described herein are a part of an
extensive investigation on commercial ammonia oxida-
tion and the production of nitric acid thereby, con-
ducted by the Bureau of Mines and the Semet-Solvay
Company in cooperation with the General Chemical
Company and the Ordnance Department, under the
direction of the Chief Chemist, Dr. Charles L. Parsons.
Bureau of Mines
Washington, D. C.
LABORATORY AND PLANT
A ROCKING ELECTRIC BRASS FURNACE1
By H. W. GlLLETT AND A. E. RHOADS
Received May 15, 1918
It seems inevitable that the .next few years will see
electric furnaces largely replacing crucible furnaces
in the brass industry, a development comparable to
that which the last few years have seen in the steel
industry.
With Klingenberg clay not available and Ceylon
graphite requiring shipping needed for other purposes,
crucibles, despite the good work done on the problem
by crucible manufacturers, the Bureau of Standards,
and others, are still, speaking generally, of much poorer
quality and many times more costly than they were
under pre-war conditions. The time is ripe for the
practical elimination of the crucible from the brass
industry.
1 Published by permission of the Director of the Bu
of Mines.
With the huge tonnage of brass required for war
purposes, the use of the small units — averaging 200
lbs. per charge — in which crucible melting is done by
the brass rolling mills, seems, and is, an anachronism.
Besides the avoidance of crucibles and the ability to
melt larger charges, electric melting (in a suitable type
of furnace) decreases the loss of metal by oxidation and
by volatilization, prevents the taking up of sulfur from
the fuel, gives better and more healthful working con-
ditions, and has many minor advantages such as
freedom from handling and storing fuel and ash. Elec-
tric furnaces give crucible quality of metal without
using crucibles.
However, not every type of electric furnace can be
used for brass melting. If brass did not differ materially
from steel in its behavior during melting, electric
furnaces would long ago have superseded crucible
460
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 6
furnaces. But brass is made up of copper and zinc,
and zinc is volatile at brass melting temperatures.
For this reason, fuel-fired furnaces of the reverberatory
type can be applied to brass only at the expense of a
zinc loss so high as to prohibit the procedure. Simi-
larly, the direct-arc type of electric furnace used for
steel melting, such as the Heroult. can be used only
on bronzes practically free from zinc, because of the
high local temperature of the melt under the arc.
Indirect-arc furnaces, such as the Rennerfelt, can
be used on brasses carrying up to about 20 per cent
zinc, but are not suitable for ordinary yellow brass,
on account of the formation of a superheated layer on
the surface of the melt directly under the arc, and the
resulting volatilization of zinc.
Induction furnaces of the ordinary horizontal ring
type, like the Rochling-Rodenhauser, cannot be used
on brass or bronze because the high electrical con-
ductivity of these alloys requires a secondary current
so high that the "pinch effect" causes rupture of the
secondary ring.
Hence it has been necessary to develop types of fur-
naces radically different from those in use for steel
in order to meet the requirements of brass.
ELECTRIC BRASS FURNACES IN" COMMERCIAL USE
There are, however, two types of steel furnace which
have been applied to brass (using the term brass loosely
to include bronze, red brass, etc.): the Snyder, a single-
phase, direct-arc furnace; and the Rennerfelt, a two-
phase, indirect-arc furnace. At the Chicago Bearing
Metal Company; Chicago, 111., two one-ton Snyders
and two one-ton Rennerfelts are melting bronze for
railroad bearings, high in lead, but practically free
from zinc. The metal losses are not much reduced
from previous practice in crucibles and open flame oil
furnaces, but the furnaces are making savings in melt-
ing cost as compared with either the crucible or the
open-flame furnaces under present conditions.
The Philadelphia Mint is melting nickel and coinage
bronze in a 1000-lb. Rennerfelt furnace. The Gerline
Brass Foundry Company, Kalamazoo, Michigan,
melts Monel metal, red brass, and brass containing
up to about 20 per cent zinc in an 800-lb. Rennerfelt.
The furnace at the Gerline plant is run on a o-hour basis,
while the other furnaces mentioned operate 18 to 24
hours a day.
Two other types of furnace designed especially for
brass melting have also found commercial use, the Baily
and the Ajax-Wyatt.
The Baily furnace uses a single-phase granular re-
sistor, the heat from which is reflected down onto the
hearth from the roof. It takes charges of about 1000
lbs. Baily furnaces are installed at the Lumen Bearing
Company, Buffalo, X. V.. Hays Mfg. Company, Erie.
Pa., Bridgeport Brass Company. Bridgeport, Conn., and
the Baltimore Copper Smelting and Rolling Company,
Baltimore. Md. The Baily furnace is applicable to
alloys of any zinc content, reduces metal losses, avoids
crucibles, and gives good working conditions. The
main drawback of this type of furnace is that the
source of heat is not close to the melt and the heat must
be reflected down from the roof. In order not to over-
heat the roof and cause its prompt failure, as well as
to hold the resistor temperature within the limits that
allow reasonable life of the resistor trough, the rate of
power input is low compared to the size of the furnace
and weight of charge. Hence the radiation losses
from walls and roof form a large proportion of the total
power. The furnace is at its best on 24-hour operation.
When 10-hour operation is necessary, it is found that
the furnace must be heated empty during all or part
of the night in order to give satisfactory output in the
daytime. Because of the high heat storage in the walls,
a furnace of this type does not respond promptly to
changes in power input, and accurate control of the
temperature of the melt is difficult.
The Ajax-Wyatt furnace is a single-phase induction
furnace in which the secondary ring is in the form of
a loop below the level of the hearth proper, so that the
hydraulic head of the metal in the hearth opposes the
rupturing effect of the "pinch" force, thus avoiding the
troubles which make horizontal-ring induction fur-
naces inapplicable to brass.
The metal heated in the secondary loop is con-
stantly ejected at one part of each opening from loop
to hearth, and colder molten metal drawn in at another
part of the opening. These fountains of hot metal
issuing from the resistor melt the charge in the hearth.
The constant circulation of metal is a most desirable
feature and gives a product of remarkably uniform
chemical composition.
Because of the compactness of the furnace, the gener-
ation of heat within the metal itself, and the stirring
action, vertical-ring induction furnaces are extremely
efficient as regards power consumption. The power
factor in the sizes so far built is satisfactory.
The furnace must be started with a charge of pre-
viously melted metal, and sufficient metal to fill the
loop must be retained when pouring. The metal in
the loop must never be allowed to solidify, or the lining
will be ruined. These facts make it difficult to change
from one alloy to another, and require that the fur-
nace be run 24 hours a day, or else receive enough
power at night to keep the metal in the loop fluid.
Ramming up and drying the refractory lining of the
loop is a job requiring care and experience, as the lining
must be perfect or its life will be short. Xo lining has
yet been found which will withstand alloys containing
over 5 per cent of lead, and the furnace has been de-
veloped mainly for yellow brass.
The furnace is fitted for rolling-mill use, where
24-hour operation on yellow brass is the rule, but is
distinctly less suitable for 1 o-hour runs or for foundries
making a variety of alloys.
Several of these furnaces are in use at the Ajax
Metal Company, Philadelphia, two at the American
Brass Company. Waterbury, Conn., and twenty-eight
at the Bridgeport Brass Company. Bridgeport. Conn.
The furnace saves zinc, avoids crucibles, and shows
so low a power consumption on 24-hour operation that
it can doubtless be used to advantage in rolling-mill
practice even under normal prices of fuel and crucibles.
June, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
461
FURNACES UNDER EXPERIMENTAL TEST
Besides the four types mentioned above, each of
which has found commercial use where conditions were
suitable, there are four other furnaces that have reached
a semi-commercial s"tage, but are still under experi-
mental development.
The Bennett furnace at the Scovill Mfg. Co., Water-
bury, Conn., is a three-phase furnace, probably of
about 750 lbs. capacity, and resembles a direct-arc
furnace. However, the voltage between electrodes
(which are automatically regulated) and bath is kept
so low that there is no true arc and the heat is generated
by a sort of contact resistance. This is said to give
low metal losses and to show a reasonably low con-
sumption of power.
The furnace has run mainly on yellow brass and is,
therefore, probably applicable to all brasses and bronzes.
The results of the work have so far been kept secret
and no detailed data are available.
The Foley furnace is a single-phase, vertical-ring
induction furnace, similar in general design to the
Ajax-Wyatt, although differing from it in many points.
One such furnace, of about 1000 lbs. capacity, has been
in experimental operation at the Bristol Brass Com-
pany, Bristol, Conn., and three 3000-lb. furnaces are
under construction., From the small amount of data
so far available on this furnace, its metal losses
and power consumption will be about the same as
in the Ajax-Wyatt; due partly to its larger size,
its power factor is somewhat lower. It has the same
disadvantages as regards starting, changing from one
alloy to another, and the necessity for 24-hour opera-
tion, as that furnace.
The General Electric furnace is a smothered-arc,
one- or two- (normally two) phase furnace, of about
1500 lbs. capacity, having four depending electrodes,
two on each side of a hearth. Between the tips of
each pair of electrodes is a carbon block to which
arcs are drawn, the arcs being smothered by granular
coke. The heat thus generated is reflected down onto
the hearth by the roof. The electrodes are automatic-
ally regulated.
After being tested at the General Electric Company,
Schenectady, N. Y., this furnace has been installed
for further test at the Chicago Plant of the Crane
Company, but is not yet considered ready for general
commercial use.
The heat transfer in this type is similar to that in the
Baily, and the furnace seems theoretically capable of
a performance of about the same order as_the Baily
with similar advantages and similar drawbacks. As
the General Electric furnace takes a higher power
input than the Baily, it may be slightly more efficient
in power consumption, but the roof is subject to even
more severe conditions and will require the use of high-
grade refractories to give a good life.
The Northrup furnace, being developed by Prof.
E. F. Northrup and the Ajax Metal Company, is an
induction furnace, heating the charge by means of
eddy currents instead of making the charge, or part of
it, the secondary of a transformer. Oscillating cur-
rent of very high frequency is used instead of alter-
nating current, and is obtained by the use of condensers
or of a special generator. A 60-kw. tapping-type
furnace is being tried out. The Northrup furnace has
a high power factor, and can take multi-phase current.
It is being developed in order to produce a furnace
suitable for 10-hour operation and for facility in chang-
ing from one alloy to another.
Since the heat is generated within the charge itself,
the eddy-current furnace should be efficient in power
consumption. This type is theoretically very promising,
but its development has not yet gone far enough to
■show what, if any, mechanical limitations the type will
have.
Many other types of furnace have been suggested
for brass melting, and a number have been tried out
more or less thoroughly, but those mentioned above
are the most prominent of the types in commercial
use or under commercial development. Most of these
are either limited in their application, or have some
drawbacks, either inherent in the type of furnace, or
not yet eliminated by long experience in their design
and use, so that no one type or make of furnace is
as yet definitely proven the best for any particular
set of conditions, and still less will any one furnace
meet all the different conditions found in the whole
range of the brass and bronze industry.
In particular, none of these types seems quite fitted
to that common set of conditions where a furnace may
be called upon to melt successive heats of alloys differ-
ing widely in composition, to handle both alloys free
from zinc and those high in zinc, and to operate cheaply
on a 9- or 10-hour day.
ROCKING ELECTRIC BRASS FURNACE
In its study of electric brass melting during the past
five years, the Bureau of Mines has tried out a rocking
type of furnace, which may perhaps help to fill this gap.
In the ordinary indirect-arc type of furnace, the heat
is applied above the melt and as hot metal is lighter
than colder metal, there is little circulation in the bath.
If the rate of heat input is at all rapid, as is necessary
for thermal efficiency, heat conduction from the top
of the melt downward does not keep pace with the
heat supply. Before the melt as a whole reaches the
proper pouring temperature, the surface is much super-
heated.
On an alloy high in zinc the surface will reach the
boiling point of the zinc in that particular alloy while
the bottom is scarcely melted; such heating creates
a high pressure of zinc vapor within the furnace, so
that if the furnace is not tightly closed zinc is lost con-
tinually. If the furnace is sealed tight, the pressure
may even blow out the roof or door. In case the fur-
nace holds tight and the pressure is not relieved till
the spout is opened for pouring a long hissing Stream
of zinc vapor then shoots out, burning in the air.
This local overheating is the cause of the failure of
the indirect-arc furnace to handle alloys high in zinc
without large metal losses.
The obvious way to overcome this trouble is to stir
the melt so vigorously that the temperature of the mell
is practically uniform and the superheating of the sur-
462
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 6
face prevented. The most practical way to stir the
melt is by the principle of the cement-mixer, by turn-
ing the furnace bodily so as to stir the contents thor-
oughly while being heated. Constant rotation of a
cylindrical furnace placed more or less horizontally,
but preferably at a slight angle with the horizontal
to produce endwise motion of the melt during rota-
tion, with electrodes entering at the ends of the drum
and an arc struck between the electrodes, should not
only stir the charge thoroughly, avoid surface over-
heating and thus prevent zinc losses, but should
also give a well-mixed alloy. By washing the walls
with metal, the heat stored in the walls and roof should
be largely taken up in the metal instead of passing
out. The power consumption should, therefore, be
low. As the walls are washed with metal their tem-
perature can rise little above the temperature of the
metal, which should give a good life of lining.
Instead of rotating the furnace through a complete
revolution — which would involve difficulty in making
brush contacts to the electrodes and in keeping the
metal out of the joints between the door and the door
opening, as this opening should be on the circum-
ference of the drum rather than on the end — it ap-
pears simpler to rock the furnace back and forth so
that the molten charge just fails to reach the door
at either end of its rocking angle.
A small furnace of this type was built and tried out.
This was rocked back and forth by hand on tracks.
It was cheaply constructed from materials at hand
in the laboratory and was not expected to give very
good results on power consumption, as the drum was
too small to allow the refractory lining to be of de-
sirable thickness.
The laboratory furnace held about 100 lbs. of charge,
and operated on 50 to 75 volts, 500 to 700 amperes,
at a power factor of 85 to go. The usual power in-
put was about 30 kw. Graphite electrodes 2 in.
in diameter were used.
A number of different alloys were melted in the
rocking furnace. In melting 1092. 1 lbs. of yellow
brass, made up of 45 per cent ingot, 55 per cent copper
and zinc, the calculated analysis being 65.6 per cent
Cu, 34.4 per cent Zn, 1080.4 lbs. of ingot were obtained,
analyzing 65.9 per cent copper, 34.1 per cent zinc.
The metal loss by weight was 1.06 per cent which
includes both volatilization and mechanical loss by
spatter in pouring. The average pouring temperature
was 10800 C.
On manganese bronze chips (40 per cent zinc),
the furnace gave a net metal loss of 3.0 per cent, while
the same lot of chips melted in oil-fired crucible fur-
naces in commercial practice gave 7.2 per cent loss.
Yellow brass chips (25 per cent zinc) gave 1.6 per
cent net loss, red brass chips (10 per cent zinc), 1.0
per cent.
A fine concentrate (20 mesh) from brass furnace
ashes obtained in the manufacture of brass of 80
per cent copper, 20 per cent zinc, analyzed 71.0
lit copper and 14.3 per cent zinc, the balance
being ash, etc., gave on melting in the furnace a re-
covery of 99 per cent of the copper and 50 per cent of
the zinc in the concentrate. This material is usually
sent to the smelter and refined in a reverberatory
furnace, not all of the copper and none of the zinc
being recovered.
Yellow brass ingot (25 per cent zinc) was remelted
with 0.5 per cent loss. Red brass (10 per cent zinc)
made up from red gates, scrap copper, yellow chips,
lead, and tin was melted with 0.5 per cent loss.
Heavy German silver scrap (18 per cent nickel,
56 per cent copper, 26 per cent zinc), which gave 1.8
per cent loss on commercial melting in coke fires, was
melted with 1.2 per cent loss.
Sound copper castings were made from metal
melted in the furnace.
Red brass of 81.5 per cent copper, 8.5 per cent zinc,
6 per cent lead, 4 per cent tin, made up from red and
yellow ingot and scrap copper, was melted in one
series of tests with the following results, the furnace
being cold at the start.
Table I
Heat
No.
Weight of
Charge
Lbs.
Time Arc
Min.
Pouring
Temp.
° C.
Kw. Hrs.
Used
Kw. Hrs
per 100
Lbs.
L34
L 35
L 36
L 37
L38
127.3
127.75
128.5
126.5
129.5
57
50
SO
37
36
1140
1180
1220
1220
1220
40
30 "A
26>A
22 >/,
19
30 Vi
25
20 'A
17>A
14'A
Total 639.55
Av. 46
Av. 1200
Total 138>/«
Av. 21"/«
The total elapsed time for the five heats, including
charging and pouring, was 5 hours. 630.9 lbs. ingot
were poured and 7.45 lbs. metal from spillings, etc.,
were recovered, giving a gross metal loss of 1.35 per
cent and a net loss of 0.2 per cent.
The power consumption, at the rate of 430 kw. hrs-
per ton on a 5-hour run. starting from the cold, and
at the rate of 295 kw. hrs. per ton when the furnace
is hot, with the metal heated to 1 200 ° C, is surprisingly
low for so small a furnace.
The results above show that the rocking furnace
is a type capable of giving low metal loss and low power
consumption. When the furnace was not rocked
while melting alloys high in zinc, pressure built up
within the furnace and zinc losses were high.
June, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
463
The laboratory tests having demonstrated the prob-
able usefulness of the type, a furnace of commercial
size was designed.
The Detroit Edison Company had long been in-
terested in electric brass furnaces as a possible outlet
for electric power, and offered to cooperate by con-
structing a rocking furnace for commercial test without
expense to the Bureau of Mines except the salaries
and expenses of its representatives while supervising
the test.
Sketches of the furnace design were given the De-
troit Edison Company, which refined the design,
made the working drawings, constructed and erected
the furnace.
The furnace is shown in Figs. I and II. The drum
is s ft. in diameter by 5 ft. long. The lining is 12 in.
thick, and consists of silocel brick on the outside,
special heat-insulating brick in the middle layer, and
corundite brick (a very refractory firebrick high in
AI2O3) in the actual hearth lining. The hearth is
3 ft. long by 3 ft. in- diameter, taking charges of 1300
lbs. and upwards. The electrodes are 4 in. diameter
graphite, threaded for continuous feed, and are ad-
justed by screw-operated supports of the lathe-slide
type. Single-phase, 60 cycle current, stepped down
to 120 or 130 volts is used, 300 kv. amp. being avail-
able. Electrode adjustment is by hand, and to
stabilize the arc an external reactance is used which
brings the power factor of furnace plus reactance,
measured at the furnace switchboard, to about 85.
The open circuit voltage falls to about 106 to 116
volts under load. The current varies between 1000
and 2000 amperes, 1650 amperes being about the
average. The power input can be varied by altering
the length of the arc, and runs from 100 to 200 kw.,
averaging about 165 kw.
The flexible leads and the water hose for electrode
cooling are given slack to allow rocking the furnace,
as is clearly shown in Fig. II.
The rocking of the furnace during melting is auto-
matically done by means of the control device shown,
with cover removed, in the lower left-hand corner
of Fig. II. This can be set to give a "safe rock"
of 80 °, the limit of motion being such that the metal
just does not run into the spout. After the charge
has begun to melt, the "safe rock" is started. It is
called the "safe rock" because the angle is such that
solid charge will not fall on the electrodes and break
them. A complete oscillation on "safe rock" takes
13V2 seconds.
During the "safe rock" the solid metal is swashed
about in the molten part of the charge and is tumbled
over, so that fresh surfaces receive direct radiation
from the arc. As melting goes on, the rocking angle
is increased by turning the handle of the control de-
vice from time to time, until, when the metal is all
melted, the furnace is on the "full rock" of about
2000. On "full rock" the metal washes the whole cir-
464
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 6
cumference of the hearth save the height of the charg-
ing door and a few inches above and below it, so that
metal 'lues not splash into the door joint. A complete
01 cillation takes 33V2 seconds.
The reversal of the 5 h. p. motor at either end of
the rocking angle is done by contactors, operated by-
solenoids, actuated by the contacts on the control
device.
When it is desired to depress the spout past the
limiting point of the automatic rock, for pouring,
the control device is switched out and the solenoids
are operated by a reversing switch.
The furnace is installed at the plant of the Michigan
Smelting and Refining Company, Detroit. Michigan,
which makes brass ingot to customers' specifications
from chips, scrap, and junk of various kinds, by means
of strict chemical control. As the firm makes no sand
castings, but ingot only, no observations on the com-
parative quality of metal melted in the electric fur-
nace and in the coke fires were possible. All the metal
melted was poured into ingot which went into the
regular output of the plant. As far as could be told
by analysis and appearance, the electrically-melted
metal was of at least as good a quality as from the coke
fires. On alloys high in lead there was somewhat less
segregation than in the metal melted in crucibles,
and on charges high in zinc, the zinc content of the
metal from the electric furnace was higher than that
from the same charges melted in the coke fires.
As there is generally much oil on the borings and
some non-metallic material in the other scrap, the
true metallic content of the charge is seldom accurately
known. Hence the net metal losses cannot be ex-
actly determined.
The metal losses were, therefore, compared with
those of the coke-fired crucible furnaces operating on
the same charge.
From 102 tons of metal melted in strict comparison
with the crucible furnaces, the rocking electric fur-
nace produced 3626 lbs. more metal from the same
charge than the coke fires, or 1.8 per cent. The
alloys melted ran from 90 to 66 per cent copper,
1 to q per cent tin. 1.5 to 26.5 per cent lead
and o to 30 per cent zinc.
The comparative metal losses on a few alloys in the
electric and the coke fires are given in Table II.
Tabi.k 11
Weight Per cent Loss Per cent Loss
Charged (Metal. Oil, Dirt) (Metal, Oil, Dirt)
Lbs. Coke Fires Electric
6576 4.6 3.2
11600 7.0 3.7
14300 2.4 1.8
11790 3.6 2.1
15840 7.1 .< 1
11805 4.0 2.4
14.VI.' 3.7 2.9
3.0 2 4
7200 8.0 5.1
The rocking furnace gave alloys and analyzed very
close to the calculated analyses, especially if the diffi-
culty of calculating the analysis of a scrap charge is
considered. Characteristic analyses arc given in Table
til.
There was no difficulty in draining the metal com-
pletely from the hearth, and alloys of different com-
position can be made one after the other without con-
Composition
Per cent
Cu Sn Pb Zn
76 8
73 4
67.5 4
tamination by metal left in from the previous heat.
Table III
Copper Tin Lead Zinc
Sought 76 8 13 3
Electric 75.9 8.3 13.1 2.7
Sought 76 8 13 3
Electric 76.2 8 12.4 3.2
Sought 85 5
Electric 85.2 4.9 4.8
Sought 83 4 6
Electric 82.9 4.4 5.7 6.9
Sought 67 1 2 30
Electric 66.6 1 2 30.4
Coke 68.4 0 5 1.7 29.3
Sought 68 1 7 24
Electric 67.9 ...
Coke 69.9 ...
Sought .60 3 37
Electric 59 7
The power consumption on io-hour operation, with
no night heating, is shown in Table IV, which gives
a resume of 5 days' operation.
The power consumption on 24-hour operation is
shown in Table V for a 4-day run.
On the basis of power, read on the high tension side
of the transformer, per ton of metal poured, the power
consumption on 10-hour operation was 336 kw. hrs.
per ton, on red brass poured at 11800 C. average.
For 24-hour operation, the figure is about 260 kw. hrs.
per ton for red brass.
The electrode consumption was 16.3 lbs. while melt-
ing 21,660 lbs. of metal, or i«/2 lbs. per ton, equiva-
lent to about 40 cents at present electrode prices. To
this must be added the loss due to accidental breakage.
There were nine breakages in melting 72 tons, four
of which were due to the charge being so bulky that
it fell against the electrodes when rocking started,
and five to the electrodes being hit while bulky ma-
terial was being charged. The design of the furnace
has now been altered so as to allow the electrode tips
to be withdrawn into the walls during the charging
of bulky material. When an electrode does break,
if nipple joints are used, the breakage is usually of
the nipple only.
In the 24-hour tests tabulated in Table V. and in
a 10-hour run just preceding the 24-hour runs, in
which the 75.25 Cu, 7.5 Sn, 14.25 Pb, 3 Zn alloy
was melted, there was charged, for the 75.25 Cu alloy,
Ingot 25200 lbs.
Red borings 1 I 2(ki lbs. 2 per cent oil = 224 lbs nonmetallic
Medium brass. . . 1540 lbs.
Scrap Cu 10987 lbs.
Scrap Pb . . . 3906 lbs.
Ingot Cu 552 lbs.
Yellow borings. . . 1400 lbs. 3 per cent oil = 42 lbs. nonmetallic
54805 266
For the 86 Cu. 6 Sn. 10 Pb alloy there was charged
Ingot 16000 lbs.
Cu 4704 lbs.
Pb 96 lbs.
20800
Total Charge. . 75605 lbs.
266 lbs. nonmetallic
75339 lbs. metallic
There was obtained
53841 lbs. good ingot !
20149 lbs. good ingot 86 Cu
73990 total good ingot, 1349 lbs gross loss, or 1.8 per cent
63 lbs. scrap 75. 25 Cu
43 Iba scrap 86 Cu
300 lbs metallics in 569 lbs skimmings \ S3 per cent
from 73 25 Cu I metallic in all
130 lbs. metallics in 246 lbs. skimmings I skimmings
from 8 ' by assay
363 Iba metallics in 429 lbs. ladle skulls from 86 Cu,
85 per cent metallic
74891 total metallic recovery, 448 lbs. net loss, or 0.6per
cent
June, 1918 TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
465
In heats 256-313, on over 3 7 'A .tons melted, the
electrode consumption, including all broken stubs and
scrap, was slightly less than 2 lbs. per ton.
Since the operation was experimental, it is not yet
possible to give exact figures on the life of a lining, but
as nearly as can be estimated the relining cost for labor
and material should be well under 50 cents per ton
with a corundite lining, when melting red brass poured
at 1150 to 12000 C. If only yellow brass poured at
noo° C.,is melted, the lining cost will be still lower.
If very hot bronze is to be produced, say at 13000 C,
the roof and upper portions of the ends should be lined
with zirkite brick.
Accurate temperature control is very easy in the
rocking furnace, since at the end of a heat, after the
"full rock," the walls are no hotter than the metal,
and there is no heating up of the charge from hotter
roof and walls when the power is shut off, as is the case
with those types of furnace where the heat is re-
flected downward from the roof. After cutting off
the arc, the temperature falls very slowly, about 2
to 3° C. per minute. By running the arc a minute
or so every 10 or 15 minutes, a charge can be held at
pouring temperature for an indefinite period.
One man can operate the furnace, with the aid of a
helper while charging. Were automatic electrode
control used, which could easily be done, one man could
probably attend to two furnaces.
The output per man hour was greater from the
rocking furnace than from the coke fires. The work-
ing conditions are much less severe and more health-
ful with the electric furnace than with the coke fires,
and a man of less rugged physique than is required
for coke fires can readily operate the rocking furnace.
Various modifications and improvements in design
were made during the tests, and others that could not
well be made on the first furnace are being incorporated
in other furnaces of this type now being built for De-
troit firms. The electrodes were at first introduced
into the furnace directly through the refractory walls.
When making yellow brass from new materials so
that addition of much spelter is required, the zinc,
vaporized during the addition of the spelter to the
molten charge, tended to condense in the clearance
between the electrode and the hole through which it
entered. This would then freeze, solder the elec-
trode in place, and cause breakage. Such trouble
was later obviated by the use of graphite sleeves about
the electrodes and by the proper arrangement and
operation of the electrode coolers. It was also found
feasible to charge the zinc with the rest of the charge
instead of speltering at the end of the heat.
Comparing the cost of melting on a 10-hour schedule
in the rocking electric furnace and in the qoke fires
of the plant at which the test was made, the sum of the
cost per ton of charge for electric power, interest and
depreciation, electrodes, linings, and for heating ladles,
is just about one-half of the cost per ton of charge of
the single item of crucibles at present prices and at
present crucible life. The value of the metal saved
by the electric furnace is about twice the cost of the
coke used by the coke fires. Hence a huge saving is
possible by electric melting under present conditions,
and even at pre-war prices for crucibles, coke, and metal
the rocking furnace will show a distinct though smaller
saving. On 24-hour operation the balance in favor
of electric melting is still more marked.
From data at hand on the power consumption of
other types of electric furnaces, it appears that, when
operated on the same alloy, heating it to the same tem-
perature, and running the same number of hours per
day, the rocking furnace is somewhat more efficient
than the direct-arc, and unrocked indirect-arc types,
very much more efficient than electric furnaces of
types in which heat is reflected onto the charge from
the roof, and very little less so than the induction fur-
naces. These conclusions follow not only from the
data at hand, but from the method of application
of heat in the various types, those with the source
of heat at a distance from the charge being less effi-
cient than those where the heat is developed close to
the charge. The induction furnaces in which the heat
is developed in the charge itself should be the most
efficient. On account of the washing of the walls
with the metal, the rocking furnace should theoretically
come next to the induction type in thermal efficiency.
In magnitude of metal losses, the rocking furnace
gives at least as good results as any other type of elec-
tric furnace. The only possible loss is from the stream
of metal while pouring, as the furnace is sealed tight
while running. Volatilization from the stream while
pouring is of course about the same in all types of
furnaces.
In closeness of control of the temperature of the
melt the rocking furnace is superior to any save the
induction type. In thorough mixing of the charge,
the rocking type is about on the same plane as the
induction type, and markedly superior to the other
types, where, in large sizes, segregation in the bath
may be a serious problem.
For example, the following shows the analysis for
copper of the first ingot from the first ladle and of the
last ingot from the last ladle, when melting 1200-lb.
charges of 60 per cent Cu, 37 per cent Zn, 3 per cent Pb.
Heat First Ingot, First Ladle Last Ingot, Last Ladle
No. Per cent Cu Per cent Cu
322 59.76 59.54
323 59.78 59.66
In ability to change from one alloy \o another, it
is superior to the vertical-ring induction type, and in
ability to operate cheaply when used but 10 hours
a day, without night heating, is ahead of the vertical-
ring induction type and of the reflected-heat type.
The rocking furnace can handle alloys of any zinc
or lead content, being superior on this score to direct-
arc, unrocked indirect-arc, and induction types. The
electrode cost compares favorably with other arc
furnaces. With equal conditions of operation, and
suitable refractories in each type, the cost of lining will
probably be about the same as with most other types.
Labor cost should be about the same in all hand-
regulated arc furnaces. With automatic regulation,
which can be applied if desired, the rocking type should
466
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 6
Table
IV — Ten-Hour Operation
Sec-
ondary Primary
Nature Wt. of
Elapsed
Sec.
Total
Weight
Pri-
Kw.h./
Kw. h./
Heat
Per cent Alloy
of Charge
Time
Kw.h.
Kw.h.
Sec.
Pouring
Poured
mary
Cwt.
Cwt.
Date No.
Cu
Sn
Pb
Zn
Charge
Lbs,
Mrs
Mn
. Arc
Motor
Power Temp.
Lbs. Kw.h.
Charged
'oured Remarks
Nov. 5 192
85
5
9
1
Average
1314
3
40
257
4
261
2000° F.
1095° C.
20
.... Furnace cooler than usual, not run
previous two days. No. 192 in-
cludes 1 hr. 20 min.. 100 Kw. hi*.
preheat
193
85
5
9
1
Average
1314
1
50
219
3
222
2050° P.
1120° C.
17
194
79
9
10
2
Little
bulkier
1304
1
35
196
2
198
2125° F.
1165° C.
IS
195
79
9
10
2
than
avej age
1304
1
30
190
2
192
2200° F.
1205° C.
14.5
196
79
9
10
2
1304
1
40
190
3
193
2200° F.
1205° C.
15
. . Time includes 20 min. charging
Heat No. 197
Day Total
5 heats
6540
10
15
1052
14
1066
2115° F.
6360
1162
16.3
18.3
1155° C.
Nov. 6 197
79
9
10
2
Little
bulkier
1304
1
45
235
3
238
2125° F.
1165° C
18.5
198
79
9
10
2
than
average
1304
1
30
199
3
202
2175° F.
1190° C.
15.5
199
79
9
10
2
Little
bulkier .
1304
1
40
186
2
188
2250° F.
1230° C.
14.5
200
79
9
10
2
than
average
1304
1
40
176
2
178
2240° F.
1225° C.
13.5
201
79
9
10
2
Little
bulkier
1304
1
30
162
2
164
2100° F.
1150° C.
12.5
202
79
9
10
2
than
average
1304
1
45
160
2
162
2125° F.
1165° C.
12 5
... Time includes 20 min. charging
Heat No. 203
Day Total
6 heats
7824
9
: 50
1118
14
1132
2185° F.
7571
1236
14.7
16.3
1195° C.
Nov. 7 203
79
9
10
2
1304
1
35
215
3
218
2125° F.
1165° C.
17
204
79
9
10
2
Little
bulkier
1304
1
40
195
2
197
2165° F.
1185° C.
15
205
79
9
10
2
than
average
1304
1
30
180
2
182
2175° F.
1190° C.
14
206
79
9
10
2
1304
1
35
173
2
175
2140° F
1170° C.
13 5
207
84
6
10
0
Very
1304
1
40
165
2
167
2150° F.
1175° C.
13
208
87.
5 5
0.
7
;x
1304
2
30
178
3
181
1950° F.
1065° C.
14
Includes 50 min. delay by broken
electrode, broken in charging
bulky charge, also 20 min.
charging Heat No. 209
Day Total
6 heats
7824
10
30
1106
14
1120
2120° F.
7583
1210
14.4
16 0
1160° C.
Nov. 8 209
84
6
10
0
Very
bulky
1300
3
00
246
2
248
2050° F.
1120° C.
19
.... Time includes 1 hr. 10 min. delay
due to broken electrode caused
by bulky charge Long delay
due to nipple being over-size and
requiring to be filed down
210
84
6
10
0
Very
1300
1
40
198
3
201
2175° F.
1190° C.
15.5
211
84
6
10
0
Very
1300
2
05
188
2
190
2175° F.
1190° C.
14.5
.... Includes 25 min. adjusting elec-
trode holder
212
84
6
10
0
Very
bulky
1300
1
30
169
3
172
2175° F.
1190° C.
13.5
213
84
6
10
0
Very
bulky
1300
1
50
170
1
171
2175° F.
1190° C.
13
. . - . Includes 20 min. charging No 214
Day Total
5 he
its
6500
10
05
971
11
982
2150° F.
1175° C.
6341
1069
15.1
16.9
Nov. 9 214
84
6
10
0
Very
bulky
1300
1
45
223
4
227
2175° F.
1190° C.
17. S
215
84
6
10
0
bulky
1300
2
05
198
3
201
2200° F.
1205° C.
15.5
216
84
6
10
0
Very
bulky
1300
1
00
195
2
197
2160° F.
1180° C.
15
217
84
6
10
0
Very
1300
1
45
189
3
192
2250° F.
1235° C.
14.5
218
84
6
10
0
Very
bulky
1300
1
25
165
2
167
2150° F.
1175° C.
13
Day Total
.5 IlLMtS
6500
8
50
970
14
984
2190° F.
6407
1073
15 2
16.7
1200° C.
show a labor cost about the same as that of any other
type.
From the electrical point of view of desirability
of a steady load, the rocking furnace does not have
so steady a load and hence, on this score, is not so
desirable as the induction furnaces or granular re-
sistor furnaces. It does not require special trans-
formers, as the granular resistor type does. It lacks
the electrical advantages of multi-phase furnaces.
In very large sizes, two arcs could be used in the rock-
ing type, but in sizes up to one ton, single-phase oper-
ation is required, and in a plant so located that the
power supply must be of limited capacity, a single-
phase arc furnace, with its fluctuating loads,' may not
be satisfactory from the electrical point of view. Such
fluctuation is no drawback in Detroit nor would it
be in most cities or large manufacturing towns.
From the results on furnaces of 125 and 1300 lbs.
capacity, it appears that the rocking type can be
built in a wide range of sizes without showing a great
loss of efficiency in the smaller sizes. This type can
doubtless be built in as large sizes as the brass industry
could normally use.
In first cost, the rocking type should be no more ex-
pensive than other electric furnaces.
While further tests in different plants and under
different conditions, which will be made at least in
part, in the near future, are needed to give accurate
June, iqi8 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
467
Table V — Twbnty-Four-Hour Operation
Kw. h.
Arc Plus Equiva
Rocking __lent
Motor
Conseq.
Day
Weight of
Elapsed
Melting
Read on
on Pri'-
Kw'
h.
Heat
Heat
Charge
Per
cent Alloy
Time
Time
Secondary
mary
per Ton
Date
No.
No.
Lbs.
Cu
Sn
Pb
Zn
Hrs.
Min.
Hrs.
Min.
Side
Side
Charged Remarks
Apr. 30
261
1
1305
75.25
7.5
14.25
3
2
09
1
47
229
Started at 6 : 30 a.m. Furnace idle
262
2
1305
75.25
7.5
14.25
3
1
53
,
28
192
since 4 : 30 p.m., Apr. 29
263
3
1305
75.25
7.5
14.25
3
1
55
22
168
264
4
1305
75.25
7.5
14.25
3
1
44
15
152
265
5
1305
75.25
7.5
14.25
3
1
44
1
15
144
266
6
1305
75.25
7.5
14.25
3
2
12
1
2
141
30 min. (included in elapsed time) adding
267
7
1305
75.25
7.5
14.25
3
1
30
0
55
153
electrode sections and taking fresh grip
268
8
1305
75.25
7.5
14.25
3
1
35
0
58
156
269
9
1305
75.25
7.5
14.25
3
1
41
1
00
151
Midnight
270
10
1305
75.25
7.5
14.25
3
1
33
1
02
146
271
11
1305
75.25
7.5
14.25
3
33
0
■59
143
272
12
1305
75.25
7.5
14.25
3
1
47
1
06
149
273
13
1305
75.25
7.5
14.25
3
2
01
1
02
150
18 min. (included) replacing broken
electrode nipple. End of heat at
5 : 40 a.m.
Day Total
16965
23
17
15
11
2074
2270
268
May 1
274
1
1305
75.25
7.5
14.25
3
2
11
1
18
143
36 min. (included) wait for helpers to
pour metal
275
2
1305
75.25
7.5
14.25
3
I
49
1
12
147
276
3
' 1305
75.25
7.5
14.25
3
1
40
1
07
152
277
4
1305
75.25
7.5
14.25
3
1
35
0
55
147
278
5
1305
75.25
7.5
14.25
3
1
45
1
12
142
279
6
1305
75.25
7.5
14.25
3
3
00
1
20
160
1 hr. 10 min. (included) replacing broken
electrode and altering cooling coil
280
7
1305
75.25
7.5
14.25
3
32
1
02
151
281
8
1305
75.25
7.5
14.25
3
1
21
0
57
146
282
9
1305
75.25
7.5
14.25
3
1
19
0
53
145
283
10
1305
75.25
7.5
14.25
3
23
0
55
151
Midnight
284
11
1305
75.25
7.5
14.25
3
31
0
56
152
285
12
1305
75.25
7.5
14.25
3
1
34
1
01
152
286
13
1305
75.25
7.5
14.25
3
1
20
0
48
141
287
14
1305
75.25
7.5
14.25
3
35
0
53
147
End of heat 5 : 20 a.m.
Day Total
18270
23
35
14
29
2076
2272
249
May 2
288
1
1305
75.25
7.5
14.25
3
1
35
1
05
150
Heat started at 6 : 35 a.m. Furnace idle
1 hr. 25 min. between shifts
289
2
1305
75.25
7.5
14.25
3
1
25
0
52
145
290
3
1305
75.25
7.5
14.25
3
1
25
0
57
143
291
4
1305
75.25
7.5
14.25
3
20
0
55
144
292
5
1305
75.25
7.5
14.25
3
1
35
1
02
144
293
6
1305
75.25
7.5
14.25
3
1
39
0
56
141
Much delay in pouring this heat, no
helpers
294
7
1300
84
6
10
0
1
31
1
04
140
295
8
1300
84
6
10
0
1
18
0
50
150
Between 294 and 295, furnace idle 45 min.
at change of shifts
296
9
1300
84
6
10
0
1
48
0
59
158
297
10
1300
84
6
10
0
1
22
0
52
151
Midnight
298
11
1300
84
6
10
0
2
13
1
05
156
39 min. (included in elapsed time) re-
placing broken electrode
299
12
1300
86
6
10
0
1
28
0
59
162
300
13
1300
84
6
10
0
1
37
1
10
179
301
14
1300
84
6
10
0
1
49
12
163
Heat ended at 5 : 20 a.m.
Day Total
18230
22
05
13
59
2126
23 18
254
May 3
302
1
1300
84
6
10
0
1
43
1
14
167
Heat started 6:45. Furnace idle 1 hr.
35 min. between shifts
303
2
1300
84
6
10
0
1
43
1
22
158
Furnace idle 1 hr. between 302 and 303,
operator in conference
304
3
1300
84
6
10
0
1
55
1
09
158
Furnace idle 1 1/2 hrs. between 303 and
306
5
1300
84
6
10
307
6
1300
84
6
10
Midnight 308
7
1300
84
6
10
309
8
1300
84
6
10
310
9
1305
75.25
7.5
14.25
311
10
1305
75.25
7.5
14.25
312
11
1305
75.25
7.5
14.25
313
12
1305
75.25
7.5
14.25
Day Total
15620
4-Day Total
69085
304. Broke electrode charging 304,
none on hand, wait for one from
machine shop
5 min. patching electrode hole between
304 and 305
Last ladle poured 6 : 55
data on the complete performance of the rocking type
of furnace, it would seem from the results so far that
it may be of distinct value in the brass industry, es-
pecially under present conditions as to crucible prices
and quality, fuel supply and prices, and metal
prices.
At the conclusion of the tests conducted by the
Bureau of Mines, which covered over 300 heats, the
experimental furnace was put on regular production
by the Michigan Smelting and Refining Company.
This company is having four one-ton rocking furnaces
built, and two are under construction for the Electro
Bronze Company, of Detroit.
The patents taken out by the Bureau of Mines on
the rocking furnace have been assigned to the Secre-
tary of the Interior as trustee, and free licenses to
operate under them can be obtained by making applica-
tion through the Director of the Bureau of Mines.
Grateful acknowledgment is made to Cornell Uni-
versity for use of the well-equipped Cornell electric
furnace laboratory in the work on the laboratory
furnace, to Dr. J. M. Lohr, formerly of the Bureau
of Mines, for aid in the work on the laboratory fur-
nace, to the Michigan Smelting and Refining Company
for facilities for the test, and to the Detroit Edison
Company, and particularly to Mr. E. L. Crosby of
the latter firm, for never-failing cooperation.
A more detailed account of the tests of the rocking
468
I III: .mi RNAL DI- INDUSTRIAL AND ENGINEERING I HI UISIRY Vol. io, No. 6
will soon be published as Bulletin 171 of
the Bureau of Mines.
BIBLIOGRAPHY
ADVANTAGES OP BLBCTKXC BRASS K8LTXNG
E V Roeber, "Manufacture of Hrass in the Electric Furnace," Eire-
and Met In, I . 3 I 190
(', II Clamer and C. Hering, "Thi Electrii I 'ui n ■• :e for Brass Melt-
; ,. .. 1 m In 1 Metal . 6 I L912), 95.
1 1 ii Miller, "The Electric Furnace for Heating Non-Ferrous Metals."
.; Lm Inst Metal n 1911 1, 257.
C. A. Hansen, "Electric Melting of Copper and Brass," Trail lm.
Inst Metals, 6 1 1912), 110.
iiaii.y PURNACB
T. P. Baily, "Annealini ind H il Treating of Steel and Melting of
Non-Ferrous Metals in the Electric Furnace," Mel and them. Eng.,
17 I 1917), 91.
SNYDSS 1'IRNAL'K
!•' T. Snyder, r. S. PatcnU 1.100,994 and 1,16
OrjNBKAI. BtBCTWC Ft RM
I l< Valentine, l S Patent 1,242,275.
RSNNSRFBLT PURNACB
I. Rennerfelt, I S Patent 1,076.518.
AJAX-WVATT FURNACE
G. H. Clamer. "Melting Brass in the Induction Furnace." J. Am.
Inst. Metals, 11 U"17), 381.
J. R. Wyatt, U. S. Patents 1. .'01,671, 1,235,628, 1,235.629 arid 1,235,630.
NOKTIIRT I' AJA.N PURMACB
B F Northrup. 'Production of High Temperature and Its Measure-
ment," Met. &• Chem. Ens 17 I 1917), 685.
PINCH EFFECT
C Hering, "A Practical Limitation of Resistance Furnaces, the
'Pinch' Phenomenon," Trans. Am. Eleclrochem. Soc, 11 (1907),
529; 16 (1909), 255.
VOLATILITY OF ZINC IN BRASS
II W Gillett, "Brass Furnace Practice in the United States." Bureau
Ol Mines, Bull 73 I 1914), 129.
J Johnston, "The Volatility of the Constituents of Brass." J. Am.
Inst. Metals. 12 (1918), 1 5
ROCKING FURNACE
H W. Gillett, and J. M. Lohr, U. S. Patent 1 .-'111 ,224.
H. W. Gillett. U. S. Patent 1,201,225.
Morse Hall
Ithaca, N. Y.
A SUMMARY OF THE PROPOSALS FOR THE UTILIZA-
TION OF NITER CAKE
By John Johnston
Received April 1, 1918
Partly owing to the great shortage of sulfuric acid
in Britain, partly in response to an appeal for sugges-
tions made by the Ministry of Munitions, there has
been considerable interest in the question of the dis-
posal of niter cake (acid sodium sulfate). Similar
interest in this matter will arise here, for there is al-
ready a shortage of sulfuric acid; it will consequently
be necessary to economize in acid, and to substitute
niter cake wherever such substitution is feasible.
Some time ago I made a search through all recent
literature available1 and compiled a summary of the
various proposals which have been made for the util-
ization and disposal of niter cake; and it has been
thought desirable to publish this summary as a means
of showing the possibilities and arousing more general
interest in this direction. Some of the proposals
are obviously not very practical — even in war time;
but it seemed better not to exclude a suggestion
even although it does not appear feasible to us now.
Niter cake, a l>y-product of the production of nitric
acid, is an acid sodium sulfate, usually containing only
slighl impurities. Its available sulfuric acid content
from $5 per cent downwards, but is usually
from 25 to ,50 per cent; this free acid may cause diffi-
culties in handling and transportation, particularly
it water, or even moisture, gets access to it. The
annual production of niter eake in the United States
was. according t<> the mog census, about 43.300 tons,
1 In the Literal atly, reference to I
11 D Io the journal reference, signifies that the original article n as
11.. 1 available and that thi > 1 he basis of the abstract
in Chemical Abstracts.
of which 27,600 tons were reported to have a value
of about S2 per ton, the remaining 15,700 tons being
reported as of no value; the amount now available
is, however, very much greater and is of the order
of 600,000 tons at least. The utilization of this ma-
terial in place of the equivalent quantity of sulfuric
acid, in so far as such substitution is possible, would
therefore result in a very appreciable economy of
sulfuric acid, the demand for which is likely to be in
excess of the supply available. The substitution of
niter cake for acid would moreover, at the present
time, result in a considerable money saving, for it
can be bought at a price of about S3 per ton at the
point of shipment, equivalent to an acid price of about
$10 per ton.
As an example of the expansion of the use of niter
cake in Britain since the war we may cite a paper
by Kilburn Scott.1 Before the war it was used to some
extent for making hydrochloric acid and sodium sul-
fate, and a small amount was sold to fertilizer plants
and to glass makers. It is now currently used in
the following processes: the extraction of grease from
wool suds and from piece scouring suds; refining of
grease; stripping color from rags, dyeing of rags, and
removing cotton from mixed fabrics in the manufac-
ture of shoddy; calico bleaching; paper making; in
the mineral water industry; and in making sulfate of
ammonia. He also discusses the methods of handling
and dissolving niter cake.2
Attention is therefore directed to the various pro-
posals outlined below, in the hope that niter cake will
be used, wherever feasible, as a means of reducing the
shortage of acid. The proposals have, for convenience
of reference, been grouped under a number of head-
ings, but it is obvious that these several categories
are not mutually exclusive.
as a pickling agent — LeChatelier and Bogitch3
discuss the advantages of using niter cake for re-
moving scale from the surface of iron, and recom-
mend a procedure for its use, namely, to work with a
solution at 8o° containing 25 per cent niter cake, the
acidity of which is maintained by further additions
of niter cake. Directions are also given in a recent
paper.4 The use of niter cake for pickling iron or
steel is the subject of a patent granted to A. K.
Eaton.5 who claims the process of "removing hammer
scale from iron and steel, which consists in sub-
jecting the scale-coated metal to the action of a
bath containing sodium bisulfate." It is reported
that a large tonnage is already used for this pur-
pose, thus releasing an equivalent amount of acid for
other purposes.
H. W. Brownsdon6 discusses its application in the
pickling of annealed brass and states that it works
1 "Economy of Acids in Metal Trades." J. Soc Chem. Ind., 36
810.
- J Sot Chem Ind.. 36
» Rev. Mttall . 13 . 191 - 949 I I 10. 2460.
i "Pickling with Niter Cake," /r,.„ trade Review, 1918, 153. I have
been informed that solutions of one-hall the concentration recommeuded
by LeChatelier .ind Bogitch are perfectij satisfactory for pickling metals.
1 [line in, 1902, "Method of Removing Scale
Oxide from the Surface ol I P0
'J. Soc. Chem. Ind., 36 I'M
June, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
469
air right provided that (a) the acid strength of the
solution is kept up to 5-6 per cent, (b) the solution is
kept hot, (c) matters are so arranged that the work
is as clean as possible. The niter cake solution is
more sluggish than a sulfuric acid solution of equal
acidity, and the difference in price (in England, acid
$20, niter cake $5 per ton) on the basis of acid con-
tent is not marked. There is therefore no marked
direct saving of money by using niter cake for pickling;
but Brownsdon considers that the use of niter cake
would make better design of annealing furnaces im-
perative, and so might indirectly result ultimately
in considerable economies.
in the textile trade — According to a report1 ex-
periments have shown that niter cake may be substi-
tuted for sulfuric acid in various operations of the tex-
tile trade; for instance, in the extraction of grease
from liquors obtained in scouring, in the refining of
grease, the extraction of cotton from mixed rags in
the making of shoddy,2 as well as in stripping color
from rags in the latter trade. For these purposes
the salt is dissolved in water by the aid of steam and
used hot. Hannay3 states that it can be used as a
sour in cotton bleaching. Matos4 states that in the
dyeing of wool niter cake may advantageously replace
the mixture of Xa2S04 and H2SO4, though, since it
may be contaminated with some iron, it is less suit-
able for the light shades.
In the textile trade, moreover, there is (in Britain)
a great demand for Epsom salts (MgS04) which may
be made by heating magnesite with niter cake.5
as a sizing agent for paper — According to a pub-
lished statement6 perfect sizing may be secured by
using half the usual quantity of alum with 20 per
cent nicer cake. Haas7 states that ordinary niter
cake is only good for sizing the lower grades of paper,
but that the purified salt should be used for the finer
grades. Sindall and Bacon8 also discuss this ques-
tion and state that 100 parts of rosin require 24 parts
NaHS04 for complete precipitation.
IN THE PRODUCTION OF AMMONIUM SULFATE In
response to a memorandum issued by the British
Ministry of Munitions, the Sulfate of Ammonia As-
sociation recommend that it be used as a temporary
expedient, the maximum proportion of niter cake to
be 10 per cent of the sulfuric acid used, and that the
solution be kept hot. The use of a greater proportion
of niter cake results in the precipitation of Na2SC>4
and in irregular working of the bath.9 According to
a recent patent,10 niter cake dissolved in water is
' Chcm. Trade J.. 58 (1916), 28; C. A., 10, 953.
= Fort, however (/. Soc. Dyers Colourisls, 30 (1914), 228; C. A., 9,
1 120], concludes that sodium sulfate injures the luster of wool by reacting
with the wool fiber
•/. Soc. Dyers Colourisls, 32 (1916), 65; C. A., 10, 21.51.
« Textile World J., 61 (1915), 25; C. A., 10, 2046.
(hem. Ind., 34 (1916), 1121.
• Papier Zlg., 40 (1915). 890; C. A., 9, 3129.
■Chem. Zlg., 40 (V916), 571; C. A.. 10, 2635.
I Paper Makers- Monthly J., 64 (1916), 202; C. A. 10, 2799.
» Chem. Trade J., 68 (1916), 342; Chem. News, 113 (1916), 175, /. Gal
Lighting. 134 11916), 74. C. .1 , 10 (1914), 1705. Compare also Cooper,
Chem. Trade J.. 68 11916), 235; J. Gas Lighting. 133 (1916), 523; < ' .1 . 10,
1422; and Gavin, Gas World, 68 (1916 9 ' I lighting, 136 (1916),
545; C. A., 11. 535.
'•Soc. ind. de produits chimiqucs, Hritish Patent 109,814 (1917).
treated with excess of gaseous ammonia, after which
the solution is saturated with carbon dioxide, and the
precipitated sodium bicarbonate washed and dried;
the mother liquor, neutralized by the addition of niter
cake solution, is diluted and cooled to or below o°
in order to separate sodium sulfate, and the residual
solution is concentrated in vacuo or otherwise to re-
cover the ammonium sulfate.
IN THE MANUFACTURE OF FERTILIZERS Strickler1
digests phosphate rock with a solution of niter cake,
concentrates the resulting solution, and cools to
crystallize the Na2S04 and separate it from the phos-
phoric acid. Kochetkov2 treated phosphate rock
with niter cake, dissolved the product in water, evap-
orated until the Na2S04 crystallized out and concen-
trated; the resulting solution contained 2 per cent
P205 and readily attacked bone meal, yielding super-
phosphate.3 Wakefield4 states that he has made
many thousands of tons of superphosphate of lime
containing 20 per cent of soluble phosphate by using
niter cake instead of sulfuric acid. Collins5 sug-
gests mixing one part of leather clippings with two
parts niter cake and heating to 300°, when much of
the nitrogen is converted into ammonium sulfate;
the product is cooled and mixed with one part of rock
phosphate, and sold as fertilizer. Some proportion
of niter cake could also be used in the fertilizer indus-
try by dissolving it in the sulfuric acid, diluted ap-
propriately.
FOR THE PRODUCTION OF SULFURIC ACID Benker6
mixes niter cake with fine sand, or finely divided sili-
cate, or anhydrous sulfates of soda, potash, or lime, in
such proportions that the mass does not melt when
it is heated. Sulfuric acid is expelled and may be
collected; Na2S04 remains behind. The purpose of
such admixtures is to minimize the rate of destruc-
tion of the apparatus, which takes place rapidly
when niter cake is heated alone; but it is questionable
in how far Benker's method is really feasible. Zahn7
claims the process of mixing niter cake with 6 to 7 per
cent water, heating, and so expelling part of the sul-
furic acid, until the mass becomes pasty, when it can
be introduced into a muffle and calcined. The Soc.
Dior fils8 mixes it with bauxite or aluminum sulfate,
and heats the mixture in a muffle so as to liberate
acid; the residue when extracted with water yields
an alkaline carbonate. They also specify the addi-
tion of coke dust to the mixture before calcining.
Prudhomme9 claims the process of heating sulfates,
with or without the addition of silica, alumina, or iron
oxide, in an electric furnace; with the simultaneoti
formation of anhydrous bases. Nibelius10 claims the
process of recovering sulfuric acid and sodium sul-
fate from niter cake by treating it with a volatile
1 CJ. S. Patent 917,502 (1909); C. A., 3, 1804.
, Inst. Agron U we, 19, 60; ' 1 , 8, 392.
■ Compare also Petri Uirin. Ann. Inst. A grott 1/ IV, 19, 142; I L.,8, 194.
. them. Ind., 34 (1916), 1121.
• Ibid.
•German Patents 204.353 (1906), 204,703 (1907); Pi ach P
)8| B63 I 1906) . British Patent 1,844 I 1907) I S Pati i I
i Patent 921,329 (1909); C 1., S, 2040; French Patent 389,898.
I French Patent 417,811.
• French Patent 400.030.
Patent 873,070 1907) I 1.2. II"''
47°
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 6
solvent, such as alcohol, to dissolve out the acid,
separating the solution from the undissolved Na2S04,
and distilling off the solvent. Uebel1 exposes niter
cake in a finely divided state to the action of hot
gases or superheated steam, in a tower, the bottom
of which is a calcining hearth. Mackenzie2 treats
niter cake to expel the H2S04 in a salt-cake furnace
by first heating the charge in a pot and, when it stiffens,
transferring it to a roaster; the vapors from the two
stages are absorbed in suitable towers. He states3
that he has recovered 10 to 12 tons of 94 to 95 per cent
acid a week from this source and that there is no trouble
in obtaining 700 to 800 lbs. acid and 1200 to 1300 lbs.
Na2S04 from each ton of niter cake. Byard4 proposes
the following schemes: (1) Blowing steam or air
into the melt and directing the mixture of acid vapors
into the sulfuric acid plant. (2) Granulating the
melt by pouring it into water and centrifuging to ob-
ta:n clean Na2S04 and an acid mixture, which can be
sprayed into a chamber of an auxiliary acid plant,
the acid so obtained being concentrated and used again
to make nitric acid, in which process the presence of
a little NaHS04 in the acid is unimportant. In this
connection it may be mentioned that Claessen6 claims
the process of briquetting Chile nitrate with 10 per
cent ground niter cake.
It is suggested6 that niter cake be roasted with iron
scale to expel the available acid in concentrated
form; this requires a high temperature, and the action
on the vessels employed is considerable. Llewellyn
and Spence and Sons' heat niter cake with iron or
pyrite, when S02 is evolved, leaving a residue from
which Na2S04 may be extracted. Stanes and Roge8
claim to obtain vitriol by roasting sulfur with twice
its weight of niter cake; they also suggest9 heating
niter cake with sulfur in a non-oxidizing atmosphere
and utilizing the sulfur dioxide produced. The sug-
gestion has also been made that niter cake be heated
with silica alone or mixed with calcium sulfate, the
S03 produced being passed to a contact plant, the resi-
due to be utilized in the manufacture of glass.10
FOR THE PRODUCTION OF Na2S04 (SALT CAKE, GLAUBER
salt) — Most of the possible uses of niter cake yield
Na2S04 as a possible by-product; the following specific
proposals have also been made. The niter cake is
ground and mixed with the proper quantity of common
salt; or, better, the still liquid material is run from
the nitric acid still into a hot salt-cake pan already
containing the requisite quantity of salt. This process
for salt cake has been worked on a considerable scale
in England, but would hardly be economical here in
general. Some patents dealing with this general
process follow: Hart" and the General Chemical
'German Patent 226.110.
« British Patent 13,907 (1915); C. A., 11, 526.
'J. Soc. Chem. Ind., 34 (1916). 1121.
'Ibid., 34 (1916). 1121.
» British Patent 6,102 (1915); J. Soc. Chem. Ind., 33 (1915), 1009.
« J. Soc. Chem. Ind.. 34 (1916), 1121.
I British Patent 103,689 (1916); C. A., 11 1732.
« British Patent 29,254 (1913); J. Soc. Chem. Ind., 33 (1915), 227.
» British Patent 18,605 (1914); J. Soc. Chem. Ind., 33 (1915), 961.
'•See Morgan, Econ. Proc. Roy. Dublin Soc, 2 (1917), 238; through J.
Soc. Chem. Ind.. 36 (1917), 504.
" U. S. Patent 698,704.
Company1 introduce a mixture of common salt and
niter cake by means of steam into a revolving cylinder,
heated almost to redness; the sulfate formed is stated
to be free from both free acid and from chloride. In a
recent communication Hart2 proposes to dissolve
the cake in water to a solution of density 1.35 and to
blow cold air through this solution contained in well-
insulated vessels; by this means a pure salt cake con-
taining less than 0.25 per cent free acid, and a solu-
tion containing mainly free acid, may be obtained.
Meyer and Oehler3 carry out the reaction between
salt and niter cake in an ordinary muffle furnace, and
state that no stirring is required if proper conditions
are maintained; namely, that the temperature should
not exceed 500°, the mass being merely sintered; this
process was worked for some time, but was later aban-
doned. The Verein Chem. Fabriken at Mannheim4
have patented a mechanical salt-cake furnace, which
has proved very efficient in working up niter cake;
this furnace has done good work for some years, ac-
cording to Lunge. The Solvay Process Company*
grinds niter cake and alkaline soda products in the
proper proportion, and heats the mixture above 1250.
Pennock6 mixes niter cake with a combining propor-
tion of soda ash (Na2C03) and a little water, and dries
the product. Ramage7 claims a similar, but more
complicated process. Rommenholler and Lohman8
mix niter cake with coke dust and ignite the mixture
in a muffle; they employ the sulfate as such, or con-
vert it into sulfide and decompose this with COj.
Haack9 mixes niter cake with common salt and coal,
and distils the mixture in a muffle, obtaining sodium
sulfide and HC1. The Chemische Fabrik Grunau10
mixes niter cake with 12 per cent sawdust and 2 per
cent coke dust, and heats in a cast-iron retort provided
with a stirring arrangement; thus obtaining neutral
sulfate and S02. The Nobel Explosives Company"
add to the liquid bisulfate as it is drawn off from
the nitric acid plant, a carbonaceous substance, such
as sawdust, peat, or the like, which yields large quanti-
ties of gas; the mixture sets on cooling to a very porous
mass which can be calcined for the production of
Na2S04 without melting.
The Phoenix Fabrik12 claims the process of mixing
the molten NaHSOj with the appropriate quantity
of pulverulent oxides, hydroxides, or carbonates of
the alkaline earths (which form difficultly soluble sul-
fates) and separating the resulting sulfates by a crys,-
tallization process. Herbert13 dissolves niter cake in
water, runs it into a lead-lined vessel provided with
a stirring arrangement, and adds ground limestone;
' British Patent 9,875 (1902).
» This Journal. 10 (1918), 238.
' British Patent 2,856 (1902); U. S. Patent 702,877; German Patent
186,398; Chem. Ztg., 1906, 1295.
< German Patent 137,906; British Patent 16,207 (1902).
» U. S. Patent 870.746.
• U. S. Patent 922.031 (1909); C. A., 1, 2040.
' U. S. Patent 871,066; C. A., 2, 1059.
• German Patent 63,189.
•German Patent 126,601.
'• British Patent 6,898 (1904).
" British Patent 21,604 (1913); C. A., 9, 1228; French Patent 464,097
(1913): C. A., 8. 3225.
'• Austrian Patent 700-12 (1912); C. .4., 7 1S89.
'• German Patent 28,769.
June, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
47i
the C02 evolved is collected, the gypsum is filtered
off, and the solution evaporated until the Na2S04
crystallizes out. Grossmann1 claims the process of
obtaining niter cake in a porous, friable form which
may be readily ground, by adding to the molten ma-
terial a carbonate such as Na2C03, or any substance
which evolves gas or vapor, with or without a diluent
such as Na2S04. Barbier2 has patented the process
of cooling a solution of niter cake of density 1 . 4 down
to about 10°, when crystals of Glauber salt separate,
and describes suitable apparatus for the purpose.
Grossmann3 treats a solution of CaS03 with niter cake
and after filtration obtains a solution containing
mainly NaOH and Na2S04; the Na2S04 is crystallized
out and the final liquor used as caustic soda. He ob-
tained, from 100 tons niter cake, 36 tons pure Na2S04
and 15 tons caustic soda; costs of production are dis-
cussed. Chatfield4 uses a solution of niter cake to
absorb ammonia from gas liquor, etc., and crystallizes
out ammonium sulfate and sodium sulfate. Hipp5
dissolves the niter cake, precipitates the heavy metals
by means of an alkaline sulfide, evaporates the solu-
tion, mixes with common salt and ignites. White6
uses it in the manufacture of soda alum. Collins7
suggests roasting potash feldspar with niter cake and
crystallizing out the alum.
It is reported that in Canada niter cake is now being
used to make sulfate pulp, on account of the shortage
of the sulfur hitherto used for making sulfite pulp.
FOR THE PRODUCTION OF MISCELLANEOUS SUB-
STANCES— In several of the above processes, hydro-
chloric acid is obtained; likewise when niter cake is
heated with calcium chloride, a process which yields
gypsum as a by-product. According to Hart,8 hydro-
chloric acid made from niter cake always contains
some sulfuric acid and often contains nitric acid and
iodine. Kerr has patented9 the process of producing
hydrochloric acid, magnesium sulfate and sodium sul-
fate by heating to 2000 a mixture of about 2 parts
niter cake and 1 part magnesium chloride, draining
off the hydrochloric acid thereby produced, and separa-
ting the sulfates by crystallization. Magnesium sul-
fate may also be made by stirring hot niter cake into
magnesite or dolomite, forming a spongy mass from
which the sulfate may be extracted with water and
] crystallized.10 Bouchard-Praceig11 and Rollo12 propose
\ the employment of niter cake as a means of decom-
posing solutions of bleaching powder, thus obtaining
free chlorine and gypsum. Cheeseman13 claims the
process of using it, after neutralizing, by making it
react with barium hydrosulfide to produce blanc fixe
1 British Patent 110.405 (1916).
» British Patent 10,450 (1902).
» British Patent 12,832 (1915); C. .4., 11, 878: /. Soc. Chcm. Ind., 36
■ 1916), 155; C. .4., 10, 1408.
•British Patent 19.530 (1893).
• U. S. Patent 726,533 (1903).
• U. S Patent 714,846 (1903).
'7. Soc. Chtm. Ind., 34 (1916), 1121.
' Tni3 Journal, 10 (1918), 238.
' U. S. Patent 1,203,357 (1916); C. A., 11, 88.
10 From Rev. des prod. chim.. cited in This Journal, 10 (1918), 228
" French Patent 221,245.
" British Patent 6,898 (1904).
1 U. S. Patent 714,145 (1902).
(BaS04) and sodium hydrosulfide. Naef? suggests
neutralizing the free acid, reducing the sulfate by
means of fine coal at a red heat, and crystallizing the
product. A similar scheme has been patented by
the Verein Chem. Fabriken.2 Parker3 proposes to
neutralize a solution of niter cake with iron, and then
to treat with sodium carbonate or hydroxide.
Grossmann4 proposes to utilize it in the production
of an extra quantity of nitric acid by mixing it with
niter and charcoal and heating the mixture under
suitable conditions.
Its use has also been suggested for the following
purposes: To increase the extraction of copper when
roasting copper pyrites by charging.it into the lower
doors of a multiple hearth furnace; alone, or with salt,
in the roasting of ores; to replace sodium carbonate
in opening up tungsten ores; as a source of acid for
leaching copper, zinc, or other metals, in the prepara-
tion of sulfates from scrap metal; for converting
chromate into dichromate; for the liberation of phenol
from its sodium salt in the process of manufacture
of phenol; in laundry work, to replace some of the weak
acids now used; in reclaiming rubber from scrap;
in the refining of petroleum; in the making and
glazing of slag bricks; as a weed killer; for flushing
drains; and as a possible means of keeping down flies
by sprinkling it on manure heaps.
In conclusion, it may be pointed out that the best
mode of using a solution of niter cake for any particular
purpose could be ascertained from the appropriate
solubility data; this involves the investigation, through-
out a range of temperature, of the three-component
system Na2S04-H2S04-H20, and of four-component
systems such as Na2S04-H2S04-FeS04-H20, investiga-
tions which would not be difficult to carry out with
the needful accuracy,6 and would be of scientific in-
terest as well as of technical importance at the present
time.6
American Zinc, Lead and Smelting Company
St. Louis, Mo.
CHEMICAL TESTS FOR THE DETECTION OF RANCIDITY
By Robert H. Kerr
Received March 7, 1918
Numerous tests have been proposed for the recog-
nition of rancidity. None of them seem, however,
to have found any wide-spread application. This
may be ascribed to two causes: first, there is con-
siderable confusion of ideas as to exactly what is
meant by the term rancidity; and second, once a fat
has become definitely rancid, its condition is so clearly
evident that no chemical test is needed to recognize it.
While it is true that the recognition of rancidity
by taste and odor is so easy that there is no need for
the use of chemical tests in the case of fats which have
definitely become rancid, there are yet many cases
> /. Soc. Chcm. Ind.. 34 (1916), 1121.
' German Patent 231,991 (1909); C. A., 6, 2709.
' British Patent 24,639 (1903).
• J. Soc. Chcm. Ind.. 36 (1917), 1035.
' Some data on the above system are presented by Le Chatelier and
Bogitch, K.-v. mllttll., 13 (1915), 949, who find that a double salt, NatSOi.-
FeSOi 2HiO, separates under certain conditions.
8 Work along this line is in progress under the direction of Professor
H. W. Foote. of Yale University.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 6
in which a reliable chemical test may prove of value.
If the fat has a strong natural odor, or has absorbed
an odor by reason of contact with an odoriferous sub-
stance, the recognition of the early stages of rancidity
may well be interfered with. Mixing of the rancid
fat with a fresh fat, particularly if the latter has a
strong natural odor, may serve to disguise its condi-
tion long enough to permit the marketing of an unfit
fat for food. Manufacturers, refiners, dealers, and
large users might find it of great advantage in many
cases to be able to recognize the onset of rancidity
before it became evident to the senses of taste and smell.
Rancidity is a chemical change in the fat due to the
action of oxygen. Its development and progress are
accelerated by certain accessory factors, notably light,
heat, presence of moisture, and contact with certain
metals, but oxygen is absolutely essential. Without
oxygen there is and can be no rancidity. The reactions
involved appear to be complex. The products formed
are numerous, and subject to variation, both with the
character of the fat and the stage of rancidity. It is
not the present purpose to discuss the products formed,
but it may be stated that aldehydes, ketones, and acids
of less molecular weight than those originally present
appear to be constant constituents of rancid fats.
Most, if not all, of the chemical tests proposed for the
recognition of rancidity depend on the presence of
one or all of these classes*of bodies, and it is to such
bodies that the characteristic odor and taste of rancid
fats are due.
Two of the many tests proposed for the detection
of rancidity have been studied in the Meat Inspection
Laboratory of the Bureau of Animal Industry at
Washington. D. C, and both have been found to be of
use. These two are the phloroglucin-hydrochloric
acid, color reaction of Kreis, and the "oxidizability
value" of Issoglio. A modification of the Kreis test
has been found to be of greatest value in judging fats
suspected of rancidity.
The Kreis test1 consists in shaking the fat with strong
hydrochloric acid and a i per cent solution of phloro-
glucin in ether. If the fat is rancid a red or pink color
is developed, the depth of color being proportional to
the degree of rancidity. Kreis ascribed the reaction
to the presence of aldehydes and ketones in the rancid
fats.
Winckel2 investigated the Kreis test and condemned
it on the following grounds: first, that it is not specific,
being given by other aldehydes and ketones than those
which occur in rancid fats; second, that the depth of
color is not exactly proportional to the degree of ran-
cidity; and third, that the test is far too delicate to be
used as a means of distinguishing sound from rancid
fats.
The Kreis test has been given a very thorough study
in the Washington Meat Inspection Laboratory.
The difficulty experienced in dealing with fats in which
rancidity is present but the characteristic taste and
odor masked by "off" or offensive odors and tastes
due to other causes and in distinguishing between such
' Vtrhandlunttn dcr Nalurforschcndtn Gesclhchafl in Basrl, 15 (1903 4),
225.
' Z. Nahr. u*d Ctnussm., 9 (1905), 90.
fats and similar fats which were not rancid, made the
need for a chemical test acute. The Kreis test was
chosen as the most promising of the chemical tests
described in the literature and was given a thorough
and careful study. The results of this study con-
firmed the objections raised by Winckel and also dis-
closed the fact that some oils, notably crude cottonseed
oil, contain bodies which cause them to give the test
when in a perfectly sweet condition. Nevertheless,
a field of usefulness was found for the test in dealing
with samples in which the characteristic odor and taste
of rancidity were obscured. Samples of this character
can be definitely and accurately classed as rancid or
not rancid by the use of the Kreis test. The test has
been in regular use since 1909 for this purpose and for
confirmation of judgment based on physical evidence
and has been found to be valuable and reliable when
used with strict regard to its limitations. As a result
of experience and testing against many hundred samples,
both of known and unknown character and condition,
the following statements regarding the test may be
made:
1 — All rancid fats react to the Kreis test.
2 — The intensity of the reaction is roughly but not exactly
proportional to the degree of rancidity.
3 — Fresh, sweet fats do not give the reaction except in certain,
special cases. Such a case is that of crude cottonseed oil which
reacts with great intensity. In this case the substance which
causes the reaction is removed by refining with caustic soda.
4 — The Kreis test is too delicate to be used alone as a criterioni.
of rancidity. If all fats which react were to be pronounced
rancid many samples which are not rancid in any sense would
have to be condemned as rancid.
5 — The Kreis test is not specific for rancid fats. It is given,
by aldehydes and ketones, other than those which occur in rancid
fats, by most of the essential oils, by crude cottonseed oil and
probably by other crude oils.
In making use of the Kreis test for the detection of
rancidity, it is necessary to guard against a reaction
due to the presence of any reacting substance, other
than those due to rancidity. If such a substance is.
present any conclusion drawn from a positive reaction
is w-orthless. While the necessity of guarding against
this source of error limits the use of the test to some
extent it does not greatly affect its value, as all of the-
animal fats and all refined vegetable oils are free from,
reacting substances. These are exactly the classes
of fats most likely to become rancid and most likely
to required laboratory examination to determine ran--
cidity.
The extreme sensitiveness of the Kreis reaction is-
not wholly a drawback. It enables one to predict
the appearance of rancidity before it becomes evident
to the senses. When a fat becomes rancid it under-
goes certain definite changes which follow one another
in orderly sequence. The time required to pass through
each stage is variable and depends on several E
but the different stages are always the same. The
appearance of the Kreis test marks the beginning of
an early stage of incipient rancidity and gives warning
of the onset of rancidity some time before the changes-
have progressed to such a point as to be evident to
the senses. Under most conditions the interval of
June, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
time between the first appearance of the Kreis test
and the appearance of sensible rancidity is sufficient
to permit the conservation of the product by immediate
use. The practical utility of this is evident.
In the use of the reaction as a criterion of rancidity,
however, its extreme sensitiveness becomes a draw-
back. If all fats which give a reaction are to be con-
demned as rancid, a great many of which are not rancid
in any true sense of the word must be condemned.
At the same time it has been found that any fat which
gives a positive Kreis test but does not have a rancid
smell or taste, is in a state of incipient rancidity, and
that the characteristic physical signs will soon develop.
For these reasons, the use of the Kreis tests is chiefly
limited to the confirmation of suspicions of rancidity
based on taste and odor and to reaching a definite
decision in those cases in which the odor and taste
of rancidity are masked by other odors and tastes.
It has proved of great value in this connection.
In applying the test to practical use it was found de-
sirable to find a means of judging its intensity. After
considerable work, a method was devised and tried out.
Trial of this method led to several changes and im-
provements. The method now in use in the Meat
Inspection Laboratories of the Bureau of Animal
Industry is based on the original method of the writer
and has been modified as a result of suggestions made
by Mr. C. H. Swanger and Mr. C. T. N. Marsh of the
Meat Inspection Laboratories of the Bureau of Animal
Industry located at New York, N. Y., and St. Louis,
Mo. The method as now used is as follows:
10 cc. of the suspected oil or melted fat are placed in a large
test tube (8 X i), and 10 ee. of strong HC1 (sp. gr. 1.19) added.
The tube is closed with a rubber stopper and shaken vigorously
for approximately 30 sec. Ten cc. of a o. 1 per cent solution
of phloroglucin in ether are then added and the tube closed and '
shaken as before. It is then allowed to stand. If the fat is
rancid, a red or pink color will appear in the acid layer. The
depth of this color is roughly but not exactly proportional to
the degree of rancidity. To determine the intensity of the re-
action the original fat is diluted with kerosene or with an oil or
fat which does not react and the intensity judged by the degree
of dilution at which a reaction ceases to be observed. In judging
this point a recognizable red or pink shade is regarded as a re-
action; a faint orange or yellow is not. The intensity of the re-
action is reported in terms of the highest dilution at which a re-
action is obtained. For example, if a fat is found to react when
so diluted that there is 1 part of the fat in 20 parts of the mixture
but not in higher dilution, it is reported as reacting in dilution
1 to 20.
In the work of the Washington Meat Inspection
Laboratory it is the custom to make two dilutions,
one containing 1 part of the suspected fat in 10 parts
of the mixture and one containing 1 part of fat in 20
parts of the mixture. Fats are thus divided into four
classes as follows:
Class 1 — Fats giving no reaction.
Class 2 — Fats giving a reaction when undiluted, but no re-
action in dilution 1 to 10.
Class 3 — Fats giving a reaction in dilution 1 to 10 but none in
dilution 1 to 20.
Class 4 — Fats giving a reaction in dilution 1 to 20.
Class 1 represents fresh sweet fats. Fats of this class
arc fit for any use and may be expected to withstand
severe exposure before becoming rancid. Class 2
represents fats which have not yet become rancid to
taste and smell, but in which those changes which will
later manifest themselves as rancidity are already in
progress. Class 3 represents a late stage of incipient
rancidity. Fats of this class are well advanced on the
road toward rancidity and their condition is usually
evident to the senses of taste and smell. Class 4
represents fats which have definitely become rancid.
One who is familiar with the taste and odor of rancid
fats has but little need for chemical tests when dealing
with this class.
Kerosene has been found most convenient for use
as an indifferent oil for diluting. Some kerosenes
have, however, been found which gave red or yellow
colors. To avoid error on this account it is recom-
mended that each lot of kerosene be tested and, if
necessary, purified. The following method of purifica-
tion has been found effective:
2000 cc. of kerosene are shaken vigorously in a large separatory
funnel with 50 cc. of HC1 (sp. gr. 1.19). After separating, the
acid is drawn off, a fresh portion of 50 cc. added and shaken
again. After separating, the kerosene is shaken with a third
portion of the acid. A few drops of the phloroglucin solution
used in the test are added before the third shaking. If the
separated acid shows a red color it is drawn off and the shaking
with successive portions of acid continued until the separated
acid ceases to show red. The kerosene is then washed three
times in the separatory funnel with 500 cc. of warm water. After
the last washing it is allowed to stand some time in a warm place
and the last portions of separated water carefully drawn off.
It is then transferred to a large beaker and heated to approxi-
mately 80 to 90 ° C, 50 g. of fuller's earth are then added, with
stirring, and the oil held at 80 to 90 ° C. with stirring for 5 min.
The fuller's earth is then removed by filtration. Kerosene puri-
fied in this way is completely indifferent in the Kreis test and will
remain so.
The "oxidizability value" test of Issoglio1 depends
on the presence in rancid fats of volatile organic bodies
which are separated by distillation with steam and esti-
mated by titration with a standard solution of potas-
sium permanganate. These substances are produced
by oxidation of the fat, are normal constituents of
rancid fats, and increase in amount with increasing
rancidity.
The method as described by Issoglio is as follows:
From 20 to 25 g. of the sample are mixed with 100 cc. of water
and distilled in a current of steam, so that 100 cc. of distillate
are collected in 10 min. Ten cc. of the homogeneous distillate
are then mixed with 50 cc. of water, 10 cc. of 20 per cent sulfuric
acid, and 50 cc. of N/100 potassium permanganate solution,
the mixture heated to the boiling point and kept boiling for 5
min. in a flask connected with a ground-in condenser. After
cooling, the liquid is treated with 50 cc. of N/100 oxalic acid and
titrated with N/100 potassium permanganate solution. If N
represents the amount of potassium permanganate required
for the oxidation and n that required in a blank test, and P the
weight of fat taken, the oxidizability value of the fat may be
expressed by the equation
X = (N — »)8o
P
Hence the oxidizability value represents the mg. of oxygen
required to oxidize the organic compounds separated under
constant conditions from the f:it
1 G. Issoglio, Ann. chim. appUcattt, 1916, 1-18.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No 6
With regard to the significance of the results ob-
tained, Issoglio states that the oxidizability value of
sound, fresh fats varies from about 3 to 10, while rancid
fats show much higher values. Oils and fats which
show a value of 15 or more are said to be rancid or to
have undergone some other change.
Comparison of results obtained by Issoglio's method
with the writer's modification of the Kreis tests is
shown by the following table:
Oxidizability
Sample
Value
No.
Material
(Issoglio)
Kreis Test
1099
Lard
14.72
Class 1
no reaction
839
Cottonseed Oil
7.92
Class 1
no reaction
1046
Coconut Oil
8.00
Class 1
no reaction
763
Tallow
8.32
Class 1
no reaction
1295
Lard
3.84
Class 1
no reaction
1047
Soy Bean Oil
13.44
Class 2
react
on less than 1
: 10
1188
Lard
4.16
Class 2
react
on less than \
: 10
1200
Lard
5.44
Class 2
react
on less than 1
: 10
1359
Lard
10.24
Class 2
react
on less than 1
: 10
1376
Lard
12.16
Class 2
react
on less than 1
: 10
923
Lard
10.56
Class 2
react
on less than 1
: 10
924
Lard
12.80
Class 2
react
on less than 1
: 10
889
Lard
19.52
Class 3
react
on between 1 :
10 and
847
Soy Bean Oil
16.96
Class 3
react
on between 1 :
10 and
329
Lard
17.28
Class 4
on more than
1 : 20
1360
Lard
10.88
Class 4
react
on more than
1 : 20
XXI
Lard
7.04
Class 4
on more than
1 : 20
1412
Inedible Grease
23.36
Class 4
react
on more than
1 : 20
XX2
Lard
18.84
Class 4
react
on more than
1 : 20
XX3
Lard
21.12
Class 4.
react
on more than
1 : 20
It is found that the results conform in the main to
the standards set. If fats of Classes i and 2 with, re-
spect to the Kreis test are regarded as sweet, and fats
of Classes 3 and 4 are rancid, the oxidizability values
of the sweet fats vary from 3.84 to 14.72, and all values
above 10, with one exception, are found in Class 2.
The oxidizability values of the rancid fats with two
exceptions are found to be above 15, the lowest value
being in fact 16.96. The two exceptions which were
found to have oxidizability values of 7.04 and 10.88,
respectively, were rancid beyond any possible question,
being strongly rancid to taste and smell, besides giving
the Kreis test in dilution 1 : 20. It would appear
fair then to regard an oxidizability value of 15 or more
as strong confirmatory evidence of rancidity.
In working with Issoglio's method it was noted that
the distillate was clear, showing that the oxidizable
organic bodies which came over were all soluble in
water. Experiments were made to determine the
relation between the total amount of water-soluble
and volatile oxidizable organic bodies. After some
preliminary experiments the following method of ex-
traction was determined upon:
25 g. of the fat are weighed into a 200 cc. Erlenmeyer flask
and 100 cc. of distilled water added. The flask is allowed to
stand on the steam bath for 2 hrs. with occasional shaking. At
the end of this time the water is separated from the fat by filtering
through a wet filter paper. The paper is closely fitted to the
funnel and thoroughly wetted. The whole contents of the flask
are poured on the wet paper. The water containing the soluble
matters extracted from the fat runs through, while the fat is
completely retained by the wet paper. The filtrate is caught in
a 100 cc. graduated flask. After cooling, the flask is made up
to the mark, shaken thoroughly and 10 cc. taken for titration
Oxidation is carried out exactly as specified by Issoglio. The
results obtained are, therefore, directly comparable, those by
the original method representing volatile organic matters sep-
arated by distillation and those by the modified method repre-
senting total water-soluble matter.
Following are some of the results obtained by the
water extraction method:
Oxidizability
Sample No.
Material
Value
Kreis Test
4155
Lard
8.96
Class 1, no reaction
4187
Lard
7.36
Class I. no reaction
4263
Lard
10.24
Class 1, no reaction
3680
Lard
15.68
Class 4. reaction 1 :
20
4154
Lard
19.84
Class 4. reaction I :
20
4327
Lard
16.00
Class 4, reaction 1 :
20
4328
Lard
14.40
Class 4, reaction 1 :
20
The results obtained were seen to be similar to those
obtained with like samples by the distillation method.
The two methods were then compared directly. For
this purpose a lot of fat which was being purposely
allowed to become rancid was chosen. This had al-
ready been under observation by Issoglio's method
for some time. As the results are of interest and as
the progress of the sample is typical they are given in
full.
Oxidizability Value
By
By
Date
Distillation
Extraction
Kreis Test
Sept. 6
7.04
Reacts
n dilution 1
20
Sept. 20
8.32
Reacts
n dilution 1
20 (increased)
Oct. 4
11.20
Reacts
n dilution 1
30
Oct. 18
12.80
Reacts
n dilution 1
30 (increased)
Nov. 1
9.28
15!04
Reacts
n dilution 1
30 (increased)
Dec. 6
10.88
13.76
Reacts
n dilution 1
SO
Jan. 8
8.96
16.00
Reacts
n dilution 1
100
It will be noted that the oxidizability value, whether
determined by distillation or by extraction with water,
does not increase uniformly but fluctuates. This is
in sharp contrast to the Kreis test which becomes
more intense at an increasing rate. Observations of
taste and odor, while they cannot be compared by any
standard, leave no room for doubt that the Kreis
test shows the true condition of affairs much more
clearly than does the oxidizability value. The oxi-
dizability value obtained by extraction with water
appears to follow the actual condition of the fat as
judged by taste and smell more closely than does that
obtained by the distillation method. As shown by the
results quoted, the water extraction method gives
slightly higher figures. As the extraction method may
be carried out more easily and with less close attention
than with the distillation method it is regarded as
preferable.
The utility of the methods described depends on
their application. Both methods must be applied
with strict regard to their limitations. The Kreis
test shows the presence of certain aldehydes and ketones.
We know that such bodies are formed in that type
of chemical change that we know as rancidity. When
we find such bodies in a fat which is by the circum-
stances of its origin and handling free from similar
bodies of natural origin, or which we know, by test,
to have been free from such bodies at a previous
time, we may then fairly accept the test as evidence
of rancidity. The method of determining the intensity
of the reaction by dilution with an indifferent oil en-
ables one to record degrees of rancidity in definite
figures, to compare the rancidity of different samples
examined at different times, to establish standards
of fitness for any purpose, and to determine definitely
whether or not any given sample conforms to those
standards. The determination of the oxidizability
value, either by Issoglio's method of distillation or
preferably by the water extraction method, is a measure
of the presence of volatile or soluble products of oxida-
tion. It yields less exact and definite information than
June, iqiI
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
475
is given by the Kreis test, yet has a certain value as
a confirmatory test. The products of oxidation on
which it depends being water-soluble and volatile, can
readily be removed from the fat by washing, or by blow-
ing with steam or air. A rancid fat, freshly washed
or blown, would have an oxidizability value little, if
any, greater than if fresh and sweet, but would be
little less the rancid on that account. A high oxi-
dizability value taken in connection with the usual
physical signs of rancidity is to be regarded as con-
firmatory evidence of rancidity. A low value cannot,
however, be held as conclusive evidence of the absence
of rancidity. A negative reaction to the Kreis test can
be so regarded. Examination of several hundred
samples, during a period of over eight years, has failed
to disclose a single sample which displayed the physical
evidences of rancidity and at the same time failed to
give the test.
If adequate precautions are taken to exclude the
known source of error and due allowance is made for
its supersensitive character, the evidence given by a
positive reaction is definite and dependable. The
method described above for determining the intensity
of the reaction affords a trustworthy and sufficiently
accurate means for the measurement of degree of ran-
cidity.
Meat Inspection Laboratory
Bureau of Animal Industry
Washington, D. C.
NOTES ON THE COLOR DESIGNATION OF OIL
VARNISHES'
By F. A. Wertz
Received January 23, 1918
In the writing of varnish specifications and in the
examination of varnish samples, it is often desirable to
designate the color of the material desired, or of the
sample examined. Thus, the varnish specifications of
some of the Government Departments and of some
of the other large varnish consumers state that the
material submitted shall not be darker in color than
that of a standard sample which is held by the con-
sumer.
The varnish manufacturer, however, usually desig-
nates the color of his products by a number, represent-
ing the color of a varnish in an arbitrarily established
color scale. Such a scale is made from a series of
varnishes, whose color is permanent to light; the
lightest varnish obtainable, usually a white dammar,
forms the one end, and the darkest commercial varnish
forms the other end of the scale. Such a scale usually
consists of ten standard samples, numbered from No.
i, the lightest, to No. io, the darkest. Any given
varnish is then designated, according to its color, as
No. 3, No. 7, etc. In practical work, this designation
is sufficiently definite for all purposes; but for manu-
facturing control work, slight differences in the depth
and even in the shade of the color often have some
particular significance. Many manufacturers, there-
fore, are not content to designate by the whole numbers,
but subdivide the scale, and described a color, for
example, as 4.6, indicating that it is lighter than No.
1 Published by permission of Director of U. S. Bureau of Standards.
S, darker than No. 4, and somewhat nearer in color to
No. 5 than to No. 4. For the use of an individual
manufacturer, this scheme is probably satisfactory,
but it is doubtful if the color scales of any two manu-
facturers coincide at more than one point, if at any.
It is desirable, therefore, to have some simple means
of designating the color of a varnish which will obviate
the necessity of retaining a standard sample of ma-
terial of satisfactory color, and which will enable the
varnish manufacturers to establish the most important
points on their color scales.
The most convenient method for this purpose is the
use of an easily prepared solution, whose color is
fixed by its composition. In attempts to find a suitable
solution a large number of colored salts in a variety
of solvents were tried, but the most satisfactory re-
sults were obtained by the use of potassium dichromate
in concentrated sulfuric acid. By varying the quantity
of dichromate, the color of almost any varnish, with
the possible exception of the very light-colored turbid
dammars, can be reproduced, so that it has been found
possible to imitate not only the depth of color but also
practically the exact color shades of a great variety
of commercial varnishes submitted to this laboratory.
No difficulty was found in thus producing a color
scale by which the color of a varnish can be defined
at least as accurately as by a 10-point scale, such as is
used by varnish manufacturers. The dilute dichrom-
ate-sulfuric acid solutions are decidedly yellow, like
the lighter varnishes, and the more concentrated
solutions are a deep rich red as are the darker varnishes.
A solution of 0.25 g. of dichromate in 100 cc. of sulfuric
acid represents a very light colored varnish; 1.0 g., a
medium colored; 2.0 g., a dark colored; and over 4 g.,
a very dark colored varnish.
The method of making the solutions consists in
dissolving a weighed quantity of pure powdered
potassium dichromate in a measured quantity of pure,
colorless, concentrated sulfuric acid of sp. gr. 1.84.
The solution and varnish, whose color is being matched,
are placed in separate, thin-walled, clear glass tubes
of the same diameter (1 to 2 cm.), to a depth of not
less than 2.5 cm., and are compared by looking trans-
versely through the column of the liquids by trans-
mitted light. The solutions corresponding approxi-
mately to the color scale of one of the large manu-
facturers are as follows:
Number Grams of KuChOt
in scale in 100 cc. H2SO4
2...'*.!!""!'"I!"!I"!""""! olio
3 0.25
4 0.35
5 0.50
6 100
7 1.50
Si; 2.00
9 4.00
10...... 8.00 +
(o) Is a pale white dammar with which no satisfactory comparison
can be made.
Upon standing, the darker colored solutions may tend
to deposit crystals of chromic anhydride. To prevent
this, it is sometimes necessary to warm the solution
and make the color comparison while the solution is
perfectly clear. Warming the acid to hasten the solu-
tion of the dichromate, or to produce a clear solution
476
THE JOURNAL OF INDUSTRIAL A X D ENGINEERING ( HEMISTRY Vol. io, No. 6
a1 the time of making a comparison, seems to have no
ffect on the color. There is always more
or less reduction of the chromic acid, if it comes into
contact with even very small particles of dust or dirt,
so that the safest procedure is to use only freshly
prepared solutions. These are easily made and the
color given by a definite quantity of dichromate is
readily reproducible.
The above-described method has been used in several
varnish specifications with very satisfactory results
and there has been favorable comment from all varnish
men who have tried the method. It is not intended
that the method should give an optically perfect
color match of a varnish, but that it should be a suffi-
ciently accurate method of designating the color of a
varnish to make it applicable for all practical purposes
where the color of a varnish is to be described or fixed.
ADDRL55L5
PLANNING A RESEARCH LABORATORY FOR AN
INDUSTRY1
By C. E. K. Mees
During the last two years the importance and value of indus-
trial research have become widely recognized, and there has been
a general awakening on the part of those who control industries
to the desirability of including in their organization a research
laboratory to act as a nucleus of scientific knowledge for the
industry, and to carry out specific investigations which are
judged to be of value.
When the executive directing such an industry, however,
looks for information as to how to proceed in order to establish
a research laboratory, he is likely to find that the specific in-
formation which he requires is by no means easy to obtain.
While there are many articles pointing out the value of a re-
. search laboratory, little has been written as to the steps which
should be taken by an industry that has determined to establish
one.
Let us take the hypothetical case of the vice president of a
company who, as a result of his reading, has become convinced
of the desirability of establishing a research laboratory, but
who, himself, has no experience in scientific work of any kind,
knows only that the greater part of scientific research is done
in university laboratories, and has no idea either of the cost of
a laboratory, of how it should be established, or of what return
he can expect from it. What is he to do in order to present a
specific case to his fellow executives, or to proceed in the es-
tablishment of a laboratory, should he be empowered to do this?
The object of this paper is to suggest a specific answer to the
problem of such an executive, putting the answer in such terms
that it may be applicable to a large number of different in-
dustries.
In considering the organization of an industrial research lab-
oratory we must deal first with the relation of the research lab-
oratory to the rest of the organization of which it is a part, and,
second, with the internal organization of the laboratory itself.
The relation of the laboratory' to the other departments of the
company will be closely associated with the origin of the lab-
oratory.
If there is a technical scientific expert in the executive staff
of the manufacturing company, he may have established the
laboratory and become its director, and in this case the labora-
tory will necessarily be very' closely associated with the work
of the executive who initiated it.
A laboratory may also be established under a separate direc-
tor, not himself associated with the executive officers of the com-
pany, but as a reference department for the executives. In
this case also it will be very closely associated with the officers
nt the company and will tend to be more concerned with ques-
tions of policy and the introduction of new products than with
any other of the problems of the company.
Iddres delivered M>ril 12, 1918, before the New Vork Section of
the Society of Chemical Industry, the American Electrochemical Society,
uud the New Vork Section of the American Chemical Society.
In a large company a research laboratory may be established
as a separate department having its own organization, and be
available as a reference department for all sections of the com-
pany, in which case its activities will cover a very wide field,
but at the same time it will not have as direct an influence upon
the policy of the company as will happen if it is closely associated
with one or more of the executive officers.
Whatever the size of the industrial concern may be, the or-
ganization of the research laboratory should be responsible di-
rectly to the management.
The work of a research laboratory almost always involves
questions of policy, and not merely manufacturing questions,
and frequently close connection with the advertising and selling
departments of the company is very necessary. In several
cases where research work has been conspicuously successful,
this has been the case.
Let us assume, therefore, that on the establishment of the re-
search laboratory we are considering, arrangements will be made
in the organization of the company by which the laboratory will
be brought into contact not only with the manufacturing sec-
tions of the company but with the financial and sales direction.
Turning next to the internal organization of an industrial
research laboratory, there are two forms of organization possi-
ble. For brevity these may be spoken of as the "departmental"
system and the "cell" system.
In the departmental system the organization is that familiar
to most businesses. The work of the laboratory' is classified
into several departments : physics, chemistry, engineering, and
so on, according to the number necessary to cover the field,
and each of these departments has a man of suitable scientific
attainments in charge of it. In a large department each of these
men will in turn have assistants responsible for sections of the
department, all the heads of departments finally being responsible
to the director of the laboratory. Under the alternative or cell
system the laboratory consists of a number of investigators of
approximately equal standing in the laboratory, each of them
responsible only to the director, and each of them engaged upon
some specific research. Each such investigator, of course, may
be provided with assistants as may be necessary.
Each of these systems has advantages and disadvantages.
Under the departmental system the advantages are strict or-
ganization, good cooperation throughout the departments.
a plentiful supply of assistants for the more able men who form
the heads of departments or sections of the departments. The
chief disadvantage is that the system tends to stifle initiative
in the younger men While it is true that research men require
to serve a considerable apprenticeship to older investigators,
there comes a time when every man wishes to try to develop
his own line of research on his own initiative and to carry out
work by himself, and while it is quite possible to provide for such
men in a departmental organization, there is some danger that
men who are really capable of original work may not get the op-
portunity to carry it out. The cell system, on the other hand,
provides a good arrangement for men of original initiative and
June, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
of the self-reliant type; it enables a man to continue a single line
of work by himself for a long time and to bring to a conclusion
work which in a departmental organization might have been
abandoned because of its apparently unremunerative character.
On the other hand, the cell system tends to exaggerate the vices
of such men. They tend to become secretive, to refuse coopera-
tion, to be even resentful if their work is inquired into, while if
a man who has developed a line of work for himself in a cell
leaves the laboratory, it may be difficult for anybody else to take
up the work, in which case a great deal of time and money is
lost, and work which should have been carried forward is left
unfinished. Another objection to the cell system is that men
who are good organizers and who are of the type of men that
can carry on work requiring many assistants do not easily find
a place in it.
In practice, some system between these two systems of or-
ganization is essential and will develop in any laboratory. It is
not possible to work a rigid departmental system, and, on the
other hand, no cell system in its most definite form could be
effective. The form of organization which is the easiest in ad-
ministration is undoubtedly some modification of the depart-
mental system, since only by this means can young students,
fresh from college, acquire adequate training and at the same time
keep in touch with different branches of their subject and avoid
the danger of overspecialization too early. A laboratory should
therefore be organized in departments with an intra-departmental
arrangement under which a young man who develops the ability
to carry out his own work may be able to take up work on his
own initiative, still retaining his position in the department and
carrying on his work under the general supervision of the chief
of his department. There will always be a tendency in the de-
partmental organization for men to desire to split away from the
department to which they are attached and become semi-
independent in the laboratory, and this tendency must be re-
sisted in the organization and by the director of the laboratory.
At the same time, it is important that too rigid a control should
not be exercised so that men feel that they are prevented from
exercising their own initiative.
A laboratory for a specific industry will generally tend to be
of what has been called the "convergent" type, that is, one in
which all the different sections of the laboratory representing
different branches of scientific work have their energies directed
towards the solution of problems relating to the same subject.
The problems of such a laboratory' will, therefore, all be inter-
related and the work of the laboratory will be directed towards
one common end.
The organization of such a convergent laboratory has been
discussed in a former paper.1 It is shown there that charts
could be prepared illustrating the organization which would be
available for almost any convergent laboratory, so that, if we
have to work out the organization of a research laboratory which
is to study any interrelated group of problems, we can do it
by the construction of similar charts. Thus, we may arrange
a chart showing the derivation of the branches of the subject
considered from the sections of pure science involved. We can
place on one side biological, physical and chemical problems,
subdividing each section so that each one represents work capable
of being handled by one man in the laboratory. It will now
be possible to draw a new chart, showing on the circumference
the different sections of the laboratory for which accommodation,
apparatus and men must be provided, and showing the relation
of these sections to the problem as a whole. Having worked
this out, it is easy to find the amount of space and the number of
men which will lie required, or which the funds available will
allow for each part of the work.
Now, before applying these charts for laboratory organiza-
tion to a specific industry, let us look at the question of the
1 This JooiiNAi., 9 H9I7), 1137.
physical organization of the laboratory itself: the building and
scientific equipment, the cost of building, and the cost of the
maintenance and operation. It may be mentioned here that
when a laboratory' is under consideration by the executive of a
company, the matters which usually concern his mind are these
physical details, and he is often greatly concerned with the
planning and cost of the building and equipment, a matter which
is quite secondary to the internal organization of the laboratory,
either as regards effect on the work or even from a financial
point of view.
The laboratory should be housed in a convenient, special
building. It is very' advisable that all research work under the
same general direction should be conducted under the same roof,
since only in this way can good cooperation between the depart-
ments be obtained, and the facilities and organization of the
whole department be available to all the workers. In technical
research, where it is often necessary to install model plants on a
small scale, this cannot always be carried out, but, as far as possi-
ble, a research laboratory should be a real building and not
merely the name for a number of scattered departments at some
distance from each other.
It is a mistake for a factory to house a research laboratory in
some abandoned building designed for other purposes. The
annual cost of research work, as will be shown later, is very high
in comparison with the cost of the building itself. The greater
part of that expenditure is on the salaries of the men carrying
out the work, and any inconveniences or disadvantages which
may be caused by their working conditions and surroundings
can easily depress the production to an extent which renders
such economies very unprofitable. The cost of the research
man, in fact, is so high that it is worth while to provide him with
the very' best facilities for carrying out his work, since, provided
money is not actually wasted on useless ornaments, these facili-
ties will always be inexpensive in comparison with the total ex-
penditure on the work.
Research laboratories are almost always too small, and it is
really desirable that, in designing such a laboratory, some system
of construction should be chosen in which expansion can be ob-
tained by the duplication of units. This is, of course, a very
difficult thing to arrange, especially in the details of the labora-
tory, but, nevertheless, it should certainly be aimed at by the
architect, since, whatever the size of the laboratory when it is
designed, it is safe to prophesy that, within a very few years ex-
pansion will be necessary, and if direct expansion is not possible,
this will take the form of detached groups of men working in
other places, an inconvenient and uneconomical arrangement.
The cost of moving in research work is not always realized.
The cost of moving into a new building may be as much as
half the total cost of the building, since the men will actually
not be working again at full speed in less than six months, and,
as a general rule, the annual expenditure is equal to the cost of
the building and equipment. It is important, therefore, in de-
signing a laboratory' to arrange, if possible, that expansion may
take place without any considerable rearrangement. An aid
to this is to make the internal divisions of a laboratory movable
as far as is possible, and while the laboratory itself should be of
fire-proof construction, it will be convenient to make partitions
of composition board and wood wherever tin- lire risk does not
prohibit this. In this way, rooms can easily be subdivided,
combined or rearranged.
Everything that has been said as to the necessity for the pro-
vision of a satisfactory building applies also to the question of
equipment, but with even greater force. It is an economic error
to allow expensive men to be short of the apparatus which they
requiri for their work. As a general rule nun will not ask for
apparatus which they do not need. There are a very few men
who might be considered to be apparatus collectors, and who seem
to have a real anxiety to surround themselves with all forms of
478
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, Xo. 6
scientific apparatus, whether they have any use for them or not;
but with the exception of these men, who are limited in number,
it may be taken that when a research worker asks for apparatus
he needs it, and must have it in some form or other to continue
his work.
The total cost of equipment for a physical laboratory represents
about two months' cost of operation, and, if economies are to
be made, it is clear they should be made in limiting the amount
of work undertaken and the consequent cost of operation, rather
than in depriving the employed workers of the necessary tools
for their work.
From various sources of published information, as well as
from personal experience, it is possible to form an estimate of
the cost of a research laboratory per scientific worker employed,
taking the term "scientific worker" to cover all graduate men
working in the laboratory. It might seem that there would be
very great variation in the cost, but, provided that we confine
ourselves to laboratories of the physical and chemical type, there
is a surprising agreement between the different figures, which
show that cost of building and equipment for a laboratory will
be between $3000 and $4000 per man; it may be taken, there-
fore, that the first cost of a laboratory will be about $3500 per
scientific worker employed. From the same sources the annual
cost of maintenance of such a research laboratory appears to be
slightly lower than the first cost. Probably $3300 per man would
be a fair estimate of the cost of maintenance, and of this we may
take 60 per cent as representing salaries and wages and the other
40 per cent all other expenses.
Let us attempt to apply the principles which have been laid
down to the design of an industrial research laboratory ap-
plicable to a specific industry, in such a form that they would be
available for the directorate of the industry to understand to
what they are committing themselves in establishing a research
laboratory, and how to proceed in order to do so.
We may select as an example of a specific industry one of a
technical manufacturing type dealing with engineering processes,
handling chemicals, and also involving certain biological con-
siderations; such an industry, for instance, as textile dyeing or
the manufacture of leather goods. Exactly the same principles,
however, would apply to industries of quite a different kind. Thus,
an industry in which there are no biological considerations will
not require some branches of a laboratory; they may need to
substitute others in their place. For some industries, physics
is of no importance and chemistry is of far more importance.
Let us, however, in order to be specific, consider the question
of a plant whose business consists in the dyeing of textiles. Let
us suppose that the industry is making a turn-over of $1,000,000
a year, of which 10 per cent is net profit, and that the directors
have decided that, in order to improve their product and ex-
tend their business, possibly to diminish costs, they will at the
outset undertake an expenditure of $15,000 a year on scientific
research. Now, let us consider what they can do for this.
In the first place, we can decide at once how many men they
can get. On the basis of $3000 per man, they should be able to
get five men for $15,000, but with very few workers in the lab-
oratory, the cost per man will be somewhat higher, and it will
be safe to assume that only four men can be obtained for the
$10,000 available for salaries. The cost of the building will
be about $10,000 and equipment about $5000. Taking the
basis of $2.00 per sq. ft. for building as a rough approximation,
we shall have a building with 5000 sq. ft. of floor space, or, di-
viding this into three floors, a building about 40 ft. square. The
work of the laboratory may be analyzed according to the chart
shown herewith. Dividing into the three main divisions of
chemistry, physics and biology, we shall get the following sec-
tions for the work: In chemistry, we shall require an analyst
and dye chemist who must understand organic chemistry, and
a colloid chemist who will study the relation between the liber and
the dyes. In physics, we shall have work to do on the testing
of the strength of materials and especially on colorimetery and
the measurement of absorption. In biology, we shall require
a man who understands the vegetable and animal fibers, their
structure and their biochemical properties. We shall also re-
quire work on the staining of fibers and photomicrography.
This will give us the chart shown.
Now, we cannot hope, of course, to represent all these depart-
ments by separate men, since we can afford to have only four
men, and in addition to the departments shown we must have
one practical dyer having actual works experience. Our men
may be grouped somewhat as follows: Our organic chemist
can look after analytical chemistry as well, that is, we must
get a man having experience in organic chemistry and some good
knowledge of dyes, who can specialize in the study of dyestuffs
and on their analysis, but who also can do what analytical
chemistry it becomes essential for the laboratory' to carry out
We may expect our colloid chemist to be a biochemist and to
take care of the microscopy. The physicist may understand
colorimetry and, at the same time, know enough general physics
to be able to look after questions involving the strength of ma-
terials. We have thus accounted for three of our four skilled
men, and the fourth must be the practical dyer, who should also
be the director of the laboratory and should have a good training
in dye chemistry and general chemistry, with a considerable
knowledge of colloid chemistry and fibers, and some knowledge
of physics. Thus, the staff of our laboratory will be completed
by the director, who will be a chemist who has had works ex-
perience in dyeing, and who must be given this works experience
before the laboratory' is commenced if a fully trained scientific
research man is not already available from the works. It is of
no use to take a man from the works who is not fully trained in
research methods and in sympathy with scientific work, and if
such a man is not already available with a knowledge of dyeing,
then the best available man must be obtained from a university
or elsewhere and given the works experience to learn dyeing
before the construction of the laboratory is attempted.
The amount available for the salaries of these men will be
about $10,000 a year, which must be distributed as seems ad-
visible with regard to the men actually chosen. The sum should
be sufficient to obtain fairly good men, as a commencing salary.
We will next consider the structure of the laboratory itself.
It must be remembered that we have three floors, each of them
containing about 1600 sq. ft. Of these, one will be required for
June, iqiS
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
479
the library, office and the dye room, which will be a small edi-
tion of a works department containing small model machines
in which all the works processes of dyeing, washing and drying
can be carried out. This may occupy about half the ground
floor, the other half being taken up by the library, staircase, and
the laboratory office, which in such a small laboratory may be
united with the library. The next floor will be devoted to chem-
istry and may be divided into two or three rooms, while the top
floor will be used for physics and will contain rooms for ordinary
physical work and for colorimetry. It will also probably be used
for microscopy, since it is unadvisable to have microscopes and
similar instruments exposed to the fumes of a chemical laboratory.
An exactly similar design to this can be made out for any other
industry, the factor of size being determined by the expenditure
which it is proposed to make, and the work being dissected in
accordance with the demands of the particular industry in ques-
tion. Space must always be kept for a small replica of those
plant operations on the investigation of which the laboratory is
working, since it will often be necessary to prove the plant opera-
tions under the direct control of the men in the laboratory and
under conditions which can be rigidly maintained at any required
point.
Now, let us consider what returns may be expected from the
work of this laboratory.
The work of an industrial research laboratory may be classified
in three divisions:
A — Work undertaken on the initiative of manufacturing
divisions for the improvement of operations, for the lowering
of cost, or in order to locate manufacturing difficulties.
B — Work undertaken with a view to the development of new
materials or of new processes. This may be initiated by the
management, by manufacturing sections, by sales divisions who
see the need for such materials or processes, or by the director
of the laboratory or his assistants.
C — Work which deals with the fundamental theory of the
subject, the results of which, if successful, will lay a foundation
for the expansion of the industry as a whole, along lines which
usually cannot be foreseen when the research work is commenced.
The work classified under Division A is, of course, common to
all industrial laboratories, and many research laboratories in
connection with manufacturing plants confine themselves almost
entirely to problems arising from the manufacturing division.
Division B includes a large portion of the work of industrial
research laboratories and the best known successes of such lab-
oratories are included in this division. A typical example is
the development of the drawn wire tungsten filament by the re-
search laboratory of the General Electric Company, a research
which, although originating from a general research on the
properties of rare metals such as would be classified under Division
C, developed into a study of tungsten with the direct purpose of
obtaining a satisfactory filament lamp from the metal. Another
example is the manufacture of indigo by the Badische Company.
Such researches usually have their basis in some more fundamental
work; the industrial work on indigo, for instance, was made
possible by the original chemical work on the structure of indigo
carried out in the German universities, which was applied on
a manufacturing scale to the preparation of the dye.
More rarely do research laboratories work on subjects classified
under Division C, that is, on the fundamental theory of their
subject, yet those who do, achieve the most conspicuous suc-
cesses. The work of Professor Abbe on the theory of the micro-
scope, and, indeed, all the work on applied optics at Jena comes
under this heading. The great success of the Zeiss Works is
directly due to the attention paid by Abbe to the development
of the fundamental theories of optics. At the General Electric
Laboratory at present much attention is being paid to the emission
of electrons from hot bodies, and from this work there have already
developed the Coolidge X-ray tube and the kenotron high fre-
quency transformer, while the possibilities of application are as
yet only just beginning to be realized.
In a study of the work of a special research laboratory all the
work done during the year was analyzed out from a classification
of the work of each part of the laboratory, and the proportionate
expense found, which should be charged to each class of the work.
This analysis showed that Division A, that is, work done for
the manufacturing departments, corresponded to about 15 per
cent of the work of the laboratory; Division B, work on new ma-
terials, 47 per cent; Division C, or fundamental work, absorbed
27 per cent, of which 22V2 per cent was devoted to the scientific
work and 5 per cent to the accompanying educational work,
while work for the assistance and information of the office force
is estimated at s'/i per cent.
Now, considering this division of the work of the laboratory,
it will be agreed that, if proper coordination exists between the
laboratory and the management of the company, work classified
under A and B will certainly be reasonably remunerative, al-
though not necessarily so completely so as to pay the dividends
on an investment in the research laboratory, which are commonly
expected from such an investment. The same may not appear
true in the case of Division C, the fundamental work, which in
the hypothetical case discussed would represent nearly a third
of the total expenditure of the laboratory; nevertheless, it is
probable that this section of the work would be likely to prove
the most remunerative of all, and the way in which this can best
be illustrated is by some examples.
Let us consider graded examples of theoretical work in
relation to their application in industry.
First, let us take the case of such work as that done by Pro-
fessor Abbe on the geometrical laws which govern the formation
of images by lenses. The connection between this and the manu-
facture of lenses is so obvious that it is at once manifest that the
discovery of any new principle in the theory' of lens optics will
react immediately upon construction in some way, either in the
form of a new product or in cheaper forms of construction.
Next, let us consider work on improved methods of testing
such, for instance, as the work done by the various bureaus of
standards or research on analytical methods. Here it can be seen
that only the possession of an accurate method of testing will
enable the manufacturer to improve his product and to guarantee
the similarity of product made at different times. Consider,
for instance, the improvements in electrical measuring methods
and instruments which have made available the standardized
electrical equipment which is now so familiar to every one.
In the third place, we may take as an example such research
work as the study of the relation between inductance and capacity
in alternating electrical circuits, which has had such an immense
influence upon the design of alternating current electrical ma-
chinery. At the present time, of course, this is a recognized
fundamental portion of electrical engineering.
Lastly, let us consider such work as that of the universities
on the photoelectric effect, the diffraction of X-rays by crystals,
or the emission of electrons by hot bodies. Of these, the last
has already found extremely important commercial application,
the second one is being adopted by several industrial research
laboratories in making a study of the structure of metals, alloys,
and other crystalline substances, while the first, so far as I know,
up to the present has not found any industrial application, and
yet, it may safely be prophesied, will be of importance to industry
within the next ten years.
It is almost impossible to name any class of physical or chemical
scientific work, from the physics of the atom to structural or-
ganic chemistry, which will not sooner or later have a direct
application and importance for the industries.
Work in a research laboratory bears a certain analogy to placer
mining for gold. A man washing gold can make a living by
steady, hard work, but nobody would take up placer mining
480
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 6
with the intention of making a living by the every-day washing.
Evi rybody hopes to find nuggets which will give them a good
profit, and possibly even a fortune In the same way a research
laboratory can produce results equivalent to a large amount of
its expenditure by steady work, but from a commercial point
of view research is undertaken in the hope of the occasional
valuable discovery rather than for the steady output of small
The analogy can be carried somewrhat further. Just as in
plai ii mining it is of no use looking for nuggets, and any miner
who neglects the routine washing in search of nuggets is likely
to starve before he finds them, in the same way a research lab-
oratory cannot look for discoveries It can onlj carry' on its
everyday work on the problems presented to it, and hope that
when some possibility of a valuable discovery presents itself
it may recognize it in time to take advantage of the fact.
There is, however, one direction in which this analogy breaks
down. When a man finds a nugget, he knows its value and its
value is definite and certain; in research work this is not the case.
Discoveries which are thought to be valuable when made often
prove worthless, while others which appear to be of no value
eventually turn out to be profitable, and frequently the value
of a discovery is not under control of the laboratory because the
adoption and exploitation of it may be in other hands.
It is sometimes thought that in order to put an industry into
a state of complete efficiency from a scientific point of view all
that is necessary is to establish a laboratory and to employ a
scientific staff to carry out research work. It is quite possible,
however, for such a laboratory to have no influence whatever
upon the general policy of the company, and only a very slight
influence upon its manufactures, the value of a laboratory de-
pending very greatly upon the closeness of its cooperation with
the other departments of the company.
It is often felt that small industries cannot afford to support
scientific research, but this argument is exactly as if it were
suggested that small industries cannot afford to support ad-
vertising. The object of spending money on research, for a small
industry' at any rate, is not to support the research but to be
supported by it, and it is scarcely an exaggeration to say that
the smaller a business is, the more important is it that it should
make use of scientific research to the greatest extent possible.
A small business is at a disadvantage in comparison with a
large one in regard to all its cost charges. In the purchase of
raw materials, in manufacturing, and in selling, its cost per unit
of output tends to be larger than in the case of big businesses,
but, on the other hand, it is at a real advantage in regard to
flexibility and enterprise. Any large business must necessarily
be cautious and conservative. The amount at stake is so large
that the penalty of error is heavy- Consider, for instance, the
mere cost of allotting half a page in a catalogue of which three
million copies are to be printed. It is clear that no business man
will allow the introduction of a new article into a catalogue for
which such an edition is necessary unless he has reason to believe
that the demand will be sufficient to pay the cost involved. That
is, the machinery of a large business is adapted for the sale of
things for which there is a large demand, but it is difficult for
it to introduce articles for which the demand will probably be
limited and doubtful. Every large business is anxious to im-
prove its goods, since it knows perfectly well that the penalty
for failure to do this is extinction, but it necessarily moves with
greatei caution and more slowly than a small business can do.
It is this very fact, rightly grasped, which enables the small
business to get its start and grow in spite of the advantage in
regard to cost possessed by its larget com] etitor, and the growth
of a small business will depend Upon its supply of ideas for new
products and new methods to a fai greatei extent than will
that of the big manufacturing concern making staple products.
Small businesses can. therefore, make far more use of a research
laboratory and get a much bigger percentage return for the ex-
penditure than any big company can hope to do. In the small
business, in fact, a research laboratory closely associated with
one of the high executive officers should begin to return a profit
within a few months of its establishment, whereas in the case of
a large company it may be years before a research laboratory
can be considered to be financially successful.
The greatest difficulty in the establishment of a research lab-
oratory in a small business is that any research laboratory will
depend for its value upon the quality of the men at the head, or,
if the laboratory is really small, of the man at the head, and a
small business often feels that it cannot afford to pay even one
good scientific man The solution of this in a technical business
might be that the research man should also be an officer of the
company, so that his cost is borne not only by the scientific
work but also by the value of the executive position which he
holds.
It may be objected that an investigator would not as a rule
prove a capable business man, but there really seems to be no
particular evidence for this common belief, and there are many
examples of men trained in science who have proved extremely
good administrators The classic example is, of course, the
organization of the great Zeiss works under Professor Abbe,
but in many cases it will be found that the technical industries
are directed b>r technical men who were themselves directly con-
cerned with development and manufacture rather than with
financial or business direction.
When the question with which this paper starts was put to
a chemist much experienced in research work, and he was asked
what he would say to an executive who requested information
as to how to proceed to establish a research laboratory', he
answered without hesitation that he would tell him to search
until he found a suitable man to be director of it, and then leave
it to the man to establish the laboratory. There is no doubt
very much truth in this view, and the success of a laboratory must
stand or fall in great measure by the quality of the man in charge
of it. But it is often desirable for business men to come to some
conclusion about research when they have in mind no man suit-
able to undertake the formation of a laboratory for them, and
it is in the hope of aiding technical or business executives in such
a position that the present paper has been written.
Eastman Kodak Company
Rochester, New York
THE AMMONIA PROGRAM FOR 1918'
By Charles W. Merrill
PRELIMINARY CONSIDERATIONS
I do not need to tell you that ammonia produced in America
prior to the war was all consumed in essential industries such as
refrigeration, domestic explosives, dry batteries, fertilizers, and
so forth. You also know that there were large imports before
the war. which, it was realized, would be cut off, and that,
furthermore, there would probably be enormous demands for
military explosives. These two factors indicated that it might
be necessary, not only to provide new sources of supply and to
economize in present uses, but also possibly to drastically cur-
tail present uses.
The War Department, fortunately, appreciated this and
planned and prepared for new plants: one a cyanamide fixation
plant, and another a plant for the conversion of sulfate to nitrate,
these both in addition to the small llaber plantalready authorized.
Both of these larger plants are reported to be weU under way.
Tin \ ue expected to begin production on a very material scale
not latei than this Fall. Private enterprise has also been active
in an endeavor to meet the increased demands. Xew by-
product coke oven, are being installed, and an aluminum nitride
1 Address before the Washington Section of the American Chemical
Society, April 11. 1918.
June, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
plant is being erected with a capacity of 25 tons of ammonia per
day.
It is thought that these new sources of supply will relieve
what might otherwise develop into a difficult situation during
the latter part of this year.
CONTROL
It was early recognized that the refrigeration of perishables
was an industry of such magnitude and extreme importance
and the supply of ammonia therefor was so vital to it, that both
should be brought under control. Therefore, the refrigeration
warehouses were licensed, and all of the manufacturers of aqua
and anhydrous ammonia were called to a conference with the
Food Administration. At this conference, the manufacturers
appointed a committee to cooperate, and executed a voluntary
agreement with the Food Administration, placing the allocation
of their output in its hands. They further agreed not to sell
anhydrous ammonia or aqua ammonia at prices in excess of
30 cents and 8'/j cents per lb., carload lots, respectively, base
price at their plants. Through this power of allocation, the War
and Navy Department requirements for their refined ammonia
products are being taken care of without disturbing the other
consumers, and, of course, in view of the above, without creating
fluctuations in prices.
Keeping in mind the fact that the present sources of ammonia
supply, with the exception of cyanamide plants, are our by-product
coke-oven and gas-producing plants, it was thought wise to put
these under license by virtue of the control of fertilizer and
fertilizer ingredients provided for in the Lever Act, and in ac-
cordance therewith, the President, at the request of the Secretary
of Agriculture, issued a proclamation to that effect, and the Secre-
tary exercises his control through the Inter-Department Am-
monia Committee, consisting of representatives of the Depart-
ments of Agriculture, War, Navy and Interior, the Council of
National Defense, and the Food Administration.
Fortunately, the ammonia control and program has been very
much simplified so far by three factors: first, the broad attitude
of the Secretary of Agriculture and Mr. Hoover; second,
the exceptional spirit of cooperation and patriotism displayed
by the great majority of producers and manufacturers of am-
monia; and third, the fact that the raw material supply so largely
centers in the hands of one firm which, not only for itself, but
for the producers it represents, is uniting in the determination
to help the Government, and to prevent profiteering.
THE PROGRAM
Unfortunately, it is not permissible to go into detailed figures
covering the program, because all of these involve the War De-
partment's confidential estimates, and, also, these necessarily
change as new emergencies arise. Nevertheless, it is possible,
and probably interesting to give you the general considerations
and principles on which it is being worked out. You will realize,
from what has been said, that the possibility of avoiding drastic
interference with existing industries depends on the magnitude
and urgency of the War Department's ammoniacal explosive
program, and the ability of that department to push the early
completion of plants to provide new sources of supply and con-
version I say "conversion" because it was early recognized
that the requirements of explosives for the immediate future
could be most quickly met and with the least disturbance of
the most essential industries by drawing from our relatively large
Supply of ammonium sulfate and converting it into ammonium
nitrate. In order to meet the demand for this ammonium sul-
fate for explosive purposes, it is necessary for the present to
secure it by commandeering orders, and the Government has
taken it over under these orders at the price of 4V2 cents bulk,
f 0. I) point of production.
1 [owever, as the producers, at our request, have refrained from
renewing all contracts, most of which have, or will shortly, ex-
pire, it will very soon be possible to supply the Government's
requirements for sulfate, simply by a pro rata allocation among
producers, in the same simple manner that has been employed
in meeting their very considerable needs for aqua and anhydrous
ammonia for purposes other than the manufacture of ammonium
nitrate. The ammonia producers, wherever they have alternate
equipment for producing ammoniacal liquor, are using it at the
present time in place of sulfate equipment. If, however, the
demand for ammonium nitrate should develop beyond the con-
version capacity, and beyond the supply already arranged for
by the neutralization method, a more serious curtailment of
supplies of ammoniacal liquor for existing industries will have to
be made. In such an event, the Inter-Department Ammonia
Committee will probably be compelled to take steps to reduce
the amounts now being allocated for ammonium chloride, for
domestic ammoniacal explosives, for refrigeration purposes,
and for other uses. If it does this, it will advise that the con-
sumption of ammonium chloride for dry batteries, without in-
suring the return thereof in exhausted batteries up to a certain
proportion of the original allotment, will be deemed to be a wasteful
practice, and subject to the penalties provided therefor in the
Lever Act. Similarly, it will probably advise that the use of
ammoniacal explosives for certain unnecessary purposes will
be held wasteful, and, furthermore, it will rule against the less
essential uses of ammonia in refrigeration.
Other curtailments will be found possible and similarly ar-
ranged for in order to provide ammonium nitrate in quantities
adequate for the actual consumption possibilities of the explosives
program.
CONSERVATION STEPS FOR SAVING AMMONIA IN REFRIGERATION
When it became evident last Fall that the use of ammonia in
the ice and refrigeration business should be reduced to a mini-
mum, in order, if possible, to release some ammonia for Govern-
ment requirements, the Food Administration made a survey of
the trade and found that there were upward of 20,000 places in
the United States in which ammonia compressors were in more
or less constant operation. These range from installations of
almost 4,000 tons daily refrigerating duty down to the little
half-ton machine installed in a butcher shop. Figures obtain-
able indicated that these machines used in their operation about
25,000,000 lbs. of NH3 per year, but the expert refrigerating
engineers who were consulted agreed that a large part of this
ammonia was wasted, and they were of the opinion that a con-
siderable proportion of this waste could be prevented if only the
people owning and operating the plants could be brought to
realize the national necessity for saving the ammonia and the
ready possibility of its accomplishment. It was evident that
a campaign of education was necessary and a small committee
of engineers and owners was called to Washington to gather
opinions and draft plans. All the leading manufacturers of
refrigerating machinery were consulted and the ideas of leading
consulting engineers either directly or indirectly obtained. The
plan finally agreed upon was to figure a reasonable limit for the
use of ammonia based on the size and character of the plant and
to have the ammonia manufacturers supply ammonia to concerns
only in such quantities as would permit them to operate their
plants so effectively as to come within these limits. The manu-
facturers of ammonia by voluntary agreement with the 1 1
Administration pledged themselves to abide by certain rules and
regulations of the Division of Chemicals which specify just how
the limits of ammonia allowances shall be arrived at.
Of course, the most important part of the ammonia-saving
campaign was to educate the owners and operators of the plants,
SO the engineers' committee in conference with representatives
of the ammonia manufacturers drew up a circular of information
and instruction which was issued by the Food Administration
to every one of the 20,0011 plant operators, on February 15, 1918.
482
THE JOURNAL OF INDUSTRIAL AND ENGINEERING < III.MISTRY Vol. 10. No. 6
This circular is headed "Urgent Requests to Owners and Operators
of Ice Making and Refrigerating Plants for Saving Ammonia,"
and the interest in it may be judged when we say that close to
100,000 copies of this pamphlet have been distributed and the
call for them still continues. It is explained in this circular
that ammonia leaks are avoidable; some means for finding them
and stopping them are pointed out; and as a practical method
for enlisting the interest of the plant employees a bonus system
is recommended.
This bonus system was strongly advised by some expert
engineers who had been studying for a series of 5 years the
ammonia problem under their charge in a system of twelve
plants. During that period the consumption of ammonia had
been reduced 75 per cent. The plan and results of this particular
experience really formed the basis for the ammonia-saving cam-
paign adopted by the Food Administration and is an interesting
example of what might be called psycho-economics. The
Superintendent of Manufacture of the series of plants referred
to resolved that the old ideas of ammonia decomposition in re-
frigerating systems hardly deserved the dignity of being called
"theories," as he believed they simply were excuses which served
to cover inattention and carelessness on the part of engineers
in stopping ammonia leaks. He concluded that the interest of
the plant engineer was necessary, and believed it could be most
effectively aroused by a money reward that would be in pro-
portion to the amount of ammonia saved in this particular plant.
He then prepared an ammonia consumption standard for each
plant and agreed to pay a certain bonus for every pound of
ammonia the actual consumption showed less than this standard.
It rapidly transpired that the engineers were able to make
material savings in ammonia, the theory of decomposition was
abandoned, and an involuntary scientific investigation followed.
The loss at the compressor piston rods was soon shown to be
a prime factor and an improved packing was invented. It seems
that the more the saving progressed, the more ways for per-
fecting it were found. The whole study from an engineering
standpoint is an example of the value of aroused attention.
This same set of engineers — so it is reported — have declared
that this year, because it is not only a money-making chance
but also a patriotic duty, they will save more ammonia than ever
before.
The last paragraph of the Food Administration's circular
describes the system of monthly reports each ice and refrigera-
tion plant must make to the Government. A series of report
cards have been sent to each of the larger plants with instruc-
tions to mail one to Washington every month. On these cards
they state the amount of ammonia originally in their plants, the
amount charged into it during the month, and the probable re-
quirements for the ensuing month. A complete file of these cards
will be maintained at the Chemical Division of the Food Ad-
ministration, and where there is evidence of undue use of am-
monia by a concern, the ammonia manufacturers selling the
supply will be cautioned against furnishing further ammonia,
unless satisfactory evidence is given that the wasteful methods
will be discontinued.
The response to this ammonia-saving campaign has been most
encouraging. If we were asked for evidence of criticism or com-
plaint, we could not point to a single letter in all our files to
show it. On the contrary, our mail fairly teems with assurances
of loyal cooperation. The ammonia manufacturer, the machine
builders, the supply houses, and the members of the Society of
Refrigerating Engineers have almost to a man written assuring
us that they and all their representatives will carry the ammonia-
saving messages wherever they go and not let the pungent smell
go unnoticed in any plant they come in contact with. One
concern wrote to their traveling men as follows:
As we suggested to you, it would be well for you to step into
any plant using ammonia, in any town that you may be in.
Lois of time to wait either between trains, or because of the
train being late, and in place of going up to the hotel and tak-
ing it easy, do your bit and go around and see these plants.
Explain to the party who is running the plant just what
ammonia means in this war. Tell him how to save it. Show
him how to locate a leak, and you can impress the fact that not
only is he doing himself a good turn by economizing, but he is
doing a part of his share to assist our Government. It will, no
doubt, take you some little time to do this, but we are willing to pay
for the time that it takes, and we want it done effectively, so
that there isn't anybody who is using ammonia in the section of
the country we travel in who will not know how to conserve his
supply.
However, we feel that the refrigerating engineers will hardly
need these reminders, for they all tell us it will be a great privilege
to save ammonia for the fighters who are risking their lives to
safeguard our liberties.
AMMONIA PRODUCTION BY COAL DISTILLATION DURING 1918
Finally, gentlemen, you will be interested, I am sure, to know
that our estimate of the probable production of ammonium
sulfate for the current year calls for 236,000 tons, equivalent,
approximately, to 58,000 tons of NH3. Similarly, the produc-
tion of NH] in ammoniacal liquor from by-product coke-oven
sources is calculated to be approximately 38,000 tons NH».
The gas plant production of ammonia is not known, as yet, with
definiteness, but in any event is not a material factor. It may
be safely concluded, however, that their production added to
the above 58,000 plus 38,000 will bring the total XHj production
from normal sources to 100,000 tons of NHj.
U. S. Food Administration
Division or Chemicals
Washington, D. C.
AMERICAN CHEMISTS WELCOMED BY THE CERCLE
DE LA CHIMIE
The following is a translation of the greeting addressed by the
President of the Cercle de la Chimie to Lieut. Col. Bacon at
the reception tendered to all American chemists in Paris on
March 24, 1918.
Colonel : In these rooms where there are gathered together
some of the most distinguished members of the Cercle de la
Chimie, it gives me pleasure to greet you, at one and the same
time a representative of the great American nation and one
of the most distinguished members of the university world
of the United States. The first of these two titles would suffice
to assure you a respectful welcome among us; the second adds
a softening degree of cordiality to our feelings. Chemist your-
self, you are here, Colonel, in the home of chemists.
In a Labor Day address in Chicago in 1900 ex-President
Roosevelt, speaking of the necessity of association, in those
energetic and lucid terms which are characteristic of his
eloquence, expressed himself thus:
In other words, the great need is fellow-feeling, sympathy,
brotherhood; and all this naturally comes from association.
It is, therefore, of vital importance that there should be such
association. The most serious disadvantage in city life is the
tendency of each man to keep isolated in his own little set, and
to look upon the vast majority of his fellow-creatures in-
differently, so that he soon comes to forget that they have the
same red blood, the same loves and hates, the same likes and
dislikes, the same desire for good, and the same perpetual
tendency, ever needing to be cheeked and corrected, to lapse
from good into evil. If only our people can be thrown together
where they act on a common ground with the same motives,
and have the same objects, we need not have much fear of their
failing to acquire a genuine respect for one another; and with
such respect there must finally come fair play for all.
The Cercle de la Chimie was born of this same need for
association to which your illustrious compatriot referred. When
we, scarcely twelve months ago, founded the Cercle de la Chimie,
we did it with the object of facilitating contact among all classes
of individuals interested in the development of French chemical
June, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
industry, offering them the opportunity to become acquainted
with each other, to consider the progress of our science, to
discuss their professional interests, to establish business rela-
tions, to manage affairs. The welcome accorded our beginnings
has gone to prove that our idea met a real need. You will find
here the scholar, the professor from our large colleges, chemical
institutes, and national institutions; here you will meet the
manufacturers, the representative of our big syndicates; you
will find the engineer and the financier who devotes his energy
to the marketing of the products of our industry; more particu-
larly you will find the chemist, from the Doctor of Science and
the graduate of our colleges to the man taught simply by ex-
perience in the laboratory; all of these in my voice bid you
welcome to-day.
The Cercle de la Chimie counts itself happy that you, Colonel,
and your distinguished collaborators show yourselves ready to
accept our hospitality, which though modest is none the less
cordial. The presence on the table in our reading room of
American journals will prove to you the interest which those
who frequent our club take in following the progress of your
science and industry. Are they not sure to find in reading these
evidences of the keen thought, daring initiative, and talent
for organization which are the characteristics of your national
spirit?
Is it rash to hope that the reception we have given you this
evening may be the beginning between American and French
chemists, of continuing friendly relations whereof we know so
well how to estimate the worth? It is to the development of
these relations, to their contribution to the approaching victory
of the allied armies which we all are preparing for in our factories
and laboratories that we now invite you, Colonel, to drink of
the wine of France.
WILLARD GIBB5 MLDAL AWARD
The Willard Gibbs Medal for 19 18 was conferred on William
M. Burton, Ph.D., in recognition of his distinguished work in
petroleum chemistry, at the meeting of the Chicago Section
of the American Chemical Society held at the City Club of
Chicago, May 17, 1918. Introductory remarks by L. M.
Tolman, chairman of the Section, were followed by an aptly
phrased presentation of the medal by Dr. Ira Remsen, in
which he paid pleasing tribute to his former student. Dr. Bur-
ton's address of acceptance and the remarks of Mr. Tolman are
printed herewith.
A reception and dinner preceded the meeting at which in-
formal addresses were made by Lucius Peter, president of the
Chicago Association of Commerce; Thomas F. Holgate, presi-
dent of Northwestern University; George N. Carman, presi-
dent of Lewis Institute; W. E. Stone, president of Purdue
University; Julius Stieglitz, director of the Department of
Chemistry, University of Chicago. — Editor.
INTRODUCTORY ADDRESS
By L. M. Tolman
In 1909 Mr. William Converse, at that time chairman of the
Chicago Section, had the idea that it would be a good thing to
found a medal which should be given as a reward for work in
chemistry, and he provided the funds to found the Willard Gibbs
Medal.
The first thought was to make it local in character but it was
soon decided that it should not have restrictions of any character
put upon it. It was provided in the rules for the award of this
medal that a jury of twelve eminent chemists, by their vote,
could award this medal to any person who, because of his
eminent work in or original contributions to pure or applied
chemistry, was deemed worthy of such an award. It was not,
therefore, limited to chemists of this country, but the jury was
given an open field to choose the one they should consider most
worthy to honor and, as you will recollect, the first chemist to
whom the award was made was Arrhenius, the famous Swedish
chemist.
The jury as it is made up at the present time is representative
of the American Chemical Society. At one time, it was pro-
vided by the rules that at least half of the members of the jury
should be from the Chicago Section, but as that seemed to have
too much of a local suggestion, it was decided that this re-
striction on the jurors should be removed and the only re-
striction now is that of the four jurors elected each year, not
more than one shall be from the same Section of the American
Chemical Society. As one reads over the present list of jurors
and those that have served on the jury in the past, he finds a
list of men composed of the most prominent chemists in this
country. Out of the twenty-eight names who have served as
jurors since the establishment of the medal, we find the names
of ten past-presidents of the American Chemical Society, and
of the present jury of twelve, we find that five have been presi-
dents of the American Chemical Society. Certainly, it is an
honor to have such a body of men give one a vote of confi-
dence.
What is a medal? Generally, a little piece of metal with an
inscription upon it; sometimes made of gold, sometimes of
silver, and sometimes of iron or copper; but the value of the
metal has little to do with the significance or value of the medal.
It is what it signifies, what it represents, and who awards it
that gives it its value, and as one looks back over the past seven
years of the award of this medal, its founder must feel
satisfied and the recipients of the medal, proud and honored.
Chemistry is to-day playing a very conspicuous part in the
history of the world. A few meetings ago, we heard from
Major Auld, of the British Commission, of the advanced organic
chemistry that is playing such an important part in the matter
of gas attacks and gas defense. We know of many other fields
where chemistry in this time of war is taking a most important
and conspicuous position, and doubtless many of the chemists
now at the front will receive medals of honor for bravery in time
of peril and for discoveries of importance, which may be of
service; but none, I believe, of these discoveries, while perhaps
more spectacular, will be of greater importance to their country
or more necessary in carrying out this war than the discoveries
of our medalist of this evening. If we look over the various
activities of the war, we must realize what a tremendous factor
gasoline is playing in this great struggle, and that we, and our
allies as well, would be at a tremendous disadvantage, if there
should be a shortage of supplies. Had it not been for the pro-
cesses and discoveries of Mr. Burton and his associates, we
might be facing that particular condition at this time. We
have but to think of aeroplanes, automobiles, and submarines
to realize the effect of a shortage of gasoline at this time.
As I look back again over tile illustrious names of the men
to whom this medal has been awarded, and over the names of
the jurymen who have served in bringing about this award, I
know of nothing that I would consider of greater value or honor
than to have been voted, under the broad terms of the rules
of this award, the honor of receiving the Willard Gibbs Medal
484
THE JOURNAL OF INDUSTRIAL AND ENGINEERING ( HEMISTRY Vol. 10. No. 6
I am sure that Mr. Burton feels as I do — that it is a reward,
a recognition, paying in part for some of the struggles and dis-
appointments which preceded the final success of his work.
Chicago, Illinois
MEDAL ADDRESS
CHEMISTRY IN THE PETROLEUM INDUSTRY
By William M. Burton
Four years ago we assembled to witness the awarding of the
Willard Gibbs Medal to Dr. Ira Rcmsen, of Johns Hopkins
University, and one year ago we met for the same purpose in
the case of Prof. Edward W. Morley, of Western Reserve Uni-
versity. Both of these gentlemen were honored preceptors of
mine, and it was indeed a
great pleasure to me to be
present on those occasions.
I never thought, however,
that I would ever be the
fortunate recipient of the
Willard Gibbs Medal, but
the unexpected and improb-
able very often occurs, and
it is so in my case. I, there-
fore, hasten to extend to the
Chicago Section of the Amer-
ican Chemical Society my
deepest appreciation of the
honor it has conferred upon
me.
This event reminds me of
a most prominent feature in
Dr. Remsen's course of in-
struction, namely, that the
best preparation for a career
in technical chemistry is
thorough training in the
pure science, and I was
equally impressed with the
introductory sentence of Dr.
Morley's address last year,
when he said "The best in-
centive for research work is
the work itself." Both of
these great teachers have
exemplified these principles
most happily in their pro-
fessional careers, and I trust
you will find my remarks
thoroughly imbued with the
influence of their invaluable
instruction.
In considering the part
that chemistry has played
in the petroleum industry, >t might not lie unwise to review,
briefly, the early history of the industry in this country.
You have all heard of the first oil well, drilled by Col K 1..
1 take, near Titusville, Pa., in 1859. Prior to that time petroleum
was found in small quantities Boating on the surface of springs
01 sin. ill streams oi watei in western Pennsylvania, ami this
oil was claimed by the Indians to have marvelous curative
properties in the treatment of every manner of disease. The white
man, with true commercial instinct, sold the oil in bottles as a
cure-all. The demand I'm the oil exceeded the supply,
and Colonel Drake conceived the idea that if the oil came to the
surface of the springs and riveis. there must be targe quantities
of it in the underlying Strata of the earth. He. therefore, with
the most primitive machinery, drilled a well near Oil Creek,
WILLIAM M. BURTON
WILLARD GIBBS MEDALIST,
in western Pennsylvania, and before he had proceeded 100
feet into the ground the oil appeared in such large volume that
it was difficult to take care of it.
At that time there was great need for a cheap and convenient
illuminating material to supplant the expensive animal and
vegetable oils which were used for that purpose. Samples of the
petroleum prior to Colonel Drake's discovery were sent to
Professor Silliman, of Yale College, who distilled the oil and
made separations according to the boiling points of the various
fractions. In his report he stated that portions of these
distillates might well be utilized for illuminating purposes.
The promoters of the oil business acted upon Professor Silli-
man's suggestions, and this was the inception of the petroleum
refining industry in this country.
For a great many years
after Prof. Silliman's investi-
gation, chemistry played a
very small part in the prac-
tical workings of the refining
of petroleum. The refiner
learned to treat the illumi-
nating oil distillate with
strong sulfuric acid and
alkalies, which improved the
character of it somewhat,
but the methods of refining
were crude and wasteful.
The only portions of the
petroleum which were used
at first comprised the frac-
tions boiling between 100°
and 300 ° C, which consti-
tuted somewhat over 50 per
cent of the total mass of
the crude oil. The low-
boiling fractions which we
now comprise in the generic
term of "naphthas" were
thrown away, as were also
the high-boiling residues,
called "tar." The tar, how-
ever, was soon utilized for
preparing lubricating oils of
very indifferent quality. It
was not untd about 1870,
when M L. Hull, of Cleve-
land, Ohio, first devised the
so-called "vapor stove," that
the naphtha fractions of the
oil were utilized. But even
then the uses for the naphtha
fractions did not cause a de-
mand equal to the supply.
and much of the naphtha was
wasted, a common prai throw it into the creeks and
rivers, where it evaporated Millions of gallons of this mate-
rial, now indispensable for automobiles, were thus lost.
These conditions continued until 1885. I'p to this time
practically the SOU source of petroleum in America was western
Pennsylvania. But 111 iss^. 01 '86, petroleum was found in
western and northwestern Ohio, near the town of Lima, and
tin fact that this oil contained from one-half to one per cent
of sulfur attracted immediate attention. The ordinary refin-
ing methods of distillation and treatment with sulfuric acid
and alkali were found to be totally inadequate to secure refined
illuminating oils of suitable quality. Therefore, the industry
turned to the chemist to solve the problem of extracting the
sulfur, and producing satisfactory products.
June, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
485
It is very curious that from the early days of the industry
until the discovery of Lima oil, there seems to have been preju-
dice on the part of practical oil men against the chemical
fraternity. Why this should have been so is not entirely clear,
but I think one reason might be the fact that manufacturers
frequently called upon chemists of general training to solve some
particular problem connected with their business, ignoring the
fact that the chemist probably had had no practical refining
experience. The chemist, therefore, probably offered suggestions
which were totally impracticable and the manufacturer, seeing
this fact, was not particularly impressed with the chemical
profession as a possible aid to his business. Whatever the
reasons may have been, it was a fact that in 1885, with the
discovery of Lima oil, there was scarcely one trained petroleum
chemist in the United States. The oil refiners, however, were
forced to turn to the chemical profession for the solution of their
problems, and the chemists had to become somewhat trained
in the refining business before they could offer a practical solu-
tion for the elimination of sulfur from the oil.
This was the starting point for a better feeling between the
chemical profession and the petroleum industry, and from that
time, more and more chemists have been employed in the re-
fining industry, until to-day the larger refineries depend almost
entirely upon chemists to manage, not only the refinery as a
whole, but the various departments of the same.
In selecting a subject for an address on an occasion like this,
it is customary for the candidate to choose as his subject the
line of work the results of which have presumably been the reason
for his being selected, and I have followed the usual procedure.
It is perhaps difficult to describe the work that has been done
without appearing to be somewhat boastful. However, the
remainder of my remarks will be devoted largely to the results
secured by the Chemical Department of the Standard Oil Com-
pany of Indiana, and I shall try to recount, briefly, the facts
concerning those things which have been accomplished, and
eliminate, so far as possible, the personal equation.
I entered the employ of the Standard Oil Company nearly
thirty years ago, at the time that the Lima oil problem was
very much in evidence, and it was peifectly clear that there
was a great field for chemical activity in the petroleum industry,
provided the refining companies were willing to educate the
chemist in the business, before expecting that the chemist would
be of much value to them. The Standard Oil Company signified
this willingness, and from 1890 until the pre :nt time there have
been a great many chemists employed by that company, most
of them being in its employ to-day, some as active chemists,
some as general managers, and some as managers of various
departments. The result has been that the refining of petro-
leum, instead of being a haphazard process, has been largely
systematized and improved, so that when we do certain things
we feel confident we will secure certain results, and the great
variety of useful products made from mid-continent petroleum
to-day indicates the part that chemistry has played in the petro-
leum industry.
As I indicated a few minutes ago, in the early days the supply
of low-boiling fractions of petroleum was largely in excess of
the demand. This condition of things existed from the in-
ception of the business until the invention of the internal com-
bustion engine. With the advent of this machine, the. demand
for low-boiling products, included in the commonly used name of
"gasoline," became tremendous.
Prior to lOOO the supply of naphtha products was greater
than the demand, and the refiners wire compelled to dispose
of the surplus for fuel and gas-making purposes.
You will recall that the automobile was devised about that
tunc, and although the use Of it grew slowly, v. Id ei
constantly increasing demand for naphtha products to run
these machines, until by the year 19 10 the demand had more
than trebled, and it was perfectly obvious that something would
have to be done to increase the supply of these products.
In those days, the average yields of various products of petro-
leum from mid-continent crude oil were about as follows:
Naphtha products 18 per cent
Kerosene or illuminating products 30 per cent
Lubricating products 10 per cent
Loss 3 per cent
leaving about 40 per cent, which was sold for gas-making or
fuel purposes in lieu of coal. It was clear that the problem
was to convert the high-boiling fractions existing in the fuel
and gas oil into low-boiling fractions needed by the internal
combustion engine. It has long been known that superheating
the vapors of petroleum at atmospheric pressure caused dissocia-
tion of the molecules, producing very low-boiling fractions
and very high-boiling fractions, as is evidenced by the ordinary
Pintsch gas, with which you are all familiar, but the low-boiling
fractions produced by these superheating methods are not
suitable for internal combustion engines, and the losses due to
fixed gases are very great. It was found that anhydrous
a'uminum chloride exerted a very marked effect upon the high-
boiling fractions, converting some of them into low-boiling
fractions entirely suitable for automobile purposes, but the very
high first cost of the aluminum chloride, together with the
fact that to make the process successful an inexpensive method
must be devised for restoring the aluminum chloride, rendered
this process out of the question. We worked for almost two
years trying to devise a practicable method for securing this
most desirable result, first by superheating and dissociation at
high temperatures, but at atmospheric pressure, and, secondly,
by the employment of various reagents, but our efforts were not
successful; on the other hand, we met failure in every direc-
tion.
It had been known for a long time that distillation of petro-
leum products under pressure resulted in their dissociation and
production of some low-boiling fractions and some high-boiling
fractions, but this process never had been applied in a practical
way for the production of motor spirits, because to a practical
refiner the distillation of oils under high pressures did not ap-
peal, owing to the extreme hazard due to explosions and fires;
but having tried everything else that suggested itself, wc
decided to attack the problem from the pressure-distillation
standpoint.
To the layman, distilling oils under pressure would present
no particular difficulty; the distillation of water is done every
day in our steam boilers, and why should one fear to do it in
the case of oil? But when you consider that the distillation
must take place at temperatures ranging from 3500 to 450° C,
where the tensile strength of steel begins to diminish very
rapidly, and when you consider that steel, at such temperatures,
in the presence of carbonaceous matter (and even free carl ion,
which often comes as the result of pressure distillation) is very
likely to absorb such carbon, become crystalline, and lose its
tensile strength, you can readily sec why the practical n
shivered at the prospect of doing work in this way We con
lilted refiners who had been in the business a great many
years. We advised with mechanical engineers for whatevei
suggestions they might offer, and it must be confessed we did
not receive very much encouragement.
Since we found, early in our work, that we would require
a pressure of about five atmospheres, you can easily see that we
approached with considerable respect the problem ol building
ipparatus thai would stand tins pressure in actual
ii , i ini n fin< ■ , foi whosi opinion 1 had 1 h
respect, said he did no! believe we could build a practical still
that would stand more than on pound pressuri pel quareinch
Vnothi 1 ted the proba
486
THE JOURNAL OF INDl STRIAL AND ENGINEERING ( HEMISTRY Vol. ,o. No. 6
po!ymerization of the vapors under heat and pressure, such as
occur when acetylene is compressed.
Howevet ri abli i o secure a very liberal sum of money
to try the scheme on a large scale, and the worst that could
happen would be to burn up our plant and fail in our efforts.
i went ahead.
The first large still we built had a charging capacity of 6,000
gallons of heavy oil, and about the first difficulty we encountered
was serious leaks around the rivet heads and along the seams.
The workmanship in building the still was good and it would
have been satisfactory as a steam boiler. We found that oil
at high temperatures and pressures leaks worse than water,
and a leak always causes a fire of an intensity directly pro-
portional to the amount of the leak It was difficult at first
to secure boilermakers who would calk these leaks while the still
was under pressure. In many cases when we calked one leak
another would form Finally nature came to our aid and we
wire gratified to observe that as the still continued in service
the leaks became less serious. The oil carbonized under the
influence of the high temperature and the carbon deposits
stopped the leaks.
There were many puzzling problems to be solved. We had to
devise a safety valve that would operate freely in spite of the
intense heat and presence of carbonaceous matter. The entire
apparatus had to be constructed in such a way as to insure
ease of operation and freedom from excessive repairs. Distil-
ling the oils under pressure resulted in the production of so-
called "fixed gases." The disposition of these gases, at first,
was troublesome. We found that in some cases the heavy
oil with which we started evolved more gas than was needed
to maintain the desired pressure in the apparatus, whereas
other oils evolved an insufficient amount of gas for this purpose.
This was an embarrassing situation, but we converted an ob-
stacle into an aid by arranging a large number of stills in parallel
so that the superfluous gases from some stills were conducted
to others that needed them and this plan gave us a perfect
method for securing uniform pressure and control, a most
essential feature in the work
The first large still we built, as I have mentioned, had a
capacity of 6,000 gallons, and by starting with fuel oil products
having boiling points ranging from 200 ° to 350 ° C, we were
able to secure a very substantial yield of a product having
boiling points ranging from 50 c up to 2000 C, and to our great
gratification the losses incurred thereby were trifling, averaging
less than 3 per cent. We were astonished, also, to find that the
boiling residues thus produced yielded a product almost
identical with the natural asphalt which is mined in large
quantities in the island of Trinidad. Evidently we are doing
artificially what Nature has done in ages gone by. :i: , distilling
1111 under pre
It would require a long time to describe how we solved some
ol the various problems that arose in connection with this
process From the single 6,000 gallon still we first built, we
now have Ovei five hundred stills of a larger capacity. At
our practical men were very loath to accept these pressure
Stills as a going proposition. They ware afraid of them. The
minute the slightest thing happened they would be likely to
run. But, fortunately, w< had no fires oi serious accidents
ioi tin firsl two 01 three yens, and when we finally did have
a rathei bad fire, the nan had secured enough self-confidence
to stand by their guns, and the damages were repaired quickly
and the work went on, so thai to day the woik of pressure
distillation is carried on in out refineries in connection with the
regular routine work, and most of us have forgotten that a
few years ago we were met with discouraging protests when we
proposed making naphtha products in this manner.
During the last five year- there have been made in this counli \
00,000 barrels of gasoline or naphtha products by the
use of these stills, and we trust that the future will show a
increased production (by this process j of this indispen-
sable material.
Although we know very little about the reactions that occur
when petroleum is distilled under pressure, it may be interesting
to speculate a little on this subject
Let us start with the paraffin Ci<H30 and see what might
happen.
C 1 ! C Hm + CH,
C11H30 = ChHjg -f" C2H4
1. II CnH28 + H2
C„H;8 = C12H„ + C2H,
Ci,H„ = 4C2H2 + 4CH, + CjH, (all gi
2C14H30 = CsHis — t II
CjoHk = CsHu + Ci2H2)
CijHw — C 1 H.L -f- C2H1
2CH, + C2H2 = C,Hin
3CH, + 2C2H2 = C;H,6
C2H2 + 2H2 = C2H$
We feel confident that the finished gasoline contains such
paraffins as CsHis, Cir,H22, and Ci2H2«, but one of the most in-
teresting results is the formation of free hydrogen as shown in
one of the above equations.
The fixed gas formed in pressure-still work gives the following
analysis:
Per cent
CH. 56.3
C:H< 25.8
Unsaturated hydrocarbons 8.5
CO 0.8
H
Condensible rapor 0.6
Undetermined 0.6
100.0
It would seem almost impossible for hydrogen to be set free
under the conditions mentioned above, but the analysis of the
gas proves this to be a fact It also seems probable that, under
the influence of heat and pressure, the gases of the different
series polymerize to form saturated products that are useful.
It is perhaps to be regretted that the chemists engaged in the
petroleum industry have contributed so little to the purely
scientific side of the subject Others have done considerable
work along this line. but. for various reasons, the petroleum
chemists have not.
The chemistry of petroleum offers a most inviting field for
scientific research, and 1 trust the time will come when this
subject will receive the attention it deserves; and when that time-
does come, I sincerely hope the chemists who have been trained
in the practical work will be in a position to do their bit for the
Miint of out knowledge of the chemistry of petroleum
It would be most unjust and unfair for me to accept at youi
hands the award of the Willard Gibbs Medal without acknowl-
edging to you the invaluable assistance that I have received
from my associates, several of whom 1 see before me in this
room They are fully entitled to their share m the honor that
goes with this nudal Some oi these gentlemen arc chemists
and sonic, although not having a thorough chemical training,
arc worthy to be called chemists
It has fallen to my 1. t to be tin director of the work I have
just outlined, but it nev -r could have been brought to .
lul termination without the valuable suggestions, indefatigable
laboi . ami loyal suppoi t of m\ ....i
Standard < mi. Company
Chicago, ti I
June, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
487
CURRENT INDUSTRIAL NEWS
IN, 21 Wcstend Park St., Glasgow, Scotland
A INEW COPPER AREA
In a paper read recently before the Royal Society of Arts,
London, Mr. W. Frecheville said that in the northern part of
Canada there is evidence of the existence of copper over a large
area. Specimens or nuggets of native copper were first obtained
from the Esquimaux who used the metal for their implements
and the occurrence was subsequently confirmed by the few travel-
lers who have been in that region; and it is interesting to note
that the specimens of rock which have been collected point to the
occurrence being geologically similar to that of the highly pro-
ductive and profitable copper mines of the Lake Superior district.
The new copper district referred to is situated east of the Great
Bear Lake and along the course of the Coppermine River which
runs north from about 65 ° latitude into Coronation Gulf in the
Arctic Ocean. Evidences of the occurrence of copper are also
reported as far east as Fathurst Inlet and on Victoria Island.
There appears to be no doubt as to the above facts and conse-
quently the present position may be summed up by saying that
there may be a great copper field somewhere in that region await-
ing development and that the locality is worthy of being carefully
examined both from a Canadian and Imperial point of view.
ELECTRIC ZINC FURNACE
According to the Bulletin Technique de la Suisse Romande, a
Cote-Pierron plant of four furnaces, each of 500 h. p. for 4,500
kg. of ore per 24 hrs., was to be opened at Maurienne, near
Epierre, at an early date. The ores, blende and galena, do not
require roasting. The ore is charged with lime and coal into the
compound furnace which is a combination of an arc resistance
and an indirect resistance furnace. The former is the smelting
furnace from which the vapors and drops of liquid metal pass
into the second furnace at once to be redistilled and condensed.
Although the particulars given are not very full, it is stated that
a liquid metal of 92 to 93 per cent zinc is gained with a loss ranging
from 6 to 9 per cent and that the electrode consumption is 12 kg.
per ton of ore.
ELECTRICAL ENERGY FROM THE VOLTERRA
"SOFFIONI"
Some time ago reference was made to the experiments made
by Prof. Luigi in central Tuscany, on the generation of electric
energy from the steam emerging from voicanic fissures in that
locality. Some additional details are given in a recent issue
of Engineering. These steam blasts contain borax and were
originally used only for the recovery of this material. The
chief problem in the utilisation of the steam for developing
energy has been to avoid corrosion from its ingredients. This
as been met by applying the steam, nut directly in turbines,
ut to heat groups of low-pressure boilers whence steam from
re water feeds the turbines. Borax is collected from the con-
tised heating steam. The turbines are each 4000 h. p. coupled
3000 kw. alternators, current being distributed at 36,000
nd 16,000 volts to Volterra, Massa, Leghorn, and Florence.
ft is now proposed to take this source of energy further in older
supply the important steel works at Alti Forni and the
lagona d'ltalia, at present using coal raised steam A scheme
' treatment for the recovery of helium and other rare gases is
ilso under consideration While it is too early to judge of the
1 results of the scheme, it is stated that the company
sold more powei than it at present conveniently produci
that the power available will be largely increased in th<
uture.
UTILIZATION OF FISH OIL
The Rheinisch Westfalische Zeitung states that the competent
authorities in Germany have prohibited the supply of herrings
to the trade except with the heads removed in order that these
may be utilized for the production of oil, albumen and phosphate
of lime. Fish offal is now utilized in Germany to produce food
for human beings as well as for animals. Offal collected from
fish-preserving factories, restaurants, etc., is dried and, after the
extraction of the oil, ground. The meal so obtained frequently
contains 50 per cent and upwards of albumen and phosphate
of lime, the latter being obtained from the bones and heads.
By chemical methods, the albumen is extracted from the fish-
meal and rendered available for human consumption. From
the oil, phosphate of lime for animal fodder is obtained by means
cf benzine, benzol, and other fat solvents. The oil is also used
for various technical purposes. Specially good kinds can be
hardened by hydrogenation and rendered suitable for production
of eatable fat. The hardened fat looks like tallow and is almost
odorless.
AUSTRALIAN GELATINE, GLUE AND SIZE
The British Commissioner at Melbourne states that, having
recently acquired 1 7 acres of land at Botany, a company is com-
pleting arrangements for the immediate erection there of large
works for the manufacture of gelatine, glue and size. The esti-
mated expenditure includes $75,000 for factory buildings and
$100,000 for plant and machinery. It is expected that the
factory will be working in April and that the products will be on
the market in the following month. The average quantity of
gelatines and glues of all kinds imported into the commonwealth
each year is about 1,400,000 lbs. The capacity of the new
factory at Botany, it is expected, will be such that the whole
of this trade will be captured. At present, the company has
two factories for the production of the same goods operating in
New Zealand from whence it is exporting a portion of its out-
put to Canada.
PURE CYANAMIDE
The Chi-mii, il Trade Journal, 62 (1918), 228, quoting from a
contemporary, gives the following as a method for the prepara-
tion of pure cyanamide. The starting material was calcium
cyanamide having a nitrogen content of 20 per cent. The yield
was 55 g. pure cyanamide per 200 g. calcium salt, corresponding
to a yield of 92 per cent. 200 g. calcium cyanamide were mixed
with 1,500 cc. water hi a 3-liter flask Into this, carbonic an-
hydride (CO;) was passed until a neutral or only slightly alkaline
action was reached. The flask was kept immersed in cold water
as the reaction causes a slight rise of temperature. If the tern
perature is kept below 400 C. there seems to be little loss of the
ether-soluble product due to polymerization to dicyanamide.
The precipitated calcium salt is filtered off and the filtrate
evaporated in vacuo, Hie evaporation being continued until a
crystalline mass separated out 011 cooling. Tin
tracted three limes with absolute ether. On distillation of the
ether, the solution which remained was concentrated ovei sul
furic acid in vacuo. In this way, 55 g. pure cyanamide in tin-
form of deliquescent needles were obtained The substance
: ive a melting n1 of 1,; C and was perfect!) soluble in
, 1!,. 1 1 in analysis the pi rcentage confc nl "i nitrogi a was found
.,;, the theoretical calculated from the formula being
67.00.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. 6
INDIGO CROP OF INDIA
Tin- official Indian Trade Journal of December 28 last pub-
lislicil a final general memorandum of the acreage and yield of
;o crop in 1917-18. The report is based upon reports
received from provinces containing practically the whole area
undei indigo in British India. The figures refer to the crop
which was [then marketed The total area is estimated at
690,600 acres, 10 per cent below the area in 1916 17 which was
770,000 acres. The total yield of dye is estimated at 87,000
cwt, as against 95, 700, the yield for the previous year, or a de-
pei cenl The season was not altogether favorable.
Heavy rainfalls and Hoods affected the crop in Bihar and Orissa
and in parts oi the 1 nited Provinces. In Sind, the crop suffered
Iri jiii low inundation in the beginning of the season.
GYPSUM DEPOSIT IN A BOILER
With regard to the discussion on the setting of plaster and the
importance of the hydrates of CaSO< in this problem, it may be
of interest to mention a recent case of deposit of practically
pure gypsum, i. e., CaS( l(.2H;l >, in a boiler. The case is reported
by Professor Goldberg in the Chemiker Zeitung. The boiler
\\ itei had been run off and a little water had been left and had
been concentrated to a mud and crystalline deposit in the course
of half a year during which the boiler was not used. Over this
crystalline deposit were found close, well-defined crystals of
gypsum, colorless or slightly yellow and containing only 0.06
per cent of iron oxide and alumina. The crystalline deposit
underneath also consisted largely of calcium sulfate but to-
gether with magnesia, oxide of iron, and silica The occurrence
of the hemi-hydrate 2CaS04.H20 in a boiler instead of the usually-
observed anhydrous salt was reported as long ago as 1838.
In boilers at pressures of several atmospheres, the CaS04
is deposited as anhydrous salt; the gypsum crystals seem only
to be formed at ordinary temperatures.
REACTIONS OF ACETYLENE
In a paper on "Some Reactions of Acetylene" read before
tlii Society of Chemical Industry, London, Prof. W. R. Hodg-
kinson described the effect particularly on iron, cobalt, and nickel
of passing acetylene and acetylene mixed with ammonia over
1 With so-called pure gas the iron was not much affected
but there was a great physical effect on nickel and cobalt. They
became brittle and showed decided corrosion and pitting. With
iron there was more or less deep carburization, this effect being
slight in the case of the other two metals. The carbon from the
acetylene was found to have actually entered the ferro-metals.
The carburization was peculiar, the carbon showing distinct
diffusion into the metal. When the acetylene was diluted with
ammonia, an almost smokeless name was produced and iron,
nickel, and cobalt were more rapidly carburized than with acetyl-
ene alone. Unfortunately, on lubsequent heating, the metals
remained brittle.
MAGNESITES
In the paper read by Mr. W. Donald at the meet-
thi l eramic Society held at Stoke on Trent, England,
the authoi state, 1 thai Creek magnesite has usually more silica
but much less ferric oxide than Australian magnesite.
telj crystalline Qreek magnesite, the mineral impurities
1 ipeciall) oxide of iron and alumina are distributed
very irregularly. This increases the difficult) of satisfactorily
calcining throughout in single filing. Canadian niaguesites
are 1 ven more irregular. In the author's opinion bj the careful
selection of material. Creek m i i could be made to com-
pare more favorably with Australian magnesite as regards
lime and silica content.
WATER LUBRICATION OF GAS EXHAUSTERS
Mr Cuillet, in an article in Journal des Usines a Gaz, recom-
mends, from his own experience, the use of water in place of
oil for the lubrication of exhausters. A steam-driven Beale ex-
hauster put into use new in October 1910 has been lubricated
in this manner and. without having once been out of service,
manifests no appreciable wear after having passed over 1000
million cu. ft. of gas. The lubrication has been effected by
siphons delivering town water of great purity, but in general
practice, according to Mr Cuillet, it is better to use ammoniacal
liquor, since a hard water under the influence of ammonia and
carbonic acid gas forms a deposit in the circular passages, causing
a block and allowing for dismantling and scraping With
ammoniacal liquor the nuisance does not occur. Exhausters
lubricated in this way have kept in excellent condition, the in-
terior surface taking a high polish.
UTILIZATION OF WASTE SULFITE LYE
The disposal of the waste sulfite liquor in the manufacture of
wood pulp or cellulose has long been a perplexing problem.
Recent experiments, says the Pulp and Paper Magazine, have
demonstrated that this waste sulfite liquor can be evaporated
to dryness and the solid substance thereby obtained may be
subjected to calcining and burning. The gases coming off may
be trapped and the ashes treated for the recovery of the sulfur
as well as the basic substances present in the original bisulfite
liquor. Incidentally, and of great economic importance, it
may be mentioned that the dry residue produces a fuel contain-
ing approximately 6000 B. t. u. per lb. A mill with a capacity
of 50 tons of pulp per day will discharge 500 tons of waste sulfite
liquor daily containing 10 per cent of organic matter which may
be thus reclaimed. The fuel available would have a heat value
equivalent to that of 25 tons of high-grade (24,000 B. t. u.)
coal. With a view to eliminating entirely the disadvantages of
burning over grates, tests have recently been made of burning
the material in suspension.
COAL SAVING
The February number of the monthly publication of the Brit-
ish Commercial Gas Association deals with the use of gas coke
for steam raising. It contains an article giving a large number
of particulars which go to prove the economy alike from an in-
dividual and a national point of view, effected by the use of
coke instead of crude coal in steam-raising plants. Illustrations
are given which show the number, variety, and importance
commercial and other undertakings which have already made
the change to great advantage. An interesting section of the
article deals with the use of coke as a fuel for road transport in
which capacity it is being largely employed to-day.
01
BRITISH BOARD OF TRADE
During the month of March, the British Board of Trade
have received inquiries regarding sources of supply for the fol-
lowing articles. Firms able to give information about these
ltc requested t<> communicate with the Board of Trade,
inghall St . London, K C,
[daces, ladies Steel strip f»/iin. to '/i in. wide X -20
to 2fi B. \V. G. put up on reels)
Sulfite pitch
Thermostats, automatic for electric
incubators
Upholsterer's springs
Wheels for tinder and petrol
( elluloid cleat traospan
■
holders (tortoise shell)
■. ishers
ined pens and pencils
el, tu isted wire
Plat pencils with sheath
Ink pots With Soluble safety lids
■ ■
i tings (or hair slides
Petrol and tinder lighters
Spangles for dress decoration
Sprinklers for perfume bottles
lighl
Maciunkkv
Making:
Scnw parts of cork-screws
Snuff
Shellac and sticklime
March
Stencils
Plant for
June, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
480
SCIENTIFIC SOCIETIES
ANNUAL MEETING OF THE CHEMISTS' CLUB
The annual meeting of the Chemists' Club was held at the
clubhouse on Wednesday evening, May 1, 1918. The treasurer
reported that out of the surplus funds $15,000 had been invested
in the Third Liberty Loan. Announcement was also made of the
acceptance of $10,000 given by Mrs. Herman A. Frasch for the
erection of a conservatory in memory of her late husband.
The conservatory %vill adjoin the club dining-room.
Dr. Milton C. Whitaker, the retiring president, was presented
with a silver tea and coffee service, the presentation being made
by Dr. Charles F. McKenna on behalf of the officers and trustees.
Election of officers for the ensuing year resulted as follows :
President: Ellwood Hendrick.
Vice Presidents: Resident, Charles H. Herty; non-resident,
Charles L. Parsons.
Secretary: J. R. M. Klotz.
Treasurer: H. M. Toch.
Trustees: T. R. Duggan, H. G. Mackenzie.
ADDRESS OF PRESIDENT-ELECT HENDRICK
We are receiving in this Club, from the retiring administration,
a great estate. It now becomes our duty to conserve it and to
administer it to good purpose.
The achievement of establishing this unique institution has
been in large part of a social nature, and we must not lose sight
of the fact that our function as a Club must continue to partake
of this quality. Unless we maintain our house as a chemists'
headquarters, as a place where good chemists feel particularly
at home, we shall fail in our purpose.
People feel at home according to their individual tastes, but
men of discrimination are disposed to favor that which is ad-
mirable. Therefore it behooves us to keep the place attractive
and, in so far as it is given to do so, distinguished. We are now
custodians of the only Club known to the profession of chemistry,
and the development of the war has thrown this profession
singularly into focus of the public eye. Whatever we say or do,
irrespective of the measure of our modesty, straightway becomes
a matter for discussion. Less than five years ago a great part
of the public seemed to think that chemistry was something
principally made in Germany. Without stultifying ourselves,
and in full appreciation of the fact that the German language,
which we forbid in conversation in the Club, is still the richest of
all in chemical literature, we hold that the science is also native
in America. Let us endeavor to prove that it is free from Ger-
man frightfulness, in word as well as in the deeds of peace.
The trustees have seen to it that there shall be no ground for
suspicion of any stain of German sympathy in war among us.
All members whether American-born or not, who are not in hearty
sympathy with the United States and its allies in the great war,
have been requested to resign — speedily to resign. The retiring
board insisted that the Club be one hundred per cent American,
and an intimate acquaintanee with the incoming members war-
rants me in saying that the temper of the new board will be the
same. We are in the heat and passion of war and there is no
room, anywhere in this building or on our roll of members, for
anyone who is against us or even neutral in the present great
light. < .in the other hand, we must avoid persecution or unkind
ness of any sort toward good Americans who are of German
origin or descent. We must remember that every man is him
self and that there is no greater mistake than to get a man
mixed up with his grandfather.
A thing that we need, seriously need, is an answer to the
question: What is a chemist? I despair of any terse phrase
that will tell it, and I am sure that it is not a quality achieved
by an academic degree. I know self-educated men who are ripe
scholars in the science as well as in the arts and the humanities;
and we all know men, academically certificated, who should not
be classed as anything better than laboratory helpers. I do
not desire to intimate that the Club should find an official answer
to the problem ; I only have in mind that we should help to estab-
lish the meaning so that the right words may be found. I also
venture the opinion that if we set a high standard for our mem-
bership requirements, we shall be taking a step in this direction
and thus do more for the profession than by any other means at
our disposal. We are fortunate in having most of the leaders
in American chemistry as our fellows. Let us keep up the stand-
ard and see to it that this house shall continue to be their real
headquarters.
I can hardly trust myself to discuss the great debt we owe to
the retiring president, Dr. Whitaker, and I bespeak his aid during
the coming year. We are under sincere obligations to the many
members who helped us to take over the adjoining building for
additional quarters, and to those who have donated their stock
in the building company. Our thanks are due to Dr. Weston
foi assistance in more ways and at more times than there is op-
portunity to enumerate. To Mrs. Herman Frasch, whose late
husband contributed largely, by his invention, to halt the march
of Prussian madness in 19 15, we are not only indebted for the
living portrait of him, but for the conservatory which is now
about to be constructed back of the dining-room, which will
make our Club unique among those of New York in this special
point of attractiveness. It will also provide for our members
a place of delectable resort.
I ask members of committees to continue in office until the
trustees shall have passed upon the nominations for the ensuing
year, in which I hope but few changes will be necessary. And
I earnestly request all members to work together during the
coming year with the same good-will that has characterized our
organization in the past. It is only by the hearty cooperation
of the membership as a whole that we can make of this Club the
great institution that it deserves to be.
139 East Fortieth Street
New York Citv
AMERICAN ELECTROCHEMICAL SOCIETY1
On Sunday, April 28, at 6 p.m., 126 members and guests of
the American Electrochemical Society left the Union Station
at Washington for a tour of the Appalachian South, having in
view a survey of the resources, water power, facilities and op-
portunities which that section of the country affords to manu-
facturers and industrial interests. The cities visited were John-
son City, Kingsport, Knoxville, and Chattanooga in Tennessee,
Sheffield I Muscle Shoals), Birmingham, and Anniston in Alabama.
The first stop was at Johnson City on the morning of April
29, where the members were guests of the Chamber of Com-
merce for breakfast at the Hotel Windsor, l.cc I'\ Miller,
president of the Chamber of Commerce, made an address of
welcome The members were then given an opportunity of
viewing the town and some of its industries by an automobile
tour through the city. An hour later the members reached
Kingsport, and were escorted by the reception committee
to the Kingsport Inn, where brief addresses were made
by V. V Kelsey. resident manager of the American Wood Re
duction Company, and J. Fred Johnson, president of the Kings
port Improvement Corporation Thi welcome bj 1
ex-Governor of Tennessee, was responded t" bj Presi
1 It is expected that a more detailed description or the plants visited
nil! be published in a later issue of Tins Journal
|00
///A. JOURNAL OF INDUSTRIAL AND ENGINEERING < HEMISTRY Vol. to, No. 6
At noon .1 luncheon compli-
mentary to thi Society was served at Rotherwood Parm, about
4 miles from the city, on the terrace in thi shadow of the stately
columned portii hi century-old farmhouse now used as
an inn. The farm attracted many of the members it i
one supplying not only many of the local demands bul shipping
its products to other parts The afternoon was spent in visit-
ing plants in the city as follows
KINGSPORT PLANTS
At the- Kingsport Extract Corporation, making hemli
chestnut extract, 24,000,000 lbs per year capacity, the mem-
■. the entire operation, from tlu- "hogging" t(j the
dried extract, and the pumping of the- liquid extract to the
Kingsport Tanning Corporation
This tanning company produces 125 hides per day and here
again the complete process was the liming of
the hides and the de-hairing by machinery to the finished
leather leaving the tanning vats and drying rooms, ready
to go (nit for ultimate manufacture elsewhere.
The wood chips residue from the extractors of the Extract
Corporation are sent to the Kingsport Pulp Corporation,
where, in conjunction with other wood treated l>y the soda
process, 60 tons of pulp per day arc produced. In this plant
the Dorr classifier and thickener are used
The Kingsport Paper Company reduces the pulp to paper, the
product now being a soft paper like blotting paper, and also
paper hoard.
The Kingsport Hosiery Mills, built within the year, where
_• LOO dozen pair- of hose are being produced daily, were of interest.
The plant is so built that it can be easily doubled in capacity
in the present building.
The Clinchfield Portland Cement Corporation, producing
400 barrels of Portland cement per day. was visited. At this
plant the Cottrell system for the precipitation of dust is being
installed and it is expected that a recovery of potash amounting
to o per cent of the dust will be made. The product is to be
converted into potassium carbonate and potassium sulfate, and
it is expected that 4 tons of these salts will be produced
daily Adjoining this plant is that of the Kingsport Lime
I orporation, built by Richard K. Meade, and producing 50 tons
per day Nearby also is the power plant of the Kingsport
Utilities Corporation, supplying power to all the industries in
the Kingsport Valley. Clinchfield coal is used and 15,000
h. p. air produced
The Kingsport Buck Corporation, where drain tile, sewer
pipe, 1 ommon building brick, face brick, etc . are being produced,
and the Federal Dyestuff and Chemical Company were visited.
The latter has the largest installation of Allen Moore cells in
the country, then' being 408 with a capacitj ol 20 tons of sodium
hydroxide and 20 tons ol chlorine per day The Hebden process
is used for dehydration of the chlorine and for the clilorination
of the products in the plant
The Kingsport Wood Reduction Corporation plant. .1
mi nt subsidized plant being built by the American Wood Re-
duction Company, was visited, togethei with the cantonments
built for the workmen who an at present employed there
During the day an exhibit of the minerals ol the Clinchfield
region was to be seen at the Kingsport Inn. In the late afternoon
motion pictures of the Clinchfield region, taken over the Clinch-
field hue from Elkhorn City, Kv . to Spartanburg, S C . were
shown in the local motion picture theater to the members of
thi Societj Dinnei complimentary to the members of the
Society was si rved at the Kingsport Inn, aftei which a business
meeting ol the Society was held The Committee reported the
il officers as follows;
President, F. J. Tone. First Vice President, Acheson Smith;
Second Vice President, II YV Gilbert; Third Vice President,
K Tumbull; Treasurer, Pedro G Salom; Secretary, Jos. W. Rich-
ards. Managers, Chas P Burgess, E I. Crosby and C. G
KNOXVILLE AND VICINITY
I. easing Kingsport at midnight. Mascot was reached early
the morning of April 30. The members of the Society were the
guests of the American Lead and Zinc Company at breakfast, after
which its plant was visited. Wilfley and Deister-Ovcrstrom
tables and the Minerals Separation, Inc., oil flotation process
are used in this plant for the concentration of the on
ore which, when mined, contains 4 per cent, is concentrated to
at with the loss of a very minute fraction of zinc sulfide.
Arriving at Knoxville, the party transferred to another
train and left for Cheoah, X C where the Aluminum Com-
pany of America is building a dam 200 feet high 40 ft
higher than Niagara Falls , and from a 1 80- foot head plans
to operate ; - 25,000 h. p.) with an
efficiency of 90.25 per cent They expect to have the power on
the busses at Alcoa in 9 months, generating at the station
[3,000 volts, transmitting 150,000 voltage of 25 cycle. The
company is planning nine dams along the river, two large and
seven small ones, giving them a total fall of 1 800 feet.
At Alcoa, several miles downstream from Cheoah. it is intended to
build another dam to be at least as high as the one at Cheoah.
These wain powei developments ire carried on through subsidi-
North Carolina being known
as the Tallassee Power Company and the other, operating in
Tennessee, as the Knoxville Power Company.
Returning to Knoxville. the party proceeded at once to the
University of Tennessee, where a technical meeting was held, at
which Mayor J E. MacMillan welcomed the members to the
city, and Dr. Brown Ayrcs, president of the University, wel-
comed them to the University. The following papers were read ;
Hydroelectric Power Possibilities i 1 the Provi.ices of Quebec and
Or.tario. Canada. 1
The Calculation of Storage Battery Capacities. C. \Y Ha2i-:i.ett.
The Sign of the Zinc Electrode W. D Bancroft
Electrical Resistivity of Porcelai a and Magnesia at High Tempera-
tures P. 11 Brace.
Precision Method for the Determination of Gases in Metals H
M. Rvdek.
Nitrogen Fixation Furnaces E K
The Society went from the University to the Agricultural Ex-
periment Farm of the University of Tennessee, where the lysimeter
with winch 1 11 Maclntyri and his staff are carrying on valuable
soil studies is located. At a complimentary dinner at the Cher-
okee Counti v Club, in the evening, Hugh M. Tate, as toastmastcr.
made an address in the course of which he argued that the
Electrochemical Society had been brought to Knoxville by the
exhibit made by the city at the Chemical Exposition last Fall
and that, therefore, the city should neglect no opportunity
to exhibit at any future National Exposition of Chemical
Industries Dr. Fink made a stimulating response. C. G.
Schluederb ".1 "The Part the United States Industries
Must Perform to Enable the Allies to Win the War.'
Kato made a brief address, followed by John A. Switzer, upon
■The Industrial Water Powers of Tennes
CH \ T TANOOGA
Arriving at Chattanooga the next morning. May 1, the party
breakfasted at Hotel Patten, alter which the local committee
escorted the members to tlu plant of the Southern Eerro Alloys
Company, when every .' i hours 2 1,000 pounds of 50 per cent
ferrosilicon are being made in Fitzgerald electric furnaces.
This is the liist ferrosilicon plant in tlu country ever opened
to anj society, and tin- was done through the kindness of Paul
I Kruesi, president of the company and a member of the
Societj Members then visited the plants of the Burdetti
Company and Wilson & Company At the latter plant
June, iotK
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
401
coconut, cotton, peanut, and soya bean oils are being refined.
The hydrogenation plant was not open to the members.
The Chattanooga Chemical Company and the Semet-Solvay
ovens of the Chattanooga Gas and Coal Products Company
were visited. Here 24 Semet-Solvay ovens using 450 tons of
coal per day have replaced 12 Roberts ovens. The members
then motored to Crystal Springs Bleachery. The return trip
to Chattanooga was made by the Crest Road, along Missionary
Ridge. An hour was spent at the Chattanooga Manufacturers'
Association exhibit in the Association Building before the So-
ciety left on a river steamer for Anthony N. Brady's $11,000,000
power plant at Hale's Bar, operated by the Chattanooga-Tennes-
see River Power Company, whose power is marketed through
the Tennessee Power Company. This is a low-head develop-
ment, having 14 vertical wheels of 3,000 kw. each (4,000
h p I, 6600 volts of 60 cycles, and 120,000 volts of 60 cycles.
SHEFFIELD AND MUSCLE SHOALS
On Thursday morning, May 2, the Society arrived at Sheffield.
Ala., where, after a breakfast at which Col. J. W. Worthington
gave an address of welcome, the members were taken in automo-
biles to visit the town of Sheffield and thence to Government
Nitrate Plant No. 1, in charge of Capt. R. W. Hempill. This
is the plant using the General Chemical Company's synthetic
process. The plant location was accepted September 10, 191 7,
the company organized October 1 , contract signed with the
J. G. White Company on October 2. On October 23 the first
load of construction material arrived and work on the buildings
began. The buildings were almost complete as the members
of the Society saw them and the installation of machinery was
going forward rapidly. The plant, costing $20,000,000, con-
sists of a gas works, a process building housing the General
Chemical Company's process, and a power house, also the con-
centration, oxidation and absorption plants, for which the Chem-
ical Construction Company have the contract. There will be
a nitrating plant and an experimental laboratory. There is
also under consideration the erection of a battery of coke ovens.
One-half of this plant is expected to be completed by June 15,
1918.
At Nitrate Plant No. 2, work was started on November 17, 191 7.
The plant construction was contracted for with the Westinghouse,
Church, Kerr Co., J. G. White Engineering Company, and the
Chemical Construction Company, and consists of a lime plant
which will burn .550,000 tons a year (the largest lime plant in
the country), a coke drying plant with 100,000 tons yearly
capacity, a liquid air plant with a capacity greater than all other
plants in the United States and Canada combined, a power house
which will produce 45.'»>i> kw., and as needed, 35,000 kw.
more will be secured from hydroelectric plants in the vicin-
ilv J. YV. Young welcomed the Society to the plant and
E. J. Pranke of the Cyauamide Company gave a descriptive
address. Those in charge of operations are Captain S. L. Coles
for the Government ; J. YV Young for the Air Nitrate Cor-
poration; G. W. Burpee, M. T. Thompson, and T. C. Oliver for
the contractors.
Leaving Plant No. 2, the party motored to Lock 6 on the
Tennessee River at Muscle Shoals, where the members viewed
the Muscle Shoals canal After a barbecue luncheon, served by
the Society's 1 ..sts, an informal meeting was held, at which
C. W. Ashcraft of the local committee was chairman.
The speakei were Col J \v Worthington, C. G. Pink,
C. A Winder, N. T. Wilcox, J. W. Richards, W G. Waldo.
Stewart J. Lloyd, and Col. A. II. White. Leaving Lock 6,
the return to Florence wai madi on 1 Government steamei
and barge, from which a fine view of the surrounding country
and <>f the site of dam No. .-. iusi above Florence, was ob
tained
BIRMINGHAM
Friday, May 2, was spent at Birmingham, where a local recep-
tion committee made up of members from the Alabama Technical
Association, the Alabama Section of the American Chemical
Society, and the Chamber of Commerce provided autos, and a
visit was made to the Tennessee Coal, Iron and Railroad
Company's Ensley plant where duplex steel is being made.
In the afternoon a visit was made to the by-product
plant of the company, which has four batteries of Koppers
ovens. Passing through the mine property at the Fairfield
Works, the party had a view of the new plate mill which is to
produce steel plate for the shipbuilding plant located at Mobile,
both of which are now under construction. The American
Steel and Wire Works at Fairfield were also visited. In the
evening the hosts entertained with a dinner at the Hotel Tut-
wiler, Arthur C. Crowder, president of the Chamber of Com-
merce, acting as toastmaster. The speakers were ex-Governor
Emmet O'Neil, C. G. Fink, J. V. N. Dorr, and H. Morrow
This was followed by a technical meeting held in the ball
room of the hotel at which Eugene A. Smith, State Geologist,
spoke on "The Mineral Resources of Alabama," and the following
papers were read and discussed:
The Electrolytic Behavior of Manganese in Sulfate Solutions. G. D. Van
Arsdale and C G. Maier
The Effect of Iron Sulfate in the Electrolytic Precipitation of Copper from
Sulfate Solution with Insoluble Lead Anodes. E. F. Kern.
Experiments with the Copper Cyanide Plating Bath. F. C Mathers.
Load-Carrying Capacities of Magnesia-Silica Mixtures at High Tempera-
tures. O. L. Kowalke and O A . H. .vacs-
Electrolytic Refining of Tin. F„ F. Kern.
Thermo-Electric Force of Some Alloys. M. A. Hunter and J W. Bacun.
Why Busy Rails Do not Rust. O P. Watts.
A New Electric Furnace. C. H. Vom Baur
The Booth-Hall Electric Furnace. W. K Booth
Electric Steel Casting. R F. Funterman.
ANNISTON
The morning of Saturday, May 4, was given over to Annistou.
After breakfast at Anniston Inn, an impressive address on the
development of their ferromanganese plants in Anniston was
made by Theodore Swann, president of the Southern Manganese
Corporation, after which the members visited the ferromanganese
furnaces of the Southern Manganese Corporation, the ferro-
manganese and Heroult furnaces of the Anniston Steel Company.
The return from Anniston to Washington was made in 24 hours,
in the special train occupied by the members for the entire tour,
in the operation of which the Southern Railway took great pride.
The geologist of their Industrial Department, J. H. Wat-
kins, was one of the members of the Society on the trip and
was always ready to give any desired information.
Charles F. Roth
Chairman, Committee in Charge
SIXTH NATIONAL TEXTILE EXPOSITION
Tin- Sixth National Textile Exposition was held at the Grand
Central Palace, New York City, April 20 to May II, 1918.
The exhibition occupied all four floors of the Palace, a fact
indicating its large size, and included exhibits of cloths and
yarns, machinery and accessories for their production, aniline
and other dyestulTs used in tluii coloring, and in addition a
fashion show was given each afternoon and evening, of gowns
and costumes designed and made in America of American-made
textiles, and dyed with American dyes.
The main and second Boors were almost wholly given over t.>
exhibits Of textile machinery and such SCO isories as "lis. lubri
cants, beltings, paints, ah c litioners and moistenei , tern
perature controllers, etc.
The exhibits of special chemical interest were those by the
dyestuffs manufacturers. The two largest were those of the
492
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. \o. 6
Marden, Orth and Hastings Corporation and the National
Aniline and Chemical Company. The exhibit of the latter
attracted much attention on account of the practical demonstra
tions of the merits of American dyes as compared with those of
German make. Samples of cotton, silk, and wool dyed with
corresponding American and German dyes were exhibited,
showing very graphically how these had stood tests for fastness
to light, fulling, scouring, and weather, with the results gratify-
ingly in favor of the American-made dyes. Approximately
fifty colors were shown in the comparative samples, including
blues, browns, greens, purples, reds, and yellows, and com-
prising direct, acid, basic, chrome, and sulfur colors as well as
some developed ones. An interesting feature of the exhibit
of this company was the working unit of a fully equipped color
testing laboratory in which the work of making these com-
parative tests was actually being carried on.
The Marden, Orth and Hastings Corporation exhibited
jointly with the Calco Chemical Company and showed samples
of the dyestuffs, coal-tar intermediates, and chemicals entering
into the manufacture of the colors which they displayed, these
including their new line of "orthaminc" colors. They also
displayed suitings, overcoatings, yarns, and raw stocks dyed
with their products and especially featured their khaki colors
in this connection.
Other exhibitors of dyestuffs and chemicals were the du Pont
Companies, Frank Hemingway, Inc.. John Campbell and Co.,
Stamford Extract Manufacturing Company, Southern Dye-
stuffs and Chemical Company, Sterling Color Company,
Williamsburg Chemical Company, Oakley Chemical Com-
pany, American Alkali and Acid Company, and the American
Dyewood Company.
The Dicks David Company, of New York City, made a
special feature in their exhibit of various fabrics dyed by American
dyers using this Company's products and demonstrating con-
clusively that American dyes arc fully the equal in purity and
strength of those imported.
An interesting exhibition of starches, gums, and dextrines
was that of Stein, Hall and Co.
The Takamine Laboratory showed their product, "Polysime,"
a de-sizing and de gumming agent. A very illuminating part
of their exhibit was the demonstration they gave of the progress
of chemical industry in Japan within the past few years.
NEW YORK SECTION, AMERICAN CHEMICAL SOCIETY
The recent investigation by the city administration of the
work of the Bureaus of the Department of Health of New
York City has resulted in the suspension of the Director of
the Bureau of Food ami Drugs, Or Lucius 1*. Hrown Follow-
ing the appointment of Dr. Royal S Copeland as Com-
missioner of Health, the Chairman of the Civil Service
Commission, Mr. James K MacBride, filed charges against
Dr. Brown, and these charges were simultaneously given to
Hi. public pre^s Accordingly Director Brown answered the
charges through the puss, and for this action was suspended by
the Commissioner of Health, pending a public hearing on
charges which air now being prepared
At the regular meeting of the New York Section of the AMER-
ICAN Chemical Society on May to, 1918, the following
resolutions wen unanimously adopted by the Section
Whereas the importance ol chemistry and the work of the
chemist has been brought clearly home to the people of this
country, particularly since the outbreak of the war, and has
resulted hi largelj increased numbers of industrial laboratories
for the careful control of manufacturing in.» usis and especially
i"i thi maintenance of standards of puritj ol products, and
Whereas tin increased demand for chemists through this
industrial expansion and through the large numbei called into
ice of the Government for the purpose of the successful
conduct of the war has created a serious shortage in the avail-
ply of chemists, and
WHEREAS it appears that there is a possibility of a serious
impairment of the efficiency of the Bureau of Food and Drugs
of the Department of Health of New York City through the
. of its activities or change in its present efficient
direction,
Therefore be it Resolved:
First : That we urge upon the duly constituted authorities
.1 in every way possible, for the full benefit of the people
of this city, the protection of the public health so largely de-
pendent upon the work of this Bureau.
Second That tvinced that in the present incumbent
of the office of Director of the Bureau of Food and Drugs,
Dr. Lucius P. Brown, the city has a most valuable administra-
tive, technical, and scientific official, selected on the basis of these
qualifications by the impartial method of Civil Service Examina-
tion, experienced in his work through long service as Food and
Drug Commissioner of Tennessee, a recognized leader among the
food and drug officials of the nation, as witnessed by his presi-
dency of their association and constant prominence upon im-
portant committees charged with the solution of fundamental
food and drug problems, a man whose integrity is beyond question
and whose marked faithfulness in administering the work of
his present position assures to the people of this city thorough
protection against adulteration of its food and drug supplies.
Third: That we commend the Commissioner of Health
for his stand that any questions which have been raised regard-
ing the administration of this important Bureau in the Depart-
ment of Health shall be given a full and public hearing, for we
are confident that through such a medium the usefulness and
high standard of the Bureau will be continued without impair-
ment.
NORTH CAROLINA ACADEMY OF SCIENCE AND NORTH
CAROLINA SECTION OF THE AMERICAN
CHEMICAL SOCIETY
Tlu Seventeenth Annual Meeting of the North Carolina
. of Science was held jointly with the Spring Meeting
of the North Carolina Section of the American CHEMICAL
SOCIETY at the State Normal College, Greensboro, N. C, on
April 26 and 27, 1918.
PAPERS PRESENTED BEFORE THE ACADEMY
The War Work of American Physicists. C. W. Edwards.
Some Important but Largely Neglected Scientific Facts. George W.
Lay
Symptoms of Disease in Plants. P. A. Wolfb.
The Sun's Eclipse, June 8, 1918: Question. John F. Lannbac.
Entrance Requirements in Science at the State Normal College.
B. W G
Extension of the Range of Prunus umbellala into North Carolina.
I S H.. i Mil-
Eliminations from and Additions to the List of North Carolina Reptiles
and Amphibians. C. S. Brimlkv
A New Species of Azalea. W C. CoKBR.
Notes on the Magnetic Compass. T. F. Hickbrson
Variations Within the Individual Sponge Towards Types of Structure
Characteristic of Other Species and Genera. H V WxLSON
New or Interesting North Carolina Fungi. H. C. BkardslEB.
Herpetological Fauna of North Carolina Compared with That of Vir-
ginia. C, S ItKlMl.KY
Further Consequences of Cross Conjugation in Spirogyra .Lantern i.
Ur.KT CONNINOHAH
A Visit to Smith's Island Lantern . \V. C. Coker.
Some Methods and Results of a Plankton Investigation of Chesa-
peake Bay (Lantern). J. J Wolfs WD Bkrt Cunningham.
Mineral Fertilizers; Their Mode of Occurrence and Distribution in
North Carolina. Collier c'onn
Notes on Buds. E W Gl
Recent Changes in Currituck Sound. COLt#XSR c\>ri»
PROGRAM <>!■' Tin: N C. SECTION. A C -
Report of Investigations on the Cause of Death of Matured Chicks
in Shell in Artificial Incubation. II B IrbucklB.
Effects of Fertilizers on Hydrogen-Ion Concentration of Soils. 1 K
1 W Mi
Action of Heat on Para-Sulfamido-Ortho-Toluic Acid.
Toluol from Spruce Turpentine. A S Wiikklkr.
The Question of the Recovery of Tin from Scrap and Cans in North
Carolina. Carlton V Mum
June, 191S
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
493
NATIONAL FERTILIZER ASSOCIATION
The Twenty-fifth Annual Convention of the National Fertil-
izer Association will be held at Hotel Traymore, Atlantic
City, N. J., the week beginning July 15. Meetings will be
held as follows:
July 15th and 16th: Meetings of the Soil Improvement Committee
of the National Fertilizer Association.
July 16th: Meeting of the Southern Fertilizer Association.
July 17th and 18th: Meetings of the National Fertilizer Associa-
tion. '
The Convention Committee appointed by President Bowker
of the National Association to take entire charge of the details
of all convention arrangements is as follows: Chairman, John
D. Toll, Philadelphia; C. M. Schultz, New York; W. Dewey
Cooke, Savannah; Irvin Wuichet, Dayton, Ohio; Horace Bowker,
New York, ex-officio. The committee will announce later the
details of the program, names of speakers, and arrangements
for entertainment.
ALABAMA TECHNICAL ASSOCIATION AND THE
ALABAMA SECTION OF THE AMERICAN
CHEMICAL SOCIETY
A joint meeting of the Alabama Technical Association and the
Alabama Section of the American Chemical Society was
held in Birmingham, Ala., on May 2, 19 18.
PROGRAM
Experimental and Extension Work in Agriculture in Alabama. Pro"
FESSOR DUGGAR.
Some of the Relations of Chemistry to Agricultural Progress. Dr.
B. B. Ross.
The Alabama Technical Association was formed last year,
its object being to maintain an organization among the technical
men of Alabama to stimulate the development of the natural
resources of the State, to foster public interest in all things bene-
ficial to the State, to advance the interests of the technical
profession in the State, and to encourage social intercourse
among its members.
The membership is made up of members of the following na-
tional societies: American Society of Mechanical Engineers,
American Institute of Mining Engineers, American Society of
Civil Engineers, American Institute of Electrical Engineers,
American Institute of Architects, and the American Chemical
Society. The officers are: President: Karl Landgrebe, Ensley,
Ala.; Vice President: H. B. Battle, Montgomery, Ala.; Secre-
tary- Treasurer: F. G. Cutter, Ensley, Ala.
AMERICAN LEATHER CHEMISTS' ASSOCIATION
The Annual Meeting of the American Leather Chemists'
Association was held at Hotel Traymore, Atlantic City,
N. J., on May 16 to 18, 1918, in conjunction with the National
Association of Tanners.
The program included reports and addresses as follows:
committee reports
Determination of Free Sulfuric Acid in Leather. J. S. Rogers.
Testing of Coal- Tar Dyes for Leather. H. R. Davies.
Testing of Dyewood Extracts. C. R. Delaney.
Effect of Hard Water on Tannins. T. A. Faust.
Comparative Analysis. R. W Griffith.
Small's Modification of the Hydrochloric Acid-Formaldehyde Method
of Separating Tannins, with Special Application to Chestnut Oak Bark
and Chestnut Wood. T. G. Greaves.
ADDRESSES
Problems for the Consideration of the American Leather Research
Laboratory. F. H. Small.
Upper Leather for Army Shoes. Fred A. Vogel.
Sole Leather for Army Shoes. Allen Rogers.
The Work of the Bureau of Standards in Leather. R. L. Wormlby.
Description of Purifying Plant for Treating Tannery Effluent. C. L.
Peck.
AMERICAN INSTITUTE OF CHEMICAL ENGINEERS
The Summer Meeting of the American Institute of Chemical
Engineers will be held at Gorham and Berlin, N. H., June 19
to June 22, 1918. Headquarters: Mt. Madison House, Gorham.
PROGRAM OF PAPERS
The Human Element in the Mill. Hugh K. Moore.
Maintenance, Construction and Organization of Sulfite Mill. Walter
H. Taft.
The Seeding Method of Graining Sugar. H. E. Zitkowski.
The Manufacturer and Fuel Situation. Wm. M. Booth.
War Pyrotechnics. G. A. Richter.
Food Conservation. Edward Gudeman.
Chemical Stoneware and Its Properties. A. Malinovszky.
Symposium on the Coal-Tar Industry
Expansion of the Coal-Tar Industry in the United States. F E.
Dodge.
Expansion of the By-Product Industry of Coal and Water-Gas Plants
in the United States. W. M. Russell.
Manufacture of Phenol. A. G. Peterkin.
Multiple Tangent System for the Manufacture of Sulfuric Acid. L. A.
Thiele.
The following plants of the Brown Company will be visited
under the leadership of Mr. Hugh K. Moore: Sulfite Mill,
the largest sulfite mill in the world; Saw Mill and Photographic
Department; The Cascade Paper Mill; Chemical Plants, in-
cluding Electrolytic and Caustic Plants; Fiber Tube Mill;
Carbon Tetrachloride Plant; Chloroform Plant; and Hydro-
genated Oil Plant.
A joint meeting with the local section of the American Chem-
ical Society will be held on Wednesday evening at the Mt.
Madison House. A unique feature of the program will be an
entertainment by the employees of the Brown Company.
RESEARCH AS AN AID TO INDUSTRIAL EFFICIENCY
The first joint meeting of the American Cotton Manufac-
turers' Association and the National Association of Cotton
Manufacturers was held in New York, May 1 to 3, 1918, in
conjunction with the Textile Exposition.
On Friday, May 3, a session was devoted to the considera-
tion of "Research asAn Aid to Industrial Efficiency," the program
having been arranged by the committee on industrial research.
The principal speakers were Dr. George E. Hale, chairman of
the National Research Council; Dr. Charles L. Reese, chemical
director of E. I. du Pont de Nemours & Co.; Dr. Edward R.
Weidlein, associate director of the Mellon Institute; and Dr.
C. E. K. Mees, of Eastman Laboratory.
Dr. Hale's subject was "Development of Research Work."
He traced the growth of industrial research in this and other
countries, illustrating it with interesting specific instances, and
offered the assistance of the National Research Council in any
movement the cotton manufacturers may undertake looking
toward the establishing and carrying on of research in connec-
tion with that industry.
Dr. Reese, speaking on "The Value of a Chemical Organiza-
tion," classified the various functions of the chemist in a well-
organized industry, distinguishing carefully between those of
the routine analytical and the research chemist.
In his address on "Science and Industry," Dr. Weidlein out-
lined the method of development of the Industrial Fellowship
System at the Mellon Institute and gave an account of the
services which the Institute is rendering to the Government
at the present time.
The addresses of Dr. Hale, Dr. Reese and Dr. Weidlein are
given in full in the May 4 issue of the Textile World Journal.
The address of Dr. Mees is printed on page 476 of this number
of This Journal.
I'M
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 6
CALENDAR OF MEETINGS
American Society of Mechanical Engineers— Worcester, Mass.,
June 4 to 7, 1918.
American Institute of Chemical Engineers — Annual Summer
Meeting, Berlin, N. H., June ig to 22, [918
American Society for Testing Materials Atlantic City, N. J ,
June 25 to 28, 1918.
National Fertilizer Association Annual Convention, Atlantic
City, X. J., week of July 15, 1918.
American Pharmaceutical Association Annual Convention,
Chicago, August 12 to 17, 1918.
American Chemical Society -Fifty-sixth Annual Meeting,
Cleveland, Ohio, September i"to 13. 1918.
National Exposition of Chemical Industries Fourth; — Grand
Central Palace, New York City, September 2.5 to 28. 1918.
ANNUAL MEETING OF THE AMERICAN CHEMICAL
SOCIETY
The officers of the A. C. S. have decided upon September 10
to 13, 19 1 8, as the date of the Fifty-Sixth Annual Meeting,
which is to be held this year in Cleveland, Ohio.
NOTES AND CORRESPONDENCE
WOMEN'S NATIONAL LEAGUE FOR THE CONSERVA-
TION OF PLATINUM
The National Chairman of the League is Mrs. Ellw 1 B.
Spear, 27 Walker Street, Cambridge, Mass. The Council is
made up as follows:
Arizona Miss Ada Comstock Miss Blanche E. Haz-
Mrs. Henry D. Ross
California
Miss Julia George
Mrs. Frank D. Ellison ard
Miss Ethel Hale Free- Mrs Charles H. Herty
man Mrs. B. C. Hesse
Mrs. Walter L. Jen- Miss Isabel Ely Lord
nings Miss Annie Louisa
Mrs. Arthur E. Ken- Macleod
Colorado neUy Miss Margaret E.
Miss Louise J. Eppieh Mrs. Kenneth L. Mark Maltby
Mrs. C. M. Lillie Mrs. Harold Murdock Mrs. Roy Martin
Mrs. Robert W. Neff
Connecticut Mrs. James F. Norris North Carolina
Mrs. Charles L. Alvord Miss KUen F. Pendle- Mrs Thomas W
Mrs. James R. Bolton ..fon„ , T . „ , Lingle
Mrs. Percy T. Walden J >ss "e'en Leah Reed M p R Venable
Mrs. Henry P. Talbot
f„. . Miss Caroline Tieknor
III"""'- Mrs. William H. Ohio
Mrs. Julius Stieglitz Walker Mrs. Cornelius Selover
Miss Marion Talbot Mrs. Austin C. Wel-
lington Oregon
Maine "^WhiJ™ ^"^ Mrs' Vincent Cook
Mm,rnhamry "'"" M^„Heiea **• WinS' Pennsylvania
Mrs. George C. Frye Miss Mary E Woolley Miss Florence Bascom
Mrs. E. W. Clark, Jr.
Winne*"'" ^Irs Theodore
Deborah Morton
Maryland
Mrs. Frank C. Mat- Mi,ss Gertrude
thews
Miss Mary L. Titcomb
H.
Massachusetts
Miss Bertha M. Boody
Miss Abbic Farwell
Brown
Mrs. Samuel V. Cole
Mrs. George W. Cole-
man
Mrs. Arthur F. Cool-
idge
Missouri
Mrs N. W. Hopkins
Miss Eva Johnston
Mr- Philip North
Moore
New York
Mrs. Henry Altman
Mrs. Wilder I). Ban-
croft
Mrs. L. Webster Fox
Miss Margaret B .
Mac Donald
Mrs. J. Willis Martin
Mrs. Howard M.
Phillips
Mrs. Alfred S. Weill
Rhode Island
Miss Sarah E. Doyle
Mrs Maud Howe
Elliott
Mrs George H. Fowler
The Pennsylvania Chairman has issued 10,000 copies of the
following letter:
TO THE WOMEN OK PENNSYLVANIA
This League is asking you to refuse to purchase, or accept
as gifts, jewelry and other articles made in whole or in part
ol platinum, for the following reasons
Ninety-live percent of the world's supply of platinum comes
from the I ral Mountains. Present conditions in Russia make
this source of supply extremely uncertain. Moreover, in 1916.
Duparc in a French report on the 1'ral deposits stated that, at
iii' present rati- of working, these would be exhausted in 1 .•
years.
The United States Geological Survey Report on Platinum
and Allied Metals in [917 shows that the total amount, mined
since its discovery in 1843 is 10,000,000 ounces. Of that amount,
one third has been used unproductively in jewelry; one-third
has been used in dentistry, much <>f which has returned to the
earth by burial; one third has been used in physical and chemical
apparatus, in chemical industry, and electrical devices
1 M11 Government needs platinum to make nitric and sulfuric
acids, which are necessary in the production of explo
Platinum is absolutely essential in the manufacture of pyrom
hich are necessary in all steel treatments no gun can be
made without the use of pyrometi 1
Some essential signal instruments are dumb without platinum.
Platinum is essential in the composition of certain delicate
gun mechanisms.
Our country's electrical defense is dependent on iridium, a
rare metal occurring with platinum and used to harden platinum
used in jewelry and electrical apparatus.
< iur industries need platinum in their control laboratories
for the manufacture of nitric and sulfuric acids, drugs, dyes,
and fertilizers.
Our educational institutions cannot afford to pay the exorbi-
tant price for the platinum essential to train men for these in-
dustries.
The control lever of all chemical industries is analytical chem-
istry, and platinum is indispensable in that line of work.
Platinum is used in making nitrates from the air for fertilizers
and munitions.
Without platinum all experiments in gases would be greatly
handicapped.
In other words, while our Government, our industries, and our
educators all have serious use for this rare metal, one-third of
the world's entire supply has been used unproductively in
jewelry.
When the price of platinum was less than gold, women had
no desire to use it in jewelry except as a setting for gems. Now
that its price is five times that of gold, over fifty per cent of the
country's supply is used annually for jewelry. Ask yourselves
the reason. Would any woman wear a lead-colored ring or
bracelet or adorn herself with lead-colored jewelry except that
its artificially produced high price has been made to give it a
false value in her eyes3 When women cease to demand platinum
jewelry, platinum jewelry will no longer be made. If you want
to have jewels set in a white metal, ask your jeweler to make
the settings of rhotanium or white gold. These alloys closely
resemble platinum and are just as well suited to the setting
of stones. Rhotanium cannot be distinguished by sight from
platinum, even by chemists. By using these alloys, you can
have your jewelry, save money, and at the same time serve your
country by conserving this rare metal for productive uses in
the war program.
This League asks that you cooperate in this most important
branch of conservation.
Very truly yours,
Louise S. Y. Weill
Pennsylvania Chairma n
West Chestnut Avbnub
Chestnut Hiix. Pa.
SEARLES LAKE OPEN TO LEASE APPLICATION
Secretary of the Interior Lane has announced that the public
surveys have been extended over the lands known as Scorica
Lake, in San Bernardino and Inyo Counties. California, and the
township plats forwarded to the United States Surveyor General
with direction that the requisite copies be promptly furnished to
the United States Land Office at Independence for tiling.
Aside from lands patented years ago and lands embraced in
subsisting mining claims, there are about 8 sq. mi of the potash
brine zone that are now open to applications for leases, pursuant
to the act of October 2. 1 .ji 7. and the regulations thereunder of
March 21, 1918
The 1 uiied State- Laud 1 iffice at Independence, Cal .has been
instructed to receive applications for leases as soon as the town-
ship plats are received, and when the plats have been formally
filed 30 days later, to forward the applications to the General
Land Office for action In the meantime publication of notice
of application may proceed as required by the regulations.
June, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
495
Parties desiring to lease the Searles Lake potash lands can
therefore now file their applications in the United States land
office at Independence, Cal. Copies of the regulations may be
procured from the Commissioner of the General Land Office,
Washington, D. C.
The Searles Lake deposit is recognized as a large and available
source of commercial potash, and two plants are manufacturing
potash from this source at present. Saturated brine deposit is
the source of potash now being produced.
A number of parties have already filed applications for leases
in the Searles Lake region.
Several applications have also been filed for leases to the
potash deposits in Wyoming. The potash leasing bill provided
that the Secretary of the Interior may issue leases for deposits
of potash in public lands in Sweetwater County, Wyoming, which
also contains a sub-deposit of coal, on condition that the coal be
restored to the United States.
It should be clearly understood that there are two classes of
leases allowed under this bill — one is for leases on the two known
deposits, Searles Lake and Sweetwater County, Wyoming, and
the other is to hunt for deposits where it is not known that
there are potash deposits.
Under the part of the act which permits exploration for unde-
termined deposits of potash a number of permits have been issued
for exploration of lands in California, Nevada, and Colorado.
A LETTER FROM FRANCE
Gas Service
A. P. O. No. 717, A. E. F.
April 5, 1918
Dear Dr. Herty:
I am in receipt of your interesting letter of March 13. Be
sure to continue to write me occasionally, for any home chemical
news is welcomed by us all. So far, no copies of the Industrial
Journal have been received, so I enjoyed the editorial separates.
Colonel Bacon and I are now located about 150 miles from
Paris, and are engaged in the organization of a strong Technical
Division for the Gas Service, A. E. F. Col. Bacon is Chief,
and I, Assistant Chief, of that Division, which attends to all
matters chemical, medical, engineering, and ordnance. Capt.
Hildebrand is acting director of the Gas Service laboratory,
a section of ours which is doing splendid work. So far our
laboratory equipment has not been received from the States,
but all necessary apparatus and chemicals have been purchased
here because of the pressing importance of many of the prob-
lems submitted to us. Our officers and men are doing fine work
under the conditions and to date about twenty reports have
been issued. Copies of these are, of course, sent to Washington.
The French scientists are cooperating with us in every way
possible, and you will be glad to know that a Paris section of
the A. C. S. is under petition.
Colonel Bacon and I have had luncheon with Lieut. Engel
several times. At present he is engaged in preparing his Ameri-
can report. His wife is a charming American lady, active in
child welfare work here.
All of us are well and working hard.
Kindest regards to you,
Sincerely yours,
(Signed) W. A. Hamor
Best regards to you and my other friends around the Chemists'
Club in New York. Wish we could drop in there for a day.
(Signed; R. F. Bacon
THE ASSOCIATION OF BRITISH CHEMICAL
MANUFACTURERS
Editor of The Journal of Industrial and Engineering Chemistry:
Tin- attention of my Council has been called In a Certain mis-
apprehension which exists in the minds of the public as ti> the
body entitled to speak on behalf of the Chemical Manufacturers
of the United Kingdom. In this connection, I would call at-
tention to a paragraph in the Report of the Committee appointed
by the Minister of Reconstruction to advise as to the procedure
which should be adopted for dealing with the Chemical Trade,
which reads as follows:
We are, however, of opinion that the Association of British
Chemical Manufacturers is the most representative Association
of the Chemical Trade at present in existence in this country,
and that it does, generally speaking, represent the Trade as
a whole.
The address of the Association of British Chemical Manu-
facturers, is 166, Piccadilly, W. 1.
Thanking you for giving publicity to this letter, I am,
Yours faithfully,
(Signed) G. Mount, Secretary
London, England
April 26, 1918
CONSERVATION OF ALCOHOL, GLYCERIN, AND
SUGAR AS USED IN MEDICINES
According to the Official Bulletin of May 2, 1918, Dr. Franklin
Martin, member of the Advisory Commission and chairman of
the General Medical Board of the Council of National Defense,
has issued the following statement:
During the past several weeks there has been considerable
discussion throughout medical and pharmaceutical circles
relative to the conservation of alcohol, glycerin, and sugar as
applied to medicinal products.
Governmental and other authorities interested, realizing that
careful consideration should be given the subject, recently met
and debated the advisability and necessity of conservation
measures from the standpoint of medical needs. In view of
the importance of alcohol, sugar, and glycerin in the manufac-
ture of pharmaceutical preparations and of the limited possi-
bilities for the conservation of alcohol and sugar therein, it was
deemed advisable to refrain at this time from recommending
conservation of sugar and alcohol in so far as their use in pharma-
ceutical preparations is concerned.
The amount of glycerin used in medicine when compared to
the available supply was found to be relatively large, and a com-
mittee was appointed to investigate formulas, manufacturing
processes, etc., requiring glycerin and to submit plans for the
curtailment of the quantity now used in case future develop-
ments should make it necessary to adopt conservation measures
in relation to medicines.
HIGH-GRADE TECHNICAL MEN AND SKILLED OPER-
ATIVES WANTED FOR UNITED STATES
ARMY ORDNANCE'
An urgent call for high-grade technical men and operatives
to fill war positions in industrial establishments was made to-
day, through the Civil Service, by the United States Army
Ordnance.
Salaries ranging from $1600 to $6000 a year will be paid the
men who qualify for the places.
Chemists and chemical engineers; men experienced in the
manufacture of gas; mechanical engineers on high pressure
apparatus; engineers to take charge of power houses; and fore-
men of machine shops are needed. Persons of military aye
accepting appointment ^'11 no1 avoid the obligations of the
Selective Service Law.
The Army Ordnance, in issuing its call for these men. is
insisting on one point. No applications will lie accepted from
Government employees or employees of linns or corporations
engaged in contracts lor the Government or its Allies unless
written assent to such application 1 given bj the I I "I Hi'
establishment that might be seriously handicapped in its wai
work by the loss of the man
496
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 6
MANUFACTURING CHEMISTS
Superintendents for plants engaged in chemical manufactur-
ing processes, especially those connected with nitrogen fixation
and the manufacturing of acids and explosives, will be paid
salaries ranging from 82400 to $6000 a year. Assistant super-
intendents of nitrate and chemical plants will be paid $1600 to
$2400 a year.
Applicants for superintendents must have a standard high
school education or its equi\ alent, and at least five years' operat-
ing experience involving chemical processes in a manufacturing
plant, or they must be college or university graduates with at
least three years of such experience. They must have been in
responsible charge of operations involving important chemical
processes for at least two years and must have earned a salary of
at least $2000 a year.
Assistant superintendents of nitrate and chemical plants
must have had at least three years' operating experience if they
are high school graduates, or one year's experience if college or
university graduates. In either case they must have earned at
le?st $1200 a year. These superintendents and assistant super-
intendents will be assigned to duty at the Ordnance Depart-
ment in Washington or elsewhere.
CHEMICAL ENGINEERS
Chemical engineers, to be paid $2400 to $6000 a year, are
wanted for duty at the Ordnance Office in Washington, and for
duty at various plants throughout the United States. These
men will have complete supervision over one or more chemical
manufacturing processes incidental to the war. They must be
thoroughly experienced and of proved executive ability. A
college or university degree in chemistry or chemical engineer-
ing and at least three years' experience in a chemical or me-
chanical industry, or a high school education or its equivalent,
and at least six years such experience in a supervisory capacity
are required.
Chemical engineers, with salaries ranging from $1600 to
$2400 a year, and assistant chemical engineers, with salaries
ranging from $1200 to $1600 a year, also are needed by the
Ordnance Office. The positions paying $1600 to S2400 are
open to men who have graduated in a course of chemical engi-
neering from a college or university and who have had at least
one year's operating experience in some chemical or mechanical
industry, or who with a high school education or its equivalent
have had at least four years' such experience. The positions paving
from Si 200 to $i6r>o a year are open to college or university
graduates in chemical engineering who have had at least six
months' operating experience, or with a high school education
have had at least three years' such experience.
GAS MANUFACTURE EXPERTS
Operatives in gas manufacture — men to operate and control
the processes of production of water gas and producer gas — are
urgently needed by the Ordnance Office. Applicants for these
positions are paid $1600 to $2 400 a year, and must have at
least five years' experience if high school graduates, or ten
years' experience if their education has been a common school
education.
MECHANICAL ENGINEERS
Salaries ranging from $1600 to $2400 will be paid junior
mechanical engineers on high pressure apparatus who wish to
do their bit toward winning the war by working for the Ordnance
Department. Experience in the operation and control of high
pressure hydraulic and gas machinery is necessary. At least
one year of such experience will be required of graduates in me-
chanical engineering courses from recognized colleges. Four
years' experience is required of high school graduates.
POWER HOUSE ENGINEERS
Power house engineers will be paid $1800 to $2400 a year
while working for the Ordnance Department. Supervision of
operation of water-tube boilers, condensers, pumps, steam
turbines, and alternating and direct current generators and
motors are among the duties of these men. Machine shop
foremen with salaries from $1800 to $2400 also are wanted by
the Army Ordnance. Ten years' experience as machinists — -
three years in a responsible supervisory capacity — is required.
Assistant operatives in the manufacture of water gas and
producer gas, mechanics experienced on high power apparatus,
and operatives of acid and chemical apparatus are wanted by
the Army Ordnance. Many positions are open. The needs
of the service, the Ordnance Department announces, are so
imperative, that applications will be received indefinitely.
Further information regarding the Army Ordnance positions
that must be filled is obtainable of the Civilian Personnel Sec-
tion, U. S. Army Ordnance, 1330 F Street, Washington, D. C.
Washington, D. C.
May 13, 1918
WASHINGTON LLTTLR
By Paui. Wooton, Union Trus
Legislation which is almost as important to many chemical
and mineral industries as the Lever Act is to the agriculture.
coal mining, and petroleum industries, has been before Congress
during the past month. The War Minerals Bill (H. R. 11259)
provides :i more drastic control over certain mineral substances
than that exercised by the fuel and food administrators. The
minerals involved are antimony, arsenic, ball clay, bismuth,
bromine, cerium, chalk, chromium, cobalt, corundum, emery, fluor-
spar, ferrosilicon, fullers' earth, graphite, grinding pebbles, iridium,
kaolin, inagncsitc, manganese, mercury, mica, molybdenum,
osmium, sea salt, platinum, palladium, paper clay, potassium,
pvi ins, radium, sulfur, thorium, tin, titanium, tungsten, uranium,
vanadium, zirconium, The bill specifies thai it is to cover
chemical compounds, alloys, and intermediate metallurgical
produi is of each of the substances enumerated.
Tlie bill was drafted originally by tin- War Minerals Com-
mittee which is composed of a representative of the American
Institute of Mining Engineers, the Geological Survey, the
Bureau of Mines, and the State Geologists' Association It
was intended to centralize authority, so as to permit the Gov
eminent to handle the mineral situation more effectively. Hear-
ings «.u conducted before the Committee on Mines ami Min-
ing of the House of Representatives. The Committee reported
the bill favorably and it was passed by the House with the elim-
ination ol the i'ii.. fixing power and with the reduction of the
Building, Washington, D. C.
appropriation from S.50,000,000 to Si 0,000,000. As soon as
the bill had passed the House, the Senate Committee on Mines
and Mining embarked upon an exhaustive hearing. The hear-
in- before the Senate Committee took on a most interesting aspect
almost immediately, due to the fact that those opposing the
bill seemed to have reserved their comment until the measure
was taken up by the Senate
President Wilson is very much interested in securing the
passage of the bill but, despite the weight of his influence be-
hind it, the Senate apparently is reluctant to give its approval
to legislation which will permit governmental interference with
industry unless it can be shown with greatest clearness that
some form of control is necessary
The great, st interest, naturally, centers around manganese
and iron pyrites, although quicksilver, antimony, platinum,
bromine, arsenic, graphite, tungsten, and others of the minerals
have come in for extended discussion. At tins writing, the
opinions of the members of the Senate Committee have not
crystallized sufficiently to Forecast the form that the bill will
have when they compute their work upon it. The price-
fijring power and the licensing feature are the main points upon
which the Senators seem most anxious to secure expressions of
opinion.
The situation with regard to manganese ore for chemical
purposes was laid before the Senate Committee by Horace H.
June, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Lamson, of John S. Lamson & Bro., New York. The firm is
engaged in importing high-grade manganese ore. While Mr.
Lamson expressed the most earnest desire to see the develop-
ment of domestic manganese mines, he recited numerous in-
stances showing the difficulties at present in securing even small
quantities of high-grade ore from domestic sources. He urged
that imports be allowed to continue until it is proved that
domestic producers can furnish uniform grades of chemical
ore. He is of the opinion that 60,000 tons of high chemical
ore will be required by American manufacturers during the next
twelve months.
Charles H. MacDowell, of the Chemical Section of the War
Industries Board, told of the arrangement between the Gov-
ernment and the Dow Chemical Co., of Midland, Mich., whereby
the Government put down seventeen additional wells on the
Dow property in order to assist in increasing the output of
bromine. As a part of the contract, the Dow Company was to
increase its bromine plant so as to take care of the additional
product. Arrangement provided for a price of thirty-five
cents a pound for the supplies used by the Government. In-
stead of turning out the product as a liquid, it was agreed to
turn it over to the Government in the form of mineral salt, so
as to make shipment easier. The Government is using bromine
in the preparation of poison gas.
Platinum is the source of no little worry to Government
officials, Mr. MacDowell told the Committee. He told how
some platinum is still being secured in Russia. The thorough-
ness of the efforts being made is attested by the fact that shoes
and other much-needed articles are being bartered for platinum
among the Russians. Mr. MacDowell's testimony carried a
measure of relief to many of those who have been anxious with
regard to platinum supplies. He declared that there is enough
platinum in the country to meet requirements if the worst should
come, but he pointed out the great difficulties that would be
met in reclaiming the platinum used in jewelry and in other forms.
Mr. MacDowell stated that it has been necessary recently to
issue 1,000 additional commandeering orders for platinum. He
is hopeful, however, that needs can be met by restricting all
non-essential uses of platinum and by securing as much as
possible of the production in Russia and Colombia. It is Mr.
MacDowell's opinion that there is enough manganese in the
United States to meet requirements for three months, even if no
further imports are permitted. Mr. MacDowell favors the
bill.
Another revelation made at the hearing was that the Govern-
ment expects to commandeer sulfur. This step has been found
necessary in order to permit of the allocation of sulfur among
the various consumers and to conserve, as far as possible, the
supplies of nearly pure sulfur produced in Louisiana and
Texas.
Some expansion has been found necessary in the Chemicals
and Explosives Section of the War Industries Board. The
work is under the direction of L. L. Summers. In addition to
his administrative duties, he pays particular attention to ex-
plosives. Charles H. MacDowell, the assistant chief, has charge
of nitrates. Other members of the staff and their assignments
are as follows:
J. H. Adams, mica; A. Brunker, R. S. Hubbard, and A. K. WBLLS,
acids and heavy chemicals; C. H. Conner, wood distillation products
platinum commandeering and requisitioning; E. J. Haley, tanning ma
terials, greases, tallows, vegetable oils and waxes; J. M. MorehEad, coal
gas products and rare gases; I. C. Darling, toluol distribution; A. G
RosENGARTEN, fine chemicals; H. W. SanPORD, ferromanganese, chromite
tungsten, and ferrosilicon; R. M. TorrencE, chemical glass, carboys, anc
chemical stoneware; W. G. Woolpolk, brimstone and pyrites; H. R
Moody, S. A. Tucker, and Iv R. Weidlein, inorganic chemicals, electrolysis
electrometallurgy, ceramics, refractories, organic compounds, and dy
stuffs.
Associated with the Chemical Section are several representa-
tives of the Navy Department. Their names and assignments
are as follows :
D. Riley, alcohol, explosives, nitrates, alkalies, chlorine, electrochem-
icals, dyestuffs, and organic chemicals; S. R. Fuller, manganese, chrome,
and ferro alloys; C. K. McDonalds, mica; S. I. Marks, tin.
Army representatives and their assignments are as follows:
Capt. Gelsciien, alcohol, nitrates, alkalies, chlorine, acids, sulfur, and
pyrites; Mr. Lockiiart. wood-distillation products, platinum, and for-
maldehyde; C. Rice, elcctrochemicals, dyestuffs, and organic chemicals;
Lieut. Col. Spruanck. explosives and nitl
Major Seth Williams is the chemical representative of the
Marine Corps attached to the War Industries Board.
497
Among the additional commodities added to the conserva-
tion list May 17 are the following: alpaca metal and articles
containing it; paper stock, sand, and shingle stock asbestos;
spelter; numerous articles containing tin; face creams contain-
ing salts of mercury.
Final figures on production of sulfuric acid have been obtained
by the Geological Survey. The results of its exhaustive calcula-
tions are in part as follows:
The production of sulfuric acid in 191 7, expressed in terms
of acid of 500 Be., was 5.967,551 short tons, valued at $71,505,-
536, to which must be added 759,039 short tons of acids of
strengths higher than 66° Be. (which cannot be calculated
for comparison with acid of 500 Be.), valued at $16,034,545.
The increase over 19 16, in the production of acid expressed
as 50 ° Be., was therefore more than 325,000 short tons in quan-
tity and $8,800,000 in value, and the increase in the production
of stronger acids was more than 315,000 short tons in quantity
and $5,225,000 in value. The value of the total production of
sulfuric acid in 191 7 was over $14,000,000 more than in 1916.
Other final figures are as follows: lithium minerals, 2062 tons;
aluminum salts, 198,452 tons; phosphate rock, 2,584,287 tons.
Numerous important matters were discussed by members
of the Chemical Advisory Board of the Bureau of Mines in a
conference last month with Charles L. Parsons, chief chemist
of the Bureau of Mines. The chemical advisory board consists
of Dr. Wm. H. Nichols, New York; Prof. S. P. Venable, Chapel
Hill, N. C; Prof. E. C. Franklin, Stanford University; Mr.
Wm. Hoskins, Chicago; Prof. H. P. Talbot, Boston; Dr. Ira
Remsen, Baltimore; Prof. T. W. Richards, Cambridge.
To prevent the useless consumption of materials and labor in
making articles for export, the War Trade Board has announced
that written approval of war missions of the country to which
exportation is intended must be secured. Exporters of certain
articles would be required to obtain the written approval of the
Food Administration or the War Industries Board before export
license would be extended. Among the articles in the latter
class are :
All acetates, acetic anhydride, acetone, all arsenic compounds, carbon
disulfide, chrome compounds, cyanides, all dyestuffs, ethyl methyl ketones,
explosives, formaldehyde, glycerin, all manganese compounds, nitrobenzol,
all potassium salts, pyrites, saccharine, chromium ore, ferro alloys, graphite,
manganese ore, mercury, mica, nickel, metallic sodium and any metal or
alloy thereof, tin, tungsten, and wolframite.
D. W. Brunton, chairman of the War Committee of Technical
Societies, is the head of a Board to which the War Department
will refer all inventions of a mechanical, electrical, or chemical
nature.
In the United States Tariff Commission's investigations of
the chemical Industries, special attention has been given to the
manufacture of oxalic acid. American laundries, which before
the war used large quantities of oxalic acid as a bleach, have
been compelled in many cases to rely upon the less satisfactory
mineral acids. A number of other businesses, especially in
the textile and tanning trades, consumed considerable amounts
of the acid, but in most instances these industries have now
found suitable substitutes.
Before the war the greater part of the oxalic acid used in the
United States was imported from Europe, chiefly from Germany,
where the industry has been firmly established for half a cen-
tury. In 1913, Germany exported 12,500,000 lbs. of oxalic
acid and slightly over 6,000,000 lbs. of this were consumed in
the United States. The balance of the American imports,
amounting to about 1,000,000 lbs., came from Norway ami
England. A great decrease in imports was noticeable 1
1915, when we received only 3,500,000 lbs. from Germany in
comparison with almost 7,000,000 lbs. in the preceding year. In
1 'iii~, imports from Germany dropped to a scant 80,000 lbs.
Until 1909, according to the statements made before thi
Committee on Ways and Means, there was but a single Amer-
ican producer of oxalic acid and the output of this firm was
practically negligible until 1911. In that year its pro
reached 2,000,000 lbs., or slightly less than one-third of the
am. unit imported during the year. The numbl I
turers of oxalic acid has always been so small that figuri 1 D
|)n),liictii>n could not lie published without revealing the opera-
tion of individual firms. However, the statistics compiled by
the Tariff Commission indicate that in general there has been
I III. JOURNAL 01 INDl STR1 1 /. \SI> ENGINEERING ( EEMISTRY Vol. 10, No. 6
no great increase in production, although in 1914, when the
1 firms were reported t < » have
begun thi manufacture. The price of oxalic acid was about 7
■ it 8 runts in nii.}, but it increased verj rapidly until April
1 old, when it reached a maximum of So cents a pound. Since then
iIh price ha dropped and during the last year it has remained
fairly constant at about 45 cents. This is due in large part to
the increasing imports of Norwegian, Dutch, and English
.11 id
The process of manufacture employed in this country re-
quires the use of caustic potash and before tin war the American
manufacturers depended entirely upon Germany for this ma-
terial. When hostilities shut off this source of supply, the
manufacturers turned to the American producers of potash
from wood ashes. The greater supplies of Nebraska and Utah
could not be utilized as these deposits yield chloride of potash
which must be further treated before caustic potash is obtained.
In Germany oxalic acid is made from producer gas and caustic
soda, and as the- gas is a waste product in several industries
this process offers a very profitable method of manufacture.
Indications are that the American manufacturers of oxalic acids
will not be able to competi with thi German producers after the
war unless a cheap supply of caustic potash becomes available.
As far as present experiments show, the sawdust process now
used in the United States will not give satisfactory results with-
out the use of caustic potash. The producer-gas process appears
more practicable, but it involves certain engineering difficulties
which American manufacturers have not yet solved.
OB1TUARIL5
ARTHUR HENRY ELLIOTT
The recent death of Dr. Elliott is deeply regretted by a large
circle of professional and other friends, who valued highly his
friendship and were always pleased to meet him. He left the
impress of his personality on the Societies to which he belonged,
and on all who came in contact with him. He was always
ready to lend a helping hand, and many young members of the
chemical and engineering professions are deeply in his debt for
assistance which he gave them in beginning their careers.
Dr. Elliott was born in London. England, in July 185 1.
He died at Peekskill, N. Y., on February 28, 1918.
Hi family name was originally Aylot and came from Nor-
mandy with William the Conqueror. He was taken to France
when he was a child and received his early education in a Con-
vent school near the Belgian border, learning French before he
learned English. On returning to England, at the suggestion of
his father, who was a physician, he took up the study of medicine.
He was so impressed, however,
by the lectures of his professors
of chemistry (Tyndall and
others) that he dropped medi-
cine, and in 1866 entered the
School of Chemistry in South
Kensington, graduating in 1869.
He also attended lectures at the
School of Mines in Jermyn
Street.
While still a student he ob-
tained a reputation as an iron
and steel analyst, reading on
March 18, 1869, an article on
the determination of carbon in
Artiiuk Hknkv I-j.ciorr ,. . t c .. T ,
cast iron, before the London
Ch( mi' al Society, which was afterwards published in the Journal
oi tin Society.
Soon after his graduation he was appointed chemist to the
9p< no alum uoiks in Manchestei when acids, alum, and other
chemicals were manufactured and the by-products of gas
wi.iks urn handled,
in [870 he entered the service of Prentice Brothers, al Stow
market, where he had to do with the manufacture of acids,
fertilizers, and especially guncotton.
In 1872 In started on a tup around the world, with a view of
joining an uncle 111 Australia, and perhaps going to China.
Arriving m New York lu presented l.ttiis to several chemists,
among them one to Proi C V Chandler, who induced him to
staj in America and became his lid long friend.
During the m si i. w \ ears lu was connected with two different
works, one in Baltimore, the other, the Highland Chemical
Works, neai Peekskill, where he made sulfuric and from .1 local
deposit of pvntis. ;is well as from imported sulfur.
In 1879 Prof. Chandler induced him to extend his chemical
studies by entering the School of Mines of Columbia University.
He joined the third class and graduated in 188 1, receiving the
degree of Ph.B. in chemistry He then took a post-graduate
course and received in 1883 the degree of Ph.D. with a major
in economic geology and a minor in the chemistry of explosives.
From 1880 to 1888 he was associated with Prof. Chandler
in his lectures at the College of Physicians and Surgeons and
at the N. Y. College of Pharmacy.
In 1886 he was appointed demonstrator in chemistry, and
in 1888 professor of physics and chemistry and director of the
laboratories in the College of Pharmacy.
In 1889 he relieved Prof. Chandler of his lectures on inorganic
chemistry entirely, lecturing on both physics and chemistry to
juniors and seniors, as well as giving laboratory instruction in
analytical chemistry and practical pharmacy, Prof. Chandler
retaining organic chemistry.
Dr. Elliott continued to discharge these duties until 1897
when he resigned.
In 1903 he was made emeritus professor of chemistry and
physics, and in 1905 he was elected a trustee, which position he
filled until his death.
In May 1SS0 he became connected with the Municipal Gas
Lighting Company and in 1884, when the consolidation of the
Nov York gas companies took place, he became engineer-
chemist to the Consolidated Gas Company, which position he
retained until his resignation in 1910.
He was retained however as consulting chemist until his
death. In 1SS5 he became associated with Prof. Chandler in
the editorship of Anthony's Photographic Bulletin, a position
which he held until the end of 1893.
In 1SS7 he married Miss Kate P. Uglow, daughter of Dr.
James Uglow, a surgeon in the Civil War. He is survived by his
widow-, three daughters, and a granddaughter.
He belonged to the following Societies and Clubs:
London Chemical American Gas Institute
American Chemical Society Society of Gas Lighting
■ 1 m ii 1 j of Chemical Industry Illuminating Engineering Society
American Institute of Chemical Engi. New York Academv of Sciences
iiccrs Columbia University Club
The Chemists' Cluh Fireside club. Flushing
American Institute of Mining Engineers The Masonic Order
PUBLICATIONS
1 "On the Determination of the Total Carbon in Cast Iron," J.
1869.
the Determination of Sulfur in Cast Iron." Chrm. Xrws,
1870 and 1871; Diniler's polyttch .' 199
Apparatus for the Rapid Analysis of Gas Mixtures." Cktm. NtBS,
1881
4 "Report on the Methods and Apparatus for Testing Inflammable
(Ills,1 2nd Annual Report of the X. Y State Hoard of Health. 1882. p ■»•»".
\ppar. .ins fot Rapid Go 1883.
'-■ I'd ol Vitriol
: "Table on Sulfuric Acid. Showing Physical Properties ol All Strengths
Published by Mis chemist. Vssn ..i i s
s. "On Nitro-Sacchai Glycerin," about 1881.
9 "Elliott's Qualitative Analysis,' 189J. 120 pages
Besides many other papers on industrial and sanitary topics. This
is certainly the record of a most industrious and useful life.
C. F. Chandler
June, 1018 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
499
JAMES HENRY SHEPARD
James Henry Shepard, B.S., professor of chemistry in the
South Dakota Agricultural College and chemist of the South
Dakota Agricultural Experiment Station, died February 21, 1918,
at St. Petersburg, Florida, from heart failure following pneu-
monia.
He was born at Lyons, Michigan, April 14, 1850, and was
graduated from the University of Michigan in 1875. The next
thirteen years were given to natural science teaching in high
schools of his native state and to the writing of an elementary
textbook on chemistry (1885), which was quite widely used, and
"Notes on Chemistry" (1886). In June 1888 he married Miss
Clara R. Durand, of Ypsilanti, Michigan, and in the fall of that
year accepted the chair of chemistry and the affiliated experiment
station position in which he remained until his death. From
1890 to 1900 he carried the added responsibilities of the College
vice presidency, and from 1895 to 1901, that of the Station direc-
torship; also, for a decade or more, beginning in 1890, he served
as chemist to the State Food Commission.
Teaching chemistry was his chief life-work. His sympathy,
alertness, enthusiasm and information made him a loved guide
and leader. His work as Station chemist was that of a pioneer
in a new territory, where a survey of resources was the first need.
His principal bulletins deal with the drinking and artesian waters
of South Dakota, with its native and introduced forage crops,
with durum wheat and its values for bread and macaroni making,
and especially with the improvement of the sugar richness of
the sugar beet.
As a food chemist, he made two studies of especial note. The
first was upon the "constants of whisky." It led to his appoint-
ment as a representative of the State Food Officials at President
Taft's hearing, June 1909,
upon the meaning of the term
"whisky." The second related
to the bleaching of flour and its
influence upon the wholesome-
ness of the product. This work
resulted in his being called by
• the United States upon the
occasion of various hearings and
trials relating to the product;
and later by the English govern-
ment in the celebrated case
against Andrews. In these
trials his knowledge of the
subject, resourcefulness, logical
mind, psychological insight, and James Henry Shepard
strength of conviction made his services invaluable.
By his death, South Dakota has lost a pioneer in higher educa-
tion and one who has done much for the development of her
agricultural resources; the pure food cause, an earnest advocate
and helpful investigator; and his friends, one of the most lovable
men they have known.
William Frear
PERSONAL NOTL5
Mr. R. C. Burt, formerly with the Barrow-Agee Laboratories,
Memphis, Tenn., has enlisted in the Sanitary Corps, Gas De-
fense Service, and has been assigned to the Gas Defense De-
tachment, Astoria, Long Island.
Mr. John C. Trimble, formerly a student in the Philadelphia
Textile School, has joined the Chemical Service Section, National
Army, and is stationed near Yonkers, N. Y.
Mr. Jerome D. Stein has resigned his position as chief
chemist of the American Zylacq Co., of Newark, N. J., to
accept a position with the Air Nitrates Corporation, Agent of
Ordnance Department, U. S. A., for the manufacture of ammo-
nium nitrate by the cyanamide process at Muscle Shoals, Ala.
Mr. Frank P. Drane, consulting chemist of Charlotte, N. C,
died of pneumonia on April 28.
Mr. Russel B. Munroe, formerly stationed in Springfield, III.,
as chief inspector for the U. S. Army at the plant of the Western
Cartridge Co., has been transferred to the Engineering Bureau,
Ordnance Department, Washington, D. C.
Mr. R. F. Tissot, formerly employed as assistant chemist
at the Tropical Paint and Oil Co., Cleveland, Ohio, has accepted
the position of assistant superintendent with the R. C. Cook
Paint Co., Kansas City, Mo.
Mr. A. M. Lynn has been transferred from the Ordnance
Training Camp at Camp Sheridan, Ala., to the Ordnance School
at the proving grounds, Aberdeen, Md.
Dr. Lina Stern, privatdozent in the University of Geneva,
has been appointed professor extraordinary of physiological
chemistry.
Miss Mildred P. Stewart has resigned her position as instructor
in physiology and chemistry at Pratt Institute, Brooklyn. N. Y.,
to take charge of the work of the Dutchess County (N. Y.)
Public Health Association, with headquarters at Poughkeepsie,
N. Y. Miss Stewart took the degree of M.A. in public health
work at the University of California in June 191 7, while on a
year's leave of absence from her work at Pratt Institute.
Miss Lillian E. Baker, for the past four years instructor in
chemistry at Pratt Institute, Brooklyn, N. Y., has resigned her
position there to accept that of instructor in chemistry at
I -liege.
Mr. J. H. Devine, formerly superintendent of Mortem ami
Maguire, paint anil varnish manufacturers, Paterson, X. J .
lias been engaged by tin- Pennsylvania Linseed Products Co.,
Pittsburgh, Pa., for demonstration work in connection with their
product, "Linotol."
At the commencement exercises at Colgate University on
May 7, 1918, the honorary degree of D.Sc. was conferred upon
Charles H. Herty, editor of This Journal.
Mr. L. C. Mazzola has accepted the position of assistant
superintendent at the Jersey City factory of the Metal and
Thermit Corporation, having direct supervision of the manu-
facture of metallic tungsten.
Mr. H. R. Dunbar, formerly teacher of chemistry at the
Sutton High School, Sutton, W. Va., is now employed as a chemist
in the fuel department of the Bureau of Alines, Washington,
D. C.
Dr. Graham Edgar of Throop College, Pasadena, Cal., has
been appointed technical assistant to the newly established
Research Information Committee, and has entered upon his
duties at the office of the National Research Council.
Mr. Alex. C. Nixon, Jr., formerly with the Solvay Process
Company as a technical assistant in the Soda Ash Department,
is now at the American University Experiment Station, Wash-
ington, D. C, engaged in chemical research on war problems.
Mr. Carl Otto, formerly with the 136th Field Artillery, United
States Army, has been transferred to the Ordnance Corps at
Washington, D. C, and has been detailed to the American
University Experiment Station for work in chemical research.
Mr. H. J. Morgan, of the General Chemical Company, has
been transferred from the Delaware Works at Marcus Hook,
Pa., to the main laboratories of the company at Laurel Hill,
Long Island, where he will be chemist in charge.
Mr. W. J. McGee, of the Bureau of Chemistry, U. S. Dept. of
Agriculture, and formerly stationed at Savannah. Ga., lias been
transferred to San Juan, Porto Rico, where he is engaged in the
inspection of food and drugs.
Captain W. 11. Ransom, Ordnance Reserve Corps, formerly
located at Wilmington, Del., has been transferred t" tin Wash-
ington office of the Inspection Division as head of the powdei
on I 1 .plosives sub-section.
Mr. E. J- Casselman, formerly engineei of tests, Washington
Steel and Ordnance Co., Washington, l> C . has accepted im-
position of assistant chemist with the Hygienic Laboratory,
Washington. D. C.
Mi W, .1. Terpenny, lor a numbei ol jn u coi cted with
the Celluloid Zapon Company of New York and more recently
foi Mi- 1 hi mi' ai depai tment foi Anderson Gui tai son
of Chicago, has licin engaged by funis, Speiden and Company
1.1 manage then Cleveland in am ii
500
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. lb, No. 6
Mr. Arthur Hough has accepted the position of consulting
chemical engineer with the Duriron Castings Company.
Miss Phyllis M. Borthwick, lecturer in physics at the Ladies'
College, Cheltenham, England, has been appointed assistant
professor of physics and chemistry at the Lady Hardinge Medical
College for Women, Delhi, India.
Mr. Joseph L. Turner, head chemist of the Bristol-Myers Co.,
Brooklyn, has been unanimously elected first vice president
of the New York Branch of the American Pharmaceutical
Association.
At the annual meeting of the Chemical Society, London, on
March si, the Longstaff Medal for 1918 was presented to
Lieutenant Colonel A. W. Crossley, for his work in the field of
hydroaromatic compounds.
Mr. L. T. Anderegg, in charge of the department of chemistry
in the high school at Decatur, 111., has accepted the position
in the Kansas State Agricultural College chemistry depart-
ment left vacant by the resignation of R. C. Wiley.
Dr. Sidney Liebovitz has suspended his consulting work in
New York City to take up some special research work at the
Mellon Institute of Industrial Research at Pittsburgh, in
collaboration with Prof. M. A. Rosanoff, head of the department
of research in pure chemistry at that Institute.
Dr. Gerald L. Wendt has been appointed assistant professor
of chemistry and curator of the Kent Chemical Laboratory at the
University of Chicago. He has charge of the instruction in
quantitative analysis and in radioactivity.
Mr. Percy G. Savage of the Norton Company has been trans-
ferred from the Worcester plant, where he had the direction
of the refractories products, to the Niagara Falls plant where he
will be engaged in electric furnace problems.
Mr. Robert Howe, formerly with the New York and Richmond
Gas Co., has taken up the duties of assistant chemist at the
Laurel Hill plant of the General Chemical Company.
Mr. C. G. Atwater, manager of the agricultural department of
the Barrett Company, has been asked by the Ordnance Bureau
of the Navy to act as consulting engineer in connection with the
proposed Navy nitrate plant and has reported for duty at Wash-
ington. Mr. Atwater is an engineer by training and has had
long experience in the practical end of ammonia production as
well as in its utilization.
Mr. George H. Brother has resigned the position of assistant
analyst, Laboratory of the Inland Revenue Department, Ottawa,
Canada, and has accepted the position of chief chemist with the
Atlantic Loading Co., where he will direct the research and
control tests on modern explosives.
Dr. A. E. Dubin, formerly in charge of the chemical labora-
tories of the Montefiore Home and Hospital, New York, has
resigned his position to accept an appointment as research
chemist with the Herman A. Metz Laboratories, Inc., New York
City.
Mr. H. T. White, formerly with the British Cordite Co., of
Nobel, Ontario, is now connected with the laboratory of the
Sherwin-Williams Company of Chicago.
During the past year, twenty-one members of the Mellon
Institute of Industrial Research, including the director,
Lieutenant Colonel Raymond F. Bacon, and assistant director,
Majoi William A. Hamor, have entered the Government service
in response to their country's call. The following is a list of
J Fellows who have gone direct from the Institute into
Service:
K. I 1 Anion. First Lieutenant. Sanitary Corps.
II. s. Bennett, First Lieutenant, Sanitary Corps.
C. O. Brown. Captain. Ordnance Department.
A. S. Crosstield. First Lieutenant, Sanitary Corps.
H. F. Ferguson, Pril I 'cpartment.
1.1 Signal Corps.
R B Hall, Second Lieutenant, Chemical Service Section.
\\ 1 Harper, Second initary Corps.
t. 1: Howson, First Lieutenant, Sanitary Corps.
cond Lieutenant, Bngineers Corps.
in ieb, Second Lieutenant, Ordnance Department.
k \\ Miller, First Lieutenant, Saint. n \
1 II Million, Second Lieutenant, Ordnance Department.
R \ Murphy, First Lieutenant, Sanitarj Corps.
I. II > Ki. ^ >;>i.iin, Chemical Service Section.
\ 11 Stewart, Cadet, Aviation Section
II. L. Trumbull. First Lieutenant. Ordnance Department,
v.* r Vawter, First Lieutenant, Sanitan Corps.
C. L. Weirich, First Lieutenant, Sanitary Corps.
Lieut. Hamilton Merrill, of the Sanitary Corps, is now con-
nected with the manufacture of gas masks at the Gas Defense
Plant, Astoria, Long Island.
Miss Edith Tapley, of Bayside, Long Island, a graduate of
Barnard College, who has been employed in the laboratory of
the General Chemical Company in Long Island City, has been
appointed chief chemist of the General Chemical Company's
plant at Kingston, Ontario, Canada.
Mr. G. F. McMahon of the Western Electric Company has
been transferred from New York to the company's Hawthorne
plant, Chicago, 111., where electrochemical work will be under his
supervision.
Dr. H. E. Wells, professor of chemistry at Washington and
Jefferson College, has been commissioned Captain in the Chemical
Service Section of the National Army.
A new chemistry building is to be erected on the campus
of the University of North Dakota. The ground has already
been broken and •contracts to the amount of $62,438 for the
construction of the building have been let by the State Board of
Regents.
Dr. R. H. Jesse, Jr., head of the department of chemistry at
the Montana State University at Missoula, has been appointed
dean of men for the institution.
Mr. Walton B. Scott has been appointed junior gas chemist
in the Offense Chemical Research Division of the Bureau of
Mines Experiment Station and assigned to the Worcester
Polytechnic Institute to work under the direction of Prof.
W. L. Jennings.
On Thursday, May 2, 1918, Miss Grace MacLeod, assistant
editor of This Journal, addressed the students who are majoring
in chemistry at Simmons College and at Wellesley College on
"The Opportunities for Women in Industrial Chemistry."
Mr. William C. Meyer, formerly chief chemist for the National
Refining Co., Coffeyville, Kansas, has enlisted, and is stationed
at the post hospital, Fort Omaha, Nebraska.
Prof. H. V. Tartar, who for the past five years has been
station chemist and associate professor of agricultural chemistry
at the Oregon Agricultural College, has accepted a position
in the department of chemistry of the University of Washington
at Seattle.
Dr. Allen Rogers has been appointed a Major in the Chemical
Service Section of the National Army. He will be in charge
of the Industrial Relations Department.
Mr. Joseph W. Hawthorne, of the Miner Laboratories, Chi-
cago, 111., has joined the U. S. Naval Reserve Force Training
School.
Mr. Kenneth L. Fox, member of the Chicago Section, A. C. S.,
has been commissioned Lieutenant of Engineers, Tank Service,
and is now at Gettysburg, Pa., with the 65th Engineers.
Mr. William J. Hajek, formerly a member of the metallurgical
staff of Crane and Co., Chicago, is now a cadet at the School of
Aviation, Rockwell Field, San Diego, Cal.
Dr. E. N. Bunting, formerly of the Chicago Section, A. C. S.,
has accepted the position of chemist with the Bausch and Lomb
Co., Rochester, X. V
The U. S. Civil Service Commission announces open competi-
tive examinations for chemical engineer and assistant chemical
engineer, for men only. The register of eligibles resulting from
the chemical engineer examination will be divided into two
grades, as follows: Grade 1, at salaries ranging from $2,400
to $6,000 a year; and Grade 2, at salaries ranging from $1,600
to S2,4oo a year. The salary for assistant chemical engineer
will range from Si, 200 to $1,600 a year. On account of the
urgent needs of the service, applications will be received until
further notice. Applicants should apply at once for Form
1312, stating the title of the examination desired, to the Civil
Service Commission, Washington, D. C.
The following additions have been made to local transpor-
tation sub-committees: Committee for Chicago: Frederick
Rayfield, of Swift and Co . C A Ailing, of Darling and Co.,
and Dewitt Brown, Armour Fertilizer Works. Columbus. O.:
S. J. Martenet, of Farmers' Fertilizer Company, has been added
to complete the list at this point Mt. Pleasant, Tenn.: Ray
P. Hoover, of Hoover and Mason. A. K. Sheldon, of the Federal
Chemical Co., Columbia, Tenn . and L: W. Faucett, Mining and
Manufacturing Company, Charleston, S. C.
Mr Paul Gross, tutor in chemistry at the College of the City
of N\\\ York, has been commissioned Second Lieutenant
in the United States Army and has reported for duty in Wash-
ington.
June, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
501
Mr. John M. Ekert, assistant engineer in the gas and oils
department of Underwriters' Laboratories, has entered the
Ordnance Department, United States Army, as supervisor of
tests at steel plants in the vicinity of Chicago and also in Ohio,
Indiana, Wisconsin and adjoining States, Physical tests,
chemical analysis, heat treatment at plants, and the instruction
of inspectors for this territory will come under Mr. Eckert's
direction.
Dr. Rudolph Gahl has resigned from the position of metal-
lurgist in charge of concentrator at the Inspiration Consolidated
Copper Company, Miami, Arizona, to devote his time to con-
sulting practice. Mr. Guy H. Ruggles, formerly mill super-
intendent of the Humboldt plant of the Consolidated Arizona
Smelting plant will succeed Dr. Gahl.
Mr. N. J. Gebert, director of the metallurgical laboratory,
Standard Roller Bearing Division of the Marlin-Rockwell
Corporation, has resigned his position and joined the staff of
Mr. Herman A. Holz, New York. Mr. Gebert will be in charge
of the metallurgical and magnetic laboratory which Mr. Holz
is equipping in the Metropolitan Tower, New York City.
Professor J. H. Ransom, for eighteen years in charge of the
work in general chemistry at Purdue University, has resigned,
to take effect at the end of the present year.
Dr. A. W. Homberger, who has been head of the chemistry
department of Wesleyan University for the past seven years,
will leave Wesleyan at the end of the Spring term to become
dean of the chemistry department of the University of Louis-
ville, Kentucky.
Assistant Professor F. E. Breithut of the College of the City
of New York on leave of absence for the duration of the war,
has been commissioned as Captain in the U. S. Army and has
reported for duty.
Dr. B. G. Feinberg, tutor iu chemistry at the College of the
City of New York, has been appointed Research Chemist in the
Ordnance Division of the United States Army.
, Mr. D. L. Williams, instructor in chemistry at the College
of the City of New York, has been called into the national service
to be in charge of the Division of Supplies of the Research De-
partment of the Gas Warfare Section of the United States
Army.
Dr. Earl C. H. Davies will resign at the close of the present
academic year as instructor of physical chemistry and electro-
chemistry at Washington University, St. Louis, Mo., to accept
the appointment as professor of chemistry and head of the
chemistry department at Butler College, Indianapolis, Ind.
INDUSTRIAL NOTL5
List of Applications Made to the Federal Trade Comm::
Pat. No.
1,139,031
711,377
795,755
Patentee
Fritz Gossel, Frankfort-on-
the-Main, Germany
Max Bazlen, Ludwigs-
.lax Bazlen, Ludwigs-
hafen - on - the - Rhine,
Germany
1 for Licenses under Enemy-Controlled Patents Pursuant to the Tr
the Enemy Act"
Assignee
Badische Anilin & Soda
Fabrik, of Ludwigshafen-
on - the - Rhine, Ger-
Patent
Manufacture of artificial
Process of
dry hydro
Applicants
Albert B. Moses. 909 Eighth
Avenue, Seattle, Wash-
ington
E. C. Klipstein & Sons Co.,
644 Greenwich St., New
York, N. Y.
E. C. Klipstein & Sons Co.,
644 Greenwich St., New
York. N. Y.
. L. Smidth & I
Church St., New
N. Y.
50
The Shepard Chemical Corporation has applied for a Delaware
charter to deal in and with chemicals, etc. It has a capital of
$1,825,000.
The toluol plant of the People's Gas Light and Coke Co., of
Chicago, which was recently completed, is now running at
capacity. It is reported that the output of the plant will be
valued in excess of $1,000,000 a year.
Orange growers in California are finding a market for all the
dried orange peelings that can be secured, the demand coming
from the. eastern manufacturers of tobacco. Until recently
the only demand for peelings has been for the manufacture of
citric acid or confectionery, but tobacco manufacturers are
calling for tons of the dried article to be used in the manufacture
of chewing tobacco. Growers are preparing to press the juice
from their cull fruit and dry the rinds to supply the new demand.
According to Drug and Chemical Markets several large German
and Austro-Hungarian concerns, including the German Oriental
Company, the North German Lloyd Steamship Company, and
the Lohmans, have formed a huge combine, to be known as the
"Europaische Handelsgesellschaft," at Bremen, to control and
centralize the import trade in war products of all kinds, and in
raw materials from Russia, Persia, Manchuria, China, Turkestan,
Rumania and Finland. It is intended to form a union of all
exporters in these countries who had pre-war business relations
with Germany and to exclude neutrals who deal with Entente
countries from all products handled and from all commerce
with the Central Powers.
Construction work has already begun on a nitric acid plant
costing $1, 000,000 to be erected at New Castle, Pa., by the
Grasseli Chemical Company.
A large wood chemicals manufacturing plant to supply the
Bient will be built at Lyles, Tenn., by the Bon An Coal
and Iron Corporation of Nashville. The initial invi itment
is to be $1,300,000 and it is planned to consume 200 cords of
wood each day. The charcoal from this wood burning will be
used for fuel in the company's charcoal iron furnace at Lyles
The plant will have a daily capacity of from 40,0 '
pounds of acetate of lime, 2000 to 3000 gallons of crude al< ohol,
and 10,000 to 20,000 bushels of charcoal.
With a capital of $4,000,000, the Alphano Humus Company
has been incorporated at Boonton, N. J., to engage in the manu-
facture of fertilizers. The incorporators are John N. Hoff,
Boonton, N. J., Richard Sellers, Bellevue, Del., and James E.
Mantee, Portland, Me.
Among the countries making a pronounced effort to attain
material freedom from dependence upon the German dyestuff
industry, Sweden is now to be enrolled. The consumption of
synthetic colors is not very large, about 900 short tons annually.
It is felt, however, that it is sufficient to warrant the establish-
ment of a domestic industry, and a company has already been
organized to finance the project. Sweden lacks the raw ma-
terial as the country has no coking coal. It is, however, richer
in chemicals than Switzerland which possesses a flourishing
dyestuff industry despite her poverty in material. The plans
of the Swedish Company embrace competition iu foreign markets.
With a capital of $4,500,000, the Independent Chemical
Company has been incorporated at Dover, Del., to manufacture
chemicals and allied products. The incorporators are W. B.
Walsh, Brooklyn, N. Y., J. A. Lyon, New York City, and V.
Harris, Pclham Manor, N. Y.
The United States Government is said lo be considering the
construction of a large new plant at New Haven, Conn., to be
located at the works of the New Haven Gas Light Company
for the production of toluol from the gas manufactured by the
New Haven Company. The gas will be trashed to extract the
benzol, which product will then be refined, producing toluol.
The new plant is estimated to cost in the neighborhood of
$100,000.
The New England Potash Co., of Hartford, Conn., which has
taken over tin- holdings of the International Feldspar Co., at
Maromas, Middletown, Conn., will erect a ten unit plant for
tin- manufacture of potash, Portland cement, ami supi
phate from feldspar.
Alcohol is being produced in Mexico from a pi; ailed "(>'l
« in, ii grows abundantly in Northern Mexico and Westen
I I hat llir plant can be gathered at a cost of from $2 to
$5 .1 ton, and that one ton produces from 18 to 25 gal. of 180
proof alcohol.
502
THE JOURNAL OF INDl STRIAL \ND ENGINEERING ( HEMISTRY Vol. 10. No.6
Thi War Industries Board has just fixed the Government
lion for toluol in tank cars and Si. 55 Per
gallon in drums for all toluol to be released for aon-militarj
purposes, and announces that the Hoard will be glad to have its
attention drawn to any instances where a higher pri
manded. No release will be granted f<>r shipment of toluol
where a price in excess of the above is asked and all
granted for other than military uses will be stamped "Released
only upon condition that prio i 5° Pir gallon
in tank cars; Si. 55 in drums."
ding i" Drug and Chemical Markets, whin the National
Aniline and Chemical Company and 6 I du Pont de Nemours
and Company applied for licenses to manufacture dyes under
German owned patents, it was found that in many instances
insufficient descriptions were given to enable any our to follow
the correct formulas. In some cases when attempts to combine
the ingredients weri made, explosions or failures from other
causes resulted. In other cases the formulas worked wit! 1
a hitch when tried ill a lal tory, bul were a failure when an
,ihni was madi to produce the dyes in commercial quantities.
Alter tin propel combinations foi the mercantile production
of dyes were established, further careful experimentation was
necessary to discover which patented formula or formulas it
to follow in order to introduce the dyes into
fabrics. It was not until these problems were solved satis-
factorily thai the licenses were approved.
According to the \i Record a company with a
capitalizal 00 has been organized to manufacture dyes
out of weeds, and glycerin 0111 ' 'llicers of the company
an A T Thompson, President, fohn J. Blijdenstein, Vice
President; George F. Seeman, Secretary Treasurer; and William
Picker, inventor of the processes. Manager. The Food Ad-
ministration declined to give Kicker a permit to buy sugar for
■ SS until Govei mneiit chemists w ere satisfied as to the
truth ■ ■ f his claims Accordingly, Kicker gave a public demon-
Stration on .March is, at which demonstration he apparently
extracted 125 lbs. of glycerin from 300 lbs. of sugar. The
glycerin dyzed and found to be 53 per cent pure.
iint satisfii d tile Government men and they have asked
for another demonstration. In the dye process Kicker claims he
1 way of extracting from common weeds a product
equal t" the best anilini
Prior to the summer of 1914 the greater part of the chemical
laboratory glassware used ill this country was imported from
Germans and Austria The cutting off of imports from these
countries caused a very serious shortage of glassware in this
country, which is not yet entirely overcome. However, within
thi i'. ' 1 wo years a number oi American manufacturers have
increased tluii production of such ware, or are manufacturing
Chemical glassware that they did not produce before.
It is probable that practically our whole available supply at
tins time is of domestic manufacture, much of which is ware-
sold under brand names which were unknown a short time ago.
In order to furnish the chemists information regarding such
domestic brands, it was decided by the United States Bureau
ol Stand. 11, Is in compari them with those of foreign make,
'flic results of these tests indicate that all of the American-made
ted an superioi to Kavalier and equal or superior to
Jena ware for general chemical laboratory use
An important discovery has bun made as a result of a sines
of experiments carried out by the Forest Products Laboratories
ol tin Canadian Government at Montreal to ascertain whether
pine oil, hitherto imported from the Southern States, could be
produced from Canadian pine Pine ml has latterly been much
used by silver mining companies foi the treatment of ore bj the
oil Dotation process, but owing to the growing demand for it
111 the 1 lilted Mil. -, C la. ', hall operators were tin eatcued with a
i 1 'fhe Canadian Government commissioned the officials
of the Forest Products Laboratories to experiment with the
view of establishing the possibility ol producing pme oil from
Canadian red pine, which is a much less resinous wood than the
Southern pine The investigation proved successful, not only
in 1 hieing pine oil, but in the discovery that a cheapei sub
stitute for flotation p in poses could be found in creosote oil
produced as a by product in wood distillation. The oils ob-
tained at the laboratory wen tested bj the Mines branch at
Ottawa and found well suited to the dotation process for re-
,iin in. metallic ores This will providi a new market for the
wo,.,! distilling indtistrv in addition 1,' relieving a situation that
was becoming serious in connection with silver mining.
Extensive experiments in Sweden have shown that wood
cellulose is an excellent cattle feed, and the Government is
] illshiug its m it ; much as possible
il the largest seizures of enemy alien property made by
the Alien Property Custodian, A. Mitchell Palmer, is that
of the B 'any, Inc. producers of a wide range of
chemicals for medicinal and technical uses, as well as of some
coal-tar intermediates and dyes. The company is capitalized
1,000, but its business and property rights are estimated
to be worth -' ily. Among the new directors are
Nicholas K. Brady, son of the late Anthony P. Brady: George
ident of the Continental Rubber Co.,
Frederick B. Lynch, of Minnesota, and Democratic National
Committeeman from that State, who is now in bustni
Wall St., N V. City, and Martin II. Glynn, of Albany, one time
Governor of New York State.
An American strontium industry is in the process of formation.
Several of the older chemical companies are making small
quantities of strontium compounds, chiefly the nitrate, and two
or time plants in the Southern part of California have been
established especially for this purpose. These plants do not
entirely take care oi the present domestic demand. This de-
mand is largely due to war conditions, as the use of signal lights
on both land and sea has been enormously increased The
most important purpose for which strontium salts are used
abroad has never been developed here, namely, the strontia or
Scheibler process for the recovery of sugar from beet sugar
molasses. Germany at the time of the outbreak of the war was
using annually 111 the sugar industry from 100,000 to 150,000
tons of strontium hydroxide. In Russia, also, where the beet-
sugar industry is well established, probably as great an amount
was used. In Italy. Great Britain, and the United States,
however, the lime or Steffens process is the one usually em-
ployed. It is generally conceded that the strontia process is
more efficient than the lime process and that the principal
difficulties connected with its establishment in this country-
have been the cheapness and facility with which lime could be
obtained on the one hand, and the expense and difficulty of
obtaining strontium hydroxide on the other. In the case of
lime, too, this is gem rally discarded after being used, while,
owing to tin 1 uia must be recovered. Because
of the present high price of sugar and the need of employing the
most efficient process foi Us recovery, this would seem to be an
excellent time to introduce the strontia process into this country.
With the introduction of this process, the need lor strontia
would increase enormously over the present demand.
The entire exhibit of the National Aniline and Chemical Com-
pany, Inc , which form, d a part of the Sixth National Textile
Exhibition in Grand Central Palace, New York, was transferred
to the 'Made in 1' S A. Exposition" of the Jordan Marsh
Company ol Boston which was held from May 15 to 25, 1918.
The Canadian Advisory Council of Scientific and Industrial
Research, a body of experts organized under government
auspices to promote industrial development and the utilization
of natural resources, has granted a sum for the carrying out
of an investigation as to the waste of sulfite liquors by the
Canadian pulp mills, and the feasibility of its being utilized as
a by-product, 'flu Council also has under consideration the
waste of ammoniacal liquor from gas works, and its utilization
for the manufacture of ammonia as a fertilizer.
War has encouraged the production of citric acid in the
United States, according to a preliminary report on this in-
dustry just made by the United States Tariff Commission.
Quantities of this acid were imported from Sicily previous to the
war, but the United States has placed it upon the restricted
import list flu Federal census reported the production of
, lbs of citric acid in 1014, which was but a slight iu-
crease over the figures repotted in 1004 and 1909. The
Statistics reported bj the Tariff Commission show that in 1915
tin I intid States produced 3.417,705 lbs. of citric acid, in
1010, 4,182,478 lbs , and in 1017. 4.032,897 lbs.
It is reported that a new process has been invented in Japan
for manufacturing glycerin directly from tallow. This new
process is said to U twice as profitable as the ordinary method
ol producing glycerin as a by-product of soap and the inventor
has made a special contract with the Tokio Gas and Electric
Company foi tin manufacture of the apparatus.
Prior to the war Japan was a large importer of medical instru-
ments from Europe, chiefly from Germany, but conditions
brought about by tin war have greatly encouraged Japanese
industry in this line, much progress having been made ill a
comparatively short period, especially in the production of
clinical instruments, which are now being supplied by Japan to
parts of tin world.
June.iigiS THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
5°3
By a ruling of Judge Foster in the Federal District Court in
New Orleans, the Union Sulphur Co., of Calcasieu Parish, will
be compelled to pay to the State of Louisiana a tax of 10 cents
per ton on all sulfur extracted from its mines.
At a meeting of the directors of the Chemical Alliance it was
decided that a fee of 3 cents per ton be charged by the importers
for each ton of Spanish pyrites distributed by them, with the
understanding that the funds received from this source would
be used in defraying the expense of the Committee on Pyrites.
Such charge has been made effective on all cargoes received
since March 20, 1918.
It is estimated by a Chilean engineer that upward of 300,000
tons of potash could be recovered yearly from refined nitrate
and from nitrate of soda exports from Chile if a proper method
of extracting potash from the nitrate were employed. This
engineer found after extensive experimentation that the nitrate
deposits in the north of Chile contained an average of 1.73
per cent of available potash.
The Aluminum Company of America will build a nitrate
plant to cost approximately $2,000,000 near Maryville, Tenn.
The factory is to produce nitrate as a by-product of the aluminum
works and hydroelectric development. It will cover seven
acres, and, it is expected, will be completed September 1. The
Government has contracted for this plant's production of
nitrate for use in the manufacture of explosives in the
$100,000,000 works it is building at Hadley's Bend, near Nash-
ville.
The Brown Instrument Company is opening a branch
office at 2086 Railway Exchange Building, St. Louis, Mo. Mr.
Paul H. Berggreen will be in charge.
The Lake Charles Naval Stores Co., with a paid-up capital
of $900,000, has taken over the Independent Naval Stores
Company leases on 60,000 acres of turpentine land in south-
western Louisiana and will continue to operate it. The officers
are: W. B. Gillican, President; A. Vizard, Vice President; B.
Chipley, Vice-President, all of New Orleans; and W. A. Hood,
Vice President and General Manager; A. Vizard, Jr., Secretary
and Treasurer, both of Lake Charles, La.
Following investigation by the sub-committee on ferro alloys
of the American Iron and Steel Institute, it has been recom-
mended that a standard of 70 per cent manganese content and
16 per cent for spiegeleisen be adopted. These recommenda-
tions are made because of the necessity of the maximum possible
conservation of shipping and the consequent need of utilizing
domestic ores to the greatest extent possible.
One of the most important of recent industrial announcements
is that the United States Steel Corporation will make cannon
for the Government, and especially significant is the fact that
the plant to be established for this manufacture is to be located
in the interior of the country where it will be as safe as possible
from enemy attacks in the event of war being brought to the
doors of America, with the possibility of invasion. General plans
are being prepared rapidly and will soon be ready for submission
to the Federal authorities. It is reported that the plant may be
established at either Pittsburgh, Pa., Cleveland, O., or Gary,
Ind.
Pittsburgh capitalists have chartered the Shenandoah Valley
Manganese Corporation of Stanley, Va., for the purpose of
developing Virginia manganese properties. This company is
capitalized at $1,500,000, and its officers are George S. Davison,
President, and Albert P. Meyer, Secretary, both of Pittsburgh.
:
GOVERNMENT PUBLICATIONS
By R. S. McBride, Burea
NOTICE — Publications for which price is indicated can be
purchased from the Superintendent of Documents, Government
Printing Office, Washington, D. C. Other publications can
usually be supplied from the Bureau or Department from which
they originate. Commerce Reports are received by all large
libraries and may be consulted there, or single numbers can be
secured by application to the Bureau of Foreign and Domestic
Commerce, Department of Commerce, Washington. The regu-
lar subscription rate for these Commerce Reports mailed daily is
$2.50 per year, payable in advance, to the Superintendent of
Documents.
BUREAU OF STANDARDS
Comparative Tests of Porcelain Laboratory Ware. C. E.
Waters. Technologic Paper 105, 8 pp. Paper, 5 cents. Pub-
lished December 10, 1917. In general there is little choice
between the five brands of porcelain tested as far as their re-
sistance to reagents is concerned. One exception is their be-
havior with caustic-soda solution, in which test the Royal Berlin
and Japanese wares were the best, if we except the apparently
abnormally high result obtained with one of the Berlin dishes.
"The two American wares and the Bavarian crucibles made a
comparatively poor showing when suddenly heated or cooled.
In both of these tests the Japanese and the Royal Berlin porcelain
and the Bavarian dishes were equally good. No Berlin cruci-
bles were available.
"A serious defect of the American and Bavarian porcelains
was the cracking of the glaze when a hot vessel was picked up
with tongs."
DEPARTMENT OF AGRICULTURE
Maple Sugar: Composition, Methods of Analysis, Effect
of Environment. A. H. Bryan. M. N. Straughn, C. G. Church,
A. GrvEN and S. !•'. Sherwood. Department Bulletin 466,
contribution from the Bureau of Chemistry, issued Nov. 3, 1917.
46 pp. Paper, 5 cents.
Standard Forms for Specification, Tests, Reports, and Meth-
ods of Sampling for Road Materials. Anonymous. Depart
meal Bulletin 555, contribution from the Office of Public Roads
l of Standards, Washington
and Rural Engineering, issued Nov. 26, 1917. 56 pp. Paper,
10 cents.
Courses in Secondary Agriculture for Southern Schools.
(Third and Fourth Years.) H. P. Barrows. Department
Bulletin 592, contribution from the States Relations Service,
issued November 5, 1917. 40 pp. Price, 5 cents. For use of
teachers in southern schools.
Manufacturing Tests of the Official Cotton Standards for
Grade. W. S. Dean and F. Taylor. Department Bulletin
591, contribution from the Bureau of Markets, issued Decem-
ber 26, 1917. 27 pp. Paper, 5 cents.
The Relation of Some of the Rarer Elements in Soils and
Plants. W. O. Robinson, L. A. Steinkoinig and C. F. Miller.
Department Bulletin 600, contribution from the Bureau of Soils,
issued December 10, 191 7. 27 pp. Price, 5 cents. A descrip-
tion of samples used and analytical results obtained in certain
investigations on the subject. Of interest to chemists generally.
The Utilization of Waste Tomato Seeds and Skins. F.
Rabak. Department Bulletin 615, contribution from the
Bureau of Plant Industry, issued Nov. 30, 1917. 15 pp. Paper,
5 cents.
Articles from the Journal of Agricultural Research
Hydrocyanic-Acid Gas as a Soil Fumigant. Iv. Ralph de Ong.
11, 421-436 (Nov. j(>, r v 1 7 J •
Enzymes of Milk and Butter. R. W. Thatcher and A. C.
Dahlberg. 11, 437-448 (Nov. 2(1, 1917).
Tests of Large-Sized Reinforced Concrete Slab Subjected to
Eccentric Concentrated Loads. A. T. Goldbeck and 11 S
Fairbank. 11, 505-520 (Dec. 3, 1917).
Movement of Soluble Salts through Soils. M. M. McCool
AND I.. C WlIEETING. II, 53I-548 (Dec. 10, mi 7
Influence of the Age of the Cow on the Composition and
Properties of M ilk and Milk Fat. C. H, Ecklbs and L. S. Pal-
mer. II, 645 '1 :'; 1 1 '"' 1 7. 1917)-
Soil Acidity and the Hydrolytic Ratio in Soils. C II Spor-
way. Hi 659 671 1 1 *ec. 17, 1917)-
5°4
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 6
Decomposition of Green and Stable Manures in Soil. R. S.
Potter and R. S. Snyder, ii, 677-698 (Dec. 24, 1917).
Effect of Time of Digestion on the Hydrolysis of Casein in the
Presence of Starch. J. S. McHarguE. 12, 1-7 (January 7).
Contribution from Kentucky Agricultural Experimental Station.
Studies in Soil Reaction as Indicated by the Hydrogen Elec-
trode. J. K. Plummer. 12, 19-30 (January 7). Contribution
from North Carolina Agricultural Experiment Station.
Pure Cultures of Wood-Rotting Fungi on Artificial Media.
W. H. Long and R. M. Harsch. 12, 33-81 (January 14).
Contribution from Bureau of Plant Industry.
Gossypol, the Toxic Substance in Cottonseed. W. A.
Withers and F. E. Carruth. 12, 83-100 (January 14).
Contribution from North Carolina Agricultural Experiment
Station.
Relation of Carbon Dioxide to Soil Reaction as Measured by
the Hydrogen Electrode. D. R. Hoagland and L. T. Sharp.
12, 139-147 (January 21). Contribution from California
Agricultural Experiment Station.
Influence of Nitrates on Nitrogen-Assimulating Bacteria.
T. L. Hills. 12, 183-227 (January 28). Contribution from
Wisconsin Agricultural Experiment Station.
Water Extractions of Soils as Criteria of Their Crop-Producing
Power. J. S. Burd. 12, 297-309 (February 11). Contribu-
tion from California Agricultural Experiment Station.
Effect of Season and Crop Growth in Modifying the Soil
Extract. G. R. Stewart. 12, 311-364 (February 11). Con-
tribution from California Agricultural Experiment Station.
The Freezing-Point Method as an Index of Variations in the
Soil Solution Due to Season and Crop Growth. D. R. Hoag-
land. 12, 369-394 (February 11). Contribution from Cali-
fornia Agricultural Experiment Station.
Efficacy of Some Anthelmintics. M. C. Hall and W. D.
Foster. 12, 397-445 (February 18). Contribution from
Bureau of Animal Industry.
TARIFF COMMISSION
The Dyestuff Situation in the Textile Industries. 24 pp.
This pamphlet is one of a series which the United States Tariff
Commission is publishing as an aid to the study and clearer
understanding of the tariff and its bearing on various industries.
In the present instance a compilation has been made of the dye-
stuffs consumed by four groups of representative textile manu-
facturers in order to study the effect the shortage of dye-stuffs
has had on the textile industry, and to ascertain the extent to
which American-made dyestuffs have replaced those of foreign
manufacture. Textile manufacturers, who of necessity use
dyestuffs, are naturally interested in dyestuff tariffs and their
varying opinions are quoted. This pamphlet is divided into
five parts, as follows:
First, a summary of the quantity and value of dyestuffs
consumed in 1913 and 1916 by 77 important companies engaged
in the manufacture of cotton, wool, and silk goods or in the
dyeing and finishing of textiles exclusive of that done in the tex-
tile mills.
Second, the relation of the dyestuff situation to the manufac-
ture of cotton goods, including a tabulation of the dyestuffs
and chemicals consumed by 23 companies in 1913 and 1916
and answers to important questions relating to the scarcity of
dyestuffs.
Third, similar information furnished by 25 important manu-
facturers of woolen and worsted goods.
Fourth, similar information furnished by 8 important manu-
facturers of silk goods.
Fifth, similar information furnished by 21 important com-
panies engaged in the dyeing and finishing of textiles exclusive
of that done in the textile mills.
The present report will be supplemented at a later date with
information which is now being collected from the manufacturers
of dyestuffs and other coal-tar products, as required by the act
of Congress approved September 8, 1916. The section of the
law dealing with dyestuffs and coal-tar products and fixing the
rates of duty thereon is printed as an appendix to this pamphlet.
BOOK RLVILW5
American Lubricants. From the Standpoint of the Consumer. By
L. B. LockharT, Consulting and Analytical Chemist. 8vo. Pp.
236. The Chemical Publishing Co., Easton, Pa., 1918. Price, S2.00.
The work comprises a brief resume of their manufacture,
method of testing, and uses. Some of the latter treated are
Internal Combustion Engines, Automobiles, Electrical Ma-
chinery, Steam Engines, Railway Lubrication, Textile Mills,
Air Compressors, etc.
The field covered is a very extensive one and it is not surprising
that some parts are open to question. For example, on page
146 one would think that the elaidin test was a specific one for
olive oil, whereas it is only one indication. It would seem also
that a description of "the Cleveland tester" mentioned in the
preface should have been included, it being widely used. In-
asmuch as "the Pennsylvania railroad pipette" was never
suitable for determining viscosity and has long been out of use,
the picture and mention of it might well have been omitted.
The work in general is clear and concise and the chapter on
Gasolines and Kerosene particularly good and timely. Mr.
Lockhart was for a number of years chemist of the North
Carolina Department of Agriculture, and while there made a
iuhiiIhi of valuable reports upon kerosene, portions of which
n reprinted and made more accessible.
A valuable feature of the book is the inclusion of practically
all the latest specifications relative to lubricants, burning oils
and gasolines, of the Navy and War Department, and the
Pennsylvania Railroad and its allied lines.
The book will no doubt "prove of practical aid" to quote
from the preface, and may be heartily and unreservedly recom-
mended to all interested in the subject. A. H. Gill
The Method of Enzyme Action. By James Be.vttv, MA.
M.D., D. P. H. P. Blakiston's Son & Co., Philadelphia,
1917. Price, Si. 75 net.
This book was written with the view to setting forth a
hypothesis of the method of enzyme action. As a preliminary
to stating this hypothesis the author has discussed in the early
pages the chemistry and physics relating to enzyme action
under the headings "Catalysis," "Colloids," "Adsorption."
"Chemical Action," etc. The gist of the matter is stated on
page 105, in these words "* * * * the whole of enzyme
action has been reduced to the action of hydrogen and hydroxy]
radicles."
Enzymes, from a chemical point of view, are the substances
closest related to organic life with which the scientist has to
deal, and they are still surrounded with the same mystery as
life itself. Having an appreciation of the complexity and
difficulties of his subject, Dr. Beatty urges his hypothesis with
the requisite reserve. In the opinion of the reviewer the action
of H and OH radicles in explaining enzyme action is the common-
sense \ iew to take.
The general review and summary of enzyme action leading
up to the statement of the hypothesis is not the least valuable
part of the publication. J. F. Brewster
June, igi8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
SOS
By Irene DcMatty
Chemistry: First Stage. F. P. Armitace. 2nd Ed. 80 pp. Price,
$0.60. Longmans, Green & Co., New York.
Chemistry: Precis de chimie. R. Lespieau. 2 Vol. 16mo. 344 pp.
Price, 4 fr. Hachette et Cie, Paris.
Chemistry in the Home. H. T. Weed. New Ed. 12mo. 386 pp.
Price, $1.20. American Book Co., New York.
Electrochemistry Applied to Sewage Disposal. F. N. Moerk. 8vo.
77 pp. Price, $1.00. Electrolytic Purification Co., Phila.
Electron Theory of Matter. O. W. Richardson. 2nd Ed. 8vo. 631
pp. Price, $4.75. G. P. Putnam's Sons, New York.
Engineers Guide: Audel's New Marine Engineers' Guide. T. Lucas
and Others. 16mo. Price, $3.00. Audel & Co., New York.
French Medical Vocabulary and Phrase Book. Joseph Marie. 2nd Ed.
P. Blakiston's Son & Co., Phila.
Gas Motor. Max Kushlan. 12mo. 366 pp. Price, $2.50. Branch
Pub., Chicago.
Hydraulics: Handbook of Hydraulics. H. W. King. 16mo. 424 pp.
Price, $3.00. McGraw-Hill Co., New York.
Lecithin and Allied Substances. Hugh Maclean. 8vo. 206 pp. Price,
$2.25. Longmans, Green & Co., New York.
Lubrication: American Lubricants. L. B. Lockhart. 8vo. 236 pp.
Price, $2.00. The Chemical Pub. Co . Easton, Pa.
Machine Design: Elements of Machine Design. H. L. Nachman. 8vo.
245 pp. Price, $2.00. John Wiley 8c Sons, Inc., New York.
Metallurgical Calculations. J. W. Richards. One Vol. Ed. 8vo. 675
pp. Price, $5.00. McGraw-Hill Co., New York.
Oil: Popular Oil Geology. Victor ZieglER. 12mo. 149 pp. Price,
S2.50. C. H. Merrifield, Golden, Colo.
Powdered Coal as Fuel. C. F. Herrington. 8vo. 190 pp. Price,
$3.00. D. Van Nostrand Co.. New York.
Roads: A Treatise on Roads and Pavements. I. O. Baker. 3rd Ed.
8vo. 666 pp. Price, $4.50. John Wiley & Sons, Inc., New York.
Sanitary Engineering: Elements of Sanitary Engineering. Mansfield
Merriman. 8vo. 250 pp. Price, $2.00. John Wiley & Sons., Inc.,
New York.
Sheet Metal Work. W. Neubecker. 8vo. 267 pp. Price, $2.00.
American Technical Society, Chicago.
Strength of Materials. E. R. Maurer. 8vo. 126 pp. Price, $1.00.
American Technical Society, Chicago.
Van Nostrand's Chemical Annual. J. C. Olsen. 4th issue. 1918. 12mo.
778 pp. Price, $3.00. D. Van Nostrand Co., New York.
RECENT JOURNAL ARTICLES
Acid Open Hearth Steel Investigation. T. D. Morgans and F. Rogers.
Blast Furnace and Steel Plant, Vol. 6 (1918), No. 5, pp. 216-217.
Acid-Resisting Iron and Its Uses in Chemical Plant. S. J. Tungay.
Journal of the Society of Chemical Industry, Vol. 37 (1918), No. 6, pp.
87t-91t.
Analysis of Aluminum Alloys. B. Colutt and W. Regan. Journal of
the Society of Chemical Industry, Vol. 37 (1918), No. 6, pp. 9It-95t.
Analysis of Intermediates. Thomas LeClEar. Color Trade Journal,
Vol. 2 (1918), No. 5, pp. 203-204.
Barium Carbonate: Possible Sources of Barium Carbonate. S. H. Dol-
bear. Mining and Scientific Press, Vol. 116 (1918), No. 18, pp.
611-612.
Brownian Movements. W. D. Bancroft. Journal of Physical Chemistry,
Vol. 22 (1918), No. 4, pp. 273-299.
Chemical Organization, Value of. C. L. Reese. Textile World Journal,
Vol 53 (1918), No. 44, pp. 161-163.
Coal: Efficient Combustion of Bituminous Coal. R' C. Hine. Industrial
Management, Vol. 55 (1918). No. 5, pp. 388-391.
Coal: Spontaneous Ignition of Bituminous Coal. J. F. Springer. Power,
Vol. 47 (1918), No. 16, pp. 536-538.
Copper: Bibliography on the Physical Properties of Copper. P. D.
Merica. Metallurgical and Chemical Engineering, Vol. 18 (1918), No.
8, pp. 409-415.
Dust Problems in Fertilizer Plants. W. G. Clark. The American Fertil-
izer, Vol. 48 (1918), No. 8, pp. 30-31.
Dyestuff Testing in the Textile Industry. E. W. Pierce. Textile World
Journal, Vol. 53 (1918), No. 43, pp. 69-71.
Electric Furnace: Modern Electric Furnace Practice. J. K Harrison.
The Iron Trade Review, Vol. 62 (1918), No. 15, pp. 913-914.
Electrical Endosmose. T. R. Briggs and Others. Journal of Physical
Chemistry, Vol. 22 (1918), No. 4, pp. 256-272.
Enzymes: Their Chemical Composition, Mode of Action, Basic Ingredient
and Synthetic Preparation. C. B, Davis. The Chemical Engineer,
Vol 26 M'dK), No 5, pp, 164-170.
Fat: The Determination of Fat in Leather. J. A. Wilson and B J
Kern'. Journal of the American Leather Chemists Association, Vol. 13
(1918) No. 4, pp. 138-141.
luirRh
Flotation: Cascade Method of Froth-Flotation. H. H. Smith. Mining
and Scientific Press, Vol. 116 (1918), Ns. 15, pp. 505-508.
Flotation in Arizona. Rudolf Gahl. Engineering and Mining Journal,
Vol. 105 (1918), No. 16, pp. 717-719.
Flotation in Relation to Gangue Minerals. J. M. McClavb. Engineering
and Mining Journal, Vol. 105 (1918), No. 16, pp. 738-739.
Flotation of Semi-Oxidized Silver Ore. E. J. Atckison. Mining and
Scientific Press, Vol. 116 (1918), No. 17, pp. 575-577.
Fuel: The Extent of the Use of Pulverized Fuel in the Industries and Its
. Possibilities in the War. F P. Coffin. General Electric Review, Vol.
21 (1918), No. 5, pp. 373-380.
Furnace Slag: Classification of Furnace Slags. Herbert Lang. Mining
and Scientific Press, Vol. 116 (1918), No. 18, pp. 619-621.
Glass: Crystals of Barium Disilicate in Optical Glass. N. L. Bowbn.
Journal of the Washington Academy of Science, Vol. 8 (1918), No. 9, pp.
265-268.
Heat Conduction: Theory of Heat Conduction and Transfer. A D.
Williams. Blast Furnace and Steel Plant, Vol. 6 (1918), No. 5, pp.
199-201.
Hydroelectric Power in Relation to Industry. J. A Johnson. Metal-
lurgical and Chemical Engineering, Vol. 18 (1918), No. 9, pp. 462-466.
Japan's Fertilizer Trade. The American Fertilizer, Vol 48 (1918), No. 8,
pp. 21-23.
Liquid Ferromanganese in Open Hearth. E. C. Hummel. Blast Furnace
and Steel Plant, Vol. 6 (1918), No. 5, pp. 201-202.
Lubricating and Other Properties of Thin Oily Films. Lord Rayleigh.
Chemical News, Vol. 117 (1918), No. 3045, pp. 160-162.
Manganese Deposits of Clark County, Nevada. F. A. Hale, Jr. Engi-
neering and Mining Journal, Vol. 105 (1918), No. 17, pp. 775-777.
Microscope to Detect Steel Impurities. John McConnell. Blast
Furnace and Steel Plant, Vol. 6 (1918), No. 5, pp. 219-221.
Microscopic Study of Welded Tires. S. W. Miller. Journal of Acetylene
Welding, Vol, 1 (1918), No. 11, pp. 472-479.
Minerals Used in the Pulp and Paper Industry. L. H. Cole. Pulp and
Paper Magazine, Vol. 16 (1918), No. 15, pp. 339-341.
Natural Gas: Making Substitutes for Natural Gas. F. Denk. The
American Drop Forger, Vol. 4 (1918), No. 4, pp. 132-135.
Oil: The Kentucky Oil Fields. W. N. Thayer. Engineering and Min-
ing Journal, Vol. 105 (1918), No. 17, pp. 781-785.
Oil-Shale Industry. A. J. Hoskin. Mining and Scientific Press, Vol.
116 (1918), No. 15, pp. 509-516.
Petroleum Industry in Kansas. W. A. Whitaker and Others. Engi-
neering and Mining Journal, Vol. 105 (1918), No. 18, pp. 817-821.
Power: An Ingenious Solution of a Power Problem. R J. Horns.
Paper, Vol. 22 (1918), No. 5, pp. 15-17.
Radioactivity of Italian Minerals: Sulla radioattivita di minerali italiani.
L. Francesconi. Cazzetta chimica ilaliana. Vol. 48 (1918). No. 3, pp.
112-113.
Radium: Some Experiments on the Extraction of Radium from American
Pitchblende Ores by Chlorination. Mrs. Ray Cable and H, Schi.undt.
Metallurgical and Chemical Engineering, Vol. 18 (1918), No. 9. pp. 460-
462.
Research: Development of Research Work. G. E. Hale Textile
World Journal, Vol. 53 (1918), No. 44, pp. 163-164.
Research: Efficiency in Industrial Research. C. W. Hill. Metallurgical
and Chemical Engineering, Vol. 18 (1918), No. 4, pp. 182-184.
Rubber: The Oxidation of Rubber. S J. Peachey and M I. eon.
Journal of the Society of Chemical Industry, Vol. 37 (1918), No 4, pp.
55-60.
Rubber and Jelutong. F. Dannerth. Metallurgical and Chemical Engi-
neering, Vol. 18 (1918), No. 6, pp. 296-298.
Salicylic Acid: The Manufacture of Salicylic Acid. Color Trade Journal,
Vol. 2 (1918), No. 5, pp. 186-188.
Science and Industry. IJ. R, Weidlein. Textile World Journal, Vol 53
(1918), No. 44, pp. 186-191.
Shale Oil: Commercial Aspects of the Shale Oil Industry. J 11 ('..
Wow Mining and Scientifii Press, Vol. 116 (1918), No. 18. pp 51 I
614.
Smelting Changes to Conserve Zinc. W. McA, Johnson. Mining and
,s, ientific Press, Vol 116 (1918), No. 16, pp. 555-556.
Solubility of Paraffins, Aromatic Naphthenes and Olefins in Liquid Sulfur
Dioxide. R. J Moore ani> others Metallurgical <m,l Chemical
leering, Vol 18 (1918), No 8, i> i> 396 402.
Solvents for Nitrocellulose. J. N. Hans. DuPent Magatdne, \ "I 8
(1918). No. '. pp 13 14.
Spruce Turpentine: Recovery of Spruce Turpentine in the Mill. A. W.
NiCKHESON Pulp and Pafet Mage in< Vol l< (1918), No 15, pp.
335-338.
Steel: Development of Steel from the Early Ages. U K. GRSAVB! ' hi
Dm/, F,,rK'r, Vol 4 (1918)., No 2, pp. 61-66.
5°6
MARKET REPORT-MAY, 1918
WHOLESALE PRICES PREVAILING IN THE NEW YORK MARKET ON MAY I S, 1918
INORGANIC CHEMICALS
Acetate of Lime 100
Alum, ammonia, lump 100
Aluminum Sulfate, (iron free)
Ammonium Carbonate, domestic
Ammonium Chloride, white
Aqua Ammonia, 26°, drums
Arsenic, white
Barium Chloride
Barium Nitrate
Barytes, prime white, foreign
Bleaching Powder, 35 per cent 100
Blue Vitriol
Borax, crystals, in bags
Boric Acid, powdered crystals
Brimstone, crude, domestic Long
Bromine, technical, bulk
Calcium Chloride, lump, 70 to 75% fused. . . .
Caustic Soda, 76 per cent 100
Chalk, light precipitated
China Clay, imported
Feldspar
Fuller's Earth, foreign, powdered
Fuller's Karth, domestic
Glauber's Salt, in bbls 100
Green Vitriol, bulk 100
Hydrochloric Acid, commercial, 20°
Iodine, resublimed
Lead Acetate, white crystals
Lead Nitrate
Litharge, American
Lithium Carbonate
Magnesium Carbonate, U. S. P
Magnesite, "Calcined"
Nitric Acid, 40°
Nitric Acid, 42°
Phosphoric Acid, 48/50%
Phosphorus, yellow
Plaster of Paris
Potassium Bichromate, casks
Potassium Bromide, granular
Potassium Carbonate, calcined, 80 @ 85%.. .
Potassium Chlorate, crystals, spot
Potassium Cyanide, bulk, 98-99 per cent
Potassium Hydroxide, 88 @ 92%
Iodide, bulk
Nitrate
Permanganate, bulk
-, flask "5
Red Lead. American, dry
Salt Cake, glass makers'
Silver Nitrate
Soapstone, in bags
Soda Ash, 58%, in bags 100
Sodium Acetate
Bicarbonate, domestic 100
Bichromate
Chlorate
Cyanide
Fluoride, commercial
Hyposulfite 100
Nitrate, 95 per cent, spot 100
Silicate, liquid, 40° Be 100
Sulfide. 60%, fused in bbls
Bisulfite, powdered
m Nitrate
Sulfur, flowers, sublimed 100
Sulfur, roll 100
Sulfuric Acid, chamber 66° B<$
Sulfuric Acid, oleum (fuming)
Talc, American white
Terra Alba, American, No. 1 100
Tin Bichloride, 50°
Tin Oxide
White Lead, American, dry
Zinc Carbonate
Zinc Chloride, commercial
Zinc Oxide, American process XX
ORGANIC CHEMICALS
Acetanilid, C. P., in bbls Lb.
Acetic Acid, 56 per cent, in bbls Lb.
Acetic Acid, glacial, 99l/i%. in carboys Lb.
Acetone, drums Lb.
Alcohol, denatured, 180 proof Gal.
Lbs.
nominal
Lbs.
@
4.50
Lb.
3 'A
@
4
Lb.
nominal
Lb.
17' <
©
18
Lb.
20
(<■>
22
Lb.
16'A
@
17
Ton
65.00
©
85.00
Lb.
12
@
13
Ton
30.00
©
35.00
Lbs
1.80
©
2.00
Lb.
8.80
©
9.00
Lb.
7 'A
©
8'A
Lb.
13'A
©
15
Ton
nominal
Lb.
75
@
85
Ton
22.00
©
25.00
Lbs.
4.25
©
4.35
Lb.
4'A
0
5
Ton
20.00
0
30.00
Ton
8.00
©
15.00
Ton
minal
Ton
20.00
©
30.00
Lbs.
1.50
@
3.00
Lbs.
1.15
©
1.25
Lb.
27.
©
2'A
Lb.
4.25
©
4.30
Lb.
17
©
18
Lb.
nomina
Potassiu
Potassiu
Potassiu
Quicksilv
Sodiuc
Sodiuc
Sodiuo
Sodiun
Sodiuo
Sodiun
Sodiuc
Sodium
Sodiuc
Sodiuc
Stront
1.40
2.00
1.50
2.50
nominal
83 'A @
17.00
0
120.00
10
@
1071
25.00
0
27.00
61'A
0
63'/.
10.00
0
12.50
2.20
0
2.65
23
0
24
3.00
0
3.25
24
0
24V.
2.60
6.25
2.50
Lbs.
4.05.
©
4.50
Lbs.
3.70
©
4.10
Ton
32.50
©
35.00
Ton
60.00
©
65.00
Ton
18.00
©
20.00
Lbs.
1
.17'/
27 V.
1 .00
©
©
Lb.
1 10
Lb.
9
©
9'A
Lb.
28
@
30
Lb.
14 .
©
15' .
Lb.
12Vi
©
16
4.85 %
90»/, %
5.40 @
Alcohol, sugar cane, 188 proof Gal.
Alcohol, wood, 95 per cent, refined Gal.
Amyl Acetate Gal.
Aniline Oil, drums extra Lb.
Benzoic Acid, ex-toluol Lb.
Benzol, pure Gal.
Camphor, refined in bulk, bbls Lb.
Carbolic Acid, U. S. P., crystals, drums Lb.
Carbon Bisulfide Lb.
Carbon Tetrachloride, drums, 100 gals Lb.
Chloroform Lb.
Citric Acid, domestic, crystals Lb.
Creosote, beech wood Lb.
Cresol, U. S. P Lb.
Dextrine, corn (carloads, bags) Lb.
Dextrine, imported potato Lb.
Ether, U. S. P. 1900 Lb.
Formaldehyde, 40 per cent Lb.
Glycerine, dynamite, drums included Lb.
Oxalic Acid, in casks Lb.
Pyrogallic Acid, resublimed, bulk Lb.
Salicylic Acid, U. S. P Lb.
Starch, cassava Lb.
Starch, corn (carloads, bags) pearl 100 Lbs.
Starch, potato, Japanese Lb.
Starch, rice Lb.
Starch, sago flour Lb.
Starch, wheat Lb.
Tannic Acid, commercial Lb.
Tartaric Acid, crystals Lb.
OILS, WAXES, ETC.
Beeswax, pure, white Lb.
Black Mineral Oil, 29 gravity Gal.
Castor Oil, No. 3 Lb.
Ceresin, yellow Lb.
Corn Oil, crude 100 Lbs.
Cottonseed Oil, crude, f . o. b. mill Lb.
Cottonseed Oil, p. s. y 100 Lbs.
Menhaden Oil, crude (southern) Gal.
Neat's-foot Oil, 20° Gal.
Paraffin, crude, 118 to 120 m. p Lb.
Paraffin Oil, high viscosity. Gal. 40
Rosin, "F" Grade. 280 lbs Bbl.
Rosin Oil. first run Gal. 41
Shellac. T.N Lb. 62
Spermaceti, cake Lb. 31
Sperm Oil, bleached winter, 38° Gal. 2.23
Spindle OU, No. 200 Gal. 36
Stearic Acid, double-pressed Lb. 23
Tallow, acidless Gal. 1 .58
Tar OU. distilled Gal. 32
Turpentine, spirits of Gal. 52
METALS
Aluminum, No. 1. ingots Lb. 32
Antimony, ordinary Lb. 12l/«
Bismuth, N. Y Lb. 3 . 50
Copper, electrolytic Lb. 2
Copper, lake Lb. 23*/i
Lead, N. V Lb. 7
Nickel, electrolytic Lb. 55
Platinum, refined, soft Oz.
Silver Oz.
Tin, Straits Lb.
Tungsten (WOj) Per Unit
Zinc, N. Y Lb.
FERTILIZER MATERIALS
Ammonium Sulfate 100 Lbs.
Blood, dried, f . o. b. Chicago Unit
Bone, 3 and 50, ground, raw Ton
Calcium Cyanamide Unit of Ammonia
Calcium Nitrite, Norwegian 100 Lbs.
Castor Meal Unit
Fish Scrap, domestic, dried, f. o b. works. . . Unit
Phosphate, acid, 16 per cent Ton
Phosphate rock, f. o. b. mine: Ton
Florida land pebble. 68 per cent Ton
Tennessee, 78-80 per cent Ton
Potassium "muriate," basis 80 per cent Ton
Pyrites, furnace size, imported Unit
Tankage, high-grade, f. o. b. Chicago Unit
62
0
64
21
m
22
33
m
34
17
0
18
17.00
m
17.25
17 ■/,
0
—
20.40
0
20.50
1.00
0
1.02
3.15
e
3.20
10
0
10'A
nominal
99»/i
nominal
6
70
0
6
4:
00
0
norainAl
nominal
is
oo
nominal
—
i
50
@
3
M
S
50
0
6.00
nominal
nominal
6.60
The Journal of Industrial
and Engineering Chemistry
Published by THE AAVERIGAN CHEMICAL SOGIETY
AT HASTON, PA.
Volume X
JULY 1, 1918
No. 7
Editor: CHARLES H. HERTY
Assistant Editor: Grace MacLeod
Advertising Manager: G. W. Nott
ADVISORY BOARD
H. E. Barnard, H. K. Benson, F. K. Cameron, B. C. Hesse, A. D. Little, A. V. H. Mory
Published monthly. Subscription price to non-members of the American Chemical Society, $6.00 yearly; single copy, 60 cents
Price per single copy to American Chemical Society members, 50 cents Foreign postage, seventy-five cents, Canada, Cuba and Mexico excepted
Entered as Second-class Matter December 19, 1908, at the Post-OfiBce at Easton, Pa., under the Act of March 3, 1879
All communications should be sent to The Journal of Industrial and Engineering Chemistry.
Telephone: Vanderbilt 1930 35 East 41st Street, New York City
Subscriptions and claims for lost copies should be referred to Charles L. Parsons, Box 505, Washington, D. C.
Eschhnbach Printing Company, Easton, Pa.
TABLE OF CONTENTS
Editorials:
Platinum at White Heat 508
The Modern Miracle 508
An Army without Reserves 508
A French Local Section 510
Original Papers:
The Manufacture of Amyl Acetate and Similar Solvents
from Petroleum Pentane. Benjamin T. Brooks,
Dillon F. Smith and Harry Essex 511
The Effect of Annealing on the Electrical Resistance
of Hardened Carbon Steels. I. P. Parkhurst 515
Volumetric Determination of Free Sulfur in Soft
Rubber Compounds. H. S. Upton 5l8
Rapid Determination of Carbon in Steel by the
Barium Carbonate Titration Method. J. R. Cain
and L. C. Maxwell 520
The Preparation and Testing of Pure Arsenious Oxide.
Robert M. Chapin 522
The Bisulfate Method of Determining Radium.
Howard H. Barker 525
A Rapid Pressure Method for the Determination of
Carbon Dioxide in Carbonates. W. H. Chapin 527
A Proximate Analysis of the Seed of the Common Pig-
weed, Amaranlhus Retroflexus L. Everhart P.
Harding and Walter A. Egge 529
The Detection of Vegetable Gums in Food Products.
A. A. Cook and A. G. Woodman 530
Uniform Nitrogen Determination in Cottonseed Meal.
J. S. McHargue 533
The Detection and Determination of Coumarin in
Factitious Vanilla Extracts. H. J. Wichmann 535
The Determination of Essential Oils in N on- Alcoholic
Flavoring Extracts. Frank M. Boyles 537
A Contribution to the Composition of Lime-Sulfur
Solutions. O. B. Winter 539
Laboratory and Plant:
A Standard Apparatus for the Determination of Sulfur
in Iron and Steel by the Evolution Method. H. B
Pulsifer 545
Determination of Acetic Acid by Distillation with
Phosphoric Acid W. Faitoute Munu 550
The Determination of Acetone. Allan J. Field 55-'
Some Results of Analysis of Airs from a Mine Fire,
A. G. Blakeley and H. H. Geist 552
A Differential Refractometer. G. A. Shook 553
A Volumenometer. J. S. Rogers and R. W. Frey. . . 554
An Evaporator for Acid Liquids. F^dward Hart 555
Conversion of Formulas. Willis H. Cole 555
Addresses:
Technical Applications of Nephelometry. Philip
Adolph Kober 556
Municipal Contribution to Conservation through Gar-
bage Utilization. Edward D. Very 563
American Garbage Disposal Industry and Its Chemical
Relation. Raymond Wells 567
The Potteries at Shek Waan, near Canton, China.
Clinton N. Laird 56S
Current Industrial News:
Niter Cake; Petroleum in the British Empire; Potash
Lye; Oil Clarifier; Canada's Export Trade; Irriga-
tion Plant; Recovery of Solvent Naphtha; Pure
Bismuth; Various Classes of Engines; Register of
Overseas Buyers; Industrial Uses of Bismuth;
Russian Monazite Sand Deposits; Mineral Output
of Great Britain; Effect of Insulation on Steam
Drums; Hardening Carbon Steel; Tungsten Fila-
ments; Tar-Still Corrosion by Chlorine; Cotton-
Sampling Machine; The Long-Range Gun; British
Board of Trade 57-
Scientific Societies:
French Section, American Chemical Society; The Ger-
man Union of Technical and Scientific Societies; Amer-
ican Pharmaceutical Association ; Calendar of Meet-
ings 575
Notes and Correspondence:
Importance of Chemists Recognized by Secretary of
\\ 'ai , Co6peration of American Chemical Societj
with the Chemical Service Section; <lu Pont Fellow
ships; Four Hundred Thousand Dollar Gift to the
Massachusetts Institute of Technology; Coal-Tar
Products for 1917 vs"
12
583
... 586
NBW I'I'HI.H \1IU\S
Market RBPORT
\v \siiincton Letter ,
Personal Notbs
Industrial Notbs
Government Publii
;o8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo.
EDITORIALS
PLATINUM AT WHITE HEAT
During the past month the subjed of platinum has
o the forefront in the thoughts of the American
For the first time, and by one of those quick
3 of general understanding which have char-
d this war period, the nation has learned the
important bearing of this element upon the part we
are to play in the war.
liief factor in arousing this interest and under-
standing has been the widespread publicity given by
ress to the stirring address delivered in the
Hou i of Representatives on June 7 by Hon. Henry T.
Rainey, Congressman from Illinois. In this address
In depicted clearly the important function of platinum
in explosives manufacture, the inadequate measures
taken for its conservation by those charged with this
ible duty, and the factors which had con-
tributed to such inadequacy.
Since the delivery of that address many things have
0 light which would prove interesting reading;
editorial discussion of these, however, will be post-
poned. Only one conviction is expressed here — the
immediate place for the platinum in this country is in
the vaults of the Treasury Department.
THE MODERN MIRACLE
cely two years have elapsed since many lines
of our industrial life were threatened with utter de-
moralization because of the shortage of dyestuffs and
medicinals resulting from the blockade of German
ports by the British navy. Textile mills faced the
imminent possibility of shutting down because of
inability to secure dyestuffs for their fabrics. Tan-
ners, lithographers, and wall paper men sought in
vain for needed coloring matter, and pharmacists'
stocks of many much-used medicinals became de-
pleted. On account of these shortages and the accom-
panying speculation in the remaining stocks, prices
soared to undreamed-of heights.
Yet within this short period of two years, one of
which has been devoted to war preparations, a miracle
has been wrought. Mills have not closed; all lines of
industrial life requiring synthetic colors are operating
under normal conditions; the sick have been provided
with ample medicinal supples; prices have been largely
d and are comparable with prices of all other
commercial products; in addition, ships have borne
to other parts of the world large quanti-
ties of dyestuffs.
ting tribute could be paid to the skill and
energy of 'he American chemist than has been done
the medium of two government announce-
ments which have been issued during the past month.
the one by the I . S. Tariff Commission and the other
by the War [ndl rd.
tit by the Tariff Commission
the results of its census of synthetic dyestuffs and
11 (page 582, this issue). Accord-
it ton of dyestuffs in the
fiscal year 1914 was 45,840.866 pounds, while in 1917
the domestic production amounted to 45,977,246
pounds. The tonnage has been made good and even
exceeded. While it is true that there is a difference
"in the relative amounts of the various classes of dyes''
in the two periods mentioned, it is interesting to note,
as the Commission's statement points out. that the
lines which have failed of their full share of develop-
ment have been exactly those to which were given
only the ad valorem duty of 30 per cent, while in those
classes which were given both the 30 per cent ad
valorem and the 5 cents per pound special duty "the
American manufacturers have shown remarkable prog-
ress." The statements of manufacturers and con-
sumers at the hearings on the Hill bill are abundantly
confirmed by the announcement of the Tariff Com-
mission. By the enactment of tariff and anti-dumping
legislation, capital was attracted to the industry,
and the chemist has made good.
As to medicinals, the War Industries Board, in an
authorized statement in the Official Bulletin of June
6. 1918, says:
"Actual or prospective shortages have come to the
notice of the Board in but few instances so far as
medicine and medicinal chemicals are concerned.* *"
Congress, capital, and chemists cooperating have
accomplished the modern miracle.
AN ARMY WITHOUT RESERVES
General Foch has aroused the enthusiasm of the allied
world by the masterly manner in which he has handled
the reserves during the recent mammoth drives of the
German army. These struggles have fitly been des-
ignated as "the battles of reserves." The morale
of all the nations joined in the contest against German
aggression has been stimulated by the conviction that
an endless flow of reserves is proceeding with all
possible haste from American to European shores.
In the matter of reserves for the armies in the field
all goes well.
The army of American chemists is now in
rapid process of complete mobilization. At last the
matter of efficient utilization of chemists has been
grasped with a firm hand by those in authority.
The orders issued by the Secretary of War on May
28, 1918 (page 580, this issuel show that the may of
previous orders has been changed to must, and under
these new orders the full strength of the chemistry
forces will soon be reached. It appears that every
possible contingency as to graduate chemists has been
provided for. Congratulations to Secretary Baker
and to those who have aided him in the preparation
of these comprehensive orders!
With the thus mobilized army of chemists all goes
well. But what about the reserves for this army?
We are preparing for a long war, how long no one
knows, but certainly as long as is necessary to insure
the triumph of the principles to which we have dedi-
cated our all. Daily grows the expansion of the con-
[uly, 101S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
ception of the vast forces we must put in the field,
on the sea and in the air. Increases in personnel
necessitate similar expansions in the program of
chemical industries, and these in turn must be manned
by chemists. It is full time therefore that serious
consideration should be given to the matter of reserves
for this army of chemists. The source of reserves is
in the universities and colleges, and we beg to urge
the most broad-minded and far-sighted consideration
of this problem by three groups of men: university
administrators, War Department officials, and leaders
in the chemical industries.
UNIVERSITY CONDITIONS
The universities represent the training camps for
the reserves of the chemistry army. These institu-
tions function through their chemistry staffs, their
physical equipment, and through the number of under-
graduates who present themselves for the chemistry
courses.
At the present moment the instructional staffs of most
of the universities are in a completely demoralized
condition. Many professors and associate professors
are on leave of absence in Washington engaged in
research on problems vital to the winning of the war
and the prevention of needless sacrifice of the lives
of our men at the front. No more important work
could engage their attention. Others are busy with
similar problems in the private laboratories of the
universities. The concentrated effort required in such
undertakings does not admit of much energy being
devoted to effective teaching. On the other hand the
university men of lower rank, the instructors and
assistants, charged primarily with the instruction of
the lower classes, are for the greater part subject to the
draft. In certain unusual cases deferred classifica-
tion has been given such men by Local Boards. These
cases, however, are sporadic and form no part of a
general policy. Continued low salaries in universities,
made necessaryby decreased budgets, the high salaries
paid in the industries, and the increased cost of living
have forced many men from the universities into the
industries. The net result is a burning of the candle
at both ends, so far as the forces for training re-
serves are concerned. Bi-terminal combustion is con-
sidered a reckless policy in all other matters, why not
in this?
In the ranks of the students, present year seniors
have already left university campuses and are now
either in uniform or in industrial plants. The matter
of post-graduate students is evidently a thing of past
history until at least the ending of the war. Further
, the operation of the draft law (in whose principles
we most emphatically believe) and the need of men
in the chemical industries have combined to lake
away from the universities many of the students in
the junior classes. Meanwhile preliminary repi
for next Fall indicate the largest enrollmenl
students intending to make chemistry their Hie
work ever known in our educational history. This is
'•uly natural in view of the greater recognition givi n
to the importance of chemistry in war work and to its
S©9
value in every channel of industrial life. These
are the men who constitute the chemistry reserves.
They will soon be in the training camps of the uni-
versities. Will they find sufficient officers present to
give them adequate instruction for their development
into efficient reserves?
To add to the complexities of the situation there is
no question about the crippled finances of the uni-
versities and of their helplessness in preventing the
present drain upon their corps of instructors.
These are the conditions, as we see them, in this
most critical year of our country's history. Certainly
such conditions demand the most earnest consideration
on the part of all who can in any way contribute to
their amelioration. From what sources may help
reasonably be expected?
ACADEMIC ASSISTANCE
First, assistance must come from the universities
themselves. Such aid cannot be in the nature of in-
creased appropriations, for university finances are al-
ready too hard hit. But they can in some instances
shake themselves loose from traditions and modify
internal organization and the character of courses to
meet as far as possible the pressing need of the times.
An example of such increased efficiency is shown by the
merger of the University and the Sheffield Scientific
Sohool departments of chemistry at Yale University,
recently announced.
It may be possible in some cases for institutions to
combine forces. Many difficulties in such a plan
present themselves, though these difficulties may not
be as great as at first thought they seem. A certain
minimum laboratory space is considered necessary per
student. Possibly this space may be more efficiently
utilized, at least in the lower classes, by repeated
using of the same space by more than one student, in
spite of the difficulty which at once suggests itself as
to responsibility for equipment. The number of men
who can be taught properly by an instructor is limited.
This is a real difficulty, and sacrifice may be necessary
here. Other courses must be taken besides chemistry
and this may present physical difficulties. Hard-
ships may be enforced upon individual students from
living conditions under such combined institutions.
This is a question of finance for which a remedy might
be found. These are but types of the many per-
plexing academic problems to whose solution the best
thought of our university men will be unstintedly
given.
AID FROM nil WAR DEPARTMENT
Second,no word of exhortation to theWar Department
1 necessary in the matter of instructors for chemical
The provision of such is only the logical
following nut of the principles now being applied in the
creation ol our armies. Reserves are of course
essential. These are of no value unless adequatelj
trained. For this training instructors are required.
In the training camps to-day are many soldiers who
could rendei effective service on the fighting front,
Vli 1 lav are ol greater service t" the army in the
5io
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 7
work of developing the raw recruit. How then can
the War Department aid in the provision of instructors
for chemistry students? In one of at least two ways:
Either by granting class exemption to instructors in
chemistry or by detailing men already in the service
to instructional work in the university lecture rooms
and laboratories. If exemption as a class should be
given, then some distinguishing emblem should accrue
to such men, for the time is at hand when peculiar
glances are cast at young men of draft age who are not
attired in khaki. If on the other hand it is deemed
best that they should be enlisted and detailed
back to universities, then it is fortunate that under
the present orders of the Secretary of War the work
of detailment would be in the hands of the Chief of the
Chemical Service Section, Lieutenant Colonel Bogert,
whose long and distinguished career as a teacher in
one of our greatest universities preeminently qualifies
him for such a duty. Time is an important factor
in the matter, however, for every day that lapses after
the opening of the universities next Fall is just so
much loss in the work these soldier instructors will be
expected to perform.
Of course the time may come when it will be advisable
to close university doors and stop many other
lines of daily effort, in the hope of putting across the
one great blow for victory. That time does not seem
to have arrived yet. Our enemies are apparently pur-
suing that policy now, and judging from the results to
date it is proving disastrous for them.
SUPPORT FROM THE CHEMICAL INDUSTRIES
Third, the future of the industries depends upon no
factor more than upon the output of chemists from
the universities. Wonderful progress has been made
in these industries in the past, particularly during the
three preceding years. Much more must be accom-
plished, if we are not to rest content simply with doing
as well as some other country has done. Within
university walls next year will be young men who some
day will have to take up the reins now so ably held by
the present leaders. Already the industries have
attracted to their staffs many valuable univer-
sity teachers. We cannot eat our cake and have
it too. Furthermore, the industries have already
drained the universities of all available students
possessing sufficient training to go into works labora-
tories. We believe that the heads of industrial labora-
tories will bear out the statement that the stand-
ard of qualifications of student accessions to in-
dustrial' staffs has within the past two years been
decidedly lowered. If this condition becomes worse
its deleterious effect will be markedly shown in the
industries during the next decade. Foresight is called for.
How can the industries aid? By giving generously
of their well earned profits of recent years to strengthen
ami build up the chemistry departments of the uni-
versities. It is not a question of charity or philan-
thropy, but can well be regarded as an investment.
With the aid of funds from this source the
pay of professors and instructors can be increased,
thereby diminishing the necessity for leaving
university ranks because of the increased cost of
living. So, too, equipment of university laboratories
can be fully maintained and improved. The account
(page 581, this issue) of the anonymous gift to the
Massachusetts Institute of Technology for the purpose
of further improvement in its equipment for chemistry
and physics shows that someone's mind is moving in
this channel. Finally, many of the ablest students
are in need of financial assistance if they are to
get the best training the universities offer. The
creation of scholarships and fellowships will do much
to alleviate this situation, aside from the stimulation
induced by prospective rewards of good work.
An important step in this direction has just been taken
by the du Pont Company in setting aside a portion
of its earnings for this purpose (page 581, this issue).
Many other ways of aiding through funds will suggest
themselves if once our industrial leaders are convinced
that in this matter they have just as important an
interest as in the purchase of raw material or in the
efficiency of plant operations.
The chem'stry army must have its reserves. Good
generalship will provide these.
A FRENCH LOCAL SECTION
Another tie joins France and America; another
offspring of the American Chemical Society takes its
place in the family of local sections. On page 575
of this issue is printed the application to the Council
for permission "to found in Paris a French section
of the Society covering the entire territory of France."
As the usual Spring meeting of the Council was not
held, this application for charter is now being voted
upon by the Directors. It requires no gift of prophecy
to predict that the vote will be of such enthusiastic
unanimity as never before characterized a vote of the
Directors. The first public announcement of the ap-
plication, made by Secretary Parsons, on the request
of President \ichols, at the recent joint outing of
the Philadelphia and Delaware Sections, was greeted
with tremendous applause.
The signatures on the application are those of dis-
tinguished French chemists intermingled with those
of American chemists, known to us all, who are now
at the front in the service of our Army, a joint brigad-
ing of French and American forces similar to that
which has been affected recently between units of the
respective armies under the leadership of that great
soldier, General Foch. The successful result of the
military union has already made itself evident on the
battlefields of France; with equal confidence we can
look forward to increased strength from the closer
cooperation of scientific forces through the medium
of the French Section.
As we read the application for charter and note the
words "the entire territory of France" we know that
these words will carry only one meaning to French
and American chemists alike, namely a restoration
of the eastern boundary of France, changed from that
of August 1O14 only in that it shall include Alsace and
Lorraine, and to that end the entire resources of this
country, men and material, are now dedicated.
All hail to the French Section!
July, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
ORIGINAL PAPERS
THE MANUFACTURE OF AMYL ACETATE AND SIMILAR
SOLVENTS FROM PETROLEUM PENTANE
By Benjamin T. Brooks, Dillon F. Smith and Harry Essex
Received March 12, 1918
In a recent paper1 we noted the effect of very high
pressures on the conversion of chlorpentane to alcohol.
In the following paper we describe a method for the
conversion of chlorpentane to the corresponding
acetates under conditions which we believe are capable
of realization on a large scale without great difficulty
and without very costly or complicated apparatus.
The present prices of amyl alcohol and acetate are,
of course, abnormal. Yet it is very doubtful if the
prices during several years before the war will be the
rule for some time after the war, unless there is a large
production from some source not now known or the
synthetic article is brought into the market in large
quantities. Before the war this country imported
annually approximately 6,000,000 lbs. of fusel oil from
Russia. The decrease in the manufacture of distilled
liquors and the spread of prohibition generally will
cause an increased shortage of amyl alcohol and
acetate.
As is well known to all familiar with fusel oil and
amyl acetate and their uses, these terms are employed
to describe the mixture of amyl alcohols, or their
acetates, together with more or less butyl and hexyl
derivatives. The composition of the natural fusel oils
varies considerably with the material fermented and
the character of the fermentation. Fernbach's re-
cently developed fermentation, yielding chiefly iso-
butyl alcohol, is an extreme case, and isobutyl alcohol
alone is too volatile for most of the technical uses of
fusel oil or amyl acetate. The following analyses
from Worden's "Nitrocellulose Industry" illustrate
what is commonly found in commercial fusel oils:
Composition of Natural Fusel Oils
From Corn Spirit
Normal propyl alcohol . 3.7
Isobutyl alcohol 15.7
Amyl alcohol 75.8
Hexyl alcohol 0.2
Fatty acids, etc 0.56
From Potato Spirit
Per cent
by wt.
Normal butyl alcohol. . . 6.8
Isobutyl alcohol 24 . 3
Amyl alcohol 67 . 8
Fatty acids, etc 0.04
The ordinary amyl acetate of commerce contains
approximately 70 per cent by weight, distilling within
the limits 135 to 140°. The above analyses make clear
the fact that it is not necessary to isolate either pure
pentane as a raw material for synthetic amyl acetate,
a single monochlorpentane to make an artificial
Stmyl acetate fulfilling all the ordinary requirements of
industrial uses.
A fairly large number of patents have been issued
i-hich have for their object the manufacture of amyl
icetate from light petroleum mixtures, chiefly pentane.
['he difficulties of most of these processes, so far as
we are acquainted with them, appear to be, first, the
formation of large proportions of dichlor and trichlor
' J. Am. Chcm. Soc, 88 (1916), 1369.
derivatives when the original hydrocarbon mixture is
chlorinated, entailing considerable loss of chlorine,
decomposition during distillation with evolution of
hydrochloric acid, corrosion of the distilling apparatus,
etc. The presence of higher chlorinated pentanes also
has the very objeationable result that on decomposition,
as during distillation, chloramylenes are formed which
are relatively stable and make their presence known
in the final synthetic amyl acetate by materially de-
creasing the solubility of many substances in this
solvent. One patentee claims that glacial acetic acid
need not be used as a solvent in the chlorpentane-
sodium acetate reaction, but acetic acid containing as
much as 30 per cent of water may successfully be em-
ployed. Our experience is that amyl acetate made
with acetic acid containing 10 per cent or more of
water, contains considerable unchanged chlorpentane,
the presence of which markedly decreases its solvent
value. The second serious difficulty, common to all
the processes known to us, consists in the formation of
relatively large amounts of amylene.
The first of the difficulties above mentioned has
been overcome almost completely and in a very simple
manner.
CHLORINATION OF PENTANE
In the earlier period of our work we lost considerable
time by attempting to develop a satisfactory method of
chlorination based on the idea that the reaction should
take place in the gaseous phase. Accordingly, a large
number of chlorinations were made by introducing
chlorine into the hydrocarbons at temperatures just
sufficient for the complete vaporization of the hydro-
carbon. In these experiments we assumed that the
chlorine and hydrocarbon gas mixture should be
thoroughly mixed before reacting, and this was at-
tempted by introducing the chlorine into the hydro-
carbon gases in the dark and then passing this mixture
through large illuminated glass tubes. In these ex-
periments it was found that once the chlorinating
action had started it would proceed very smoothly in
diffused daylight and that ultraviolet light as a
catalyzing agent was not necessary; indeed, the re-
action often proceeded with considerable violence and
the separation of some free carbon. It was difficult
to regulate accurately the ratio of hydrocarbon vapors
to the chlorine introduced, and the formation of
dichlor and trichlor derivatives was unavoidable. The
yields of monochloride derivatives were ob-
when the chlorine-hydrocarbon mixture con-
tained a large excess of hydrocarbons, namely, 2 to 4
times the ratio necessary to form the monochloride
ives. By employing mixtures containing 3
1 hydrocarbon to one of chlorine, a yield of
monochloride of 88 per cent of the theoretical was ob-
is, 88 per cent of the chlorinated material
was monochloride. The large volume of hydrogen
chloride formed in this reaction carries off large amounts
vapor, this fact necessitating the ab-
SI2
THE JOURNAL OF INDUSTRIAL A VD ENGINEERING I HEMISTRY Vol.
io. No. -
on of i he hydrogen chloridi in cold v.
order to recover this pentane. I' was easily apparent
thai the manufacture on a lai oi crude chlor-
pentane by this method would entail great practical
difficulties, and would certainly add a great deal to the
cost of this comparatively simple operation.
After a number of preliminary experiments, which
tlo1 I"- recorded here, a method w;
which has proved to be quite satisfactory and which
has served for the preparation of large quanl
these chlorinated hydrocarbons. The simplicity of the
method makes it entirely adaptable to large scale
opei itions, and a fairly large experience with it over
more than one year's time shows that the chlorinated
product consists of the monochlorides to the extent of
90 to 94 per cent.
The principle of the method simply consists in main-
taining always a very large excess of hydrocarbon as
compared with chlorine and also, which is very im-
portant, a very large ratio of hydrocarbon to
chlorinated products. In brief, the method consists
in passing chlorine through a large number of small
orifices into a large quantity of cold crude pentane, and
stopping the chlorination before the concentration of
the chlorine derivatives becomes greater than about
20 per cent of the mixture. In practice, escaping
hydrogen chloride is absorbed in cold water and the
pentane thus recovered is returned to the reaction
vessel. The presence of moisture is not objectionable.
it seems to be desirable. Illumination of the
reaction mixture is not absolutely necessary, although
we have employed a high-power tungsten light bulb
in the upper part of the reaction vessel, the light
catalyzing the reaction at the start. This reaction
exhibits a peculiar phenomenon. At first the pentane
l>l' rs to dissolve the chlorine unchanged, but after
an interval of about ten minutes the color of free
chlorine quickly fades and disappears and then chlorine
may be passed in very rapidly, reacting as fast as
ed. The liquid should be kept chilled to at
least 10° to prevent too great vaporization of pentane
with the hydrochloric acid formed.1
The control of the process can readily be accom-
plished by observing the specific gravity of the mixture.
since a specific gravity of 0.820 corresponds to about
jo per cent of monochlorides, when a crude pentane
on boiling at 25 to 450 is taken for chlorination.
In order to illustrate the per cent of suitable crude
pentane contained in a high grade of gasoline. 76 ° Be.,
1 hi following table of fractions obtained by slow
distillation through suitable column is given:
Boiling Point
!Vr cent by Volume
28-30°
30-35°
0 17.8 pei cent -
litablc to
\0
5 S Acetate
in i
5 0
45-50°
6 6
50-55°
8 5
8.5
60-70°
Casing head or natural gas gasoline naturally con-
tains the largest per cent of pentane and when suitable
provision is madi to avoid losing the butane, as by
1 Hro.il,;., Essex and Smith t nited States Patent No 1,191,196.
ing in a heavier gasoline, this raw material
should prove the most economical.
The fractional distillation of the monochlorides
furnishes another opportunity to reject material of un-
suitable boiling point. A distillation analysis of the
monochlorides employed in most of the work here de-
Us having been made from a crude
pentane fraction boiling point 25 to 45 °, is given
below:
Boiling Point
Per cent by W
igbt
3.8
100-110°
4f, 6
110-120
27 4
120-130°
14.4
130-140°
5 3
bove 140'-
2.4
Several results which are typical of those obtained
by chlorinating the cold pentane are given below.
The per cent yield is calculated on the per cent of
monochlorides in the total chlorinated hydrocarbon,
not on the amount of pentane originally taken. Thus
if the yield is 90 per cent, the balance of 10 per cent is
a higher chlorinated product.
I — Chlorination <<f Crcde Pentane. Boiling Point J5 4^
\\ 1
Lost
with
Time HC1
Grams Hours Per cen
5500 4.5 13.4
5500 5.5 35.0
5500 4.0 29.0
1500 4 11 25.0
-•11711 5 > 28.0
3700 6.0 25.0
Concentration of chlorides
when chlorination was stop]
Mono-
Wt. In- chlorides
Product changed 9.5-140° Dichlorides
(.'.rams Grams Grams Grams
5233 3908 1155 170
4108 2555 1371 182
4206 3312 884 10
2698 1775 611 47
1492 975 407 110
2781 2309 444 28
Per cent monochlorides in
If desired, a pentane fraction of much smaller
boiling point range can be employed as the initial raw
material, and this will result naturally in a final acetate
of smaller range of boiling points. The fractional
distillation to obtain most of the crude pentane used
in our work was carried out in a small 50-gallon ex-
perimental apparatus. More homogeneous fractions
would be obtainable from larger stills provided with
suitable columns, such as those employed for the
rectifying of crude benzols.
A small amount of hydrochloric acid is formed
during the distillation of the crude chlorpentane, due
to slight decomposition of the chlorides. The amount
of decomposition resulting from this cause is so small,
however, that no appreciable diminution of the yield
of crude chlorpentane results. This fact has to be
taken account of. however, in the choice of apparatus
for distillation, as will be brought out later.
CONVERSION 01 CHLORPENTAN1 INTO VMM ACETAT1
Although the conversion of chlorpentane into amyl |
acetate by heating with anhydrous sodium acetate is,
at first sight, merely a direct application of a standard
method of organic synthesis, we found it necessa
to carry out a large number of experiments in order
determine the optimum conditions, particularly
regards temperature and pressure, nature of solver
effect of agitating the reaction mixture, yield fror
July, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
513
various gasoline fractions, material of construction
for apparatus, effect of catalysts, and possible utiliza-
tion of the by-product amylene.
Early in the course of the work we determined that
somewhat better yields of acetate are obtainable with
the lower boiling fractions than from hydrocarbons
of higher boiling point. Kerosene chlorides are highly
unstable, decomposing slowly at room temperature
to such a degree that in several cases the pressure
of the HC1 developed was sufficient to expel the cork
from well stoppered containers. The tendency of the
alkyl chlorides to decompose with the formation of
defines increases with those of higher molecular
weight, as is shown by the following results.
Table II — Yield of Acetate from Chlorinated G
Boiling Point Yield Acetate Olefines
Original Per cent Per cent
Hydrocarbon of Theory of Theory
28-30° 50
30-35° 49
35-40° 49
45-50° 46
50-55° 46
55-60° *3
60-65° 42
65-70° 38
Calculated for pentane
Calculated for pentane
Calculated for pentane
Calculated for 50 per cent pentane
Calculated for 50 per cent hexane
Calculated for 50 per cent hexane
Calculated for 50 per cent hexane
Calculated for 50 per cent hexane
1 Heated 1 1 hours at 190-195° in autoclave, not stirred.
Owing to the large amount of solid material in the
reaction mixture, anhydrous sodium acetate at the
beginning and sodium chloride toward the end of the
operation, we carried out several comparative experi-
ments to determine the effect of continual agitation
of the contents of the autoclave. When the reaction
mixture is not agitated, a hard, nearly solid salt cake
forms, which prevents further reaction.
Autoclave
stationary
Autoclave
rotated
Autoclave
stationary
Reaction Mixture
580 g. Chlorides
750 g. Sodium acetate
375 g. Acetic acid
375 g. Amyl acetate
580 g. Chlorides
750 g. Sodium acetate
375 g. Acetic acid
375 g. Amyl acetate
730 g. Chlorides
800 g. Sodium acetate
472 g. Acetic acid
ul., rides
650 g. Sodium acetate
750 g. Acetic acid
458
300
The presence of water in the glacial acetic acid
retards the reaction very markedly, acetates made in
this way containing relatively large amounts of un-
changed chlorides, as illustrated by the following
experiments.
Table IV — Influence of the Water
Solvent Hours
Acetic acid, 99 per cent 15
Acetic acid, 90 per cent 15
Reaction M
Yield
Acetate
Per cent
of Theory
4: 3
38.0
TIRE
Chlorine
i Product
Per cent
2.0
5.3
The presence of a solvent is necessary if a product
free from chlorides is desired. The result obtained
without a solvent is shown in Experiments n and 19,
Table V. in which it will be noted that the per cent of
unchanged chlorides in the product is very high.
A few substances, BaCl2, FeCl3, and CuCl. were
tried for their possible catalytic effect, but no benefit
could be noticed in the results.
It is possible that the amylenes resulting in the
treatment of the chlorpentane mixture, as herein
noted, are derived largely from secondary or even
tertiary chlorides or acetates. We tested the stability
of commercial amyl acetate, consisting almost entirely
of acetates of primary alcohols and found that during
8 hours at 205 ° and about 300 lbs. pressure in a copper
lined autoclave, only 6.5 per cent of amylenes were
formed. After cooling, the autoclave showed a pres-
sure of 60 lbs., due to gaseous products of the decom-
position, probably C02 and ethylene.
We have not had the opportunity to examine the
constitution of the amyl acetates made from the
petroleum fractions, as the primary object in view
was the commercial utility and value of the product.
We find that the solvent power of synthetic amyl
acetate for cellulose esters and gums is such that by
these tests alone the natural and synthetic acetates
cannot be differentiated from each other. If, how-
ever, the acetate contains two or more per cent of
chlorine in the form of unchanged chlorides, its solvent
power for gums and resins is markedly diminished.
A number of typical results are included in Table V.
UTILIZATION OF AMYLENES
We believe it is very doubtful if the amylenes,
obtained as a by-product in the conversion of the
chlorpentanes to acetates, can profitably be converted
into alcohols or acetates. So-called hydration of
amylenes and other olefines to the corresponding
alcohols has been investigated by us and the results
I-
Ml
to
Chloride
| .r.nii
Sodium
, Acetate
Grama
Solvent
Crams
94
89
51
IK
50
400
730
7 VI
50
4(H)
900
100 g. Acetone
500 g. Absolute alcohol
>iic acid
470 g. Acetic acid
17
580
7SII
375 g. Acetic acid
375 g. Amyl acetate
19
1 1
1 inn
950
1422
1215
None
None
5
S80
750
7 SO g. Acetic acid
7
580
750
tic acid
175 k. Acetic acid
375 g. Amyl acetate
Ta
BLE Y
Yield
Chlorine
Yield An tate
Crudi \<i
tate
in
Corrected
Temp.
Pressure
Per cent <,f
Product
Per cent of
° C.
Pounds
Theoreti
al
Per etui
Theoretical
Remarks
180-190
60
1911
li! '
) 14
s', 2
Product contained free
220
51 5
11 <)
4'i :
193 'MM
iso
ss 11
41 4
[95 -200
230
55.4
1 .2
5.1.4
195-200
170
47 0
1 1 O
314
20S .'Hi
lllll
IS i
(, 1
16 1.
195-200
400
430
41 11
1.0
41 .2
HI g, BaCb in reaction
.'ill I
45.0
3.5
319
30 g FeCli added
195-200
50.0
0 9
48.8
514
THE JOURNAL OF IXDVSTRIAL AND ENGINEERING ( BEMISTRY Vol. 10. No. 7
Amyl Acetate
Flow Sheet — Quantities for ONe Day
CllLORINATION
Chlorine. 5620 lbs
or 110 cells
Condensing Wate
2700 lbs. HC1 in weak soln
Dichlorpentane Loss
Amyl Acetate
Flow Sheet — Acetylation
Cryst. Sodium Acetate
Pentane, 107S gal. X
18.000 gal. storage tank Mtiting pans, fused Acetate
^_ Rcc. Pentane , 3225 gal.
5,000 gal. storage tank
Autoclaves, copper lined
MonocbJorpentane
Glacial Acetic
Acid, storage tank
Wash water
Washing tanks Salt and Sodium Acetate
Solution
Sodium Acetate*
Evaporator
Recovered Pentane, 3225 gal.
MonocbJorpentane, 6750 lbs.
8.000 gal. storage tank
embodied in a separate paper.1 With sulfuric
acid the principal results are polymerization to
heavier, more viscous oils (not tars), the forma-
tion of alcohols and of acid and neutral esters of
sulfuric acid. We have not been able to obtain
yields of alcohol as high as noted by Wischnegradsky1
in the case of amylene made from natural fusel oil.
The yields obtained by us are given in the following
table, and it will he noted that with 50 per cent acid
very little change was effected and with 05 per cent
acid at 5.00 mostly polymers were formed.
Tabu VI— Addition of Water to Amylene-Hexene Mixti-re nv mi.
puric Acid of Varying Concentrations
E ;
50 — 5
2
1.0
90.0
1.0
8.0
75 0
.5
18.0
45.0
16.0
21.0
75 —10
16.0
54.0
17.0
13.0
75 0
2
10 0
67.0
9.0
14.0
...Is) 0
2.5
10.0
57.0
15.0
18.0
75 —15
2
10.0
12.0
8.0
85 —15
32.0
14.0
32.0
85 + 1 vol. —10
13.0
56.0
18.0
13.0
acetic acid
5.0 11.0 75 0
In view of the readiness with which olefines react
with many mineral acids, such as II. Mb. HC1, HBr,
.tnd in some cases eve': HCN and 11 S, we
thought it possible that under certain conditions
acetic acid might react with the amylcnes direct.
Accordingly the conditions of the usual acetylation
1 J. .lm. Chrm. Soc.. 41 11918), 822.
> Inn , 190 (1877). 328.
Crystallizing pan
Acetic Acid, glacial
' Amyl Acetate, storage
were tried on amylene itself. A quantity of crude
amylene, 125 g., boiling point 30 to 60°, was heated
in an autoclave at 200 ° for 5 hrs. with an equal weight
of glacial acetic acid. From the reaction product we
isolated only 4.5 g. oil boiling at 100 to 135 ° and 4.0
g. residue above 13 5 °, these fractions consisting of
polymers of the original amylenes. In another ex-
periment 00 g. amylene were heated 20 hrs. at 1000
with 00 g. acetic acid and 30 g. zinc chloride and the
result was 14.5 g. polymers boiling over ioo°. A
reaction mixture duplicating the last was let stand 30
hrs. at 20 to 24 °, obtaining 8 g. polymers.
It is not the purpose of the present paper to go into
the details of producing a given output of synthetic
amyl acetate. However, a brief discussion of the
character of the apparatus required and a conservative
estimate of costs should make clear that the commercial
manufacture of synthetic amyl acetate is entirely
feasible. In view of the amount of amyl acetate
annually consumed in the United States alone and the
amount of the synthetic acetate which might con-
servatively be expected to find a ready place in the
market we have, tor the sake of definiteness. based
estimates on a daily production of 600 gal. of synthetic
amyl acetate. The figures used are based upon a
yield of monochlorides of 90 per cent, a low average
lor the method described, and a yield on acetylating
of 55 per cent of the theory, a result actually at-
tainable and probably exceeded. The minor by-
products, amylene, common salt, and hydrochloric acid,
have not been given any value in the estimate. It
has been assumed that the crude pentane would be
July, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
SiS
furnished in tanks or steel drums, being most ad-
vantageously manufactured at the source of pro-
duction of casing head gasoline. The price of such an
article in fairly large quantities bears no relation
whatever to the prescription doses of pentane sold for
photometric work. It has also been assumed that
the most advantageous location for such a plant would
be in the neighborhood of a chlorine-caustic soda plant,
where the chlorine would be available for use without
liquefaction. The diagrams indicate roughly the flow
of material.
APPARATUS REQUIRED
I — STORAGE FOR
(a) Crude pentane, 18,000 gal. steel tank.
(6) Crude chlorinated product, pentane and chlorpentane,
18,000 gal. lead-lined steel tank.
(c) Distilled chlorpentane, 8,000 gal. lead-lined tank.
(d) Sodium acetate, crystalline, 100 ton covered wooden
bins.
(e) Glacial acetic acid, 10,000 gal., 5 wooden tanks,
2,000 gal. each.
(/) Amyl acetate, finished, 15,000 gal., 3 steel tanks, 5,000
gal. each.
2 CHLORINATION
3 units complete, each consisting of one 500 gal. earthen-
ware vessel1 fitted with lead coil for cold water or brine,
glass Hart condenser of the type used for nitric acid,
and earthenware receiver for separating recovered pentane
and aqueous HC1.
3 — STILLS
2 Steam jacket Duriron stills, 1000 gal. charge capacity for
rectifying chlorpentane.
1 Steam jacket copper still" for rectifying amyl acetate,
acetic acid, and amylene mixture, capacity 900 gal.
4 — ACETVLATION
3 Copper-lined steel autoclaves, jacketed, heated by hot
oil circulation, provided with agitators of copper or
Duriron, capacity 900 gal. each.
5 — ACCESSORIES
1 Centrifugal extractor, 30 in. copper mesh basket, for
separating salt from reaction mixture.
1 Agitator, copper, for washing amyl acetate with soda ash
solution, capacity 900 gal.
1 Wooden tank with chain type agitator for washing ex-
cess sodium acetate from salt, capacity 500 gal.
2 Crystallizing pans, iron, in brick setting, slow direct fire
for recovering sodium acetate, 300 gal. each.
3 Melting pans, steel in brick setting, slow direct fire for
fusing sodium acetate, capacity 200 lbs. sodium acetate
each.
1 Motor for agitating autoclave, 8 h. p. steam, 200 boiler
h. p. for distillation, heating building, pumping, etc.
4 Dump cars and track for conveying salt, sodium acetate,
etc.
1 Motor, 8 h. p., for operating pumps.
3 Low-pressure rotary pumps for pumping pentane, amyl
acetate, etc.
Estimated Cost of Synthetic Amyl Acetate on the Basis of 600
Gallons Daily Production
Daily Costs
Gasoline, 990 gal. at 40 cts $ 396.00
Chlorine, 5200 lbs. at 2.5 cts 130.00
Acetate of soda. 4880 lbs. cryst. acetate at 15 cts 732.00
Soda ash, 1450 lbs. at 3 cts 43.50
Interest on $35,000 at 6 per cent, and depreciation at 20 per cent
per annum 30.30
Labor, one chemist at $8.00, 10 laborers at $4.00 48.00
Fuel and Power 40 . 00
Total Daily Costs $1419.80
Value op Products
Amyl acetate, 600 gal. at $4.50 per gal $2700.00
Total daily costs 1419.80
Daily Profit $1 280 . 20
Mellon Institute of Industrial Research
Pittsburgh
nriLDiNGS
i Shed for storing acetate of soda.
i Building for chlorinating pentane and distillation of
chlorpentane, fireproof asbestos board,
i Building for acetylating and distillation of amyl acetate,
t Building for boilers and fusing sodium acetate.
1 Suitable vessels of this size are regularly manufactured.
THE EFFECT OF ANNEALING ON THE ELECTRICAL
RESISTANCE OF HARDENED CARBON STEELS1
By I. P. ParkhursT
Received November 24, 1917
The electrical resistance of steels as affected by im-
purities or by different heat treatments applied over
wide ranges of temperature, has attracted the atten-
tion of several investigators. A resume of previous
work is here given.
RESUME OF PREVIOUS WORK
W. H. Johnson2 made a study of the electrical re-
sistance of steels in order to determine the effect of
impurities. The resistance of seven samples of differ-
ent analyses was measured. The impurities were
found to increase the resistance, but the data ob-
tained were not sufficient to allow of specific conclu-
sions.
A. Campbell3 determined the effect of stress on
the resistance of iron and iron-nickel wires. Prac-
tically no change was observed up to the breaking
point.
H. Le Chatelier4 investigated the effect of high tem-
peratures on the resistance of iron, steel, hard steel,
iron-nickel, platinum, etc. His measurements were
made in an atmosphere of hydrogen. In a 0.6 per
cent carbon steel he observed breaks in the tempera-
ture-resistance curves at 710 and 820° C.
H. Le Chatelier5 studied the effect of hardening
and tempering on the resistance of steels. His re-
sults showed that the resistance was increased by
hardening and decreased by tempering.
L. Compredon6 made a study similar to that of W.
H. Johnson, referred to above, and obtained similar
results.
J. De War and J. A. Fleming7 determined the re-
sistance of iron and nickel at temperatures down to
the boiling point of oxygen. They found that the
resistance decreased rapidly with the decrease in tem-
perature.
' Read in abstract .a the Metallurgical Symposium, Boston Meeting,
American Chemical Society, September 1917.
"I nemical Composition and Electrical Resistance of Steel Wire."
J. Iron and Hied Inst., 19 (1881), No. 2, 605.
"Electrical Properties," Engineering, 63 HSH7), 4<>s.
I "Electrical Resistance "1 iron and Us Alloys at High Temperatures."
( ompt. raul . 110 (1890), 283.
' "Effect of Tempering on the Electric Resistance of Steel," Compt.
find . 112 i 189! I. I".
• "Electro conductivity of Steel," l.r Genie Civil, 19 (1891), 309.
I "Electrical Resistance of Iron." Phil. Man.. 34 (1892), 326.
5i6
THE JOURNAL OF IX DUST RIAL AND ENGINEERING < HEMISTRY Vol. 10, \"o.
F. Osmond1 investigated the effects of carbon,
silicon, nickel and manganese on the resistance of
steels. He found that the resistance was increased
by all these elements, and especially by silicon, nickel
and manganese. The temperature coefficient fell
in a parabolic curve with increase in resistance.
H. Le Chatelier2 studied in detail the effects of car-
bon, silicon, and manganese on the resistance of steels.
Carbon was found to increase the resistance of 7
microhms for 1 per cent, silicon 14 microhms for 1
per cent, and manganese 3 microhms for 1 per cent.
' . Benedicks' investigated the effect of impurities
on the resistance of iron and steel. He used commer-
cial iron and steel varying from 0.08 to 1.7 per cent.
C. and varying in amounts of silicon, manganese,
phosphorus, and sulfur. Calculating the percentages
of silicon and manganese to equivalent carbon, he
proposed the following formula
p = 7.6 + 26.8 1 (',
in which p is the resistance of the steel, 7.6 the re-
sistance of pure iron, and 2C the sum of the per-
centages, in terms of carbon, of the impurities in the
iron.
\1. I'ortevin4 determined the resistance of ter-
nary steels, including alloys with nickel, chromium,
tungsten, aluminum, molybdenum, vanadium, titanium,
boron and thallium. He discussed also the influence
of titanium on the arrest points.
A. P. Schleicher and W. Guertler5 studied the re-
sistance of alloys containing 35.25, 30.6 and 25.2
per cent nickel. It was observed that there was a
pronounced discontinuity in the resistance at about
420° C. for the steel containing 35.25 per cent nickel,
and at 700° C. for the one containing 30.6 per cent
nickel. The alloy containing 25.2 per cent nickel
gave, in the original condition, abnormally low values,
but the resistance increased with each heating until
it became stabilized with a discontinuity at 900° C.
A. I'ortevin6 heated steel bars in a salt bath at
750 and 9000 C. for varying lengths of time and after
quenching, measured the increase in resistance.
K. Honda7 investigated the influence of high tem-
peratures on the electrical resistance and magnetic
properties of iron, steel, and nickel. He concluded
that the magnetic transformation was not an allo-
tropic change, but a gradual change of the property
of a phase, due to a change in temperature.
G. K. Burgess and I. N. Kellburg8 measured the
electrical resistance of pure iron from o to 900 ° C.
The resistance increased with a gradually rising rate
ml Steel," /.<j Lumitre Ellc-
1 "The Electrical Resi !
triquc, 46 (1893), 93.
■"The Electric Resistanct "t Steel
agemeni [><■!!* L'Industric Nationale, 3 p '43
"Electric Resistance of Ir,>n and Steel
(1903).
'"Electric Resistance ol Steel," Rami d, r
1«>4.
i lectric Resistance of Iron-Nickel Alloys," Z. Elt
(1914). 273.
'"Influence of Ili^h remperatures on Magnetic
rend.. 158 (19141. 51.
'"Influence of High Temperatures on Magnet
11 (1914), 183
s "Electric Resistance of Iron .it Varying Temperatures," /. Wash
i . 4 (1914), 436.
Bulletin </'■ l<i >-.;/(. ,/7-n. 'iti
. 40. [51,
Properties
Properties," RntU
to .A. There was an inflection at A2 and an abrupt
fall in resistance at 894 ° C. The reverse change took
place at approximately the same temperature. The
I was 25° C. The change at A3 was progressive
and thermoelectrically nonreversible. The change
at A2 was reversible.
P. Mahler1 studied the influence of carbon and
manganese on the resistance of steel. The specific
resistance increased 7 microhms for 1 per cent of
carbon, and 5 microhms for 1 per cent of manganese.
Mahler believes that occluded gases increase the
resistance, and points out that hydrogen is known
to do so.
Edward D. Campbell-'3 investigated the effect of
annealing on the resistance of quenched steels. He
measured the resistance of the quenched steels and
subjected them in turn to temperatures of 100,
200, 300° C etc. The annealing at 100° C. was
prolonged for 4S hrs. The time of annealing at the
other temperatures was from 1 to 2 hrs. He plotted
curves showing the resistance against the tempera-
ture of annealing.
OBJECT OF THE PRESENT INVESTIGATION
The object of the investigation here presented was
to determine the rate of softening of quenched steels,
under conditions in which the temperature of anneal-
ing is kept constant. Changes in the electrical re-
sistance were used as a measure of the changes in
hardness.
Fig. I — Apparatus for Quenching Coils
The work was carried out by first quenching the
steel and measuring the resistance. This was fol-
lowed by annealing the steel for a definite time at a
definite temperature, and again measuring the re-
sistance. This procedure was repeated at the same
temperature but with an increasing interval of time,
followed by another measurement of the resistance.
The total period of annealing for the different speci-
mens varied from 90 to 190 hrs. The results were
then plottetl as time against resistance.
EXPERIMENTAL
The steels were treated in the form of a wire coil.
The specimens were prepared by forging steel bars
1 "Electric Resistance of Steel," Rr.ut de MUaUurtit 12
"The Influence of Heat Treatment on the Thermoelectric Properties
and Specific Resistance of Carbon Steels." J. />.>* and Sled Inst.. |2], 94
(1916). EM
Bquiatomic Solutions of Iron Possess Equal Resistances?"
12 1917 >. 1.
July, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Si7
down to ' 1 in. round. The pieces of this size, about
4 in. long, were drawn down to wires varying from
0.014 to 0.019 in. in diameter (0.355 to 0.482
mm.). From 20 to 50 cm. of this wire were used as a
specimen. The specimens were heated and quenched
in a vacuum, being contained in a silica tube which
was heated in an electric combustion furnace. Tem-
peratures were measured with a platinum-platinum-
rhodium thermocouple.
The arrangement for heating and quenching is
shown in Fig. I. The specimen was placed in the
glass extension of the silica tube. The tube was then
placed in the tube furnace and kept there for 5 min.
At the end of this time it was evacuated, withdrawn
from the furnace, inverted, and replaced in the fur-
nace. After about 1 min. it was again withdrawn
and the specimen quenched. The object of this pro-
cedure was to bring the coil to the desired tempera-
ture as quickly as possible, in order to prevent oxida-
tion. It was necessary to guard carefully against
oxidation, since the coils were long and slender. It
will be shown later that the effect of oxidation was
small.
After measuring the resistance, the method of which
will be explained later, the coil was annealed at a definite
temperature. The temperatures chosen were 125,
150, 175 and 2500 C. For the first three tempera-
tures the specimens were annealed in a constant
temperature paraffin bath, which was heated on an
electric hot plate to a temperature which was a few
degrees below that desired. The temperature was then
further raised and adjusted by means of a resistance
coil in the bath. The current in the coil was regulated
through a thermostat regulator and a relay. The
temperature was constant to about one degree.
For the first 5 min. the specimen was immersed
directly in the paraffin. For longer annealing the
specimen was placed in a tube immersed in the paraffin.
The reason for putting the coil directly in the paraffin
was to allow a closer determination of the time of
annealing. The specimen would take up the tempera-
ture of the liquid much more quickly than that of
air, hence the time of annealing could be more ac-
curately measured in the paraffin than in air. For
longer annealing, a small difference in time would
make much less difference in the results, hence the
tub'.- was used. This was desirable whenever possi-
ble in order to prevent any chance of carbonization.
For annealing at 2500 C. a constant temperature
oven was used, in which the temperature varied about
5° C.
For measuring the resistance of the specimens, they
were immersed in a tube of alcohol, which was placed
in a thermostat regulated to 30° C. The maximum
variation of the temperature was 0.05° C.
The resistance was measured with a Kohlrausch
bridge used as shown in the diagram in Fig. II. The
unknown resistance X and a known resistance, R,
arc connected in series, and in parallel with them is
the slide wire of the bridge. The bridge is balanced
with each end of each resistance, thus making four
readings. If the readings for the known resistance
are a and b, and those for the unknown resistance c and d,
then
X _ d — c
R ~ b — a
This method was used in order to eliminate the effect
of contact resistance. The double-throw switch was
used in order to eliminate the effects of all thermo-
electromotive forces and generated electromotive
forces.
R Kno
Resistance
X Unknown
Resistance
3 Battery
<5 Switch
•3' Switch
G Galvanometer
H Bridge
Fig. II — Apparatus for Measuring Resistance
The resistance meastirements themselves were ac-
curate to one part in one thousand. However, the
impossibility of placing the contacts at exactly the
same point each time increased the error. This added
error depended on the length of the coil. For both
contacts it was not more than 0.5 mm. This would
give a possible error of 0.25 per cent for coil No. 5,
which was the shortest, and o. 1 per cent for the longer
coils. This makes a total probable error of from 0.2
to 0.35 per cent.
The analyses of the specimens and the dimensions
of the coils are given in the following tables:
Table I
C
-Analyses of Specimens-
Si
Mn
Per cent Per cent Per cent Per cent Per cent
0.05 0.006 0.021 0.055 0.025
0.09 0.059 0.013 0.044 0.019
. 0.18 0.025 0.090 0.068 0.092
0. 25 " 058 0. ID9 0.075 0.036
. 0.45 0.122 0.112 0.092 0.106
Dimensions
of Coils
Diameter Length
Mil
Mi:
II )55 514
0.368 500
ii is ' 486
ii4.ll 503
0.431 196
The results of the resistance measurements are
plotted in the following curves, which show the effect
oi the duration of annealing on the resistance of the
steels.
Si8
Till: JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. ;
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CONCLUSIONS
The total change in resistance increases with the
carbon content of the steel. The change is very rapid
at the beginning of the annealing and becomes slower
as the resistance decreases. However, there was no
indication in any case that the change was complete
at the end of the test.
Since the resistance of a steel changes with the hard-
ness, the curves are a fair indication of the varying
rates at which hardened steels are softened by an-
nealing at a constant temperature. The larger part
of the change is completed within a few minutes,
but the change is not entirely complete in 113 hrs.
Division of Metallurgy and Applied Chemistry
University of Kansas, Lawrence
VOLUMETRIC DETERMINATION OF FREE SULFUR IN
SOFT RUBBER COMPOUNDS
By H. s. Upton
Received October 5, 1917
The published and accepted methods of determin-
ing free sulfur in a rubber compound are more or less
tedious, and, where manufacturing operations are de-
pendent upon them, are the cause many times of
serious delays. These delays, the cost of materials
required, and the time consumed by the determining
process, make these methods expensive. It was with
this in mind that the following method was evolved
and results obtained both in conservation of time
iterials and also in accuracy lead us to believe
it may be of int< hers who are using the
<>ds.
M I I 11(11)
The proposi depends on t] I sulfur
when heated with an alcoholic potash solution is con-
verted into a mixture of potassium sulfide and potas-
sium thiosulfate, both of which may be titrated with
id iodine by usual methods as given in this
article, The free sulfur is determined in the acetone
extrad from tin- rubber compound. The resinous
extrad of certain commercial rubbers and the extract
of other compounding materials are acted Upon by
the alcoholic potash solution and by various standard
solutions used in analysis, thereby rendering neces-
sary the application of corrections. The amount of
correction or blank used in titrating is determined
by the nature and amount of the various ingredients
in the extract from the rubber compound. This
limits the use of the method with confidence to a sam-
ple of rubber, the composition of which is known to
the analyst. The proposed method can be used suc-
cessfully where a large number of tests are being run
on a compound made up to a certain formula, for
example, insulated wire compounds, boot and shoe
compounds, etc.
The equation generally given for the oxidation of
sulfur by a water solution of potassium hydroxide is:
4S + 6K0H = 3H20 + K2S203 + 2K2S
This varies with change of conditions. When using
an alcoholic potash solution instead of potash in
water more thiosulfate is formed than is indicated in
the equation and in some cases the conversion to this
product is complete. Using this principle, a method
has been worked out which is as follows:
PROCEDURE
Extract a 2-g. sample of rubber compound with
acetone into a 300 cc. Erlenmeyer flask until the free
sulfur has been removed. A similar compound,
which is known to be free of free sulfur, is tested at
the same time. This is used to determine the blanks
in the subsequent titrations.
Evaporate the acetone gently until little remains,
completing the drying in an oven at ioo° C. This
operation need not take longer than a half hour. The
sulfur in the dried extract is oxidized to thiosulfate
with 25 to 50 cc. of 5 per cent alcoholic
potash solution by boiling gently for one hour, using
a small glass funnel placed in the neck of the flask
for a condenser. Remove from heat. Wash and re-
move funnel from flask. Add 25 to 50 cc. of ammo-
nium zirj solution1 and just bring to boiling.
1 This solution is maile as follows- 10 g. of zinc oxide arc dissolved in
dilute hydrochloric a,i<i
liter
The solution is made alkalii
The solution is n
ith ammonia
nade up to ft
July, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Si9
This precipitates the sulfide as its zinc salt, leaving
the thiosulfate in solution.
Cool to room temperature in water. Acidify with
glacial acetic acid, adding 3 cc. in excess. Dilute to
200 cc. Titrate with N/25 iodine and starch. This
gives the sulfur present as thiosulfate. The precipi-
tate of zinc sulfide is not acted upon by the acetic
acid.
Add ammonium hydroxide to destroy the acidity
and a trace of iodine. Add hydrochloric acid to
acidity, having 5 cc. in excess. This dissolves the zinc
sulfide and liberates hydrogen sulfide. Titrate the
liberated sulfide with iodine and calculate to sulfur.
The titration in each case is carried to a permanent
blue, lasting half a minute. The end-point is generally
very distinct.
The determination of thiosulfate is called (a) titra-
tion, and that of the sulfide, (6) titration. The sum
of (a) and (b) titrations gives the total free sulfur.
The sulfur-free sample is tested at the same time as
the sample containing free sulfur and blanks for (a)
and (6) titrations found. In a straight rubber com-
pound blank (a) is about 1 cc. and blank (b) is o. 5 cc.
of iodine. Often all the sulfur in a pure rubber com-
I pound is converted completely to thiosulfate and (b)
] titration may be omitted. When this is the case
make the solution acid with hydrochloric, adding
5 cc. in excess, and carry out the determination as for
thiosulfate, instead of making acid with acetic.
It is important that the solution should be kept
cool during the determination. The different re-
agents should be measured as their quantity tends to
vary the results. Solutions should be kept to approxi-
mately the same volume, as this affects the iodine
blank. Two hundred cubic centimeters of solution
are a convenient volume to work with. In the process
of treating sulfur with alcoholic potash a white crys-
talline precipitate of potassium thiosulfate is some-
times found. This is almost insoluble in 95 per cent
alcohol but dissolves readily in the more dilute solu-
tion. Potassium sulfhydrate (KSH) may be formed
by the action of alcoholic potash, but it is oxidized to
potassium sulfide when the potash is present in excess.
! The strength of the standard iodine solution is de-
termined at least twice a week, as it becomes weaker
on standing, due to the volatilization of the iodine.
Weight Per cent of
of Acetone Sulfur Equivalent
Sample Sample Extract G. per Cc.
No. Grams Tested (a) (6)
1 2.0000 4.00 0.002598 0.000647
2 2.0000 4.00 0.002598 0.000647
3 2.0000 4.00 0.002598 0.000647
4 2.0000 4.00 0.002598 0.000647
5 2.0000 4.00 0.002598 0.000647
6 2.0000 4.00 0.002598 0.000647
7 2.0000 4.00 0.002598 0.000647
8 2.0000 4.00 0.002598 0.000647
9 2.0000 4.00 0.002598 0.000637
10 2.0000 25.00 0.002598 0.000647
11 2.0000 25.00 0.002598 0.000647
12 2.0000 28.50 0.002598 0.000647
13 2.0000 22.85 0.002598 0.000647
14 2.0000 22.85 0.002598 0.000647
15 2.0000 24.50 0.002598 0.000647
16 2.0000 25.00 0.002598 0.000647
17' 1.0000 8.00 0.002586 0.000646
18' 1.0000 8.00 0.002586 0.000646
19' I OOOli 8.00 0.002586 0 000646
... 1.0000 8.00 0.002586 0. 00064O
1 Smoked sheet cured with 5 per cent sulfur
I
FACTORS AND CALCULATIONS
It is very convenient to use factors in calculating
the results. The factor for (a) titration of sulfur is
0.50536 times the value of i cc. of standard iodine
solution. This is found from the following equation:
2K2S203 + 2I = 2KI + K2S406
Factor for (6) titration for sulfur is 0.12630 times
the value of 1 cc. of standard iodine solution and is
found from the following equation:
H2S + 2I = 2HI + S
An example of calculation where 0.0328 g. of sulfur
or 1 . 64 per cent on a 2-g. sample was known to be
present is as follows:
1 cc. Standard Iodine = 0.005139 g. of Iodine
(a) Titration: 1 cc. Standard Iodi:
g. of Sulfur
(6) Titration. 1 cc. Standard Iodi
g. of Sulfur
Blank (o) = 1.00 cc.
(a) Titration required 12 00 cc.
0.005139 X 0.50536 = 0.002597
0.005139 X 0. 12630 = 0.000649
lank (b) = 0.50 cc.
1.00 cc. (Blank) = 1 1 00
Iodii
11.00 cc. X 0.002597 -=- 2 (2 g. sample) = 0.0143 g. of Sulfur
(6) Titration required 5 . 80 cc. — 0. 50 cc. (Blank) = 5 . 30 cc. Iodine
5.30 cc. X 0.000649 H- 2 (2 g. sample) = 0.0017 g. of Sulfur
(a) Titration + (6) Titration = 0.0160 g. or 1.60 per cent of Sulfur
By this method 0.1 g. of sulfur may be titrated with good results.
There has not been time to experiment with larger amounts of sulfur.
Some actual determinations by this method are
given below. They are average results from a large
number of determinations of many different com-
pounds.
The most active types of various substances liable
to react with the reagents were tested to see if they
would interfere with the determination. Linseed oil,
while not used extensively in rubber compounding,
is chosen for this purpose, for it has high saponifica-
tion, iodine absorption and oxidation values. These
determinations were carried out according to the pro-
cedure for free sulfur in rubber compounds.
A much larger quantity of material in each case
was tested than would be present in an analysis.
Only starch seemed to have any effect which would
interfere with the determination. It is well known
that correct results are impossible in an iodine titra-
tion with much starch present. Starch would not be
liable to occur in a rubber mixture and at least would
not appear in the acetone extract.
(a) Titration
(a) Blank
(6) Titration
(6) Blank
Free S by
Standard
Standard
Standard
Standard
Free S by
Fuming Nitric
I Used
I Used
I Used
I Used
New Method Method
Cc.
Cc.
Cc.
Cc.
Per cent
Per cent
2.20
1.00
0.40
0.50
0.16
0.21
1.20
1.00
0.40
0.50
0.03
0.15
4.00
1.00
0.40
0.50
0.39
0.37
3.80
1.00
0.85
0.50
0.38
0.30
3.70
1.00
0.35
0.50
0.35
0.39
2.65
1.00
0.25
0.50
0.22
0.22
2.50
1.00
0.25
0.50
0.20
0.21
2.05
1.00
0.25
0.50
0.14
0. 16
1.55
1.00
0.25
0.50
0.07
0.12
12.95
1.00
6.70
0.50
1.75
1.65
12.45
1.00
4.75
0.50
1.61
1.58
12.00
1.00
5.80
0.50
1.60
1.64
14.40
1.00
2.50
0.50
1.81
2.08
15.70
1 .00
2.70
0.50
1.98
2.13
10. 10
1.00
2.40
0.50
1.29
1.40
9.30
1.00
4.70
0.50
1.21
1.33
187.0
1.00
0.90
0.50
4.62
4.53
17.70
1.00
2.80
0.50
4.48
4.48
18.70
1.00
0.60
0.50
4.60
4.62
I , 00
i on
0 SO
o 50
4 14
1 11
520
THE JOURNAL OF INDUSTRIAL AND ENGINEERING I HEMISTRY Vol. 10. Xo. 7
Material
Tbsted
Blank of Reagents.
Blank of R
Sulfur
Sulfur.
Sulfur
Sulfur
Potato Starch
Potato Starch
Potato Starch
Potato Starch
Potato Starch
Pol atO Starch
Po tl irch
Potato Starch
Rosin
Rosin
Linseed Oil
Linseed Oil
Linseed Oil
.cetone Extract <>f Smoked Sheet
Rubber to Determine Blank with
Reagents
M R, . . .
Ceresine.
Ceresine,
Weigh!
(0) Titration
(4) Titratior
of
: of Standard
Standard
Standard
Standard
Standard
by New
Free S
Sample
Extract I \ alue
! i
1 1 sed
Method
Present
1 G. per Cc.
Cc.
Cc.
Cc.
Gram
Gram
0.005121
0.30
None
0.005121
None
00
0.004798
(i 60
0.40
0.0200
n 0200
0 0 ''in
11 0
- 00
11 60
5.15
0.0200
0.0200
(1 1
-
11 60
11 411
0 021 1
0.0200
II 1
0.005141
60
11 4(1
0.1007
0.1000
11 004727
14.55
11 60
0.75
11 40
11 0326
'i 0200
11 5000
0.0(14727
13.65
0.40
0.5000
0.004727
11 60
1 7(1
0 40
0.004727
12.55
11 60
0.40
n.0200
0.5000
13 50
11 60
0.40
0.40
0.0200
11 ,iili(i
0.004727
14.25
0.40
11 40
0.0316
'i 0200
0.004727
14 20
11 60
0.40
0 11.
11 004727
13.40
0 40
0 40
0.0200
10
0.005121
X llll
11 60
S 60
0.40
0 0201
8.00
.1 60
0.40
0.0203
0 0200
0.00 1 1
8.70
0 10
. n 005121
8.00
4.40
0.40
0.0207
.1 0500
1 5121
8.50
11 .,11
■ 0
II 40
0.0219
0 02OO
1 0000
4 L!
(i 1
11 55
None
1 0000
4.01
0.004768
0 mi
0. SO
None
1 1"
3.90 0 004 < -
1.00
11 SO
None
None
1 0000
4 W
0.1 11 11 68
00
None
None
1 0000
3.51
0.005121
None
None
1 0000
3.81
11 OHM 21
0.80
1 . 0000
4 (in 0.005121
,, 0
., so
None
4.00 0.005121
II .11
(i 40
None
None
1 . 0000
11 004727
8.85
11 60
5.50
0 40
0.0221
0.0200
1 . 0000
0.004727
8 ',u
0.60
5.60
11 40
0.0222
II
0.004727
10.00
-■■
0.40
0.0230
1 . 0000
III llll
11 60
0.40
0
0.0200
1 . 0(100
0.004727
10.70
11 60
3.10
0.40
0.0249
0.0200
1.0000
0.004727
9.15
0.60
3.55
0.40
0.0210
0.0200
The above is a tabulation of results:
The advantages of this method are its accuracy,
ease of manipulation, rapidity, and cheapness.
When the dried acetone extract from a rubber com-
pound is obtained, eighteen samples may easily be
determined in 21/-: hrs. The operator need not
spend more than an hour's time in actual manipula-
tion. This method may be used to determine sulfur,
and mixtures of soluble sulfides and thiosulfates.
Atlantic Insulated Wire and Cable Company
Stamford, Connecticut
RAPID DETERMINATION OF CARBON IN STEEL BY THE
BARIUM CARBONATE TITRATION METHOD1
By J. R. Cain and L. C. Maxwell
Received May 3, 1918
INTRODUCTION
Bi • ause of the increased demands now made on the
testing and steel works laboratories which analyze
steel delivered on government contracts, and because
nl the reduced number of chemists available for such
work, it becomes desirable to increase the efficiency
of laboratories in all possible ways. Short-cuts or
simplifications which will reduce the time required
for determination by standard methods, or reliable
in w methods which require less time than those now
in use are of value in contributing towards ini
output of work. With this idea the following modifica-
tion nt the barium carbonate titration method originally
described by Cain- has been developed. The work
carried on recently a1 the Bureau of Standards
in connection with a military problem where speed was
considered important.
The barium carbonate method is much used, es-
pecially by testing laboratories which usually have to
analyze steels of unknown composition from many
sources. It has been recognized that this VD
as heretofore used is not as rapid as the soda lime
in i In nl. but it is also felt by many that it is less sub-
ject to disturbing influences and is in most respects
i Published by permission of the Directoi of the Bureau »>( Standards,
' Bureau of Standard I apa No 33
simpler than the latter method. It is believed that the
modifications herein recommended put the barium
carbonate titration method more nearly on the same
basis with the soda-lime method as to time requirement,
with but little loss in accuracy, and with added sim-
plicity in manipulation. The time required per de-
termination has been reduced 50 per cent and it is now
possible for a chemist during an 8-hr. day to make
50 determinations by the barium carbonate titration
method.
The procedure recommended in the cited paper was
briefly as follows:
The combustion of the steel was carried out by
admitting oxygen at a moderate rate to the combustion
tube. Xo details were given in that paper as to fur-
nace temperatures at the time the boat was inserted
in the furnace, nor as to whether the boat was allowed
to preheat before admitting oxygen. Actually, the
results given in the paper were obtained by placing the
cold boat in a furnace kept at 1000 to 10500 and ad-
mitting the oxygen immediately; the passage of the
oxygen at the moderate rate specified was continued
for 20 to 25 min. The oxides thus obtained were fre-
quently not well fused. If an incomplete combustion
was suspected, the oxides were crushed and reburned.
This method of burning corresponded to practice
ere at that time. The barium carbon-
ate was tillered under an atmosphere free from carbon
dioxide, using a special apparatus illustrated and de-
scribe.] in the cited publication. The filter consisted
oi a carbon tube fitted with a perforated porcelain
plate; on this was placed a bed of coarse quartz par-
ticles, and on this a layer of asbestos. When filtra-
tion was finished the porcelain plate and superimposed
layers of quartz and asbestos were transferred to a
wide-mouth llask, treated with excess of the standard
hloric acid, and the solution titrated
sodium hydroxide, using methyl orange as indicator.
Various precautions in manipulation and filti
were described. These precautions, the necessity for
Qg a filter of this type each time, and the slow-
July, 1 91 8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
ness of the combustion all contributed toward making
the barium carbonate method as described longer than
others in use. This was compensated by the high
degree of accuracy attainable and the insurance against
numerous sources of error, as detailed in the paper.
The present method saves time in the following ways:
1 — Admission of oxygen at a very rapid rate to the
burning sample with automatic provision against too
rapid passage at the exit end of the combustion tube.
(This would cause loss of carbon.) This rapid ad-
mission of oxygen, coupled with the use of a preheated
boat and the practice of allowing the sample to pre-
heat in the furnace a minute before admitting oxygen,
gives complete combustion of a 2-g. sample in 1 ' 2
to 2 min. If combustion is allowed to take place
gradually, instead of rapidly, as specified, the rapid
method herein described cannot be used. The criteria
of a successful combustion by this method are:
(a) Well-fused oxides in which no trace of the orig-
inal grains of steel is apparent.
lb) Much accelerated oxygen inflow during the
actual combustion of the sample.
(1 ) Vivid incandescence while the sample is burning,
visible if a quartz combustion tube is used.
Should these signs of a good combustion be lacking,
determinations should be rejected.
2 — Use of glass plungers to take up dead space in
the forward end of the combustion tube so as to de-
crease the amount of gas that has to be flushed out at
each determination.
3 — Rapid filtration as described in Section 6.
4 — The delivery of all the reagents from reservoirs
by air pressure.
The main prerequisite for the use of the modified
method is a laboratory atmosphere not contaminated
with excessive amounts of carbon dioxide, so that the
barium carbonate may be filtered in a simple apparatus
not requiring exclusion of the carbon dioxide contained
in the laboratory air. This requirement is met by
any modern laboratory with even fairly good ventila-
tion and without an excessive number of gas burners
operating at one time in a confined space. Practically
this point may be tested by comparing blanks run
with the filtering apparatus described in the original
paper1 and that herein recommended. If the differ-
ence in the blanks is such as would cause an error
exceeding 0.005 per cent carbon when a 2-g. sample
is used, ;'. c. 0.0001 g. carbon, either the longer method
must be used or steps taken to reduce the carbon di-
oxide content of the laboratory atmosphere.
I FURNACES AND TEMPERATURE
An electric furnace operating at not less than 1063 °
C. (the melting point of pure gold) is used.- Such a
furnace may be obtained upon specification or as a
standard article from manufacturers or may be con-
structed by the operator. The furnace should be
equipped with a rheostat so designed with respect
1 Lix. cil.
1 Lower temperatures may be used with very fine chips, the tempera-
ture recommended will burn successfully chips that will just pass a 10-mesh
to the line voltage that initially the furnace gives the
proper temperature with nearly all the rheostat re-
sistance inserted. As the furnace is used its winding
deteriorates and increases in resistance, and this should
be compensated by removing resistance on the rheostat
so as to maintain the furnace temperature as specified.
If the temperature is too low when all the rheostat
resistance is removed, the furnace must be supplied
with a new winding. Temperatures are checked by
the melting point of pure gold. A piece of this metal
is flattened out, placed on a clean porcelain or alundum
boat and left in the furnace (previously brought to
full heat) for 10 min. If the gold is not then melted
the temperature is too low.1 The same piece of gold
may be used repeatedly provided care is taken always
to place it on a clean surface of either alundum or porce-
lain.
2 BOATS AND LINING MATERIALS
Boats may be of alundum, porcelain, platinum or
nickel. Nickel boats may be made very cheaply by
cutting a sheet of nickel of proper size at the corners
and bending these up. Such boats should be ignited
in the furnace in a current of oxygen until free from
carbon. To protect the combustion tube from the
effects of spattering oxides it is provided with a sleeve
of nickel sheet (also ignited until free from carbon).
Boats are lined with alundum sand, free from materials
causing a blank. The special grade supplied by the
Norton Company is quite satisfactory.
3 COMBUSTION TUBES AND CATALYZER
Combustion tubes may be standard forms of porce-
lain or well-glazed quartz, or in fact, any material
which has been carefully tested for freedom from
porosity. To facilitate fitting of stoppers the cross-
section at the end should be circular. In the forward
end of the tube a roll of copper gauze 3 in. long and
of a diameter sufficient to fill the tube is inserted so
that it is heated by thermal conduction from the heated
zone of the furnace to a temperature of 200 to 300° C.
The copper should not, however, be placed so far in
the furnace that there is danger of its melting. The
copper is then oxidized by bringing the furnace to a
proper temperature while passing oxygen. This copper
oxide serves to oxidize any carbon monoxide that
might be formed, also any sulfur dioxide, which is
oxidized and fixed as copper sulfate. Should too great
an accumulation of copper sulfate take place the cata-
lyzer should be renewed.
4 RATE OF FLOW OF OXYGEN
The rate at which oxygen is admitted to the for-
ward end of the tube should be not less than 10 to 15 1.
per min. At the exit end of the tube the rate should
not exceed 225 cc. per min. This latter rate of flow
is attained most simply by constricting a glass capil-
lary tube inserted in the forward stopper of the com-
bustion tube so that the desired rate of outflow is
obtained with the specified rate of inflow. A plug of
glass wool precedes the capillary. The rate of out-
flow is especially important, for if this is much ex-
1 The melting point of pure silver (960.5° C). determined la the Bame
way, is a convenient check on the lower temperature limit.
5"
THE JOl RNAL OF INDUSTRIAL AND ENGINEERING ( HEMISTRY Vol. 10. Xo. 7
■', carbon dioxide will be carried past the absorp-
tion tube containing I n hydroxide. The
dead space in the combustion tube in front of the copper
oxide catalyzer is taken up with a glass tube closed
at both ends. This 1 amount of gas to
be flushed out of the tube a1 mbustion, and
materially shortens the time requin termina-
t ion.
5- MEYER ABSORPTION TUBES AND BARIUM HYDROXIDE
SOLI I 1
The form of Meyer tube shown in the cited
lias many advantages and may be obtained from dealers
on specification. It should be filled with sufficient
barium hydroxide solution (25 g. Ba(OH)j.2HjO
per liter) so that when gas is passing for a determina-
tion the liquid fills all the small bulbs and one-half
the large bulb at the exit end. The barium hydroxide
solution is held in a 10-I. bottle and is delivered by
pressure of air free from carbon dioxide.
6 FILTERING AND WASHING
A Buchner funnel fitted to a suction flask and sup-
plied with two superimposed, open-grain, 7-cm. filter
papers is used for nitrations. Much time is saved by
not having to fold and fit the papers. The large sur-
xposed insures rapid filtration. The Meyer
tube is washed three times, using care to reach all
points. The precipitate on the filter is then washed
four times, washing the top of the funnel carefully.
The wash water is free from carbon dioxide and is
delivered from a large glass reservoir by air pressure.
7 STANDARD ACID AND ALKALI
Tenth-normal hydrochloric acid is used. This may
be conveniently standardized against weighed portions
of chemically pure sodium carbonate which has been
fused in a platinum crucible and cooled in a current
of pure, dry carbon dioxide. The carbon dioxide is
conveniently obtained by heating acid sodium car-
bonate in a hard glass test tube and passing the liber-
ated gas through a calcium chloride tower. The alkali
is standardized sodium hydroxide solution adjusted
to be equivalent to the acid. Methyl orange is used
as iin indicator. Both acid and alkali are delivered
from the respective stock bottles to the burettes by
air pressure.
8 — PROCEDI Kl
The furnace being at the proper temperature and
the filled Meyer tube connected, 2 g. of steel are wi
and transferred to the boat filled with alundum sand.
This should have been placed in the hot furnace
previous to weighing the sample and then removed
so that at the time of placing the sample on it its
temperature is just below a visible red. (This will
not cause loss of carbon unless the particles of the
sample are extremely small less than 60 mesh.)
The boat is then immediately placed in the furnace
and allowed to heat for one minute with no 0
passing. During this time a second sample is being
I (the balance should be placed in the same
room with the furnace for convenience). Oxygen
is now admitted at the I'd in Section 4.
and at the end of 5 min.. if the combustion li
successful (see Introduction), the Meyer tube may
be disconnected and the boat removed from the fur-
nace to cool sufficiently for introducing the second
sample. The filtration and washing of the barium
carbonate is then carried out as described. By this
time the boat is ready for the second sample, which
has already been weighed out. The combustion of
this sample is then started, using another Meyer
tube. The absorption tube used for the previous
on is now washed out by adding to it
from the burette the necessary amount of standard
acid (this being usually about 5 cc. more than is ac-
tually needed to dissolve the carbonate). The acid
is transferred from the Meyer tube to a wide-mouth
flask, as is also the filter paper carrying the precipitate.
The Meyer tube, after washing twice with water, is
filled with barium hydroxide solution for the next
determination. The flask containing the precipitate
is placed on the hot plate until the carbonate is dis-
solved.1 Titrations are conveniently made when
several flasks are ready. During filtration, washing,
etc., of the first determination, the combustion of the
second proceeds, but there is still time before its com-
pletion for the operator to adjust the acid burette
for the second determination, to fit papers to the
Buchner funnel, and to weigh out the third sample.
Table I — Results Obtained by Modified Barit-m Carbonate Titra-
tion Method on Bureau of Standards Analyzed Standard
Samples
Certificate
Value Carbon Found bv Mean Varia-
(by Direct Method Herein tion from
Sample Combustion) Described Number of Certificate
No. Per cent Per cent Determinations Value
35 1.03 1.016 to 1.027 3 — 0 01
23 (i 80S 0.81 3 +0. 005(a)
106 0.373 0.380 2 +0. 007(a)
21o 0.617 0.605to0.620 12 — 0.005
(a) The corresponding differences in the determinations of carbon in
Sample 23 given in the cited paper were: 0.000 per cent. 0.000 per cent.
0.000 per cent, and — 0.005 per cent; in 106 they were: 0.001 per cent and
— 0.001 per cent.
Bureau of Standards
Washington. D. C.
THE PREPARATION AND TESTING OF PURE ARSENIOTJS
OXIDE2
By Robert M. Chapin
Received March 12, 1918
INTRODUCTION
A supply of assuredly pure arsenious oxide is an
important matter to the modern analytical chemist.
Analytical methods that involve titration with stand-
ard iodine, by virtue of their accuracy and convenience,
are constantly finding new applications in addition
to the already considerable list, and for standardizing
such iodine solutions pure arsenious oxide is generally
useful and frequently used. Moreover, employment
of the substance as an alkalimetric standard has been
advocated by Menzies and McCarthy.3
From textbooks and various papers dealing
with the applications mentioned above, it appears
that pure arsenious oxide is very easily obtained.
Typical are the statements of Menzies and McCarthy*
\\.m<1 long continued healing, which apparently causes some action
on the filter pupcr involving a slight error in the determination.
5 Published by permission of the Secretary of Agriculture.
" J. Am. Ch/m. StK . 37 (1915), 2021.
July, 191S
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
S23
that it "may be purchased commercially at a low price
already in a high state of purity," and that "it may
readily be purified further both by recrystallization,
if necessary, and by sublimation." The experience
of the writer points to the contrary. Commercial
specimens, even of "guaranteed analysis," may be
far from pure. Sublimation alone is not a dependable
method of purification, and, unless proper conditions
prevail, preliminary recrystallization may not be an
adequate supplementary measure. In fact it is en-
tirely possible, after recrystallization and sublimation,
to end with a "purified" arsenious oxide more impure
than the original material. Finally, extant methods
for testing are inadequate for detecting the presence
of important amounts of certain impurities. Par-
ticularly is this true of antimonous oxide, certainly
an important impurity and one not unlikely to be
present, but for the detection of which, aside from the
dubious test of the Pharmacopoeia, there seems to
be no practical method extant.
As impurities commonly present in commercial
white arsenic, Scott1 gives "Si02, Sb203, Fe203, NiO,
CoO, CaO, S03, Cu, Pb, and Zn." The United
States Pharmacopoeia IX prescribes tests for As2S3,
Sb, Sn, Cd. Thorpe2 mentions the presence of bis-
muth, sulfur and carbonaceous matter from the fuel.
TESTS FOR PURITY
1. insoluble — To i g. of the powdered sample in
a wet3 test tube add 10 cc. of a mixture of 1 vol. con-
centrated ammonia (sp. gr. 0.90) with 2 vols, water.
Heat with shaking to very gentle boiling. The solu-
tion should be perfectly clear and colorless with no
trace of insoluble residue.
2. heavy metals — To the solution obtained under
(1) add 10 cc. clear and fresh saturated hydrogen sul-
fide water, mix, and heat just to boiling. No precipi-
tate, turbidity, or color other than a faint yellow should
appear.
3. antimonous oxide — If necessary, filter the hot
solution obtained under (2) into another test tube,
otherwise cool at once in water and finally place in
ice water for 15 min. No turbidity should appear
(less than 0.15 per cent Sb203).
4. sulfur, sulfides — Dissolve in a test tube, with
heat, 1 g. of the sample in 10 cc. normal caustic soda
solution, add 1 drop of lead acetate solution, and mix.
No coloration should appear (less than 0.005 Per cent
sulfur).
5. nonvolatile — Under a hood cautiously heat 1
g. of the sample in a weighed crucible, raising the heat
at the end to barely perceptible redness. The material
during sublimation should show no darkening (car-
bonaceous matter) and should leave a nonvolatile
residue of less than 0.05 per cent.
Tests 1, 4 and 5 are essentially those of Krauch'
merely modified in details as experience indicated
1 "Standard Methods of Chemical Analysis," Wilfred W. Scott. D.
Van Nostrand Co., 19 I 7.
» Dictionary of Applied Chemistry, 1 (1912).
1 To prevent the substance caking on the glass.
' "Chemical Reagents; Their Purity and Tests," E. Merck; Translation
by Schenck. D. Van Nostrand Co.. 1907.
desirable. Tests 2 and 3, however, are new. Test 2
hardly needs further remark. Test 3 depends on the
fact that antimonous sulfide is somewhat soluble in
hot ammonia,1 but separates on cooling, excess of
arsenious oxide precluding the presence of ammonium
sulfide.
The strength of the ammonia may vary consider-
ably without, injury, but the delicacy of the test can-
not be increased by using relatively more substance.
In fact it is sensibly diminished thereby, probably
as the effect of mass action exerted by the arsenious
oxide. Merely cooling to about 20 ° C. will eventually
bring out even small amounts of antimony. At this
temperature a little over 0.20 per cent is soon plain,
but smaller amounts require so much time that the
use of ice water is desirable. The first indication of a
positive test is an opalescence much like decomposing
hydrogen sulfide water. This slowly increases to a
yellow turbidity which would tempt the inexperienced
to assert positively that the test was a failure and
that arsenious sulfide was coming out. Soon, however,
examination by transmitted light will reveal a dis-
tinct orange tint, and coagulation to characteristic
red flocks will ensue after a sufficient time. Pure
arsenious oxide with pure reagents will show no trace
of turbidity, even on long standing.
The ultimate sensibility of the test is distinctly
greater than above indicated, for by letting the tube
stand in ice water for 2 hrs. it apparently becomes
possible to detect down to 0.10 per cent Sb203. But
in this connection it must be remembered that, iodi-
metrically at any rate, small quantities of antimonous
oxide will act exactly like arsenious oxide except for
the difference in molecular weights. .Therefore, the
presence of 0.15 per cent of antimonous oxide is equiva-
lent to less than 0.05 per cent of inert matter, a limit
sufficient for all purposes except those of such a high
degree of accuracy that special purification of com-
mercial material would be imperative in any event.
For experiments on the antimony test, crystallized
arsenious oxide was prepared from a mother liquor
assuredly freed from antimonous oxide by the removal
of an extra and liberal crop of crystals after the regular
test on the preceding crop was negative as later
described. Antimonous oxide was introduced in the
form of a 0.23 per cent solution of tartar emetic, equiva-
lent to a 0.1 per cent solution of the oxide, the desired
amount being added to the test tube already contain-
ing both the arsenious oxide and the ammonia, but
before boiling.
The sulfur test was checked by means of pure ar-
senious sulfide, dissolved in freshly boiled normal
caustic soda.
The matter of tests for pharmaceutical purity being
outside the writer's present field of work will be only
briefly discussed. Careful sublimation of one gram
in a hard glass test tube appears to yield considerable
information regarding nonvolatile residue, arsenious
sulfide, metallic arsenic, and organii matter. But a
test for antimony is certainly desirable. The test in
> "Qualitative Chemical Analysis," Prescott & Johnson, 7th Edition,
1916.
524
I III: JOl RNAL 01 INDUSTRIAL AND ENGINEERING CHEMISTRY Vol.
10. No.
the form specified for determining chemical purity is
probably too delicate, though it may be made less so
by changes of concentration oi bj i ooling at a higher
Apparently the best way of reducing
i to employ i , solution of definite
strength in place of ammonia as a solvent. For ex-
ample, using 10 cc. of normal caustic soda on a one-
gram sample, and cooling in I une per cent
of Sb;C>3 in the sample quickly gives a heavy precipi-
tate, while with 0.6 per cent SbjOa the test remains
for a period much longer than 15 min.
Caustic soda might al 0 erve for the detection of in-
soluble matter in pharmaceutical testing.
The present assay method of the Pharmacopoeia
must necessarily be inaccurate if antimonous oxide is
present, and the only recourse seems to be distillation
with hydrochloric acid.1
PREPARATION OP PUR] IRSENI0T7S "XIDE
The production of pure arsenious oxide on a manu-
facturing scale is not here considered: merely its
preparation in the laboratory. Under such conditions
sublimation cannot be depended on to separate vola-
tile impurities. Among these must be included an-
timonous oxide, as may be easily demonstrated by the
specific test for that substance now available. It
evidently possesses a sufficient vapor tension at tem-
peratures ordinarily employed, even in careful work.
for subliming arsenious oxide to produce appreciable
contamination. Since volatile impurities — including
carbonaceous matter which will produce elementary
arsenic — are apparently quite as important as the
nonvolatile, measures to eliminate them ought to
precede final sublimation if a reasonably pure product
is to be assured.
The classic step preliminary to sublimation is crys-
tallization. The writer has been unable to discover
any more practical means for attaining the desired
end. But the process of crystallization to be employed
is usually very sketchily outlined. Either water or
hydrochloric acid of varying strength is specified as
olvenl and few details are given. It seems to
caped notice that arsenious oxide during crys-
tallization strongly adsorbs many impurities — par-
ticularly antimonous oxide — present with it in solu-
tion. Consequently a "recrystallized" product may
be more impure than the original material. Frac-
tional crystallization is the obvious recourse, and
properly carried out is very effective and not especially
tedious. The absence of antimonous oxide is a rational
and convenient index of the success of the operation.
As solvents for arsenious oxide, ammoniacal solu-
tions and strong hydrochloric acid solutions are
temptingly effective, bu1 unfortunately both are also
effective solvents for accompanying impurities. Water
usually dissolves far less of the impurities, so that
its disadvantages as a solvenl are outweighed by the
simplicity of the ensuing fractional crystallization.
The final crystals, however, are best deposited from
a slightly acid solution.
1 Most recently studied by Koark and McDonnell, This Jovknal. 8
1916), 327.
^ To 2 liters of boiling distilled1 water in a 3-liter
"boiling flask" are slowly added 1 50 g. powdered, white
arsenic made into a cream with a little water. The
mixture is boiled briskly for about i1 , hrs. or until
the volume is reduced to about 1600 cc, then is re-
moved from the heat and allowed to settle for a few
minutes. If the liquid tends to settle fairly clear it
may be filtered at once through a fluted paper, but if
it remains pronouncedly milky it will filter badly and
must be clarified. To this end it is decanted from the
■it into another flask, brought to boiling, treated
with milk of lime prepared from 2 g.! pure CaO,
boiled 10 min.. then filtered.
The filtrate is bo in a stout beaker until
4 or 5 g. of solid have separated. Bumping will not
ious if the flame is lowered sufficiently. It is
then decanted, boiling-hot, through a rapid fluted
paper into another stout beaker kept hot during filtra-
tion, either on the steam bath or over a flame, and the
filtrate kept close to the boiling point while the test
for antimony is made on the deposited arsenious oxide
in the first beaker. For the purpose in view a com-
paratively coarse and rapid test is adequate. A
quantity of the moist substance which is judged to be
equivalent to about one gram dry is brought into a
test tube and the test made as usual except that cooling
for 5 min. under running tap water is sufficient.
Unless antimony is very plainly present in the deposit,
the mother liquor is cert ainly antimony-free. Some-
times no antimony will be found even when much was
present in the original substance for it appears to be
practically wholly adsorbed by solid arsenious oxide
if a sufficient quantity of the latter remains undissolved.
Conversely, if solid arsenious oxide is absent, anti-
monous oxide may pass into the filtrate in large amount.
evidently being much more soluble in a solution of
arsenious oxide than in pure water.
If the test for antimony is positive it will be neces-
sary to take off successive crops of crystals in the same
way until a negative test finally results. Fractional
crystallization by cooling is not advised for the reason
that at temperatures below S50 the formation of
crystalline from amorphous arsenious oxide progresses
with such rapidity that the process is likely to get
out of control.
The antimony-free mother liquor is treated with
approximately either one or one and one-half per cent
of its volume of concentrated hydrochloric acid, de-
pending on whether lime was employed for clarifica-
tion, and boiled down in a beaker to evident satura-
tion. After a final filtration, it is cooled rapidly with
frequent stirring to prevent the formation of crusts,
then let stand over night. After being well stirred up.
the crystals are filtered with suction and washed chlo-
ride-free. The yield naturally varies much, but will
commonly be around 7; g. The crystals will probably
be very nearly pure, but the writer has never been
able to secure any which did not show slight darkening
during sublimation.
For sublimation the apparatus of Menzies and
ipurilies.
1 Tap w.iii-r may introdu
Thifl Quantity hus so fa
e undesirable organic i
proved sufficient.
July, iqiS THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
525
McCarthy1 is convenient but of small capacity. On
a larger scale excellent results may be obtained with
a stout-walled 250 cc. Erlenmeyer flask of rather hard
glass, charged with 75 g. arsenious oxide evenly spread
over the bottom. The flask is set in a fiat sand bath,
and the sand brought about one-half inch above the
level of the material within. The mouth of the flask
is covered with a porcelain crucible cover, and the
bath is heated under a hood with a sufficiently powerful
burner of the ring or stove type. The sublimation
may require 7 hrs. and should not be intermittent
for the flask, once cooled, is likely to crack when re-
heated. It is finished when a line of clear glass ap-
pears all around the flask above the sand. When
completely cool, the flask is removed from the bath
and with cautious handling the bottom is cut off
with a hot point just below the line of the sublimate.
The latter may then be easily removed with a knife
blade. It is best to reject the portion in the neck of
the flask, for volatile impurities will tend to concen-
trate there. The writer prefers to reject also the
glassy ring of sublimate just above the sand level.
With proper management the yield is excellent, very
little being lost by volatilization.
CONCLUSION
It must be admitted that arsenious oxide lacks some
of the qualities desirable in a standard substance for
volumetric analysis. Nevertheless it is capable of
affording extremely accurate results and for the
purpose of directly standardizing iodine solutions
there seems to be no other substance2 which can fully
take its place. Since it must be used, the chemist
must possess practical and reliable methods for de-
termining whether commercial samples are sufficiently
pure for ordinary analytical work, while in case of
deficiency, or when the material must be of the highest
purity, dependable methods of preparation must
be available. It is believed that these needs are met
by the methods of preparation and testing here pre-
sented. Especially are methods given for detecting
and eliminating an impurity to which far too little
attention has been given in the past, viz., antimonous
oxide.
Biochemic Division, Bureau of Animal Industry
Department op Agriculture, Washington, D. C.
THE BISULFATE METHOD OF DETERMINING RADIUM
By Howard H. Barker
Received December 5, 1917
The quantitative determination of the small amounts
of radium in radioactive ores and various products
obtained in their treatment for the recovery of radium
is generally conducted by the emanation method. It
is based upon the fact that the gaseous disintegration
product of radium- the emanation — can be completely
separated from radioactive materials and that the
equilibrium quantity is proportional to the radium
content. Very small quantities of radium emanation
' /-or. i it.
'Antimony potassium tartrate, advocated by Mctzl (Z. anorg. Chcm..
48 1906), LS6), is well known to be efflorescent whin crystallized. The
present writer has been unable to dry it to strictly constant weight in
agreement with the theoreticat composition of the anhydrous
are capable of exact measurement by electrical methods,
for which carefully standardized electroscopes have
come into general use.
The care and accuracy with which the emanation
is separated from the specimen under examination are
very essential in quantitative work and demand skil-
ful manipulation, especially in the case of solids. Since
heat alone rarely affects a complete separation of the
emanation from the radioactive solids, the recognized
methods of determining radium involve chemical
treatment that will result in a solution or in decomposi-
tion of the material by fusion. Our experiments test
the applicability of fusion with bisulfate, for the separa-
tion of radium emanation, and afford a comparison of
this method with other methods recognized as more
or less standard.
Our work deals with substances which are not sus-
ceptible of direct solution in water or acids. The
emanation is separated by direct fusion with sodium or
potassium bisulfate or mixtures of the two. Since
solids generally emit, at ordinary temperatures, variable
proportions of the emanation continually produced by
the radium present, the customary procedure is to
first expel the emanation, that is, reduce it to zero,
and then seal up the sample, allow it to stand for a
definite time — a day or longer — and finally separate
the accumulated emanation by fusing again. The
equilibrium amount is then conveniently obtained by
reference to a table of growth of radium emanation.1
Plum2 made use of potassium bisulfate for radium
determination in his study of methods of separating
the radioactive constituents from carnotite ores.
Schlundt3 employed potassium bisulfate in a few of his
experiments on the quantitative determination of
radium mainly by fusion with mixed alkali carbonates.
The experiments that follow I hope will serve to estab-
lish the reliability of the bisulfate method and also its
range of applicability.
PLAN OF EXPERIMENTS
Representative carnotite ores and the radium-bear-
ing products obtained therefrom were selected for the
determinations of radium which were conducted by at
least two other methods for comparison with the bi-
sulfate method. The samples include (i) two carno-
tite-bearing sandstones from different localities and
differing considerably in composition and radium con-
tent, (2) a siliceous concentrate obtained from an ore
by chemical treatment in which the radium has been
concentrated about fifteen-fold, (3) a sample of first
sulfate containing about 600 parts of radium per billion
of total weight, one-fourth of which is barium sulfate,
(4) one sample of tailings, the sandy residue lefl after
the extraction of radium from the ore, (5) a by-product
very rich in gypsum, but containing also vanadium,
iron and uranium compounds.
The radium was determined in case of these samples
by at leaSl three methods.
> Eolowrat, /. Radium, 6. 195; also Curie, "TraMde Etad
I.P 419;CA«ffl KaUnder, 1(1914), 361; Rutherford, "Ra • •",., Sub t.mces
.,11.1 1 heii Radiations," 1913. 66S
1 lm.1 ft<in Sd . 37 1 1915), 1811.
Im Eieclrochem Sot . 26 (1V14), 163.
526
THE JOURNAL OF INDUSTRIAL AND ENGINEERING I EEMISTRY Vol.
No.
METHODS of SEPARATING THE EMANATION
i — Preparation of a refined radium-barium sulfate
by fusing a weighed sample, to which a small quantity
of barium compound has been added, with 3 to 5 times
its weight of a mixture of sodium and potassium car-
After leaching the melt with water, the in-
soluble carbonates are dissolved in dilute hydrochloric-
acid and pure radium-barium sulfate is precipitated
by the addition of a few drops of sulfuric acid. The
11 1 Typb op Apparatus for Boiunc On ICmanation from
Mixed Cardonatb Fusion
refined sulfate thus obtained is fused in a platinum
boat with a mixture of sodium and potassium carbonates
and is then sealed and stored for a certain period after
which the accumulated emanation is again separated,
collected and transferred to a standardized electro-
scope.1
2 — Direct separation of the emanation from the melt
is obtained by fusion of the sample in a platinum
crucible with mixed carbonates of sodium and potas-
1 Further details are given by I.ind. Tins Journal. 7 (1915). 1024,
•nd in I' S. Bureau of Mines. Bull. 104. 94.
sium. The melt is poured into a clean iron mortar.
The crucible may be rinsed out by fusing a little more
of the carbonates in it. The melt is powdered and
sealed up in a thin-walled glass bulb, B, shown in Fig. I.
After standing for a day or longer the emanation that
has accumulated during the period of storage is separated
by dissolving the carbonate in nitric or hydrochloric
acid. The gas burette E of the apparatus used for
this operation (Fig. I) is filled with a boiling hot solu-
tion of caustic soda through the levelling reservoir G
by closing cock D and having F open. Then, after
closing F, the levelling bulb G is lowered to a position
below the outlet tube D in order that subsequent
boiling will be conducted under slightly diminished
pressure. This precaution also enables one to detect
small air leaks in the apparatus. The bulb B contain-
ing the powdered carbonate is so adjusted in the 3-hole
rubber stopper of the wide-mouth flask A, the boiler,
that it is cracked by forcing down the stopper. The
cock D is then opened and moderately strong acid is
admitted gradually from the drop funnel C . When the
sample is siliceous and the carbonate fusion exceeds
5 g., the capacity of the boiler should be at least 250 cc,
and it is sometimes advantageous to have a little water
in it to distribute the carbonate when the bulb is broken
and in this way prevent the formation of a coating of
silicic acid over the dry powder when acid is admitted.
If the volume of air remaining in the boiler still exceeds
the capacity of the burette, the air may be partly dis-
placed by carbon dioxide before connecting up with the
burette. As the decomposition of the carbonate pro-
ceeds the solution is heated and finally boiled until the
liquid in the gas burette is forced down by water vapor
to the level of D. The gas is then transferred quanti-
tatively to an air-tight electroscope.
3 — The bisulfate method consists in making a fusion
of the material whose radium content is to be deter-
mined with either sodium or potassium bisulfate alone,
or better, a mixture of the two in a hard glass pyrex
tube of suitable dimensions. Hard glass pyrex tubes
25 cm. by 2.5 cm. were used in most of the determina-
tions. The material and the bisulfate are thoroughly
mixed before introducing into the tube, after which
they are fused and boiling continued long enough to
expel the last traces of emanation. The sides of the
tube are washed down by introducing a little fresh
bisulfate into the tube, allowing it to fuse and run down
into the melt. The test tube is sealed with a stopper
carrying two outlet tubes, one extending to within an
inch or two of the melt, and the other just reaching
through the stopper. After the emanation has been
allowed to accumulate for a given definite period, the
tube is connected up with the evacuated ionization
chamber of an electroscope as shown in Fig. II. The
micro drying bulb next to the ionization chamber con-
tains concentrated sulfuric acid, whose function is to
remove moisture from the air and emanation before
entering the electroscope. The other drying bulb con-
nected to the test tube on the ionization chamber s
of the apparatus contains a fairly strong solution of
caustic soda to remove any traces of sulfuric acid dis-
tilled over in the operation. The drying bulb hitched
July, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
527
to the other side of the test tube contains concentrated
sulfuric acid or water, and is there primarily for noting
the inflow of air into the system. It also serves for
detecting any leaks in the line of connection. All
rubber connections are wired, and the tips of the glass
tubes are not broken until all connections have been
made. Before breaking the capillary tips, the inter-
mediate system is placed under a slight vacuum. The
tips are then broken and by adjusting the stopcocks
of the evacuated ionization chamber the flow of air
through the chain is regulated. Heat is now gently
applied until the mass is molten, after which it is boiled
for about 5 min. Sometimes it is a little difficult
to get good boiling at this stage, but I find where an
equal mixture of the fused bisulfate and crystals is
used, that this difficulty seldom appears. The emana-
tion is swept into the chamber by a slow, steady current
of air which is maintained during heating until atmos-
pheric pressure is nearly attained in the chamber.
Readings of the rate of discharge are made 3 hrs.
after the introduction of the gas, the same as in the
other methods.
RESULTS AND DISCUSSION
The results obtained are summarized in the following
table. The values represent duplicate determinations
for the most part, but some of them are triplicate.
The values in the table represent grams of radium per
gram of material X io~9.
Material
Carnotite No. 1 .
CarnotiteNo. 2.
Concentrate. . ,
Tailing's.
First Sulfate
By-products. . . .
Wt. of
Sample
1 .00
1 . 00
0.50
! 00
0.05
2.00
Table I
Refined
Sulfate
5.15
10.60
29.90
0.90
676.00
1.26
Mixed
Carbonate Bisulfate
5.18 5.22
10.00 10.40
30.00 29.40
0.94 1.00
680.00 678.00
1.24 1.27
The good agreement in the values shows that from
the standpoint of accuracy in radium determination,
no one method has any advantage for the classes of
materials examined. The bisulfate method, however,
presents some advantages which deserve recognition.
I — It has been established that the bisulfate method
may be used in liberating the emanation from samples
of pitchblende, whose radium content is known, used
in the standardization of electroscopes. There are
two advantages worthy of mention which the bisulfate
method has in this operation over the solution method:
(a) It is not necessary to take into consideration the
"emanating power" of the pitchblende in the case of
the bisulfate method, while it is in the case of the solu-
tion method; (b) The same carefully weighed samples
of pitchblende may be used for several standardizations
by resealing the bisulfate melt after the emanation
has been driven off and collected for standardization.
II — Besides simplicity of operation, the bisulfate
method is by far the most rapid procedure. Not only
is the actual time required for the final separation of
■the emanation shorter than in the other procedure, but
the time in work expended in preparing a sample and
getting it sealed up is reduced to a few minutes.
Ill — The chances for loss due to manipulation are
reduced to one operation, when the material is trans-
ferred to the test tube. In both of the other methods
great care must be exercised in avoiding losses when
fusions are in progress. Instead of one, two to three
transfers of materials occur in the other methods.
IV — The cost of the operation is reduced. If one
is careful the test tubes may be used for several deter-
minations. In the refined sulfate method the small
platinum boats, costing at least a dollar each are not
good for more than 5 to 6 determinations. The use
of larger platinum vessels is essential in the other
methods, while in the bisulfate method all fusions are
made in hard glass test tubes.
V — After the final separation of emanation by the
bisulfate method, the material remains and is ready for
another determination in case an accident occurs.
When the material under examination contains
thorium, then the gas cannot be transferred directly
to the electroscope during fusion, but must be collected
in a gas burette to allow the decay of thorium emana-
tion.
I wish to thank Mr. J. C. Simpkins, who assisted me
at the outset in this work,' and Dr. H. Schlundt for his
helpful suggestions.
Chemical Products Company
Denver, Colorado
A RAPID PRESSURE METHOD FOR THE DETERMINA-
TION OF CARBON DIOXIDE IN CARBONATES
By W. H. Chapin
Received October 3, 1917
By use of the apparatus sketched below carbon
dioxide may be very quickly determined in any car-
bonate which is soluble in cold hydrochloric acid.
The accuracy of the method is equal to that attainable
with the absorption method, except possibly when
the latter is in the hands of a very skilled manipulator
who has had long practice with the method.
The principle is very simple: The carbonate is
allowed to dissolve in dilute HC1 contained in a flask
of known volume to which is attached a small mercury
manometer. The change in pressure is read off,
and by a simple calculation the weight and percentage
of C02 are obtained. The necessary details are given
in the procedure,
52C
THE JOURNAL OF INDUSTRIAL AND'ENGINEERING CHEMISTRY Vol.
No.
APPAKA I ' S
The flask is made from a 600 cc. distilling flask
by cutting off the side tube and sealing on the manom-
eter tube in its place. The latter should have a bore
of 5 mm. If too small, the capillary effect will inter-
fere with accurate reading, and if 100 large the move-
ment of the mercury changes the volume of the ap-
paratus too much.
Attached to the manometer tube is a sliding scale
of celluloid 15 cm. long and graduated in millimeters.
This scale is made from a 15 cm. (6 in.) ruler by cutting
out one side as seen in the sketch. It is held in place
by means of small metal clips which may be slipped
out of the way when reading. By use of a small lens
it is possible to read the position of the mercury to
'/5 mm. The inside of the manometer tube and the
mercury used in it must be '\<-;<u and dry or no ac-
curate readings can be expected.
The capsule used for weighing out the sample is
suspended by a thread as seen, the latter being caught
and held in the stopcock until it is desired to drop the
sample into the acid. This capsule may be made of
copper or any metal no1 displacing hydrogen from the
arid
The stopper should be of rubber, smooth and close
tit ting. Its tightness may always be insured by we1 ting
slightly at the moment of inserting. It should be
adjusted to a mark on the neck of the flask.
To keep the temperature of the apparatus constant
and to make it easy to determine, the bulb of the flask
is kept immersed in water at room temperature. The
thermometer used in reading the temperature is kept
standing in this water.
ire using the apparatus, its capacity is deter-
mined by fdling with water from the bottom of the
near arm of the manometer to the stopcock, and
weighing. To prevent the water going too far in the
manomi rubber connector is placed over the
open end and then closed by means of a pinchcock.
If this is opened slightly after the flask is filled the
may be adjusted to any position.
First set up the apparatus as seen in the sketch,
surrounding the bulb with water at room temperature.
Fill the flask with carbon dioxide from a generator or
pressure cylinder, and then run in by means of a pipette
10 cc. of 3 N HC1 which has also been saturate'! with
carbon dioxide.1 Weigh out a sample of the powdered
carbonate into the capsule (0.7 g. where the COj
content is about 20 per cent, and 0.4 g. where it is as
high as 40 per cent). Suspend the loaded capsule as
seen in the sketch, taking care to moisten the stopper
well and to press it down to the mark. This may
cause a slight compression of the gas in the flask and
a consequent rise in the mercury, but the effect may
be corrected by holding the end of the thread and open-
ing the stopcock for a moment while gently tapping
the manometer tube. When all is ready place a finger
over the end of the stopcock tube, taking care not to
catch the thread, and then open the cock so as to let
the capsule drop. After this immediately close the
cock again. The carbonate usually dissolves within
a minute, but it is always best to watch the manometer
for about 5 min. for further rise, tapping gently in
the meantime. Finally, when the reaction is complete,
adjust the scale so that the lower end corresponds with
the meniscus in the near arm of the tube and then read
off the height of the column in the other arm. Great
care must be taken to get exact adjustment and to
avoid parallax. Read to centimeters and tenths and
estimate to hundredths. Also take the temperature
accurately.
We now have the volume of the CCK at room tempera-
ture. V, (vol. of flask minus 10 cc. occupied by acid).
We also have the pressure P of the CO* (as read on
tin' manometer). Finally, we have the temperature I.
We can get the weight of the CO« by calculating down
to standard conditions and multiplying into the weight
of 1 cc. of COj under standard conditions (c 001065 g.).
We then have:
V, X_P X -'73 X 0.001065
760 X (-'73 + I"*
Since the factors \'t, 275. 0.001965 and 760 are always
the same, we may work out the value of the fraction
1 If the acid is not first saturated with COl a part of the gas evolved
during the reaction will remain in solution. If the flask is not first filled
with COj a part of the gas dissolved in the HO will at first be given off,
ami later during the determination, when the pressure of the CI I
gas will again go into solution Where the pressure of the COl in the flask
is one whole atmosphere at the start, no gas will he given off from the
acid, ami since the change in pressure during the determination will be
comparatively slight, very little will then go into solution. It is best to
keep the stock of HCI in a gas wash bottle connected with a fCipp generator,
where C I > 111. i\ a any 'ime he forced through it. The tube through which
the COl IS led into the apparatus when tilling with this gas is attached to
the wash bottle Thus every time the apparatus is filled just that much
v I' passes through the acid.
Wt. Of CO; =
July, iqiS
THE JOVRXAL OF INDUSTRIAL AXD EXGIXEERIXG CHEMISTRY
5^9
V, X 273 X 0.001965
760
and call this the constant for the apparatus, K. We
then have:
KP
Wt. of CO,
+ t
The percentage of C02 in the carbonate then follows,
thus
100 KP
Percentage of C02 •= -. ; — . v . „r. 7 . .
(273 + I) X Wt. of sample
By use of logarithms the necessary calculation may be
made in less than 2 min. The total time con-
sumed in making a determination, including the weigh-
ing and calculation, need not be over 15 min.
After completing a determination the capsule may
be lifted out of the apparatus by means of a wire hook,
and the spent acid may be drawn out with a pipette.
The apparatus is then ready for the next determination
without even refilling with C02.
Calcite
Per cent CO:
43.53
43.67
43 . 40
43 . 52
Av., 43.51
By ignition
43.59
Results
Argilla
Z4.71
24.34
24.67
24.36
24.59
Av. 24.53.
By absorption method
24.47(0)
34.74
34.40
By absorption method
34.59
34.30
(a) Average of 100 determinations varying from 24.1 per cent to 24.8
per cent.
Severance Chemical Laboratory
Oberlu* College, Oberlin, Ohio
A PROXIMATE ANALYSIS OF THE SEED OF THE
COMMON PIGWEED, AMARANTHUS
RETROFLEXUS L
By Everhart P. Harding and Walter A. Eoge
Received August 3, 1917
It was thought by the authors of this paper that
the partially carbonized bracts of the seeds of this
common plant might make a good filtering medium
for decolorizing sugar and other colored solutions.
This suggested other possible uses of the seeds which
led to their proximate analysis.
DESCRIPTION OF PLANT1
This variety of pigweed is commonly called "red
root." "rough pigweed," "green amaranthus" and
"Chinaman's greens." It is an annual weed which
grows from a well-formed and fairly deep-rooted
tap root. The root is generally red. The plant
grows from i to 3 ft. high and is branched, the branches
coming obliquely from the stem. The stem and
leaves are rough. The plant flowers from July to
September. These flowers are very inconspicuous,
appearing in the angle formed by the stem and leaf
stalk. The seeds are oval, black and shiny, and
ripen during August, or before. The weed occurs
in all parts of the State of Minnesota and thrives in
all kinds of soil, but prefers a rich loam. It is common
in gardens and waste places and does most injury
by crowding out crop plants.
' Minnesota Agricultural experiment Station, Bull. 129. March 1913,
p. 37
PREPARATION OF SAMPLE
The seeds were stripped from plants growing in
Waseca County in the southern part of Minnesota.
They were cleaned by removing foreign matter and
chaff (bracts). The separation and removal of the
bracts was difficult and tedious. Approximately 75
per cent of the seeds were black and fully matured,
the rest were red, showing varying degrees of maturity.
The sample was rapidly ground to 20-mesh size and
the moisture determined on a portion of this size to
represent total moisture in the seeds. The rest was
air-dried for 7 days and then ground to a 72-mesh
size. Moisture and all other determinations were
made on this size sample.
ANALYSIS
moisture in 20- and 72-MESH samples — One-
gram samples were dried in an electric drying oven
at exactly ioo° C. Preliminary tests showed that
14 and 4 hrs., respectively, were required to bring
the 20- and 72-mesh samples to constant weight.
-— 20-Mesh^ . 72- Mesh .
I II I II III
Moisture content, grams 0.1127 0.1129 0.0860 0.0860 0.0860
Average percentage of moisture 11.28 8.60
ash — Ash was determined on one-gram samples
in an electric muffle at a temperature of 6200 C.
1 11 in
Ash content in grams 0.0445 0.0448 0.0446
Average percentage of ash 4 . 46
It was very difficult to burn the substance com-
pletely to an ash over a Bunsen burner.
DETERMINATION OF OIL (ETHER EXTRACT) About
one-gram portions of the material, dried respectively
to constant weight in an air oven and in a vacuum
sulfuric acid desiccator, were extracted in Soxhlet
extractors with anhydrous, alcohol-free ethyl ether
to completion, which required 16 hrs.
i II in IV
Oven dried, grams oil 0.0798 0.0793 0.0788 0.0791
Desiccator dried, grams oil 0.0814 0.0788 0.0801
Oven dried, average percentage of oil . . 7.92
Desiccator dried . average percentage of oil 8 . 46
The dried oil dissolved in cold sulfuric ether, but
not in cold petroleum ether.
protein — Protein was determined by Gunning's
modification of Kjeldahl's method, using one-gram
samples and the nitrogen conversion factor 6.25.
1 II III IV
Protein content, grams 0.1880 0.1873 0 1867 0.1880
Average percentage of protein 19.13
STARCH DETERMINATION (ACID CONVERSION METHOD)
— Three-gram samples were used. The usual acid
conversion1 of starch into dextrose was made and the
amount of dextrose determined by the Munson-
Walker method.'- The seeds occupied a volume of
2.10 cc„ for which allowance was made. Aliquot
parts of the solution equivalent to 0.30 g. of substance
were used in the reductions and the starch conversion
factor of 0.90 was used.
The following amounts of reduced cuprous oxide
and the corresponding weights of dextrose and starch
were found.
' Sachse. them. Zcntr. 1877, 732; Bureau nl Chemistry, I S Dept.
of Agriculture, Bull. 107.
* Browne. J. 4m. (hem Sat . 1906. 43?
530
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 7
11
in
CusO, mg 299.6 298.0 297.5 298.4 300.1 299.4
Dextrose, mg 137.0 136.2 135.95 136.40 137.25 136.90
Starch, mg 123.3 122.6 122.4 122.7 123.5 123.2
Percentage of starch 41.09 40.91 40.98
Average percentage of starch 40.96
staki ii in ii i \ii\ation (diastase method) — Three-
gram samples were used and the diastase conversion
carried out as outlined in Leach's "Food Inspection
and Analysis," p. 284. The Munson- Walker method
was used for determining the amount of dextrose.
The reductions were determined on an aliquot part
of a definite volume equivalent to 0.240 g. of material.
For the conversion 0.60 g. of commercial diastase
with a reduction equivalent of 33.1 mg. of cuprous
oxide was used.
11
in
CutO, mg 233.9 234.1 232.8 233.3 232.8 232.0
Dextrose, mg 89.40 89.50 88.85 89.10 88.85 88.46
Starch, mg 80.46 80.55 79.96 80.19 79.96 79.61
Percentage of
starch 33.53 33.56 33.32 33.41 33.32 33.17
Average percentage of starch 33.39
DETERMINATION OF SUGAR (REDUCING SUGARS) The
determination of sugar was difficult on account of
the colloidal condition of the sugar extract. This
difficulty was finally overcome by keeping the solution
just slightly alkaline, which seemed to settle the col-
loids. Filtering was avoided as far as possible by
increasing the volume of the solution and pipetting
an aliquot volume.
Five-gram samples were boiled in 150 cc. of 50 per
cent neutral alcohol for an hour on a steam bath with
reflux condenser. The solution was cooled to room
temperature and the volume made up to 500 cc. with
05 per cent alcohol made just alkaline. After thor-
oughly mixing and settling over night, 400 cc. were
pipetted off with continuous suction and evaporated
on a water bath to 20 cc. This volume was made up
to 250 cc, using 2 cc. of lead acetate to clarify. After
clarifying, 200 cc. were pipetted with continuous
suction into a beaker and the excess of lead precipi-
tated with anhydrous sodium carbonate. The solu-
tion was filtered and 30 cc. of the filtrate used for
determining the sugar by the Munson-Walker method.
From an aliquot part of the solution equivalent to
0.80 g. of material only a mere trace of Cu?0 was
formed.
MIXATION OF SUGAR (AFTER INVERSION')
Fifty cubic centimeters of the solution in the pre-
ceding determination from which the excess lead
was precipitated were pipetted into a ioo-cc. graduated
flask, s cc. of concentrated hydrochloric acid added,
the volume made up to 100 cc. with distilled water,
and allowed to remain over night at about 200 C.
11
CutO. mg 21.00 21.40 21.90 21 10
9.40 9.56 9.76 9.44
Percentage of dextrose 2.35 2.39 2.44 2.36
Average percentage of dextrose
Percentage calculated as cane sugar 2.15
The acid was nearly neutralized and the sugar de-
termined in an aliquot part of the solution, equivalent
to 0.40 g. of material, by the Munson-Walker method.
determination of crude fiber — This determina-
tion was made on 2-g. samples containing 8.57 per
cent of moisture. Kennedy's modification1 of Sweeney's
method was used and modified by filtering and ig-
niting in alundum crucibles.
11
in
IV
Crude fiber and ash, grams 0.2585 0.2650 0.2590 0.2580
Ash, grams 0.0358 0.0380 0.0398 0.0382
Crude fiber, grams 0.2127 0.2220 0.2192 0.2198
Percentage crude fiber 10.63 11.1100 10.96 10.99
Average per cent crude fiber 10.92
tannin- Qualitative tests showed tannin.
SUMMARY
. Percentages on %
20-Mesh 72-Mesh
Constituents as Received Air-Dried
Moisture 1 1 . 28
Ash 4.33
Oil (ether extract) 7 . 03
Protein 18.57
Starch (diastase) 32 . 40
Starch (acid conversion) 39.77
Oven-
Dried
0.00
Desiccator-
Dried
7.92
20.93
36.52
44.83
Percentages
20-Mesh 72-Mesh
Received Air-Dried
Constituents
Hemicellulose (starch by acid conversion
minus starch of diastase) 7.37 7 . 59
Sugar reducing trace trace
Sugar (after inversion) 2.32 2.39
Sugar (after inversion computed to cane
sugar) 2.08 2.15
Crudefiber 10.59 10.92
Tannin and other undetermined substance
by difference 6.35 6.52 7.17
The proximate analysis shows that the seeds would
make a good component part of a stock food and as.
seeds of related species have been found to contain
considerable amounts of potassium nitrate, the rather
high protein content would suggest that they might,
be valuable as a chicken or bird food.
Chemical Laboratory
University of Minnesota
Minneapolis
THE DETECTION OF VEGETABLE GUMS IN FOOD
PRODUCTS
By A. A. Cook and A. G. "Woodman
Received May 2, 1918
The use of gums in food products is dependent
mainly on their physical properties, the most note-
worthy of which is their colloidal nature. This
property enables the gum substance to hold within
itself relatively large quantities of water and still
impart a decided "body" to the mixture. Their use
is specifically, then, as thickeners and binders in such
food products as marshmallow preparations, ice cream,
custards, pie fillings, egg substitutes, and flavoring
emulsions. The gums ordinarily employed are gum
arabic, gum tragacanth, Indian gum, agar-agar,
and commercial dextrin. Gelatin, egg albumin, and
commercial glucose, as well as starch, are also used
for the same purpose.
EXISTING METHODS
The methods which have been proposed for the de-
tection of this class of materials are based for the
most part on isolated reactions for a particular gum,
depending on some color or solubility test of the crude
gum itself, and having no reference to the detection
of small amounts of the gum in a complex food mixture.
Of the few that are more general perhaps the best.
This Journal, 4 (1912), 600.
July, 101S 7 F THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
531
known are those proposed by Patrick,1 and Howard,2
and the group scheme devised by Congdon.3 The
first two of these were suggested only for ice cream and,
while quite simple and easily performed, are unsatis-
factory for complicated food mixtures and entirely
useless so far as identification of the gum is concerned.
The more pretentious scheme of Congdon appeared
quite promising and was given a thorough trial on
food products and on known mixtures with gums.
The results obtained were, however, very disappointing.
Congdon's procedure is evidently based on quali-
tative tests made on the crude gums, no provision
being made for separating the gum from the other
components of the complex food mixture, no matter
how seriously these interfere with precipitation or
color tests. Further, some of the tests included in
the scheme were found to be neither specific nor
conclusive even with the gum itself.
SEPARATION OF THE GUM
As the basis for a workable scheme it was decided
at the outset that on account of the complex food
mixtures to which gums are added, all tests for the
identification of the thickener should be limited to
tests made on the relatively pure gum substance,
previously separated from the food product. This,
of necessity, eliminates many of the tests described
in the literature for the individual gums, most of
which are dependent on impurities naturally occurring
in the raw gums, and limits the available reactions
for an orderly scheme largely to the precipitation
tests. All such tests that could be found in the litera-
ture, and the action of all available solvents were
carefully studied on solutions of gum arabic, agar,
gum tragacanth, Indian gum, dextrin, gelatin, and
egg albumin. Since Indian gum is not so specific
a term as "arabic" or "tragacanth" and includes at
least two different species, two samples of this gum,
of entirely different appearance and obtained from
different sources, were used.
After much experimentation, which need not be
detailed here, the following systematic procedure
was finally adopted for the separation of the gum
in a comparatively pure condition from the food prod-
uct. This procedure consists, in brief, in precipitating
the protein of the food mixture by heating with acetic
acid and tannin, and then precipitating the gums from
the filtrate by acetone. In this way the sugars and
other acetone-soluble materials are left in the filtrate.
Since milk is a common ingredient of the class of foods
in question, soluble phosphates have also to be re-
moved by an extra precipitation with ammonia.
Finally, the redissolved gums are precipitated relatively
pure by alcohol. The procedure is summarized in
Table I.
Table I — The Separation of Gums
A — ELIMINATION OF PROTEINS
1 — Dilute sample to suitable concentration with water, add
5 cc. dilute acetic acid and 25 cc. of 10 per cent tannin
solution, and heat mixture for 20 to 30 min. Centrifuge and
filter. Discard precipitate.
1 U. S. Dept. of Agr., Bur. of Chem., Bull. 116, 24.
' J. Am. Chem. Soc, M (1907), 1622.
•This Journal, 7 (1915), 606.
Note— Casein, coagulable proteins, and some of the
gelatin precipitated. Fats and other insoluble substances
included in precipitate.
2 — Add 40 to 50 cc. more tannin solution to nitrate from Ai
and heat for short time. Centrifuge and filter. Discard
precipitate.
Note — Remainder of gelatin and soluble proteins pre-
cipitated.
B — SEPARATION OF GUMS AND DEXTRIN FROM SUGARS
1 — Treat clear filtrate from A2 with twice its volume of
acetone. Centrifuge and filter. Discard filtrate. Wash
precipitate twice with acetone.
Note — Precipitate includes gums and dextrin. No
precipitate shows absence of gums, dextrin, and milk
solids.
2 — Dissolve precipitate from Bi in 50 cc. of warm water
slightly acidified with acetic acid and add 10 cc. of ammonia
(sp. gr. 0.90). Centrifuge and filter. Discard precipitate.
Note — Calcium phosphate from milk solids precipitated.
C — ISOLATION OF PURE GUM SUBSTANCE
Add acetic acid to filtrate from B2 until slightly acid. Add
alcohol, one volume at a time, until a well defined pre-
cipitate appears.
Note — Gums and dextrin precipitated in fairly pure
condition. No precipitate with five volumes of alcohol
indicates absence of gums and dextrin.
Within certain limitations, which will be discussed
later, this procedure is capable of separating gums
and dextrin from complex food mixtures. In the
numerous experiments on which it was based the
amount of gum present varied from 0.1 to over
1.0 g. and the weight of sample from 50 to 200 g.
It is certain that amounts of gum as small as 0.1 g.
can be separated by the procedure from ordinary food
mixtures. It should be remembered in this con-
nection, however, that some gums are more readily
detected than others when present in equivalent
amounts. Tragacanth, for example, is much easier
to detect In small quantities than either arabic or
agar. The relation of the amounts of other precipit able
matter, especially protein, is also of some importance
since the gums tend to be carried down mechanically
in the precipitation of protein, hence the ratio of
protein to gum may be so great that the procedure
will fail to detect the gum through mechanical loss.
Table II
Approximate Volumes
of Alcohol Necessary
for Precipitation Characteristic
Vols. Al- Vol. Gum Appearance of
cohol Solution Gum Precipitate in Air
Agar 3-4 1 Finely divided white Usually remains soft
precipitate; settles and non-coherent
Arabic 2 1 White flocciilent pre- Becomes dry and
cipitate; settles powdery
quickly; neither
sticky nor coherent
Indian.... 2-3 1 Stringy precipitate; Becomes dark col -
becomes very co- ored; tough co-
herent after settling herent layer
Tragacanth 2 1 Coherent, jelly-like Flattens down, be-
mass; floats in eotnini; a semi-
clots in upper transparent co-
part of solution herent layer
Dextrin... 3 1 White, fine prccipi- Tends to become
tate; settles slow- hard on long
ly; very sticky standing
IDENTIFICATION 01 III E GUM
Certain of the precipitation tests for the gums,
which have been used as the basis for the foregoing
method of separation, serve also fairly well for the
Characteristics
of Gum Precipitate
After Standing
for Some Tune
THE JOURNAL OF INDUSTRIAL AND ENGINEERING ( HEMISTRY Vol. 10, No.
identification of the gums. It suffices in general to
the approximate volume of alcohol required for
the final precipitation and the nature and appearance
of the alcohol precipitate. It is advantageous in this
connection to pour off most of the alcohol after the
ipitate has settled and moist gum pre-
cipitin' to stand expo air for a short time.
noting its behavior when drying. Table II presents
in concise form the characteristic differences which
own by the common gums.
( ONJ [RMATORV TESTS
While the characteristic differences described in
the preceding table have been the chief reliance in
identifying the gums, a number of the tests described
in the literature have been examined to determine
their value as confirmatory tests. Most of these,
as previously stated, depend on impurities present in
the crude gum and hence, as would be expected,
proved of little value when applied to the separated
gum precipitate. Several procedures, however, were
found even under these conditions to be distinctly
helpful. Chief of these was the presence of charac-
teristic diatoms in the agar. The test is a well-known
one and consists in identifying under the microscope
the peculiar diatoms which are associated with agar,
chiefly Arachnoidiscus Ehrenbergii and various species
of Cocconeis, after destroying the organic matter by
digestion with acid. The characteristic appearance
of these diatoms will be found figured in most standard
texts on food analysis.
The procedure consisted in destroying the organic
matter of the sample by heating with nitric and sul-
furic acids until the solution became colorless, diluting
the concentrated acid solution with water, centrifuging
to collect the siliceous residue, and examining this
under the microscope. The test may be applied to
the original material, but much time will be saved by
using the tannin precipitate obtained in Ai of Table I.
Since this precipitate is separated by the centrifuge it
will obviously contain all the relatively heavy particles,
including the diatoms, and its use will eliminate the
interference due to soluble carbohydrates, as cane
sugar, commercial glucose, etc., which use up time and
acid in the digestion. This procedure was tried re-
i dly on many samples of agar including the purest
bacteriological material, and on food mixtures con-
taining agar, and the presence of the characteristic
diatoms noted in every case. Although this test ac-
tually depends on the presence of "impurities" in the
gum, it was found that the diatoms are so widely dis-
tributed in commercial samples and remain so con-
sistently in the tannin precipitate that the test was
eful.
The volatile acidity of Indian gum was also found
of value as a confirmatory test. It has been noted
by several authors that the species of gum coming
under the classification of Indian gum have the charac-
teristic property of developing an acetic odor when
exposed to the air, and Emery1 has made this eliarac-
ii the basis of a method for the detection of
i Tins Journal, « (191
Indian gum as an adulterant of gum tragacanth. The
method consists, in brief, of accelerating the hydrolysis
of the gum by heating with acid, distilling, and titrating
icetic acid produced. Emery gives the following
typical figt sed as cc. of N/io acid per gram
of gum:
-nth 3
Indian pm 25.4-28.3
Emery's method was applied to the dried gum pre-
cipitates obtained in the systematic procedure of
Table I and the following results were obtained:
Table III
Gum Volatile Acidity
Indian gum, No. 1 20.3
Indian gum, No 3 16.4
■ 1 for 4 mos. after precipitating) 16.1
Indian gum. No. 4 9.5
Indian gum, No. 5 14.8
Tragacanth, No. I 3.5
Tragacanth. No. 2 2.3
Tragacanth, No. 3
Gum arabic 0. 25
Dextrin 1.0
These figures show that the differences found by
Emery hold for the precipitated gums, although to
a less marked degree. The method, although rather
long and tedious, has distinct value as a confirmatory
test on gum precipitates when Indian gum is suspected
and the characteristics described in Table II are not
conclusive.
LIMITATIONS OF THE METHOD
The delicacy of the method under favorable condi-
tions has been pointed out in a previous paragraph.
There are, however, certain limitations to its useful-
ness which should be definitely noted.
First, the successful use of the procedure for the
identification of the gums depends primarily upon the
ability to recognize the different visible characteristics
of the gum precipitates. It is, therefore, highly de-
sirable that before using the procedure for analytical
purposes the analyst should know the various gum
precipitates "by sight." This can be readily ac-
complished with the aid of a few prepared solutions
of the gums concerned.
The identification of the gums where more than
one is present in the food mixture is a more difficult
matter. With some combinations of gums a partial
separation can be accomplished by the fractional pre-
cipitation of the procedure, but with such a combina-
tion as dextrin and agar-agar, or Indian gum and
tragacanth, this would be practically impossible,
although there might be indications as to the presence
of both gums.
A more serious matter is the possible presence of
two substances which interfere distinctly with the
separation and identification of the true gums. These
are pectin and commercial glucose. The first of
these is perhaps less important since, although it is
somewhat similar to the gums and would to a certain
extent be precipitated with them in the procedure,
few of the commercial food products in which gums
are used ordinarily would be likely to contain fruit
pectins. The most likely combinations would be
fruit pie fillings and jellies and jams made from apple
stock, food products in which the presence of gums has
been noted.
July, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
533
In the few cases where from the source of the sample
the presence of pectin might be expected, its removal
prior to the alcoholic separation of the gums may be
aided by observing the following precautions:
(1) In adding the acetic acid to the ammoniacal
solution (C of Table I), it should be added slowly,
the mixture stirred, and allowed to stand for some
time with occasional shaking. The removal of pectin
at this point may be accelerated by adding a few
drops of a tannin-iron solution before the ammonia
and acetic acid treatment.
(2) Small amounts of alcohol, one-quarter to one-
half of a volume, are added with stirring to the am-
moniacal solution.
(3) When the amount of iron present is slight,
judging from the color of the solution, as well as the
precipitates, a few drops of a ferric chloride solution
are added to the aqueous solution of the acetone
precipitate (Bi of Table I).
Of greater practical importance is the presence of
commercial glucose in products which also contain
gum, a combination which is common in commercial
products like marshmallow creams. The interfering
factor here is of course dextrin and this is precipitated
with the final gum precipitate by alcohol, although
the scheme of fractional precipitation outlined in
Table I should give some indication of its presence.
Numerous tests have shown that in the case of
Indian gum and gum tragacanth commercial glucose
interferes but little with their detection and identi-
fication, even when the ratio between the quantities
of glucose and gum is as high as 40 to 1 for Indian gum
and 120 to 1 for gum tragacanth. In the case of gum
arabic the interference of commercial glucose is dis-
tinctly noticeable when the ratio of glucose to gum is
20 to 1, a portion of the dextrin precipitating with 2
volumes of alcohol along with the gum arabic, and by
its sticky character masking the flocculent, non-
coherent characteristic of the gum arabic. With agar,
although no experiments were carried out, the inter-
ference would be still greater. Since the amount of
commercial glucose present in a marshmallow paste,
for example, is likely to exceed the ratio given for gum
arabic, in such cases an additional step in the procedure
may be needed.
This additional step is based on the fact that dextrin
is more readily hydrolyzed by boiling with dilute
acid than are the gums. It is carried out on the pre-
cipitate obtained with two volumes of alcohol, which
will contain the greater part of the gum arabic and a
portion of the dextrin. 0.5 g. of the dried gum pre-
cipitate is heated for 5 min. with 50 cc. of water and
2.5 cc. of concentrated hydrochloric acid (sp. gr.
1.20). The hydrolysis is conveniently carried out in
a large test tube immersed in boiling water.
Experiments on known mixtures have shown that
in this way one part of gum arabic may be detected
in a mixture with 4 parts of dextrin, a delicacy which
allows the detection of the gum in the presence of a
considerable proportion of commercial glucose. Fur-
ther, it must be remembered that the precipitate ob-
tained with 2 volumes of alcohol would not contain
the whole of the dextrin involved, for the larger part
of this, as has been shown, would come down only
with the third volume of alcohol. The precipitate to
be hydrolyzed would, therefore, contain the gum with
a small amount only of the dextrin present in the orig-
inal mixture. Without question, then, the procedure
is quite delicate and is capable of detecting relatively
small quantities of gum arabic in the presence of com-
mercial glucose.
SUMMARY
A method is described for the separation of the more
common gums from food products based upon elimina-
tion of proteins by acetic acid and tannin and precipi-
tation of the gums by acetone and finally alcohol.
The separated gums are identified mainly by their
fractional precipitation with alcohol and the charac-
teristic appearance of the precipitated pure gum.
The necessary modification of the method in the
presence of such interfering substances as milk solids,
pectin, and commercial glucose is described.
The method described is capable of detecting with
ordinary commercial products 0.1 g. of gum in 100 g.
of a complex food mixture.
Massachusetts Institute of Technology
Cambridge, Mass.
UNIFORM NITROGEN DETERMINATION IN COTTON-
SEED MEAL
By J. S. McHargue
Received April 13, 1918
Chemists often have trouble in obtaining uniform
results in duplicating nitrogen determinations on
cottonseed meal. Since cottonseed meal is so ex-
tensively used as a source of protein in feeds, it is a
matter of considerable importance whether or not all
serious errors have been eliminated in a nitrogen
determination on this material.
The object of this paper is to call attention to pro-
cedures common among chemists which are often the
cause of considerable error in the determination of
nitrogen in cottonseed meal.
During the past year the writer has been called upon
to check a number of cottonseed meal samples in
which the amount of nitrogen was in question. On a
few of these samples duplicate determinations of
nitrogen showed variations ranging from as much as
0.50 to 1.50 per cent of protein, while other samples
of cottonseed meal gave almost identical results upon
duplication. The samples upon which varying results
were obtained naturally suggested further investiga-
tion in regard to the cause of the variations.
Self has shown that nitrogen can be lost by volatiliza-
tion during the digestion if a large excess of potassium
sulfate has been added. He attributes this loss to the
formation of KHSO, when an excess of H2SOi has been
boiled off.
The following experiments were made to determine
whether or not nitrogen was lost in ,'i eiitliiusci-d nn-:il
1 Pharm. J., 88, 384-5; Chtm \bs 1 1 mer.). 6 (1912), 2048.
534
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING < HEMISTRY Vol. 10, Xo.
digestion when there was considerable variation in the
amount of Na2S04 added.
Six 0.7005 g. portions of cottonseed meal were
weighed and transferred into 800 cc. Kjeldahl digestion
flasks. 25 cc. of H2SO4 and the amount of the re-
agents indicated in the table were added to each flask
and the digestion carried on at a brisk boil for 2 hrs.
After cooling, the contents of the flasks were diluted,
made alkaline, the mercury or copper precipitated with
sodium polysulfide1 and the ammonia distilled in the
usual way. The results were a follows:
Tabus I
Reagents Added Results
Anhyd. Na^SO* Mercury N Obtained Protein
G. G. Percent Percent
A 2 0.7 6.32 39.50
B 4 0.7 6.30 39.37
C 12 0.7 6.29 39.31
CuSO..5Hi0
\ 2 0.5 6.16 38.50
B 4 0.5 6.32 39.50
C 12 0.5 6.38 39.87
From the foregoing results it is to be observed that
there is a gradual diminution in the nitrogen determina-
tions receiving mercury as the amount of Na2S04 is
increased, whereas in those digested with copper
sulfate there is a gradual increase in the nitrogen as
the NajSOj increases. The results obtained with
mercury agree with the findings of Self.
Robertson2 has also noted slightly higher results
where copper sulfate replaced mercury in the digestion.
The loss in nitrogen in the presence of mercury can be
assumed to be due either to volatilization of a nitrogen
compound during the digestion or to the formation of a
mercurammonium compound which is not decomposed
during distillation. While the losses of nitrogen in the
experiments digested with mercury are noteworthy
they are not sufficiently great to account for the varia-
tions often experienced in nitrogen determinations on
cottonseed meal. Hence it was necessary to continue
the search for other sources of error.
Further experiments were made on a sample of
cottonseed meal which had baffled the wits of another
chemist in regard to its nitrogen content. Six nitrogen
determinations were made on this sample for the
purpose of showing the variations between determina-
tions and to test the efficiency of Na2S04 versus
K2SO4 in cottonseed meal digestions. In three of the
determinations 7 g. of K2S04 were used in each diges-
tion and 6 g. of Na2SOi in each of the remaining
determinations. Mercury was used as the catalyst
and the amount of acid and time of digestion were the
same as in previous experiments. The results ob-
tained were as follows:
Table II
Potassium Sodium
Sulfate Sulfate
Per cent Per cent
Nitrogen Nitrogen
A 6.90 6.71
H 6.92 6.75
C 6.74 6.64
Average 6.85 6.70
Per cent Per cent
Protein Protein
Average 42.81 41.87
Maximum 43.25 42.19
Minimum 42.13 41.50
Difference 1.12 0 . 69
1 Sodium polysulfide can now be obtained from Messrs. Charles Cooper
& Co.. 194 Worth Street, New York.
» Brackctt and Haskins. "Nitrogen." J t <> I C, 1. No. 3, 395.
In the averages of the above experiments there is a
difference of 0.15 per cent nitrogen or 0.94 per cent
protein in favor of the K2SO< digestions. The differ-
ence between the maximum and minimum results in
the K2SO, digestions is 0.18 per cent nitrogen or 1.12
nt protein. In the XajSOi digestions these
differences are 0.11 per cent nitrogen or 0.69 per cent
protein, a little more than one-half the difference in the
K2SO4 digestions. It is also to be noted that the
results for "C" in each digestion are decidedly off in
comparison with the results for "A" and "B."
In order to locate the cause of the "off" results in the
foregoing determinations the following series of experi-
ments was carried out:
One hundred grams of cottonseed meal were trans-
ferred onto a series of sieves of 20, 40, and 60 mesh,
and after placing a few coins on each sieve the whole
was shaken for about 25 min. That portion of
the sample remaining on the 20 mesh sieve was 13.58
per cent, on the 40 mesh 30.82 per cent, on the 60
mesh 16.71 per cent, and the portion that passed
through the 60 mesh was 38.89 per cent. The parts
into which the sample was divided by sieving were
bottled separately and six nitrogen determinations
made on each sample. The amount of the reagents
and the time of digestion were the same as in the
previous experiment.
Table III shows the results obtained for nitrogen
on each of the samples with K^SOi and Na2S0i.
Table III
Greater Between 20 Between 40 Less than
than 20 mesh and 40 mesh and 60 mesh 60 mesh
Per cent N Per cent N Percent N Percent N
With K'SO, A4.84 4.76 7.01 7.69
B4.72 4.66 7.00 7.65
C4.65 4.66 6.85 7.64
Average 4.74 4.69 6.95 7.66
Equivalent to protein 29.62 29.31 43.44 47.88
Range of N 0.19 0.10 0.16 0.05
Equivalent to protein 1.19 0.62 1.00 0.31
Per cent N Per cent N Per cent N Per cent N
With NaiSO. A4.72 4.72 6.98 7.65
B4.54 4.67 6.96 7.65
C4.52 4.63 6.93 7.62
Average 4.59 4.67 6.96 7.64
Equivalent to protein 28.69 29.19 43.50 47.75
Range of N 0.20 0.09 0.05 0.03
Equivalent to protein 1.25 0.56 0.31 0.18
N by K...SO. > N by Na:SOi 0.15 0.02 — O.01 0.02
From the results presented in the foregoing table
on the nitrogen determinations of the different sized
particles that were contained in the sample of cotton-
seed meal, it is to be observed that there is a gradual
diminution in the variations of the different nitrogen
determinations as wc approach the fine ground ma-
terial. On the 20 mesh sample there is a difference of
0.20 per cent nitrogen, which is equivalent to 1.25
per cent of protein, in the averages of the two different
digestions, while on the 40 mesh sample there is a
difference in the averages of the two different digestions
of 0.02 per cent nitrogen, which is equivalent to a
difference of 0.12 per cent of protein. There is also a
striking diminution in the difference between the
averages of the two methods of digestion on the 60
mesh sample as compared with the difference on the 40
mesh sample. It is also to be noted that there is less
variation in the results obtained in the sodium sulfate
digestions than in the potassium sulfate digestions.
July, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY 53s
From the results in Table III it is to be con- were only obtained after 4 hrs. of digestion. How-
eluded that another and perhaps the greater cause of ever, the addition of larger amounts of sodium sulfate
irregularities in nitrogen determinations in cottonseed will reduce the time of digestion, 12 g. being sufficient
meal is due to the lack of regrinding the larger particles to bring about complete digestion in 2 hrs.
to a sufficient degree of fineness to obtain a homo- It was observed that in determinations in which
geneous mixture in weighing out portions for digestion. copper was used as the catalyst, the precipitation of
In order to confirm this conclusion more definitely, the copper as sulfide greatly facilitates the boiling and
about 300 g. of cottonseed meal were sifted with coins reduces the time of distillation as compared with
on a 40 mesh sieve for about 25 min. The greater determinations in which the copper was not precipi-
part of the coarse particles that remained on the sieve tated previously to starting the distillation,
were hulls and were ground to pass through the 40 Approximately 300 cc. of liquid should remain in the
mesh sieve. The two portions were again thoroughly flask after distillation, since alkali will distil over if the
mixed and quaitered down to a 100 g. sample. Upon solutions are concentrated to a much less volume,
this sample the following experiments were made for A large excess of alkali should always be avoided,
the purpose of testing, first, the uniformity of the Blanks were run on all of the reagents and deducted
results obtained on the material treated in the above from each determination,
manner, and second, the time necessary to complete a „««■/« ttc™«<.
, J r CONCLUSIONS
digestion on cottonseed meal. „ , . .... ,
•p c c 4. 1 •* j from the data presented in this paper the following
Pour series of experiments of twelve nitrogen de- , . , , . , , . . s
+„ _,•- +• u j t>i. j- i.- • 4.1 conclusions may be drawn in regard to obtaining uni-
termmations each were made. The digestions m these , . , . . & s
, . . , - , torm nitrogen determinations on cottonseed meal,
series 01 experiments were carried on for 1, 2. 3 and 4 _,,,., . . , . . .
, ,. , T , . ., ,, ,. .. 1 — the chief source of irregularity in nitrogen de-
hrs., respectively. In each series all the digestions . . , , , , ,
, , « ,. . „ , , , . i_'il-i j terminations on cottonseed meal may be due to a lack
were heated gently at first and then to a brisk boil, and /•••,-, , _. . ,
t. , ,, ., . ,. , TT of grinding the sample to a sufficient degree of fineness
after about 45 mm. all the solutions were clear. Upon , , % A , • , . , , „
j- ami i( r ,, ,>_ , ^ • 1 (.4° mesh) to obtain a homogeneous mixture of hulls
distillation the following results were obtained: , , . . , .
and meal for weighing out a charge.
Table IV — Showing the Effect of Different Periods of Digestion
with Mercury, Copper Sulfate, Potassium Sulfate, and Sodium 2 When mercury is used as the catalyst a digestion
Sulfate on a Sample of Cottonseed Meal . ,,.,,.,..
i hour 2 hours 3 hours 4 hours pertod of more than 2 hrs. of brisk boiling in an excess
Per cent N Per cent N Per cent N Per cent N Qf sulfur;c acid apparently Causes a loss of nitrogen.
7 g. K,SO. + 0.7 g. Hg + 25 cc. H2SO. «/ ■ a 4.1. * 1 + *t.
A 6 10 6 26 6.22 6.12 3 — When copper sulfate is used as the catalyst the
^ £[f |-^ g-j* g'2? digestion period will depend upon the amount of sodium
, ,, ~~m , „. „ ,_ sulfate added, 12 g. being sufficient to bring about a
Average 6.14 6.25 6.24 6.17 ° °
Protein 38.38 39.06 39.0 38.56 complete digestion in 2 hrs.
6 g n«so. + 0.7 g. Hg + 25 cc h2so, 4— The precipitation of the copper as sulfide facili-
A 6.13 6.26 6.20 6.24 r r r l
B 6.14 6.28 6.22 6.22 tates the boiling and shortens the time of distillation.
C 6.18 6.25 .6.26 6.12 & , .
5 — Sodium sulfate is just as efficient as potassium
Average 6.15 6.27 6.23 6.19 ,c , ■ , , ,•
Protein 38.44 39.19 38.94 38.69 sulfate in cottonseed meal digestions.
7 g. K2SO4 + 0.5 g. CuS04.5HiO + 25 cc. H2SO4 6 — The writer suggests the use of the following
b ; 6^18 6^22 6.25 6^34 charge: 0.7005 g. of cottonseed meal, 0.3 g. CuS04 or
c JLlf — — JJ1 0.5 g. CuS04.sH20, 12 g. Na2S04 + 25 cc. H2S04, and
Average 6.18 6.22 6.30 6.32 brisk boilino- for 2 hrs
Protein 38.63 38.88 39.38 39.50 uiibK uoillllg iui 2 nib.
6 g. Na2SO« + 0.5 g. CuSO<.5HiO + 25 cc. HiSO< Kentucky Agricultural Experiment Station
A 6.18 6.21 6.26 6.36 Lexington, Kentucky
B 6.17 6.29 6.34 6.34
C 6.16 6.24 6.28 6.33
Pr'oYeln'....'. 38.11 3?! 06 39.1? 39163 THE DETECTION AND DETERMINATION OF COUMARIN
Table V— Showing the Average Percentage of Protein for Each IN FACTITIOUS VANILLA EXTRACTS
Digestion Period with Mercury and with Copper Sulfate
With mercury... 38.41 39.13 38.97 38.62 By H. J. Wichmann
With copper. . . . 38.60 38.97 39.35 39.57 Received March 18, 1918
In comparing the results obtained under the different A quick qualitative test for coumarin is very de-
conditions of digestion, as shown in the foregoing table, sirable for separating those extracts that contain it
the following points are of most interest. from those thai do not The number of extracts that
In all of the one-hour digestions the results for contain coumarin without a declaration of its presence
nitrogen are low; therefore, a longer period than 1 hr. on the label is so small that the extra work of making
is necessary for a complete digestion of cottonseed the double extraction, as in the modified Hess-Pres-
meal. In the experiments in which mercury was used cott method, seems entiri fluous and Un-
as the catalyst, the 2-hr. digestions gave the necessary. The method of testing for coumarin de-
maximum results. Longer periods of digestion ap- scribed in IT. S. Department of Agriculture, Bureau of
parently caused a slight loss of nitrogen, negligible Chemistry, Circular 95 has, in the hands of the writer,
after 3 hrs., but appreciable at the end of 4 hrs.' diges- efficient for this purpose. The method there
tion. outlined requires the distilling of the extract to a low
In the experiments in which copper lulfate and 6 g. volume, evaporating the distillate containing vanillin
of sodium sulfate were used, the maximum results and coumarin. if the latter is present, with i cc. of
S36
THE JOURNAL 01 INDl STRIAL AND ENGINEERING < HEMISTRY Vol. 10, No. 7
50 per cent potassium hydroxide, followed by fusion.
ylic and protocatechuii acids formed from
the coumarin and vanillin by the fusion arc separated
by distilling the acidified solutions of these acids or
separating them with benzene, the former being
ith steam and soluble in benzene, properties
not possessed by the latter. The writer prefers the
ne method of separation because of its simplicity.
The method, however, requires some preliminary
experience before very small quantities of coumarin
can with certainty be detected. One precaution
necessary is not to carry on the distillation so far that
yellow decomposition products result, but to stop just
short of that point; otherwise it will be difficult to
make a clean-cut fusion.
T. R. Dean1 modified the original method. It was
recognized in the original article that certain volatile
salicylate-forming compounds like saccharin should
not be present. If they are present a qualitative test
will indicate coumarin, but a subsequent quantitative
determination would give no weighable quantity.
because both salicylic acid and saccharin would be
removed with the vanillin thus leaving no coumarin
where it would be expected. This disagreement be-
tween qualitative and quantitative results would
indicate salicylate-forming compounds, the identity
of which would have to be determined by further work.
Dean's modification simplifies the original method in
that the fusion is not complicated by the presence of
vanillin and other organic matter. Such matter may
cause a destruction of the salicylates if sufficient
alkali has not been added.
When a vanilla extract is extracted with ether a
certain amount of coloring matter always accompanies
the vanillin. In the case of an alcoholic extract this
is always more than if it had been dealcoholized.
However, the amount of coloring matter is greatly
reduced in either case if the solution is alkaline. Dean
recommends using a dealcoholized extract, preferably
the residue from an alcohol distillation. Experiments
by the writer have shown, however, that it is not
necessary to dealcoholize before testing for coumarin.
an further simplifications have been introduced
and attention is called to the peculiar color changes
that coumarin undergoes when heated with con-
centrated potassium hydroxide. These are interesting
and characteristic and furnish the first indication of the
nee of coumarin. The method is as follows:
Ten cc. of extract an- made alkaline with 10 per cent sodium
hydroxide, then diluted with 15 cc. of water to reduce the
alcoholic strength ami extracted with 20 cc. of ether in a separa-
tors funnel. The ether solution will be slightly colored when
tin brown lower layer has been drawn off. A few cc. of strong
alcoholic potassium hydroxide solution are added, the mixture
shaken and then washed with 10 cc. of water. The ether layer
will thru lie found to be white. This procedure removes all
organic acids, vanillin, coloring matter or saccharin that might
be present One cc. of 50 per cent potassium hydroxide solu-
tion is i.l, icid in a test tube and the ether solution of coumarin
poured over it. Alter thoroughly shaking, the ether is hastily
evaporated. The tube is then placed over a free flame, the
watei evaporated and the potassium hydroxide fused. If
coumarin is present in any amount a change of color will he
1 This Journal, 7 (1915), 519.
noticed as the evaporation of the water proceeds and fusion
begins. Even very small quantities of coumarin in strong, hot
potassium hydroxide solution will show a greenish yellow color
that suddenly disappears as the heating is continued. The
disappearance of the color shows that the coumarin has been
converted into the salicylate anil heating should he discon-
tinued The melt is taken up with a few cc. of water, the solu-
tion acidified with sulfuric acid and extracted in a small separa-
tory funnel with 5 to 10 cc. ol benzene Benzene is preferred
to any other solvent because of its low density, low solvent
power for mineral acids, and because it will not dissolve any
protocatechuic acid formed from vanillin that might possibly
have been carried over with the ether. The acid solution is
removed from the separately funnel and the benzene washed
with a few cc. of water. After washing, the benzene is filtered
into a test tube and tested for salicylic acid with a cc. or two of
water containing a few drops of ferric chloride solution. If no
color develops on shaking, one or two drops of A' 10 sodium
hydroxide should be added to neutralize any trace of mineral
acid that may lie present and which prevents the development
of the purple color.
This test can be conducted easily in 15 min.. takes
only 10 cc. of extract, and does not require dealcoholiza-
tion or any complicated apparatus. The only evapora-
tion necessary, that of the ether, can be done on a
steam bath without appreciable loss of coumarin
The change of color on fusion indicates its own end-
point and gives, together with the purple salicylate
color, a double test for coumarin. Coumarin is changed
to salts of coumaric acid by hot concentrated potassium
hydroxide. The development of the yellow color
shows this phase and the sudden disappearance of the
color indicates the conversion into a colorless salicyl-
ate. The delicacy is unquestionably great since the
writer has obtained a very decided purple color with
10 cc. of extract containing only 0.005 Per cent of
coumarin. This modified method is considered simpler
than the original and can be conducted in a shorter
time.
This qualitative test has not been made quantita-
tive. The results obtained so far by fusing pure
coumarin with potassium hydroxide in test tubes,
extracting the salicylic acid and matching the color
developed against standard solutions, have been from
2 to 15 per cent too low. This is probably due to a
slight volatilization of coumarin before the alkali can
attack and hold it. However, results by a gravimetric
met hod. to be described later, have been so satis-
factory as to accuracy, speed and ability to determine
small quantities that a colorimetric method is hardly-
necessary.
The Hess-Prescott method directs that the extract
be dealcoholized before the vanillin and coumarin are
extracted. The vanillin is then removed from the
ether by a number of extractions with 2 per cent
ammonia, the coumarin remaining in the ether. Un-
published results of the writer indicate that it is
possible to titrate vanillin in non-aqueous solutions
with alcoholic sodium ethylate or potash. The
sodium-vanillin salt can then be removed from the
solvent by washing with water. Coumarin is not
affected by the vanillin titration. Therefore, it re-
mains in the solvent and. after the vanillin salt has
been washed out, can be determined by evaporation,
July, iqiS THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
drying and weighing. Excess alcoholic alkali can be
used without affecting the coumarin results if it is not
desired to determine the vanillin volumetrically.
It has been found that benzene, chloroform and ether
are the best solvents for extracting vanillin and
coumarin from either aqueous or alcoholic solutions.
Forty cc. of chloroform, ioo cc. of benzene and 60 cc.
of ether in four or five extractions will extract quanti-
tatively large amounts of vanillin from water and
alcohol solutions up to 25 per cent strength. Since a
half aliquot is usually taken for analysis this corre-
sponds to 50 per cent alcohol in the extract which is
probably more than the average commercial extract
contains. Benzene, chloroform and ether all extract
acids and coloring matter from vanillin extracts treated
with lead acetate, ether extracting by far the most.
Hence ether cannot be used if the vanillin is to be
determined by titration, because the acetic acid it
extracts at the same time cannot be removed by wash-
ing. Benzene or chloroform can be used for such
purposes. There is, therefore, a possibility of com-
bining a volumetric vanillin with a gravimetric
coumarin determination in such cases where the
qualitative test shows the presence of the latter. The
details of a volumetric vanillin determination will be
published later. However, if results for coumarin
only are desired, it is recommended that ether be used
as the extracting solvent as it has decided advantages
in such cases. It evaporates more quickly and the
extractions and washings are speedier because ether
and water can be separated faster than water and
chloroform or water and benzene. While ether ex-
tracts considerably more coloring matter and acid than
benzene or chloroform from vanilla solutions, these
impurities are neutralized by the alkali and removed
with the vanillin in the subsequent washing with water.
A water-white solution of coumarin in ether remains.
The ether can be evaporated and the coumarin dried
and weighed. No dealcoholization is necessary and
the results can be obtained speedily. It is not rec-
ommended in quantitative work to extract the
coumarin from alkaline vanilla solutions as in the
qualitative method, because emulsions are liable to
form, and coloring matter must be removed anyhow.
In many cases where speed is desirable it would be
advantageous to determine coumarin in one portion
and the vanillin by colorimetric or other methods in
another.
To show the results that can be obtained by the
above method the following data are submitted:
To 50 cc. of vanilla extract various quantities of coumarin
were added, the vanilla solutions then treated with lead acetate
without dealcoholization. made up to 100 cc, filtered, and the
excess lead precipitated wilh dry potassium oxalate. The re-
moval of the lead facilitates extraction because it reduces emul-
sion formation. Fifty cc. of the solutions thus prepared were
extracted with ether, benzene or chloroform, as indicated in the
table, a few drops of phenolphthalein solution and excess alco-
holic alkali added and the vanillin salt removed by washing
With several 10 cc. portions of water. The disappearance of the
red phenolphthalein color in the wash water is an indication of
sufficient washing. The washed solutions containing the cou-
marin were evaporated and the coumarin dried and weighed.
The results are given in Table I.
Table I
Quantity of
Coumarin extracting Number Coumarin Coumarin
added Extracting solvent of recovered recovered
Mg. solvent Cc. extractions Mg. Per cent
25.0 Benzene 100 5 24.5 98.0
24.5 Benzene 100 5 24.0 97.9
24.5 Chloroform 40 4 24.0 97.9
25.0 Chloroform 40 4 25.2 100.4
25.0 Ether 80 4 25.2 100.4
25.0 Ether 80 4 24.8 99.2
5.0 Ether 80 4 4.8 96.0
10.0 Ether 80 4 10.2 102.0
15.0 Ether 80 4 15.0 100.0
25.0 Ether 80 4 24.5 98.0
50.0 Ether 80 4 49.3 98.6
The results shown in the table indicate that an
accurate quantitative determination of coumarin can
be made by the method outlined above. Quicker
methods for lead number and vanillin, to correspond
with the coumarin method, are in preparation.
SUMMARY
A simple and quick modification of the original
method for the detection of coumarin in factitious
vanilla extracts has been developed. While quantita-
tive results based on the qualitative method are too
low, another method has been given which is shown
to be both quick and accurate for the determination of
coumarin.
U. S. Department of Agriculture
Food and Drug Inspection Laboratory
Denver, Colorado
THE DETERMINATION OF ESSENTIAL OILS IN NON-
ALCOHOLIC FLAVORING EXTRACTS
By Frank M. Boyles
Received March 28, 1918
There has been appearing for some years on the
American market, in increasing numbers, a variety
of so-called non-alcoholic flavoring extracts which
consist essentially of an emulsion of the respective
essential oils in mucilage of acacia, tragacanth, karaya,
or other gums. Glycerin is quite often present.
In making a survey of these products, the writer
tried first the method suggested by Redfern1 which
was found to be quite unsatisfactory; first, because
the procedure of precipitating the gum from 25 cc.
of the sample with 25 cc. of 05 per cent alcohol and
filtering through a Gooch into a 100 cc. flask and
making up to the mark was too tedious and time-
consuming; and second, because the writer did not
in this case, and never has been able to obtain con-
cordant results by the method of Howard- to which
Redfern refers. Indeed this method is even less
adaptable to the non-alcoholic extracts than to the
ordinary alcoholic extracts, for the reason that the
former contain, in a number of cases, as much as four
times more oil than the strictly standard alcoholic
extracts and there is always danger, if not certainty,
of losing oil through volatilization when from 10 to
20 per cent is present .
Taking advantage of the fact that many gums arc
precipitated by lead subacetate, the following pro
cedure was tried: 5 CC. of the emulsion were diluted
with 20 cc water and transferred to a Babcock milk
■ This Iouknal. 8 (1916) 1 N
1 lm. Chem. Soc, 30 (1908), 608.
S3«
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING ( HEMISTRY Vol. 10, No. 7
bottle and the gum precipitated by lead subacetate
and centrifuged. The precipitated gum came to the
top and the volume of oil could not be read. This
was then modified by adding chloroform to absorb
the oil after precipitation of the gum. On centrifuging
this mixture the gum precipitate settled to the bottom
of the bottle with the chloroform, and upon decanting
the supernatant liquid, adding ether, and heating to
expel the chloroform as recommended by Howard
and then diluting with water and centrifuging, the
gum precipitate came to b the oil and again
interfered with the reading of the volume of the oil.
Finally the following method which consists simply
of making an alcoholic extract from the emulsion and
proceeding according to the official method1 was
found to give satisfactory and concordant results for
tin lemon and orange extracts.
METHOD
Measure 10 cc. of the emulsion into a graduated cylinder,
transfer as much as possible to a 50 ee. flask, rinse the cylinder
with 10 cc. portions of 95 per cent alcohol, and with the aid of
a glass rod transfer all of the emulsion and precipitated gum
to the flask, rill to the mark, shake thoroughly, let stand about
30 min. Filter through a folded filter and determine the oil
in a 20 cc. portion of the filtrate by the official method.1 The
per cent of oil found in the filtrate is multiplied by 5 to give
the pur cent of oil in the original emulsion.
The gum is completely precipitated and it is more
expeditious to throw down the gum in the volumetric
flask and to make up to volume and use an aliquot
mi the filtrate than to precipitate the gum and at-
tem] wash the oil from it into the flask, ft is
possible to pipette the aliquot directly from the flask,
but as the precipitated gum gathers at the shoulder
of the flask and frequently stops the outlet of the pipette
this procedure offers little advantage over filtering,
as it is not necessary to avoid transferring the gum to
the filter.
In the case of extracts containing less than 5 per
cent oil it is necessary to use more sample than speci-
fied in the directions given.
Non-alcoholic extracts of lemon and orange contain-
ing 10 per cent of the respective oils were prepared
e 1 ording to the formula
Essential oil 20 cc.
TraSacanth 3 g.
Glycerin 40 cc.
Water, q. s 200 cc.
I he results obtained on these extracts are given in
Table I. Results obtained on co : non-alcoholic
extract ai e al ti i given.
Table I
iif rcial Exti i.i -
Oil Found
Pel * i ii i
7.0
17 cl
15.0
14 0
6 S
7.5
19.0
19 5
.'.l ll
Preps
Strength < til Pound
cenl Pel cenl
Orange 10 10
HI 10
10
io 10
I .,,!.„, io 10
Lemon 10 9 5
Lemon 10 1"
I. cm, mi
Lemon . .
Lemon
quite accurate results could be obtained by ordinary
steam distillation.
It is necessary first to run blank experiments on
pure oils to determine just what percentage of re-
covery can be accomplished with the particular ap-
paratus at hand.
Using a 200 cc. side-neck distilling flask with outlet
tube midway of the neck and a cassia flask as receiver,
the writer has consistently recovered 95 per cent of
lemon and orange oils when proceeding as follows:
Measure 10 cc. of the extract into a graduated cylinder and
transfer it by means of about 35 cc. water to a side-neck dis-
tilling flask and distil with steam into a 100 cc. cassia flask. In
the case of lemon and orange oils 95 per cent of the oil is re-
covered so that the amount found must be multiplied by 100
and divided by 95.
Table II gives the results obtained by steam dis-
tillation on the 10 per cent extracts described above.
Table
II
Strength
Per cenl
10
. . 10
Oil Found
Per cent
10.0
9.5
10
10
10
.. 10
9.7
10.0
10.0
9.5
Por cassia, cinnamon, and clove extracts, the fol-
lowing modification of the official method1 is suc-
cessful.
Dilute 10 cc. of the sample with 95 per cent alcohol to 50 cc.
as in the case of lemon and orange. Filter. Place 10 cc. of
the filtrate in a separators- funnel containing 50 cc. water, add
1 cc. HC1 (1 : 1), and shake out 4 times with 25 cc. portions
of ether. Wash the cotnl lined ether extracts twice with water
and then shake for a few minutes with about 5 g. granular
calcium chloride
Place a small piece of cotton in the outlet of the separators'
funnel and draw the ether into a tared beaker. Evaporate
the ether on a boiling water bath, place in desiccator for 3 min.
and weigh; divide the weight by the specific gravity of the oil
to find the per cent of oil by volume.
Table III gives the results on cassia, cinnamon and
clove extracts containing 10 per cent of the respective
oils and prepared according to the formula given under
lemon and orange. Results on commercial extracts
are also given.
Table III
Commercial Kxtracts
Found
Per cent
13.5
12. -I
Prepared Hxtracts
Strength
Found
Pel eent
Per cent
Cassia
10
9.83
Cassia
10
9.90
10
Cinnamon
. 10
9.90
Cinnamon
10
9.96
i Lnnamon
10
9.90
Clove
Hi
10.0
Clove
10
9.89
Clove
10
9.95
Almond, anise, and nutmeg extracts of the non-
alcoholic type are converted into alcoholic extracts
as in the case of lemon and orange and an aliquot
portion analyzed by the official methods.2
PEPPERMIN 1 I \ 1 K IC 1
A standard extract was made up containing 10
per cent peppermint oil by the formula given under
lemon and orange. 10 cc. of this were made up to
□ Redfern's statement it was found that
' "Re 1 ol I 01 \i thod "
■ "Report of Com. on Methods of Analysis,
/, l.O. A.t P >"
July, i9i8 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
for only i min.
per cent oil found.
for only 45 sec.,
50 cc. with 95 per cent alcohol, filtered, and an attempt
made to assay the nitrate by the official method1
with the following results. These results are cal-
culated to the original extract.
1 — Following the method as given, 2 per cent of
oils found.
2 — Heating was carried on
(shaking at 15 sec. intervals), 8
3 — Heating was continued
S per cent oil found.
4 — Heating was continued for only 20 sec, n
per cent oil found.
5 — Heating was continued for 25 sec, 8 per cent oil
found.
6 — Heating was continued for 20 sec. and then the
suction was continued for an additional 15 sec
without heat, 9 per cent oil found.
7 — Heating was continued for 20 sec and the
suction for an additional 10 sec. without heat, 9 per
cent oil found.
The writer's experience with this method has been
most unsatisfactory, even moderate agreement in
duplicate determinations has never been attained.
The method leaves too much to chance. If the flask
is not disconnected from the suction the instant the
last of the solvent is drawn off, there is a loss of oil,
and we have not been able to discover any means
whereby we can be assured when this instant is at
hand.
Steam distillation gives very good results for pepper-
mint if one determines beforehand what per cent of
oil can be recovered with the apparatus in blank
experiments using known quantities of pure oil. The
writer has found this recovery to be 90 per cent, so
that the quantity of oil found is multiplied by 100
and divided by 90 to find the amount present in the
extract.
Proceeding according to the directions given for
lemon and orange extracts for steam distillation the
following results were obtained on a 10 per cent non-
alcoholic extract and on commercial extracts.
Table IV
Percent
Peppermint 10
Peppermint 10
Peppermint 10
Chemical Laboratories
McCormick and Company
Baltimore, Maryland
Per cent
10
9.8
lercial Extracts
Per cent
II. 0
12.8
7.2
A CONTRIBUTION TO THE COMPOSITION OF LIME-
SULFUR SOLUTIONS2
By O. B. Winter
Received April 19, 1918
The principal constituents of lime-sulfur solutions
are calcium polysulfides and calcium thiosulfate.
Small amounts of calcium sulfate and possibly of
calcium sulfite are also present, and the claim has been
made that the solutions may contain other com-
pounds such as hydrogen sulfide, calcium hydrosul-
1 "Report of Com. on Methods of Analysis," J. A. 0. A. C, p. 268.
s This work was done in the chemical laboratory of the Michigan
Agricultural College Experiment Station and the results arc publish' I "i
the permission of the Director.
539
fide, calcium hydroxyhydrosulfide, different calcium
oxysulfides, free lime, and free sulfur. How much of
each of these compounds is liable to be present? It
is the purpose of this paper to discuss some of the work
done in this laboratory which pertains to the above
question.
HYDROGEN SULFIDE, H2S. CALCIUM HYDROS ULFIDE ,
Ca(SH)2. CALCIUM HYDROXYHYDROSULFIDE,
CaSHOH
In reviewing the literature on the composition of
lime-sulfur spray, it is interesting to note the discus-
sions on the theoretical composition of the solution,
together with the absence (except in a few articles) of
even an attempt to prove the existence of certain of
the compounds discussed. Divers and Shimidzu1
give detailed methods for preparing some of the above-
mentioned compounds and state some of their proper-
ties, but their work has nothing whatever to do with
an ordinary lime-sulfur solution. Roark2 discusses
the possible existence of these compounds in a lime-
sulfur solution, but does not give experimental proof
of their presence. Tartar and Bradley3 conclude that
they are not present in appreciable amounts. Thomp-
son and Whittier4 claim the presence of hydrosulfide
sulfur and give experimental data which they believe
justifies their claim. Green6 says, "We have, how-
ever, never been able to detect definitely the presence
of hydrosulfide or free sulfuretted hydrogen in lime-
sulfur solutions."
It may be possible to prepare a lime-sulfur solution
which contains hydrogen sulfide, calcium hydrosul-
fide, or calcium hydroxyhydrosulfide, but it has yet
to be shown conclusively that any of these compounds
are present in appreciable quantities in a "straight"6
lime-sulfur solution either as a result of the prepara-
tion of the solution, or of hydrolysis or other action
taking place during storage under normal conditions.
It is also interesting to note that writers seem to have
different opinions regarding the chemical actions which
take place in lime-sulfur solutions, and for this reason
literature is quite confusing in regard to the formation
of any of the above-mentioned compounds. For ex-
ample, the action of water on a polysulfide is repre-
sented as follows by different chemists:
Divers and Shimidzu:7
CaS5 + 2H20 = Ca(SH)(OH) + 3S + HSS + 0
Ca(SH)(OH) + 202 + H2S = CaS203 + 2Ha0
Auld:8
CaS* + 2H,0 = Ca(0H)2 + H2S»
H2SX = H2S + (*— i)S
Roark:7
zCaSx -h 2H20 = Ca(SH)2 + Ca(OH), + 2S«_,
■ J. Chan. Soc, 45 (1884), 270-91.
'J. A. O. A C, [1| 1 (1915), 81.
" This Journal, 2 (1910), 271-7.
• Delaware Agricultural College Experiment Station, Bull. 105 (1914), 8.
' Union of S. Africa Dcpt. of Agr.. 3rd and 4th Report of the Director
of Vet Research, 1915, p. 179.
» Hy a "straight" lime sulfur solution is meant a solution prepared from
ordinary commercial lime and sulfur to which no foreinn substance has been
added, and which has stn,,<l lot several days
' hoc. ■ il
I III m Sot . [1 I 107 | 191 J), 18 !
I 111. JOURNAL OF INDUSTRIAL AND ENGINEERING < HEMISTRY Vol. 10. No. 7
Ca(SH). + H20 = Ca SH OH) • H -
also CaS5 + 2H,0 = Ci OKI i! r- 4S
itt:1 Up to a certain dilution no decompi
takes place when freshly boiled; distilled water is
added to a lime-sulfur solution.
A similar disagreement might be given for many
of the other reactions which are supposed to take
place in boiling, storing, or diluting a lime-sulfur
solution.
Experiments in this laboratory show that any one
of the compounds mentioned above containing the
SH radical) may be detected by titrating an aliquot
of the solution with standard iodine, determining the
end-point by the disappearance of the yellow color,
and by titrating an equal aliquot with the same solu-
tion determining the end-point with nitroprusside2 of
sodium. When the polysulfide has been entirely
decomposed the solution loses the yellow color, while
the blue color of the nitroprusside of sodium remains
as long as there is any sulfur present either in the form
of a sulfide or in the form of any compound contain-
ing the (SH) radical. If the two above titrations
agree, none of the above-mentioned compounds are
present. The following two eqtiations represent the
reactions which undoubtedly take place:
CaS* + Ca(SH). + H,S + I; =
Cal2 + Ca(SH)2 + H:S + S* (Titrated to dis-
appearance of yellow color)
CaSx + Ca(SH)j + H2S + 4I2 =
2CaI2 + S(I+3) + 4HI (Titrated with nitroprus-
side of sodium as indicator)
One might anticipate that the difference between
the two titrations would be a measure of the amount
of sulfur present other than sulfides, but we have
not been able to prove this since the color end-point
in the presence of a considerable quantity of a com-
pound containing the (SH) radical does not appear
sharp. However, the method is sufficiently accurate
to show the presence or absence of any of these com-
pounds.
It might be well to state here that other experiments
have shown that when compounds containing the
(SH) radical are present in a solution, an aliquot
titrated with standard zinc chloride, using nickel
sulfate as indicator, is higher than one titrated with
standard hydrochloric acid, using methyl orange as
indicator. This may be explained by the following
ions:
1 • 3ZnCl: =
Clj + ZnSv + 2ZnS + 2HCI
CaS, + Ca(SH)s + 4HCI = zCaCU + jH,S + Ss_,
If any of the compounds referred to above are
formed in an ordinary lime-sulfur solution, they must
1 J. A. 0. A. C, [II 1 1 1913
In titrating with nitroprusside of sodium .is .tn indicator for sulfur
compounds, it is essential thai the indicator should noi be added until tlu-
end poinl is practical!) reached since if the blue color is well developed n
is almost impossibli i" change back u> .1 colorless solution. If necessary.
a fiu extra samples should be titrated, and those with the persisting color
discarded
be unstable in the presence of other existing com-
pounds, since the two iodine titrations mentioned in
a preceding paragraph agree in every "straight"
lime-sulfur solution that has been tested in this labora-
tory, whether prepared with an excess of lime or sulfur,
whether freshly boiled or of long standing, and whether
concentrated or dilute. Therefore we believe that
none of the above-mentioned compounds exist in ap-
preciable quantities in a "straight" lime-sulfur solu-
tion; and vice versa, if the spray contains any of these
compounds, which can easily be detected, it is not
a "straight" lime-sulfur solution.
FREE LIME
Roark' makes the statement that "While not more
than a trace of calcium hydroxide [CaiOH)3] may
be present in a freshly prepared lime-sulfur solution,
it is formed in appreciable amounts upon dilution,
according to the reaction
- 2H;0 = Ca(.OH), + H2S
and would be present, therefore, in lime-sulfur solu-
tions which had stood for some time and become
partially decomposed." He gives no proof of its
actual existence. Thompson and Whittier- claim
that. "Free calcium hydroxide may occur either from
simple solution, where an excess of lime has been used,
or it may result from hydrolysis of the polysulfide."
They found "free lime present when the ratio of lime
to sulfur exceeded a certain definite figure, increasing
in amount as this ratio increased until the limit of
the solubility of calcium hydroxide was reached."
They say nothing about how long the solutions in which
they found free lime had stood before making the
analyses, and show no data to prove the statement
that "free lime may result from the hydrolysis of the
polysulfide." Tartar and Bradley3 reported that
no free lime or only a trace was found by them in
lime-sulfur solutions. They say, "It appears that if
there is hydroxide in the freshly prepared solution it
either unites with some of the sulfur already in com-
bination to form more polysulfide. or it unites directly
with the polysulfide to form oxysulfides which crys-
tallize out of the more concentrated solutions."
Chapm* says. "If originally made with an es
lime or if not boiled long enough, excess of lir.
first present in solution, but if such a preparation be
allowed to stand quietly and cool off in the cooking
vat, the indications are that the undissolved lime soon
■set lies down, while the small amount of dissolved
lime rapidly reacts with polysulfide according to equa-
tion
iol"aS. - ;C ' Ml i :i\.S • H "
so that in this case also, unless the cooled solution is
again stirred up with the sediment, a plus r<
figure can never be present in the end*' — in other
words, no free lime can be present. GreenJ claims
t Lo,
1 Delaware Agricultural College Exp - 105 I), 11
i This Jodrnai I
' U. S Dept. of Agr., Bull. Ml 1916 13
1 ii ,.i S Africa Dept. of Awr Srd and 4th Report of the Directca
of Vet Research, 191S. p. 180.
July, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY 54i
that a trace of free lime is usually present but that the were freshly prepared from materials containing an
amount is very small. excess of sulfur. (2) That Method I shows no free
In view of the above apparent differences of opin- lime or only a trace in the commercial concentrates
ion, an attempt was made to prove either the pres- which had stood from one to ten years, some of which
ence or absence of free lime in an ordinary lime-sulfur had undergone considerable oxidation, whereas Method
solution. II shows its presence in all of these samples. (3)
Two different methods have been used by analysts That both methods show free lime in Sample I, which
for determining the amount of free lime in a lime- had been recently prepared from materials eontain-
sulfur solution. The one (Method I)1 is by titrating ing an excess of lime, but that Method II shows the
with 0.1 N hydrochloric acid, using methyl orange larger amount. (4) That Method I shows very little
as indicator, and with 0.1 N ammoniacal zinc chloride free lime in Sample J (Sample I after standing two
solution using nickel sulfate as an outside indicator. 4ays), whereas Method II shows more than when first
In this method, the hydrochloric acid titration indi- prepared. (5) That when a given amount of free
cates the lime combined with sulfur as polysulfides lime was added to a sample in which neither method
plus the free lime, while the zinc chloride titration in- indicated its presence, making Sample K, Method I
dicates only the former. The difference between the shows nearly all that was added, while Method II
two titrations is a measure of the free lime. The shows slightly more than the amount added. (6)
other (Method II)2 is by removing the free lime as That while Method I shows no free lime in Sample L
calcium sulfate by means of magnesium sulfate solu- (Sample A after having been exposed to the air for
tion (the magnesium being precipitated as magnesium several hours and oxidation had begun), Method II
hydroxide and filtered out). The solution is titrated shows its presence.
with standard acid before and after the removal of From the above data it is evident that the two
the free lime. The difference between the two acid methods do not agree. Which is correct? When
titrations is held by the authors to be a measure of we consider the known facts that hydrochloric acid
the free lime. The results recorded in Table I were reacts with calcium polysulfides and calcium hydroxide
obtained by these two methods on 10 cc. of lime-sulfur as follows:
concentrates diluted to 200 cc, of which 10 cc. were CaS 4- ^HCl = CaCU + H->S 4- S
taken for analysis: Ca(OH)! + 2HCI = CaCl2 + 2H20;
Table I
^-0 1 /v^HCi'-i11 ' that ammoniacal zinc chloride reacts with calcium
, , . Before After polysulfide according to the equation
. Method I , adding adding r J
Sample 0.I.VHC1 O.IA'ZnCl: CaO MgSOi MgSOi CaO
no. cc. cc. g. Co. cc. g. CaSx + ZnCl2 = ZnS.v + CaCl2;
A 8.60 8.65 0.0000 8.60 8.60 0.0000
b 8.40 8.40 o.oooo 8.40 8.35 o.oooi and that in the presence of ammonium chloride, am-
C 40.35 40.25 0.0003 40.35 37.90 0.0069 ^
D 12.65 12.65 o.oooo 12.65 n.90 0.0021 moniacal zinc chloride does not react with calcium
E 18.38 18.40 0.0000 18.38 18.30 0.0002 , ... ,, . ... .. ,
f 17.98 17.96 o.oooo 17.98 17.65 o.ooo9 hvdroxide, it seems impossible that titrations made
G 17.43 17.48 0.0000 17.43 17.00 0.0012 .... , , ,, ■ •, j ■ ,, ■■, ,j
h... . 12.80 u.82 o.oooo 12.80 12.08 o.oo20 with hydrochloric acid and zinc chloride could agree
) g-fg |||g gjjg^ 'IM \\ l°5 %■%$* in the presence of free lime. Further, when free lime
i i T84o a.w o oooo '8.40 loo o.'ooii was added to a lime-sulfur solution, it was practically
all accounted for by the difference between the above-
In explanation of the above table, it may be well mentioned titrations immediately after the addition,
to state that Samples A and B were prepared in the Therefore 'the author contends that Method I is ac-
laboratory using an excess of sulfur and were analyzed curate for determining free lime in a lime-sulfur solu-
soon after their preparation. Samples C to H, in- ^ n
elusive, were commercial concentrates which had stood gince Method I, as given above, has been noted in
in the laboratory from one to ten years, of which some literature and has been shown to be accurate, it seemed
had previously been opened for analysis and a large worth while t0 investigate Method II more thoroughly,
amount of oxidation products had formed. Sample Concerning this method Thompson and Whittier1
I was prepared in the laboratory using an excess of state that when magnesium sulfate is added to a
lime and analyzed immediately after its preparation. iime-sulfur solution containing free calcium hydroxide.
Sample J was the same as Sample I, except that the magnesium hydroxide is precipitated quantitatively
analysis was made two days after its preparation. ai,d calcium sulfate formed, thus neutralizing the solu-
Sample K was the same as Sample A, except that tion and afforciing a method for determining the free
0.0062 g. of calcium oxide had been added in the Hme From othl.r sources in literature, it is well
form of lime water in diluting to 200 cc. Sample L known that magnesium hydroxide is precipitated when
was the same as Sample A after it had been standing, g soilHion 0f calcium hydroxide is treated with mag-
osed to the air, for several hours, and oxidation had llesium sulfate. However, this reaction is hardly
begun. From a study of this table it will be noted: considered sufficiently complete for quantitative de-
(i) That neither of the two methods show an apprecia- terminations, and too, magnesium'-' salts react with
ble amount of free lime in Samples A and B, which sulfides as follows:
1 Tais Journal, 1 (1910), 273. 1 Delawan Lgricu 'I ( ollegi Bxpt. Sta., Bull 105 (1914), 11.
1 Delaware Agricultural College Kxpt. Sta., Hull. 108 (1914), 11. ' j Mineon, "Quel Chem Anal ," mi. Ed (1904), p. 215.
542
I 111. JOl RNAL OF INDUSTRIAL AND ENGINEERING ( HEMISTRY Vol. 10, No. 7
MgS0< +2.\a,S + 2H20 =
Mg(OH), + NasSO< + zNaSH
Divers and Shimidzu, in an article on "Magnesium
Hydrosulfide Solution and Its Use in Chemico-Legal
Cases as a Source of Hydrogen Sulfide,"1 state that,
"The poly(-penta)sulfide that may be in solution is
only very slightly decomposed even at boiling heat,"
thus indicating that the polysulfide of magnesium is a
stable compound. Therefore, it appears possible that
when a lime-sulfur solution is treated with magnesium
sulfate, chemical action may take place even if there
is no free lime present.
In order to throw more light on the above question,
the precipitate which came down on adding magnesium
sulfate was tested for the presence of sulfur, and was
found to contain a small amount. This would indi-
cate that the magnesium sulfate acted on some sulfur
compound. However, the precipitate was amorphous
and it seemed possible that some of the lime-sulfur
solution might have been occluded. Therefore the
test was not considered conclusive. The samples
of concentrates which formed a precipitate with mag-
nesium sulfate were diluted for analyses, with and
without the addition of magnesium sulfate. Some of
these were titrated for monosulfide and thiosulfate
sulfur with standard iodine solution determining the
end-point by disappearance of color and also by the
use of nitroprusside of sodium. The following re-
sults were obtained:
Table II
I for Monosulfide I for Thiosulfate
—With MgSOi^ -—Without MgSO(^ After After
Color- Sodium Color- Sodium Titra- Titra-
less Solu- Nitro- less Solu- Nitro- ting Col- ting Col-
Soln. tion prusside tion prusside umn 3 umn 5
No. Cc. Cc. Cc. Cc. Ppt. Cc. Cc.
1... 8.14 8.32 8.50 8.52 Very little 7.05 7.05
7.05 Lost
2... 25.60 26.35 27.63 27.63 Much
These data show that when magnesium sulfate are
added to lime-sulfur solutions, some compound is
formed which causes a blue color with nitroprusside
of sodium after the polysulfides have been decom-
posed and the solution has become colorless; and that
the thiosulfate content remains the same. Since the
solution is colorless but reacts with nitroprusside of
sodium, it apparently contains a compound having
the (SH) radical, e. g., hydrogen sulfide, calcium
hydrosulfide, calcium hydroxyhydrosulfide, or the
eorresponding salts of magnesium.
Other: i pared solutions were titrated with
hydrochloric acid ami with zinc chloride, and the
folli >\\ ing i . tied :
Table III
With MsSO, With..., i
0 .11V 0.1 .V 0. 1 A
I1C1 ZnCli HC1 ZnCl.
No. I Cc. Cc.
I> 11.90 12.12 12.65 12.65
E 18.30 18.40 18.38 18.40
F. ....... 65 17.70 17.98 17.96
G 17.00 17.20 17.43 1748
H 12.08 12.40 12.80 1
These data show that the titration of the treated
sample with standard hydr< d is lower than
thai of tli<' untreated. Thi he loss of some
calcium compound. It also shows that the titra
tion of the treated sample with ammoniacal zinc
1 J. Chrm. Soc, 46 (1884), 699.
chloride is slightly higher than with hydrochloric
acid. This also is significant. It indicates the forma-
tion of some new compound, and this compound must
contain the (SH) radical.
The io cc. aliquots of a lime-sulfur solution which
indicated no free lime by Method II were placed in
each of two ioo cc. graduated flasks. One of these
(a) was diluted to the mark with freshly boiled dis-
tilled water, and to the other (b) was added a large
excess of io per cent magnesium sulfate solution and
then also diluted to the mark with freshly boiled
distilled water. Both solutions were allowed to stand
about 12 hrs. The former remained perfectly
clear, as was anticipated; the latter also remained
clear for several minutes, then gradually became
cloudy and by the end of the i 2 hrs. a large number
of crystals had formed, which, on examination, under a
polarizing microscope, were readily identified as cal-
cium sulfate (CaSOj.2H:0). These solutions were
then analyzed and the following results were ob-
tained:
Table IV
Mono-S MISHh-S Thio-S Sulfide-S CaO
Sample Gram Gram Gram Gram Gram
a 0.0302 0.0000 0.0330 0.1505 0.0813
b 0.0279 0.0012 0 0333 0.1377 0.0154
In the above table the samples were titrated with
iodine to the end-point determined by disappearance
of color and also to the end-point determined by nitro-
prusside of sodium, and the difference between these
two titrations was considered as sulfur in the form
of compounds containing the (SK) radical and is indi-
cated as M(SH)»-S. The results in this table show
that there was a slight loss in the monosulfide equiva-
lent and in the polysulfide sulfur; that the thiosulfate
sulfur remained practically the same; that a small
amount of some compound containing the (SH)
radical was formed; and that there was a loss of about
8i per cent of the lime. In other words, they show that
a large amount of calcium had disappeared while the
loss in the monosulfide equivalent, thiosulfate. and
sulfide sulfur were comparatively small. A micro-
scopic examination showed conclusively that calcium
sulfate was precipitated from the solutions. Xow
the following calculations may be made:
0.0333 X ,. = 0.0291 g. CaO necessary to combine with 0.0333 g.
64
S in Thio-S
0.0279 X = 0.0488 g. CaO necessary to combine with 0.0279 g.
S in Mono-S.
Total. . 0.0779.g. CaO
From these it will be seen that there should be
°-°7 79 S- oi CaO in the solution, while there are only
0.0154 g. by actual determination. Evidently mag-
nesium has replaced some of the calcium, and the solu-
tion now also contains magnesium polysulfide and a
small quantity of some compound containing tlu SH
radical. These compounds were not present in the
original solution and must have been formed by the
■nn sulfate. It will also be
length of time the solution is allowed to
stand and the quantity of magnesium sulfate •
are important factors in this reaction. And it ap-
pears that the lower polysulfides, or possibly the oxy-
July, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
sulfides of calcium are acted on more readily than the
higher polysulfides, since solutions prepared by using
an excess of lime in which lower polysulfides and possi-
bly oxysulfides are present, react more quickly and
with a less concentrated solution of magnesium sul-
fate than do those in which an excess of sulfur is used
and only the higher polysulfides are present. From
these data as well as those in Tables I, II and III, we
must conclude that magnesium sulfate reacts with
some compound in a lime-sulfur solution other than
free lime, and in some solutions, at least, this com-
pound is calcium polysulfide. Therefore Method II
cannot be considered accurate for determining free
lime in a lime-sulfur solution.
Having presented evidence which we believe is
sufficient to show that Method I is an accurate measure
of the free lime in a lime-sulfur solution, and that
Method II cannot be considered accurate for this
work, a few more solutions were prepared using differ-
ent proportions of lime and sulfur, and a few more
concentrates were diluted with lime water. These
were analyzed by the former method, some imme-
diately and some after standing several days. The
results, together with explanatory remarks, are found
in Table V:
Table V
A710
Sample HC1
No. Cc.
20.17
20.15
29.90
30.00
20.17
20.15
29.50
30.00
CaO
0.0000
0.0000
0.0011
0.0000
Remarks
S : CaO = 3:1. Analyzed im-
mediately after boiling
Same as 1 after standing well
stoppered for three days
S : CaO =1:1. Analyzed im-
mediately after boiling
Same as 3 after standing well
stoppered for three days
Sample K in Table I
Same as 5 after standing well
stoppered for three days
Commercial concentrate diluted
with lime water (0.0106 g.
CaO)
Same as 7 after standing exposed
to air for fourteen days
The results in Table V, similar to those in Table I,
are in accord with the contention that free lime is
present in a freshly boiled lime-sulfur solution pre-
pared by using an excess of lime, but they are con-
trary to the contention that free lime will remain in
such a solution or that it is formed by hydrolysis.
The only conclusions that can be drawn from the two
tables are that the small amount of free lime which
may be present immediately after preparing a lime-
sulfur solution, gradually disappears on standing,
and that immediately after adding free lime to a
lime-sulfur solution nearly all the lime exists in the
free state, but that chemical action takes place slowly,
and after some time all the free lime has entered into
chemical combination. Therefore, the inference is
that the ordinary commercial lime-sulfur solution,
either concentrated or dilute, does not contain an ap-
preciable amount of free lime.
FREK SULFI'K
Thompson and Whittier1 show that the residue
which separates from a lime-sulfur solution prepared
with an excess of sulfur in an atmosphere of nitrogen,
filtered while hot and kept in a completely filled, tightly
1 Delaware Agricultural College Expt. Sta., Hull. 106 (1914), 20.
stoppered receptacle, is mainly free sulfur. Auld1
mentions the fact that when a lime-sulfur solution was
prepared in an atmosphere of nitrogen and an excess
of sulfur was used, a polysulfide was formed which
analyzed to be the pentasulfide or slightly higher,
and that on standing free sulfur separated out. He
believes that sulfur may exist as free sulfur in solu-
tion. Harris2 prepared the pentasulfide by simply
using a reflux condenser, and free sulfur crystals were
found by the author in some of his solutions after
they had stood several years. Tartar and Bradley3
succeeded in extracting free sulfur from a lime-sulfur
solution and found that the quantity extracted grad-
ually decreased with the increase of the time of ex-
traction, but found no definite end-point. Ramsey4
contends that the so-called polysulfide sulfur is loosely
combined and that free sulfur exists in the solution.
Green5 says, "We regard our data as effectually dis-
posing of the contentions both of Auld and Ramsey in
regard to loosely attached sulfur, and sulfur in solu-
tion." He believes that the polysulfide sulfur is
firmly combined and that there is no free sulfur in
solution. Thompson and Whittier conclude from
their work that no sulfide lower than the pentasulfide
is formed and that free sulfur is held in solution.
During the progress of this investigation samples
were prepared with and without the use of a reflux
condenser, using an excess of sulfur. Those with the
condenser approximated the pentasulfide, while those
without were lower. In both cases, when the solu-
tions were filtered while hot into flasks which were
completely filled and well stoppered and the solutions
allowed to cool, crystals which proved to be free
sulfur separated out. Even when allowed to cool
before filtering and then kept as mentioned above,
free sulfur separated out of the more concentrated
solutions.
Table VI gives the results of complete analyses on
a solution prepared from materials containing an ex-
cess of sulfur and kept the lengths of time indicated.
The analyses were made on 10 cc. aliquots of the
diluted concentrate.
Table VI
Time of Sulfur Total Ratio
Soln. stand- Crys- Mono-S Thio-S S-S Total-S CaO S-S :
No. ing tals Gram Gram Gram Gram Gram Mono-S
I A(a).. Still None 0.0441 0.0430 0.2153 0.2620 0.1188 1 :4.88
IB. . 12 hrs. Few 0.0445 0.0492 0.2148 0.2639 0.1212 1:4.83
1C 32days Many 0.0444 0.0496 0.2110 0.2606 0.1211 1:4.76
(«) This solution was less concentrated than the other two because it
had not cooled.
This table shows a loss in sulfur from the solution,
and the loss lies in the polysulfide sulfur. The fact
that before the deposition of the sulfur, the ratio of
the sulfide sulfur to the monosulfide sulfur was less
than 5, and that as more sulfur was deposited this
ratio was lowered, makes it appear that the free sulfur
deposited in these solutions probably came from the
breaking down of the higher polysulfides and not from
free sulfur in solution. However, whether this ex-
1 .; ( hem, S01 . 107 (1915), 484.
mp 1, 1 , 1 ,,\ Bxp Sta Teeh. Bull. 6 (1911), 10.
; Tims Journal, 2 (1910), '. 1
1 ./. Agr. Sd . [2] 6 (1914), 194-201.
1 nion ,1 ifrica Dept. <>( AKr , ir.l and 4tn Report c,r the Directoi
„i Vet. Research, 1915. p. I1'.'.
544
TEE JOl RNAL 01 INDUSTRIAL AND ENGINEERING ( HEMISTRY Vol. 10, No.
planation is satisfactory or not, apparently makes
little difference, since free sulfur in such a solution
would undoubtedly have properties similar to those
of sulfur loosely combined, as in the case of the higher
polysulfides.
OXYSULFIDES OF CALCIUM
Most lime-sulfur investigators agree that when
lime and sulfur are boiled in water, with the lime in
excess of the ratio i : 2.28, and the solution is al-
lowed to stand in a closed vessel, certain oxysulfides
of calcium separate out. However, they do not agree
exactly as to the constitution of these compounds.
It has been suggested that they are not ordinary oxy-
sulfides1 as carbon oxysulfide COS, uranium oxysulfide
U202S, manganese oxysulfide Mn2OS, etc., but that
they are compounds made up of a calcium polysulfide
and calcium oxide; and that the chief difficulty in the
question of their composition is to determine what
polysulfide enters into their structure and whether
or not this polysulfide is constant.
Undoubtedly the most important evidence con-
cerning these oxysulfides has come from an investiga-
tion of the crystals themselves, even though the re-
sults of different analyses of these crystals do not
agree as well as might be desired. Considering the
facts that no solvent has been found by which the
crystals can be purified by recrystallization and that
they cannot even be washed entirely free from im-
purities, it is almost surprising to find that different
chemists agree as well as they do on their composi-
tion and properties. However, since there are the
:nentioned difficulties in dealing with the crys-
tals, it seemed advisable to compare the work done
along this line in this laboratory with that of others.
In doing this, lime-sulfur solutions were prepared by
taking one part of calcium oxide, one part of sulfur
and five parts of water, boiling without a reflux con-
denser until the escaping vapor showed the presence
of hydrogen sulfide, filtering while hot, and placing in
well-stoppered flasks, some of which were filled com-
pletely while others were only partially filled. In
all cases oranj lies separated, even when the
flasks were completely filled, showing that they were
not dependent on the oxygen of the air for their forma-
tion. (In the more dilute solutions crystals formed
only in the partially filled flasks.)
Several batches of these crystals were purifie.l by
separating them from the mother liquor by filtering
through hardened filter paper in a Gooch crucible,
washing a few times with small amounts of cold water
(io° C.)i a few times with small amounts of 95 per
cent alcohol, several times with absolute alcohol,
ether, carbon disulfide, and then with ether again.
They were dried in a vacuum desiccator over calcium
chloride.
The crystals purified as given above had an orange-
red color. They were found to be insoluble in and
her. petroleum ether, chloro-
form, carbon disulfide, carbon tetrachloride, pyridine,
ilute alcohol. They were decomposed by hot
Id water, forming a solution similar in appear-
1 Ann., 224 (1884), 178.
ance and reaction to a dilute lime sulfur solution, and
leaving a white, amorphous residue. When treated
with 95 per cent alcohol, pyridine containing water,
or with a small volume of cold water they were de-
composed, forming a solution similar to the above;
but some of the crystals retained their original shape,
losing only the orange-red color. On heating, the
crystals were gradually decomposed, leaving a white
substance which did not melt or burn. Under the
microscope the smaller crystals appeared like orange-
red four-sided prisms with parallel cleavage. Be-
tween crossed Nicols, the extinction appeared parallel
in one position and at an angle of about 30 ° in an-
other. The white amorphous residue, as well as the
white crystal-shaped masses which remained after
treating with cold water, was found to be calcium
oxide.
Samples of different batches of these crystals were
analyzed by treating with sodium hydroxide solution,
oxidizing with sodium peroxide, acidifying with hydro-
chloric acid, and then determining the total lime and
total sulfur in the usual manner. The results are
shown in Table VII:
TABLB VII
Total Total
Sample S Ca Ratio
No. Per cent Per cent S/Ca
1 20.92 28.28 1.34
2 20.75 27.11 1.27
3 22.09 28.77 1.28
4 21.83 25.47 1.17
5 21.08 25.11 1.19
6 20.70 27.30 1.31
Average 21.23 27.01 1.27
From the above results it is evident that the mole-
cules making up the crystals contain as many atoms
of sulfur as of calcium, since the theoretical ratio of
sulfur to calcium in such a molecule is 1.25, which is
almost identical with the average of the above de-
termined ratios.
On titrating several water solutions of the crystals
with standard iodine and comparing the end-point
determined by color with that determined with nitro-
prusside of sodium, it was found that the two end-
points were the same, showing the absence of the
(SH) radical, and therefore the absence of any of the
compounds containing this radical.
That lime is set free when the crystals are decom-
posed with cold water is shown by the following:
Two samples of crystals were shaken in flasks com-
pletely filled with freshly boiled distilled water until
decomposition was complete. The solutions were
then filtered and aliquots titrated with o. i N hydro-
chloric acid and with o.i N zinc chloride. The fol-
lowing results were obtained:
Tabus VTII
Souj. HC1 ZnCU CaO
N'o Cc. Gram
1 5.49 2.80 0.0075
16.04 7.95 0.0226
The genera] properties of these crystals seem to
indicate that they are the Herschell's1 crystals de-
scribed in the literature, and a partial analysis shows
that their percentage composition agrees with one of
the formulas given by Geuther:'
> Ann., Mi (1884), 181-192.
• Ibid
July, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
(2CaO.CaS3.nH2O)
as is shown by the following:
Table IX
Geuther's formula — 2CaO.CaS3.HH2O
Per cent
Per cent
-Theory
26.9
.. 27.01
21.6
21.23
Percentage composition-
It should be noted, however, that one property is
shown by the mother liquor from which the crystals
separate which is very difficult to explain if the crys-
tals in solution are considered as being composed of
calcium, oxide in combination with calcium polysulfide.
This is shown by the fact that when aliquots of such a
solution are titrated with standard hydrochloric
acid, standard zinc chloride, and standard iodine, the
three titrations agree. This will be seen in the fol-
lowing table where 10 cc. of lime-sulfur concentrates
containing the orange-red needles were diluted to
100 cc. with freshly boiled distilled water and 10 cc.
aliquots were titrated.
Table X
Sample 0. 1 N HCI 0. 1 N ZnCl: 0 1 N I
If the mother liquor from which the crystals separate
contains in solution a compound which has for its
formula 2CaO.CaS3.nH2O, it is difficult to explain
the above results, since hydrochloric acid, zinc chloride,
and iodine could hardly give equal titrations on a
solution containing the molecules mentioned. No
attempt to explain this will be made at this time, but
it should be emphasized that whatever the explana-
tion may be, the fact remains that the three titra-
tions do agree.
SUMMARY
I — Compounds containing the (SH) radical, as
hydrogen sulfide, calcium hydrosulfide, calcium hy-
droxyhydrosulfide, and the corresponding salts of
other metals, may be detected in a lime-sulfur solu-
tion by comparing the titration of the solution with
standard iodine to the disappearance of the yellow
color with that when the end-point is determined by
the use of nitroprusside of sodium.
II — A "straight" lime-sulfur solution does not con-
tain an appreciable amount of any of the above-men-
tioned compounds.
Ill — The difference between the titrations of a
"straight" lime-sulfur solution with standard hydro-
chloric acid and standard ammoniacal zinc chloride
is a measure of the free lime in the solution.
IV — When an excess of lime is used in the prepara-
tion of a lime-sulfur solution and the solution is freshly
prepared, or when recently diluted with lime-water, it
contains free lime; but on standing, the free lime
gradually disappears. Therefore an ordinary lime-
sulfur solution cannot contain free lime.
V — When magnesium sulfate is added to a lime-
sulfur solution the following may be noted: (1)
There is a slight decrease in the monosulfide sulfur
and the sulfide sulfur contents. (2) The thiosulfate
sulfur content remains practically constant. (3) The
magnesium replaces part of the calcium forming mag-
nesium polysulfide and under proper conditions cal-
cium sulfate crystallizes out. (4) A compound con-
taining the (SH) radical is formed.
VI — The magnesium sulfate method for deter-
mining free lime in a lime-sulfur solution is inaccurate.
VII — There appears to be no free sulfur in a lime-
sulfur solution, and the sulfur that separates out on
standing undoubtedly comes from the higher poly-
sulfides.
VIII — When a concentrated lime-sulfur solution is
prepared with an excess of lime, orange-red needles
separate out. The properties of these crystals indi-
cate that they are the same as those described in the
literature as Herschel's crystals, and as being com-
posed of calcium oxide combined with calcium poly-
sulfide. Their analysis agrees most closely with that
of Geuther, who gives for their formula the following:
2CaO.CaS3.nH2O. However, it seems improbable
that they exist in solution in the form indicated by
this formula.
ACKNOWLEDGMENT
This work was suggested by Prof. A. J. Patten of
this laboratory, and was carried out largely under
his direction. I wish to express my great apprecia-
tion for the. continued interest manifested throughout
and for his kind advice and criticism.
Michigan Agricultural College Experiment Station
East Lansing. Michigan
LABORATORY AND PLANT
A STANDARD APPARATUS FOR THE DETERMINATION
OF SULFUR IN IRON AND STEEL BY THE
EVOLUTION METHOD
By H. B. Pulsifer
Received April 3, 1918
While investigating the determination of sulfur
in iron and steel as briefly described in This Joikxai.. 8
(1916), 1 1 1 5, the author was led to make a fi
terminations by the evolution method. After the
several estimations with dilute acid, both diri
annealed, as recorded in the following columns, it
was decided to conclude the work with other scries
using concentrated hydrochloric acid.
The excellent results obtainable with hot concen-
trated acid have been reported almost since the in-
ception of the method nearly a hundred years ago;
but Williams,1 in 1892, was apparently the first one
to compare results and demonstrate that concentrated
acid would furnish far higher and more correct results
than dilute acid. During the years following, numer-
ous investigators,2 both American and European,
I J. Eng. Soc. West. Pcnn.. 8 (1892), 328.
i Schindler, Z. angew. Chcm , 6 (1893), 11; Schneider, Otslerr. Z. Berg.
41 (1893), 365; I'liillips. /, Am. Chem Sot . 17 (1895), 891;
,,,-Konlorcls Annaler, 60 (1905), 187; Schulte, SlaM »
(1906). 985; Kinder, Ibid., »B (1908). 249; Orthej / angew (hem.,
21 I 101 1359 ..mI 1393.
546
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 7
confirmed his conclusions and, going even further,
presented exhaustive data to show that quick solu-
tion in hot concentrated acid dissolved all ordinary
sulfides and evolved the sulfur as hydrogen sulfide
from all sorts of the ferrous alloys. In particular
the abundant formation of methyl sulfide generated
by dilute acid on materials of high combined carbon
was entirely overcome by dissolving in the hot con-
centrated acid. Several designed and used a form of
apparatus to return as much as possible of the dis-
tilled acid to the flask, thus maintaining the strength
of the solution until the action is complete. The un-
suttability of using rubber with the concentrated
acid has long been known so that the better types of
apparatus have been constructed wholly of glass.
Rubber stoppers in contact with hot concentrated
hydrochloric acid for 15 min. may easily evolve far
more sulfide than most irons contain, 5 g. being taken.
Most of the types of European apparatus appear-
ing rather impracticable and there being none at all
available in this country, Messrs. Kimer and Amend,
of New York, kindly attempted to construct a special
flask after the design shown in Fig. I. They were un-
able to make one without using a solid stopper and
increasing the ground joints from 3 to 8. The flask,
however, serves very well; it is seen set up in opera-
tion in Fig. II. Shortly afterwards Schaar & Com-
pany, of Chicago, were interested in the matter and
were able to procure several excellent units, after the
exact original design, from Japan. These flasks have
only the three ground joints and are highly satisfac-
tory. After making several hundred determina-
tions with the battery of three, one solid and two with
hollow stoppers, as indicated in Fig. Ill, the author has
no changes or alterations to make in the original de-
sign. If the large main stopper is kept slightly greased
it withstands the internal pressure perfectly yet is
easily removed with a slight twisting motion. With a
battery of 3 units one operator can continuously make
9 determinations per hour, including weighing out the
samples and titrating the results. With enough flasks
an operator and assistant ought to make more than
20 determinations an hour.
Fia. II
Arrangement of single flask showing hydrogen generator, wash bottles,
flask, and beaker of absorbent solution. The cooling water is led into the
coil through the tubes at the left.
As this type of apparatus and the results obtainable
are apparently slightly recognized in this country it
is thought worth while to again record the manner of
operation and the sort of results one gets. The
samples used were either those checked by other
methods or supplied by the Bureau of Standards.
With the reflux apparatus and using 40 cc. of hydro-
chloric acid (sp. gr. 1. 19) 5 g. of iron can be dissolved
and the solution held at gentle ebullition for 15 min.,
leaving the final solution of more than half its original
strength. The use of hydrogen to wash out the sul-
fide obviates vigorous boiling as commonly advoca-
ted. Thus at the end of the operation the acid is
considerably more concentrated than at the start
when 1 : 1 acid is used. Without the reflux only from
1 4 to ' 3 of the original acid may remain in the flask
at the end under the same heat influence. It is
naturally presumed that the hot concentrated acid
is responsible for the uniformly high results obtained.
The cooling coil in the neck of the flask assists in
holding back droplets of the solution which would
Otherwise carry ferrous chloride over into the absorb-
July, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
ing solution; for this reason the catch-bulb frequently
used has been omitted. The amount of iron carried
over varies greatly with the character of the dissolving
and the heat used. Using the hydrogen or carbon
dioxide stream ' to sweep out the hydrogen sulfide
there is evidently no advantage in heating to more
than the gentlest ebullition. Many measurements
showed from a trace to 5 mg. of iron carried over into
the ammoniacal cadmium chloride solution. With
only 0.01 mg. or less of iron carried over, as is usually
the case with this apparatus, the cadmium sulfide
precipitate is a clear lemon-yellow. From 0.02 to
0.05 mg. iron makes the precipitate darken to orange,
then becoming reddish with over 1 mg. iron. The
ferrous hydroxide present in this small amount quickly
oxidizes to ferric and takes no part in the subsequent
titration with iodine. As iodine is liberated from
iodide solution by both ferric salts and hydrochloric
acid the solution should not stand unduly after the
addition of the iodine and before the back titration
with thiosulfate. The author finds 2 min. ample to
effect the solution of the cadmium sulfide with the
strength of acid used; with longer standing iodine is
gradually liberated and the solutions turn blue again.
Permanganate and Oxalate
KMn
Ot per cc.
NaiC2(
KM
qO(
To color
(0.4717) (a)
0
3500
45
79
0
02
0
003607
0
3500
45
78
0
02
0
003608
0
3500
45
78
0
02
0
003608
0
3500
45
85
0
02
0
003602
0
3500
45
80
0
02
0
003606
Av„ 0.003606
u) Factor for changing weight of oxalate to weight of permanganate.
Permanganate and Thiosulfate
CMnO.
NasStOi
Ratio
15.51
49.91
0.3108
15.00
48.22
0.3111
15.04
48.30
0.3114
15.01
48.30
0.3108
15.00
48.21
0.3111
15.02
48.35
0.3107
14.97
48.11
0.3112
Av.
0.3110
Iodine and Thiosulfate
Iodine
Na;S:03
Ratio
49.82
47.10
1.058
49.80
47.21
1.055
49.62
47.08
1.054
49.91
47.22
1.057
49.76
47.11
1.056
49.80
47.22
1.055
49.78
47.19
1.055
1 cc. KMnO. is equivalent to 0.001829 g. S (factor = 0.5072).
1 cc. KMnO* is equivalent to 3.395 cc. iodine solution.
1 cc. iodine solution on 5 g. sample in percentage equals 0.01077 per
The standardization of the iodine solution is best
accomplished through a thiosulfate and permanganate
solution against standard sodium oxalate as supplied
by the Bureau of Standards. The author prefers
large bottles of all the reagents, in bulk from 20 to
50 liters, and made up some months in advance. If
preserved in the dark the solutions will alter so slowly
that checking once a week is sufficient. As illustra-
ting the precision and uniformity of the standardiza-
tion work contrasted with the unequal distribution
of sulfur in the metals, the above figures may be
presented. It will be noticed that the variations be-
tween individual measurements are of the order of
1 part in 1,000 in the standardizations, while on the
metal samples the sulfur content as measured by
repetition under identical conditions will quite likely
vary as much as 1 part in 5.
PROCEDURE
The procedure used on the following samples to ob-
tain the figures .in the last column, marked "Cone.
HC1," is as follows:
5 g- of the well-mixed sample are weighed on a watch-glass
to within 1 mg. and cautiously brushed into the flask so as not
to fall against the sides. 40 cc. of hydrochloric acid (sp. gr.
1 . 19) is poured into the upper bulb. The stopper is placed in
position. The absorbent solution is prepared by putting 300
cc. distilled water in a tall form of 500 cc. beaker; to this is added
20 cc. of ammonia (sp. gr. 0.90) and 10 cc. of ammoniacal cad-
mium chloride solution (300 g. CdCl2, 500 cc. ammonia (sp.
gr. 0.90) and 500 cc. distilled water). The exit tube is adjusted
in the beaker and a cover glass arranged as well as may be.
The cooling water is regulated.
Battery of three flasks with hydrogen generator and water and gas
connections. An analyst can maintain a rate of 9 determinations an hour
with three flasks.
Hydrogen from HC1 on zinc passed through alkaline KMu04
and a safety bottle is then let in to force the acid down on the
metal and the burner beneath is lighted. The burner has
previously been adjusted so that it will just keep the solution
in gentle ebullition. The stream of hydrogen may be passed
through continuously to the end or closed off during the peak
of the gas evolution. Within 5 or 10 mir . the sample will prob-
ably completely dissolve. If a series of bottles be substituted in
place of the single beaker the results will come no higher nor
will the slightest trace of a precipitate be found in the second
bottle. Inserting a wisp of glass wool in the beginning of the
exit tube will decrease the amount of iron passing over, but
will not influence the results.
At the end of 15 min. the flame is removed; the exit tube is
withdrawn from the beaker; the hydrogen is shut off; the stopper
is loosened and the coil washed down into the flask, after which
the stopper is hung on the side support (Fig. Ill) ready for the
next time; the outside of the exit tube is washed off into the
beaker and the flask emptied and rinsed ready for the next run.
With the iodine solution in the burette at a known mirk
and 10 cc. of starch solution added to the solution beneath,
50 cc. of concentrated hydrochloric acid are poured in and iodine
added to a strong permanent blue. Two minutes may be al-
lowed for the complete solution of the cadmium sulfide, after
which the blue color is discharged with the thiosulfate solution
If carbon dioxide is used as wash, one must add the hydro-
chloric acid with much care, especially if bicarbonate has separa-
ted and fallen to the bottom. This copious gas evolution, de-
S4«
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 7
laying the work and once in a while spoiling a run, is a serious
objection to the use of dioxide.
The separation of the figures into groups in the column under
"Cone. HO" results from runs made at different times, or from
variations in the method such as the use of dioxide, three ab-
sorbent bottles, filtering the cadmium sulfide, a filter of glass
wool, putting sulfates in the flask. Filtering the sulfide raises
the blank and increases the results; no justification for the
added uncertainty has been found.
Blanks arc carried out exactly as a determination omitting the
metal in the flask. They should be inserted often enough to
establish a uniform deduction from the total iodine. With the
materials used for nearly all of the author's work the blank was
between 0.20 and 0.40 cc.
The samples in the following sets of analyses have been
numbered to correspond with the work previously reported and
referred to in the opening paragraph. Numbers omitted could
not be investigated because of inadequate sample.
Sample 9 — Ship Plate
Sample 2 — Foundry Ir
T. C. = 3.45, G. C. = 3.23, Si
P = 0.78, Mn = 0.53
Nitric
Bamber
s Chloric
Dil. HC1
Cc
nc. HC
0.011
0.018
0.016
Direct
0.021
0.009
0.015
0.017
0.008
0.021
0.008
0.017
0.010
0.010
0.023
0.008
0.020
Av., 0.014
0.008
0.019
\v.
0.009
Also
0.005
0.004
0.007
Av., 0.018
0.007
Av., 0.008
Annealed
0.010
0.018
0.021
0.023
0.023
0.023
Av.
0.005
0.009
Av.,
0.021
Faster sol
0.010
0.003
0.008
0.002
Av., 0.009
0.004
Av.
0.003
Q
lick soln
0.002
0.002
0.003
Av.
0.002
Sample 3—
-"Vismera"
prom Inland Steel
Nitric
Bamber
s Chloric
Dil. HC1
Cone
. HC1
0.007
Not rut
0.012
Not run
0.034
0.031
0.009
0.018
0.034
0.033
0.012
Av., 0.015
0.033
0.030
Av.
0.009
Av.
0.033
0.036
0.034
0.034
0.034
0.034
0.033
0.032
0.033
0.034
0.037
0.033
0.036
0.029
0.029
0.031
0.029
0.032
Sample 4 — Foundry Iron
Nitric I
amber's
Chloric
Dil. 1IC1
Cc
nc. HCI
0.015
0.021
0.023
Direct
0.013
0.022
0.022
0.013
0.024
0.028 0.020
0.013
0.021 Av.
0.023
0.016
0.026
0.026 0.019
0.013 Av.
0.021
0.013
0.024
0.028 0.031
0.011
0.018
0.023
0 026 0.018
0.013
Av.
0.015
0.021
0.024
0.022 0.019
0.031 0.032
Annealed
0.023
0.032 0.020
0.014
0.032 0.022
0.015
0.022
Av.
0.015
Av.
Av.
0.023
0.028 0.022
0.026
Sample 5 — M
ld Steel
Nitric
Bamber's
Chloric
Di
. HCI
Cc
nc. HCI
0.017
0.021
0.015
Direct
0.049
0.021
0.019
0.016
0
021
0.034
0.017
0.019 A
v., 0.016
0
020
0.037
i., 0.018
0.021
0.020
Av., 0.
020
0.037
0.040
A
0 0 !0
Anne
0.
0.
Av., 0.
lied
015
015
015
A v..
0.036
0.038
0.038
0.036
0.038
Sample
8 — Iroquois Iron No. 3
Nitric
Bamber's
Chloric
nil hci
Cc
Bl HCI
0.030
0 041
0.034
Direct
0.039
0.038 0.034
0.030
0.038
nun
0.029
0.032 0.036
0 H 10
0.028
ii 034 Av
ii nil
o ,
0.038
0.035 0.036
. 0 "I"
(i 020
0.028
0.034 0.032
o 032
0.020
0.030
0.030 0.038
A\
., 0.035
A
v., 0.021
\nnealei
0.036
0.041
0.023
0.034
0.035 0.039
0.038
0.036
0.031
0.024
Li
0.033
0.034 0.036
Av., 0.024
Av
0.034
Nitric
Bamber's Chloric
Dil.
HCI
Cone. HCI
0.032
0.032 0.033
Direct
0.044
0.031
0.028 0.027
0.033
0.047
0.032
0.034 Av., 0.030
0.032
0.046
0.034
Av., 0.031
Av., 0.033
0.048
Av., 0.032
0.048
Annealed
0.044
0
032
0.048
0
032
0.048
0
030
Av., 0.047
0
029
Av.. 0.031
Sample 12 —
Bureau Standards D,
6A and 6B
, S, ox. = 0.044 and 0.046
Nitric
Bamber's Chloric
Dil. HCI
Cone. HCI
6a
6a 6a
66 6f>
0.038
0.046 0.046
Not run
0.062 0.058
0.040
0.042 0.039
0.057 0.062
0.037
0.046 Av.. 0.043
0.061 0.066
0.039 Av., 0.045
0.062 0.047
Av., 0.039
Av.
Av.
0.069 0.056
0.048 0.046
0.062 0.051
0.055 0.067
0.057 0.059
0.058 0.063
0.066
0.068 0.057
6a
0.062
0.055
0.061
0.056
0.053
0.060
0.068
Sample 13 — Am. Fdy
Assn. Stand. A, 2nd
Nitric
Bamber's Chloric
Dil. HCI
Cone. HC
0.052
0.057 0.052
Direct
0.061 0.049
0.051
0.056 0.049
0.041
0.048 0.053
0.045
0.058 0.054
0.041
0.061 0.051
0.053
0.059 Av., 0.052 Av., 0.041
0.055 0.049
0.047
0.062
0.060 0.050
Av., 0.050
0.063
Annealed
0.053 0.052
Av.,
0.038
0.052 0.062
0.039
0.057
0.041
0.661
Sample 15 — Foundry Iron, T. C. = 3.69, G.
P = 0.65, Mn = 0.48
Nitric
0.063
0.060
0.063
0.062
0.067
0.066 A\
, 0.064
Bamber's .
0.068
0.075
0.073
0.067
Chloric
0.059
0.064
0.061
0.068
Dil. HCI
Direct
0.047
0.047
Av., 0.047
Annealed
0.050
0.050
0.048
0.045
Av., 0.048
Av., 0.061 0.062
C. = 3.34, Si = 2.06,
Cone. HCI
0.069 0.089 0.069
0.069 0.071 0.068
0.074 0.076 0.074
0.076 0.087 0.083
0.069 0.080 0.072
0.070 0.072 0.078
0.081 0.080
0.071 0.077
0.076 0.074
0.067 0.074 0.062
0.076 0.079 0.071
0.073 0.068 0.080
0.071 0.075 0.080
0.066 0.073 0.083
0.076 0.067 0.084
0.080
0.079
0.079
0.089
0.087
0.086
. 0.072 0.073 0.080
Total Av., 0.076
Sampi.f. 16 — Am. Fdy. Assn. Stand. B, 2nd, S, ox. = 0.070,
Nitric Bamber's
0.078
0.06S
0.070
0.070
0 in''
Chloric Dil. HCI
0.070 Direct
0.067 0.059
,0.069 0.059
0.058
Av, 0.059
Annealed
0.060
0.063
0.053
Av., 0.059
Sample 17 — Special Small Ingot
0.077
0.069
0.081
0.080
0.075
0.078
Av., 0.076
Mine Bamber's Chloric
0.075 0.084 0.076
0.076 0.083 0.072
0.079 Av., 0.084 Av., 0.074
v., 0.077
Dil. HCI
Direct
0.061
0.061
0.064
0.058
Av., 0.061
Annealed
0.055
0.055
0.055
0.056
At., 0.055
one. HCI
0.092
0.087
0.090
0.085
0.088
0.087
0.072
0.084
0.084
0.080
0.077
0.080
0.076
. 0.079
July, 191S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Sample 18 — Foundry Iron, Special Small Ingot
Nitric
Bamber's Chloric Dil. HC1 Cone. HC1
0.081
0.094 0
079 Direct
0.077
0.081
0.095 0
080 0.066
0.069
0.082
0.089 Av., 0
080 0.067
0.068
0.084
Av., 0.092
0.080
0.085
0.078
0.066
0.070
lv., 0.081
Av., 0.069
0.076
Av.. 0.074
Annealed
0.063
0.065
0.064
0.059
Av., 0.063
Sa»
ple 19 — Foundry
[ron, Special Small Ingot
Nitric
Bamber's Chloric
Dil. HC1
Cone. HC1
0.106
0.103 0.098
Direct
0.094 0.097
0.101
0.104 0.097
0.060
0.096 0.101
0.097
0. 103 Av., 0.098
0.060
0.091 0.094
0. 100 A\
., 0.103
0.058
0.095 0.093
, 0.101
0.063
Av., 0.060
0.092 0.091
0.096
Annealed
0.094
0.075
0.094
0.077
0.095
0.072 Av.
0.094 0.095
0.066 Av.
0.095
Av., 0.073
Sam
ple 20 — Foundry
Special Iron, Small Ingot
Nitric
Bamber's Chloric
Dil. HC1
Cone. HO
0.113
0.140 0.129
Direct
0.092 0.092
0.116
0.138 0.128
0.074
0.086 0.090
0.121
0.131 0.136
0.066
0.096 0.090
0.119 Av
., 0.136 Av., 0.131
0.074
0.096 0.093
0.117
0.065
0.101 0.098
Av., 0.070
0.097
0.111
Annealed Av.
0.097 0.093
0.088
0.086
0.086
0.075
0.074
Av., 0.081
Sample 21 — -Foundry Iron, Special Small Ingot
Nitric
Bamber's Chloric Dil. HC1 Cone. HC1
0.176
0.140 0.
199 Direct
0.132
0.176
0.138 0.
172 0.136
0.134
0.182
0.131 Av., 0.
186 0.131
0.141
0.171
Av., 0.136
0.127
Av., 0.136
0.184
0.131
0.182
0.139
0.184
0.126
v., 0. 179
0.132
Av., 0.132
Annealed
0.158
0.141
0.155
0.156
0.152
0.137
0.151
Av., 0.150
Sample 22— Foundry 1
ron, Special Small Ingot
Nitric
Bamber's Chloric
Dil. HC1
Cone. HC1
0.265
0.269 0.261
Direct
0.261
0.265 0.260
0.188
0.163 0.187
0.255
0.266 Av., 0.261
0.222
0.146 0.186
0.255 Av
, 0.267
0.190
0.183 0.183
0.259
0.205
0.169 0.186
0.188
0.187 0.186
0.172
0.186
Av., 0.194
0.142
0.177
Annealed Av.,
0.169 0.185
0.234
0.196
0.243
0.208
0.227
Av., 0.222
Sample 23—
Foundry Iron
Nitric Bamber's Chloric
Dil. HC1
Cone. HC1
0.015
0.024 Not run Direct
0.016
0.020
0.010
0.018 0.014 0.019
0.016
0.023
0.010
0.016 0.018 0.020
Av
,0.022
Av., 0.010
0.017 0.024 0.022
0.014 0.020
Annealed
0.016
0.015
0.017
0.015 Av.
0.016 0.019 0.020
Av., 0 015 Tot
al Av., 0.018
Sample 24 — High S Steel
Nitric
Bamber's Chloric Dil. HC1
Cone. HC1
0.120
Not run Not run Not run
0.125
0.116
0.113
0. 109
0.116
U II.
0.123
. 0. 114
0.119
0.123
0.124
Av., 0.121
Sample 25 — Bureau Standards B. O. H.,
0.032
Nitric Bamber's Chloric
Not run Not run Not run
No. 15a, S prom 0.021 to
Dil. HC1
Not run
Total Av.
Cone. HC1
0.044 0.049
0.044 0.046
0.042 0.048
0.049 0.049
0.063 0.047
0.049 0.054
0.047 0.049
0.048
Sample 26 — Bureau Standards B. O. H., No. 126, S from 0 018 to
0.025
Nitric Bamber's Chloric Dil. HCI Cone. HCI
Not run Not run Not run Not run 0.023 0.028
0.025 0.029
0.026 0.027
0.023 0.029
0.024 0.028
0.023 0.023
0.023 0.025
Av., 0.024 0.027
Total Av.. 0.026
No. 13o, S prom 0.022 to
uple 27 — Bureau Standards B. O. H.,
0.035
Nitric Bamber's Chloric
Not run Not run Not run
Dil. HCI
Not run
HCI
0.034 0.034
Sample 28 — Bureau Standa
Nitric
Not run
Bamber's
Not run
ds B. O. H.
0.041
Chloric
Not run
0.033 0.036
0.028 0.034
0.035 0.033
0.033 0.031
0.035 0.039
0.034 0.033
Av., 0.033 0.034
Total Av., 0.034
No. 14a, S FROM 0.031 TO
Dil. HCI
Not run
Sample 29 — Bureau Standards B. O. H., No. 1
0.033
Nitric Bamber's Chloric Dil. HCI
Not run Not run Not run Not run
Cone. HCI
0.037 0.045
0.039 0.041
0.036 0.044
0.035 0.044
0.036 0.038
0.036 0.036
0.037 0.039
Av., 0.037 0.041
ital Av., 0.039
, S from 0.027 TO
Cone. HCI
0.045 0.049 0.064
0.049 0.047 0.054
0.051 0.054 0.056
0.044 0.052
0.044 0.057
0.049 0.067
, 0.048 0.048 0.055
0.065
0.052
0.049
Av., 0.062
Total Av, 0.051
SUMMARY
An evolution flask for the determination of sulfur
in iron and steel has been designed and used for over
300 determinations of sulfur in 23 samples of metal
whose sulfur content has been carefully ascertained
by other methods.
The apparatus is designed to obviate the use of
rubber and provide a reflux condenser to maintain
the acid solution at maximum strength, at the same
time preventing the boiling over of the solution and
washing the gas which goes over into the absorbing
solution. If a current of hydrogen or carbon dioxide
is continuously passed through, the hydrogen sulfide
is effectively washed out and it is impossible for the
absorbent solution to suck back. The author broke
one flask by running in the acid onto the metal when
the bottom of the flask was too hot, and another broke
when the cooling water connection parted and the
cold water ran down the side. The first accident
came through attempting to speed up the runs and
not cool the asbestos between times. If the flame is
shut off immediately on ending a run and only re-
lighted as the last act of starting a new run, this danger
55°
THE JOURNAL Of INDUSTRIAL AXD ENGINEERING CHEMISTRY Vol. io, No. 7
is avoided. After learning this, over 300 determina-
tions were made without accident. The breaking
of the water connection resulted from the multiplicity
of ground joints in the substitute flask; such an acci-
dent is hardly possible with the original design.
The cost of a flask is of no consequence if the re-
sults are considered worth having. The cost per de-
termination will depend on the number of runs that
can be made before it is damaged. If 1,000 deter-
minations should be the average life on an original
cost of Si 0.00 the cost is 1 cent per determination.
The manipulation is simple and only by gross care-
lessness should an analyst break the apparatus by
handling. With the cooling water running and the
hydrogen passing through, the flask can be left boiling
over the flame indefinitely without damage.
The results which can be obtained with the apparatus
are uniformly high, often above those obtainable by
any other method. In only two instances with the
samples studied did the dilute acid give more sulfur
than the concentrated. These were both high sulfur
materials and the sulfur from both of these samples
easily separates as elemental sulfur; in using the nitric
acid oxidation method the globule of sulfur, which may
float about if the solution in hot acid is rapid, has to
be oxidized by long digestion. The high results which
one obtains as in Samples 2 and 3 might keep
one in doubt as to the source of all the sulfur, were
not the abundant cadmium sulfide precipitates di-
rectly in front of one and undeniably of the right pro-
portions. The excellent agreement on some Bureau
of Standards samples and the high figures on others
emphasizes the advantage of standardization of the
iodine solution against sodium oxalate.
A glance at the results shows the fallacy of using
1 : 1 hydrochloric acid, whether the sample has been
annealed or not. If the sample is very high in sulfur,
dilute acid will liberate more hydrogen sulfide in a
1 5-min. interval than the concentrated acid, proba-
bly because of more elemental sulfur being formed
in the latter case. In this case neither will give as
high results as an oxidation method but that, too,
must be extended to oxidize the separated sulfur.
Others have found that a slow digestion carried out
for hours will finally bring the evolution sulfur result
as high as the oxidation figure, even on these high
sulfur materials. For sulfurs not over 0.10 per
cent the proposed method is therefore as accurate
as any method; for sulfur over 0.10 per cent the
analyst must be strictly on his guard.
The advantages of the evolution method are that it
gives the true amounts of sulfur present in the sample,
the method is exceedingly rapid, the method is the
most direct of any yet devised, and only two containers
are used. Oxidation methods using nitric acid are all
highly liable to loss of sulfur because of the excessive
gas formation. The successive nitrations, evapora-
tions, and precipitations in the oxidation and fusion
methods (carried to excess in the latter method) ren-
der these methods reliable only under the most rigid
conditions of laboratory, chemical, and manipula-
tive control. This unfortunate condition is most
vividly presented in the distributed results of the
Bureau of Standards showing the average result as
obtained by the best analysts, all using the same
method, with the extreme results usually differing
by as much as 1 part in 5. There is certainly some-
thing more than the inherent heterogeneity of the
samples at fault when the average results diff er so
widely.
Montana State School op Mines
Butte. Montana
DETERMINATION OF ACETIC ACID BY DISTILLATION
WITH PHOSPHORIC ACID
By W. Faitoctb Munn
Received December 12, 1916
On account of the scarcity of literature dealing
with methods for the determination of acetic acid
in organic mixtures other than the analysis of cal-
cium acetate, it was thought advisable to work
along this line and devise, if possible, a new method
which would be simple, rapid and accurate, even
in the presence of carbon dioxide.
Although the determination as finally carried
out bears relation to the regular phosphoric acid
distillation method such as is described in the well-
known books on technical methods, I think it suf-
ficiently different, due to a number of changes and
additions, to describe in detail.
This method has been used by the writer more
particularly for determining acetic acid in calcium
acetate residues and dry soda and sulfite liquors
than for commercial calcium acetate assays and has
given in all cases excellent results. Of course, if
other volatile organic acids are present they will
be estimated with the acetic acid and the analysis
will therefore have to be continued so as to further
separate these acids before calculating the results
as acetic acid. In most cases the amounts of other
volatile acids contaminating the acetic acid are very
small and for most analyses such as are desired for
technical information may be neglected.
The principle of the method is the decomposition
of the acetate by means of phosphoric acid, dis-
tilling the acid vapors liberated and collecting them
in a known amount of a standard barium hydroxide
solution which is in excess, finally determining by
titrating back with standard acid.
Before describing the method as finally carried
out a few remarks relative to the methods now in
use and described in books on quantitative analysis
will be given.
Lunge's ',Chemisch-technische L'ntersuchungs-
methoden," dritter Band. Seite - or the
translated edition, Vol. 3, p. 307, directs that the
acetate be distilled to dryness two or three times,
the resulting distillates being combined and the
amount of acid therein determined by titration
with alkali.
Allen's "Cornmereial Organic Analysis." Vol. I,
and Treadwell's "Quantitative Analysis" describe
methods similar to that of Lunge.
July, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
SSi
The methods described by A. G. Stillwell1 and
T. S. Gladding2 differ from Lunge's, mainly in the
way of collecting the distillate, i. e., absorbing the
acid vapors in standard alkali as they are evolved
and collected.
W. M. Grosvenor3 points out the error liable
to be introduced if any appreciable amount of car-
bon dioxide is present, but does not eliminate this
error in his method should such be the case.
The procedures as given above tend to cause a
great deal of bumping as the contents of the dis-
tilling flask become more concentrated and there-
fore more syrupy and the distillation often becomes
very irregular. This is more noticeable when an
organic residue is being acted upon than when acetic
acid in acetate of lime is being determined.
There are three improvements in the following
method by the writer, viz., (1) making the distilla-
tion bulbs and condenser tube in one piece (of
V4 in- glass tubing and of the shape shown in the
drawing), thus making one less joint and, as the
apparatus is much smaller bore, enabling one to
obtain more concordant and accurate results in
a shorter time; (2) the use of a slight suction on the
latter end of the apparatus, thus preventing bumping
to a very great extent, the accumulation of vapors
in the flask and reducing the time required to make
the determination; (3) the use of a standard solu-
tion of barium hydroxide for absorbing the acid
vapors. (On account of the use of a current of
air drawn through the apparatus it is necessary to
provide the inlet of the flask with a soda-lime tube.)
The flask A, of about 500 cc. capacity, is fitted
with a two-hole rubber stopper, one hole of which
contains the distillation bulbs and the other a thistle
tube bent as shown in the figure. A soda-lime
tube, C, and a dropping funnel, D, are connected
to the thistle tube. As the dropping funnel con-
tains dilute phosphoric acid, the air drawn through
the apparatus during the distillation must enter
through the soda-lime tube.
The cooling jacket for the condenser tube is made
from '/< in. glass tubing. After drawing down the
1 J. S;c. Chem. hid., 1904, 305.
• Tins Journal., 1 (1909), 250.
1 "Analysis of Commercial Acetate of Lime," J. Sue. Chem. Ind.. 1904,
ends and sealing on the water-tube connections, it
is slipped on in the usual manner. The remainder
of the apparatus needs no explanation as it can be
clearly understood by glancing at the figure.
A known amount of a saturated, or nearly so,
standard barium hydroxide solution is quickly run
into the Erlenmeyer flask B, enough being added
so as to still have an excess at the end of the de-
termination.
S g. of the dry sample, if it is a residue from a dry
distillation, or a varying amount depending upon
the nature of the substance, are placed in the flask
A, and after fitting the corks, a dilute solution of
phosphoric acid (20 cc. H20 plus 40 cc. 85 per cent
phosphoric acid) is added through the funnel D.
The stopcock of the funnel is now quickly closed
and a slight suction (water pump) started through
the apparatus. The flask and contents, which should
be on a sand bath, are gradually heated until the
liquid boils. After the temperature has reached
the boiling point the flame is regulated so as to just
keep the contents boiling lightly. The rate of suc-
tion is then adjusted so that the bubbles issuing
from the tube in flask B are not more than 10 to
15 per minute.
As soon as the distillation and suction have been
adjusted, a dilute solution of phosphoric acid is
made up (50 cc. H20 to 25 cc. 85 per cent phosphoric
acid) and poured into the dropping funnel. This
dilute acid is allowed to drop into the distilling
flask at the same rate as the condensed vapors distil
(about io-to 15 drops per minute). It may be said
at this point that the concentrations just given for
the phosphoric acid may vary considerably, depend-
ing upon the material under examination.
100 cc. Ba(OH)2 solution used, equivalent to 153 .30 cc. A"/10 Ba(OH)i
AVlO HC1 used to neutralize excess 90.30 <
iV/10 Ba(OH)i equiv. to acetic acid plus CO2 63.00.
N HC1 used to dissolve BaCOj 10.56 c
N NaOH used to neutralize excess HC1 6 . 25 <
JV HCI equivalent to BaCOa
JV/10 HCI equivalent to BaCOi
From Ba(OH)i
Subtract cc. HCI equivalent to BaCOj
.id.
4.31 cc
43.10 cc
63.00 cc
43.10 (
19.90 .
AV10 Ba(OH)2 equivalent to acetic ;
19.9 X 0.006 x 10Q _ 2.39 per cent acetic acid
At the end of the run, which is generally complete
in an hour and a half, phenolphthalein is added to
the barium hydroxide solution and the excess of
alkali determined by titration with N/10 hydro-
chloric acid. Normal hydrochloric acid is now
added to dissolve the barium carbonate and the ex-
cess of acid then present is neutralized by the addi-
tion of normal sodium hydroxide and methyl
orange for indicator. (As there is often a yellow
color present in the liquid before adding the methyl
orange for the second titration, the end-point
showing when the excess hydrochloric acid has been
neutralized is very indistinct. If the end-point
is determined by using the methyl orange on
552 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. -
plate, it is very definite.) The acetic acid in 5 g. of the kobinf.au and eollins method as modified
sample is estimated on preceding page. by L. F. Kebler1 was found by the author to give
A sample of carbonate of lime (about 40.00 per the most accurate results. The presence of alcohol
cent C02), part of the residue from the manufacture and the time of shaking did not influence the per-
of acetone by heating calcium acetate, was treated centage of acetone.
by the above method and the following figures The acetone that was used in trying out these
obtained : methods was Merck's reagent guaranteed by them
AVio Bafoiih used yr 09 cc. to be 99 to ioo per cent. The percentages of acetone
AT/io hci to titrate back 67 02 cc. obtained in four determinations using the Robineau
w/io(BaOH),equiv.toCO,p oTcT" and Rollins method were as follows:
N HCI added 5.63cc. Determination No. I II III IV
W NaOH to titrate back 2 63 cc. Acetone, per cent 96.37 96.37 95.89 95.74
a iici equiv. to CO: 3 oo cc. or 30 cc. .v/io nci There remained 4 per cent unaccounted for. The
30.07 — 30. oocc. = 0.07 cc. .v/io (BaOH): or 0.008 per cent acetic acid Bureau of Standards at Washington advised check-
, , , , , , t , ing the purity of the acetone by means of the specific
As this sample had been re-heated for a long time ° r J _. „„^„„s „„ • ■ tU^
* , . , , gravity and referred to Timmerman2 as giving the
before this analysis was made, the chance of any T . , . . • ,,
' , , . • • best value obtainable.
acetate still being present was reduced to a mini- „c,,.<; .."/.«
_ & v , 0/-. The specific gravity I found was 0.80716 15 /4
mum. The presence of a large amount of tO: * „*• » 1 „ ;.. »-„,-. .."/.■> „\.:„\.
, v . br ... .. and Timmerman s value is 0.79574 15 ,4 , which
therefore does not seem to interfere with the acetic . , m„. .. tv-„.„ „„j
would indicate the presence of water. Krug and
acid determination. ,, „, , , , .. . . o ^ , ,_ „„„+ „f „,„«.„
.... , , . McElroy3 found that at 20 C, one per cent of water
While the above procedure appears somewhat . * „ .... - ,
..„,_.; . , u raises the specific gravity 0.0031. Squibb' found
complicated at first glance, it does not prove to be 0 , _„:«.„ j tu„ „„„„;<:„
F b . ' . . ,. . « j that at 15 one per cent of water raised the specific
so, as the distillation after once it is adjusted, needs „„;«„ „„„;*„ ~( >ra„i,>,
' ,. , . , „ . '. gravity 0.0029. The specific gravity of Merck s
very little attention, thus allowing the person in * 0/0+1. „ f„,„ tu„^ 1^
, J , ' , . acetone was 0.80716 15 /4 , therefore, there could
charge to attend to other duties. , ,_ , .
s be 3.6S per cent of water present, assuming as correct
. Lederi.e Laboratories _.. . , » . .
New York City Timmerman s value for anhydrous acetone.
The author wishes to express his thanks to Dr.
I. W. Fay, of the Polytechnic Institute of Brooklyn,
THE DETERMINATION OF ACETONE ., . /'. , . ' .
for his advice during the work.
By Allan J. Field
ROSEBANK
Received June 20, 1917 • Staten Island, N. Y.
The purpose of this investigation was to find an
accurate method for the determination of acetone
in methyl alcohol. All of the published methods SOME RESULTS OF ANALYSIS OF AIRS FROM A
were investigated with results as follows: MINE FIRE
messinger's method1 is a volumetric method By a. g. blakeley and h. h. Geist
depending upon the reaction between iodine and Received September 15. 1917
acetone to f< rm iodoform. Messinger claims that There is no doubt that gas analysis has found con-
accurate results can be obtained by this method, siderable use in locating mine fires and especially in
A criticism by Vaubel and Scheuer2 of this method following the progress of these underground fires.
is that when thiosulfate is used in titrating back, Not a great deal of data has been published, however,
the results are always too low-, and, therefore, they The writers, therefore, considered it proper that they
recommend the use of arsenious acid instead of the publish some data which may be of interest to those
thiosulfate. The writer tested this method, using connected with mining work, particularly with anthra-
thiosulfate as well as the arsenious acid, but could cite coal mining.
not get accurate results. The precautions recom- The mine at which the samples were taken is an
mended by Collischon3 were observed but the results anthracite coal mine, a mine considered as a rather
were not satisfactory. I found that if, after the addi- gaseous mine, or one generating a fairly large quantity
tion of the N / 5 iodine solution, the mixture is shaken of methane or fire damp.
for 5 min., a low result is obtained, while shaking for On November 18, 1916, several men were overcome
20 min. gives a higher result, the percentage varying while at work inside the mine. On November 19, a
with the length of time of agitation. These cxperi- lire was discovered. Batteries were erected for the
ments were tried on a pi me solution without purpose of smothering out the fire by cutting off all
the presence of alcohol. Winn methyl alcohol was the fresh air supply.
present the percentage of acetone found was several In order to carry out this investigation pipes were
per cent higher. The increase could not be due to extended through the batteries, these pipes being closed
the alcohol furnishing the extra amount of acetone by means of valves at the outer ends. From time to
as the quantity it contained was duly considered. , ,„.,,.,„ s i9 .
' Btr., SI (1888), 3366. ! Bui. soc. chim. btlg.. 24 (1910
« Z. angew. Chem., 18 (1905), 214. ' J Anal. Afpl. Chem . 6 (1892), 187.
' Z anal. Chem.. 89 (1890), 562. ' -' Am. Chem Soc., 17 11895). 200.
July, 191S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY 553
time these valves were opened and air samples taken. are enclosed in a metal case which opens, as indicated,
These samples were taken in such a way as to accurately and which may be rotated by means of an arm ter-
represent the air behind the battery, or in other words, minating in a micrometer screw, M. The smallest
the air from the fire zone. division on the micrometer corresponds to a differ-
The carbon monoxide was determined by the iodine ence in index of about 0.00005. The face of each
pentoxide method, more than one liter of air being prism is divided into two parts, A and B, by means
passed over the heated iodine pentoxide in each de- of a groove so that a drop of the standard liquid may
termination. be placed on one face (either A or B) and a drop of
The results given in Tables 1 and 2 seem to need no the liquid to be tested on the other face. For ex-
further explanation. ample, since the temperature coefficient of most solu-
The mine fire zone was partially opened in August tions is nearly that of water, water may be used as a
191 7, and no further air samples were tested. standard when measuring the index of solutions.
Table l — 7th Level, Gangway Battery To obtain a dividing line free from color it is neces-
Carbon , . ■
Carbon Carbon Dioxide in sary to use a monochromatic source of light, such as
Date of Oxygen Dioxide Monoxide Methane Black Damp1 j • n ,. - . _.
Sampling Percent Percent Percent Percent Percent a SOdlum name, Or Some Compensating device. The
Dec 1. 1916 >8$° °-*> 0008 2.40 8.28 former is sometimes inconvenient and the latter would
Dec. 5 16.40 1.16 0.0057 2.33 5.85
Dec. 12 15.80 1.34 o.oo34 4.27 6.47 considerably increase the cost of the instrument. A
Dec. 19 16.00 1.61 0.015 3.28 7.80 , * . , , _
Dec. 26 15.66 i.69 o.oi 3.66 7.72 monochromatic red glass, G, was used in connec-
Jan.5. 1917 14.00 1.71 0.006 4.46 5.87 x- •., , . ■ ,- ,. T , ., - . ,,
jan. ii 14.30 2.ii 0.004 4.51 7.66 tlon- with an electric light, L, and it was found that
jan! 25::::: :::::: uilo I'.ll 0:002 I'M Ia\ the dividing line is nearly as sharp as that which ob-
**{;•?,, }^-?o |.04 0.005 5.ib 9.20 tains when a sodium flame is used. The lamp used
Mar. s".. '.'.'.: :::::: }3.io 2:38 0.0016 3^7 7 78 was a 7.5 watt, novolt, frosted globe tungsten and
Mar. 22 13.90 1 .60 None 3 . 55 5.23
Apr. 5 12.42 2.43 None 4.38 6.62
Apr. 18 13.11 2.34 None 3.35 6.79
May 3 13.10 2.67 None 4.12 7.93 \yHJ
May 17 10.20 3.20 None 6.35 7.06 -< \JJ(
May 31 9.90 2.22 None 4.96 4.59 (f\ a'W
June 14 8.70 3.42 None 7.87 6.70 V\ ■"• ■»
June 28 9.00 3.32 None 6.60 6.53
July 12 6.40 4.21 None 8.14 6.82
July 26 4.80 4.47 None 10.90 6.71
Table 2 — 7th Level, Monkey Battery \ \ J^^T^^ \ \
Carbon \ \ i^^OT \ r> iTKlD
Carbon Carbon Dioxide in \ \ ^^nTO* \-°
Date of Oxygen Dioxide Monoxide Methane Black Damp1 \ \s> •' ^^^^^^T^'R
Sampling Per cent Per cent Per cent Per cent Per cent ^*- *
Dec. 1, 1916 13.63 2.09 0.019 5.97 7.13 Mfj
Dec. 5 12.00 2.11 0.009 3.35 5.29 < ff . >A P
Dec. 12 11.51 2.17 0.0044 6.22 5.52
Dec. 19 14.10 2.30 0.029 4.73 8.14
Dec. 26 13.78 1.98 0.016 5.15 6.73
Jan. 5. 1917 9.80 2.12 0.01 5.62 4.40 p\
Jan. 11 10.80 3.31 0.0068 6.20 7.77
Jan. 18 10.20 3.40 0.006 5.63 7.39
Jan. 25 10.73 3.46 0.007 4.76 7.80 ll L ,') I L
Feb. 9 9.40 4.10 0.008 6.34 8.35
Feb. 22 11.10 3.67 0.0017 5.25 8.72
Mar. 8 10.00 3.43 None 5.76 7.32 Fig. I Fig. II
Mar. 22 11.40 3.62 None 4.96 8.85
Apr. 5 9.10 3.97 None 6.13 7.82 ' ...
Apr. 18 10.20 3.65 None 3.81 7.63 it was made a part of the instrument so that no ad-
May 3 10.00 3.40 None 6.44 7.36 . , , , T, .
May 17 7.30 4.40 None 7.02 7.52 justing was necessary when once in place. It is more
jine ii "".::::::::: 3.30 tisn None 9:03 0:36 convenient than daylight and it also produces a more
june28::::::::::: 3:20 4.86 None 10.05 6:47 uniform new
July 12 3.30 4.96 None 11.88 6.81 uniiorm neiu.
J^y 26 2-80 4-84 None 10-17 6 ■-'•' The refractometer was originally designed to measure
■ Foster and Haidane, "The investigation of Mine Air," p. 124. the difference in index between hemolyzed and un-
to Philadelphia & Readlng Coal and Iron Company hemolyzed blood, as it was discovered by Dr. F. H.
Pottsville, Pennsylvania Howard and the writer, some time ago, that the amount
of hemoglobin present in a given sample of blood causes
A DIFFERENTIAL REFRACTOMETER its index to vary markedly and, furthermore, that the
By G. a. Shook difference in. index (hemolyzed and unhcmolyzcd blood)
Received February 16, 1918 depends only upon the amount of hemoglobin present.
This instrument is the result of an attempt to de- Since the absorption bands of blood are in the green
velop a simple but accurate refractometer for measuring and blue parts of the spectrum a red glass is well
the difference in refractive index between two liquids. adapted to this sort of measurement.
It is of the Abbe" type but so constructed that two After passing through the refracting prisms the
liquids may be examined simultaneously and, there- light enters a telescope, T, provided with cross-wires
fore, if the index of one is known and if both have the as shown. Between the telescope objective, O, and
same temperature coefficient, the index of the liquid the prisms is a diaphram, D, provided with a shutter,
in question may be accurately determined without S, and by adjusting this shutter the light from either
knowing its temperature. A or B may be cut out. For instance, when the light
The instrument as constructed by the writer is from B is intercepted, the dividing line A', due to
shown diagrammatically in Fig. I, and the optical the light from A, is seen; and when S intercepts the
system in Fig. II. The refracting prisms P, P light from A, then B' is in the field. The distance
554
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 7
between these lines is measured by means of the microm-
eter M.
When red light is used a difference in index can
be measured with an accuracy of about one in the
fourth decimal place (». c, ± o. 0001), but with sodium
light the accuracy is about ±0.00005; that is, if one
measures the difference between the two lines by means
of the micrometer, cleans the prisms, and makes a
second measurement, the two values of the index
difference calculated therefrom will agree within
0.0001 for red light and within 0.00005 for sodium
light.
The relation between the micrometer reading and
the difference in index is very nearly linear, so that
by means of two solutions of known index and a com-
parison solution, the instrument can be easily cali-
brated.
Williams College
Williamstown. Mass.
A VOLUMENOMETER
By J. S. Rogers and R. W. Frey
Received February 19, 1918
Although there are numerous types of mercury
displacement apparatus for measuring volume none
has been found satisfactory for comparatively large
pieces of leather. The apparatus described here,
while based on the well-known displacement princi-
ple, possesses, it is believed, some new features. It is
not only satisfactory for large pieces, but also permits
of a decided economy in mercury since the chamber
for immersion is in the shape of a rectangular paral-
lelopiped instead of a cylinder or sphere. The appara-
tus was designed primarily for measuring test pieces
of a maximum size 71 ;\ X 3 in. in connection with the
development of methods of determining loss from a
mechanical wearing test of leather. It has also been
found to be very useful in determining the apparent
density of leather.
A description of the volumenometer and photo-
graphs (Figs. I and II) follow: The immersion vessel
consists essentially of the tank A and top B. both of
cast iron and having accurately ground surfaces, C,
so that the top, when clamped on by means of the bolts,
D, make a mercury-tight joint. The tank A has a
chamber. E. 11 8 in. wide, S in. long, and 31 - in. deep,
and the walls of this chamber are continued in the
top B in such a manner that they converge to the
small opening F in which is sealed, with shellac, the
short thistle tube G. The top has two posts, H,*_to
which the pieces to be measured are fastened.
In the metal tube I, which passes through the wall
of the tank from the bottom of the chamber E, is
sealed a heavy capillary glass Y-tube, J, fitted with the
mercury-sealed stopcocks K. One arm of the Y-tube
is connected with the bulb L, and the other arm with
the burette M. Both the bulb and the burette are
connected with the vacuum system.
By means of N and 0 the zero points on the two glass
tubes may be easily adjusted to coincide with the
level of the mercury, which may change slightly from
time to time, due to temperature variations and me-
chanical loss. This adjustable zero device consists
of a small threaded metal sleeve fastened on the glass
tube and fitted with a nut. Resting on the nut is a
loose-fitting glass sleeve having a fine graduation.
By turning the nut the graduation on the glass sleeve
may be raised or lowered as desired.
All metal surfaces to which the mercury would have
access are treated with bakelite, and the entire ap-
paratus is securely mounted on a large wooden tray.
The bulb and burette are also properly supported.
The operation of the apparatus is conducted as fol-
lows: With the top removed and the stopcocks open,
completely fill the tank with mercury, being careful
not to form any air traps in the Y-tube. Then draw
the mercury well up into the bulb and burette, and
after closing the stopcocks add sufficient mercury to
fill that part of the chamber in the top of the tank.
Place the top in the tank and fasten it securely by the
four bolts, D. By opening the stopcocks let the mer-
cury down from the bulb and burette until it stands
at the same level in all parts of the apparat'
the two adjustable zeros. X and 0. so that the gradua-
tions on the glass sleeves coincide with the menisci
of the mercury, and take the zero reading on the burette.
Now draw the mercury again well up into the bulb
and burette, close the stopcocks and remove the top.
Fasten the piece to be measured onto the posts H
(Fig. I), replace and secure the top. Open the stop-
cock communicating with the bulb L and let the mer-
cury run down slowly to the zero mark at N on the
stem of the bulb and close the stopcock. Then open
the stopcock connecting the burette and allow the
mercury to gradually lower until it fills the tank and
rises to the zero mark at 0 on the tube G. close the
stopcock and read the burette (Fig. II). The differ-
ence in readings will give the volume of the piece.
July, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
5SS
In making a series of measurements, if care is taken
in removing the pieces so as to avoid loss of mercury,
the zero reading and adjustments need only be made
after about every eight measurements.
The dust and dirt which slowly accumulate on the
surface of the mercury in the tank may be very easily
swept off with a small camel's hair brush. In fact, a
slight layer of dust is somewhat desirable as it forms
an envelope around the piece when immersed and helps
to prevent the absorption of mercury.
An objection to the apparatus is that it requires
two persons to operate it most satisfactorily and ex-
peditiously. Furthermore, unless care is exercised in
removing the pieces some mercury is likely to be lost.
No doubt a more satisfactory means of fastening the
piece could be devised which would overcome the ten-
dency to lose mercury which collects around the screws,
and which would decidedly shorten the time required
for securing and removing the pieces.
A few of the measurements made with the apparatus
are given here. These volumes were obtained on the
same series of samples on different days, but always
under the same temperature and relative humidity
conditions of 700 F. and 65 per cent relative humidity,
the apparatus being set up in the constant tempera-
ture and humidity room.
Samples Volur
SI 35. 15
S2 29.35
S3 39.75
S4 36.85
LI 39.45
L2 41.85
Cc.
Samples
Volutin
in Cc.
35.20
L3
40.05
40.05
29.40
L4
39 . 80
39.80
39.80
1.5
42.95
42.95
36.90
u
... 47.85
47.90
39 . 50
L7
37.20
37.20
41.90
L8
34.40
34.40
A piece of hard rubber has been used as a standard
to check the apparatus, and its volume . determined
at frequent intervals during a period of several months
has ranged from 89.10 to 89.13 cc. The volume of
this same piece calculated from loss in weight in water
at 700 F. gave 89. 14 cc.
CONCLUSIONS
An apparatus has been devised which is satisfac-
tory for measuring the volume of comparatively large
pieces of leather. The measurements can be dupli-
cated and are reasonably accurate.
Leather and Paper Laboratory
Bureau of Chemistry, Department of Agriculture
Washington, D. C.
AN EVAPORATOR FOR ACID LIQUIDS
FOK THE ECONOMICAL EVAPORATION OF ACID LIQUIDS OR
OF ANY LIQUID DISCOLORED BY CONTACT WITH METALS
By Ed
Received February 7, 1918
This system of evaporation for which United States
letters patent have been granted but not yet issued
(Application No. 202,189) is especially indicated
where the solvent is water. The tubes (Fig. 3 is a
cross-section) which may be of any number and of
any desired size and length (3-in. glass tubes 4 ft. long
are recommended for most purposes) are supported
on gas pipe covered with asbestos paper as shown in
Fig. 3; cross-stirrup supports are not shown. There
*%
Jfy.S
lp^r:S
■*&•
are three i-in. openings in each tube to permit the
introduction of liquid and the escape of steam. These
openings may, of course, take the form of tubes,
and the solvent may be condensed if desired.
The fire grate and course of the fire gases are indi-
cated by the arrows in Fig. 1. Two, three or more
sets of tubes may be used (two are shown) and the
liquid warmed in the first set boils and evaporates
in the second, and is collected and discharged by the
end manifold, shown in Fig. 2, into crystallizers. The
concentration of the discharged liquid is controlled
absolutely and with great accuracy by the feed.
Hart Laboratories
Easton, Pennsylvania
CONVERSION OF FORMULAS
By Willis H. Cole
Received February 8, 1918
In practically .ill industries in the United States
pounds and gallons are still the units of measure,
while in the laboratories of these factories the metric
system is almost universally used. Thus the indus-
trial chemist is called upon to make many conversions
SS6
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 7
of formulas as made on a large scale in pounds and gal-
lons, into a size suitable for laboratory batches, in grams
and cubic centimeters. I have seen many good chemists
waste all the way from minutes to hours doing this,
looking up conversion tables and multiplying. By
aid of 'li>' following simple rule, great saving of time
uracy is effected. Call the gallons cc, and
multiply the pounds by 0.12 (for very accurate work,
0.1108) to get grams. These figures may then be
multiplied by any factor which will give a convenient
sized batch for laboratory purposes.
China Wood Oil.
Prepared Linseed Oil
Turpentine
Petroleum Spirits- . . .
Example I
Varnish Formula
Factory Batch
100 lbs.
. . . . I"
. . . . 4 gals.
! 5 gals.
. 7 gals.
Convenient
Lab. Batch
24 g.
52 gals.
In this case you will see that there are more
ingredients measured by volume than by weight.
Should this condition be the reverse, it is more efficient
to change the rule, calling pounds, grams; and multi-
plying gallons by 81/* (for very accurate work, 8.3455)
to get cc. Here follows a formula to illustrate this
method.
Example II
Flat White Enamel
Factory Batch C
Zinc Oxide 90 lbs.
Lithopone 90 lbs.
Whiting 25 lbs.
Silica 25 lbs.
Varnish 12 gals
Benzine 10 gals.
Yield 28 gals. 233.3 cc. 116.6cc.
The factors used hold for U. S. Standard gallons
only and not for Imperial gallons.
Research Laboratory
Muller & Schumann Co., Brooklyn, N. Y.
Convenient
onversion
Lab. Batch
90 g.
45 g.
90 g.
45 g.
25 g.
12.5 g.
25 g.
12.5 g.
100 cc.
50 cc.
83 . 3 cc.
41.6 cc.
ADDRESSES
TECHNICAL APPLICATIONS OF NEPHELOMETRY1
By Philip Adolph Kober
I — INTRODUCTION
Something over two years ago I had the privilege and honor
of reading a paper2 before the New York Section of the American
Chemical Society on nephelometry in which I gave briefly the
history of photometric analysis and a description of the develop-
ment of nephelometric instruments. At the invitation and with
the encouragement of your honorable Chairman, Dr. Alexander,
I shall now venture to put before you some technical applica-
tions of nephelometry, which, owing to war and other conditions,
I regret, are not nearly as complete as I originally planned to
have them.
As most of you know, the method is based upon the measure-
ment of the brightness of the light reflected by cloud — in other
words, by the particles in suspension — very much as in an
ultramicroscope. The intensity of the light reflected is a func-
tion of the quantity of suspended particles, when other conditions
are constant.
The principle of the nephelometer can best be shown by
the diagrammatic sketch, shown in Fig. I.
Fig. I
The path of light in nephelometer.
Let A and B represent tubes containing a precipitate in the
form of a suspension, and I, represent a strong light which throws
its uniform beam on tubes A and B at right angles; then a and
b will be the lij;lit in the eyepiece due to the reflections from the
two suspensions If tube A, for example, contained distilled
water and the instrument were perfect, no light at a would be
1 Lecture and demonstration given before the N. Y. Sections of the
Society of Chemical Industry. American Chemical Society, and American
Electrochemical Society. Chemists' Club, October 19. 1917.
1 Kober and Craves, This Journal. 7 (1915), 84).
Fig. II
Lamp house and instrument, showing the concentrated filament lamp,
air space, condenser, and lamp house. When the doors (not shown) are
closed, no light is visible except in the eyepiece. The inclined angle of
the instrument, which allows air bubbles to escape from underneath the
plungers, and the exact position and angle of reflectors are not shown in
the sketch.
visible. As soon as the smallest amount of suspension is pro-
duced in the tube A, light is obtained in a in approximate pro-
portion to the amount of suspended matter. This light a is
never measured absolutely, but is always matched at b, which
is that reflected by the precipitate of a standard solution — a
known amount of the substance to be determined dissolved in a
known volume.
The matching of the two lights could be done by changing
the standard solution step by step until it would be exactly that
of the unknown. In practice this would be tedious and. there-
fore, instruments were designed to eliminate this in whole or
in part.
Fig. II shows a diagrammatic sketch of such instru-
ment and lamp house, and is known as a nephelometer-colorim-
eter,' because it is both a nephelometer and colorimeter.
Fig. Ill shows the instrument without the lamp house, particu-
larly the scales, verniers, and the screw arrangement for raising
and lowering the cups, which is used to match the reflected light
from the suspensions.
1 J. Biol Chrm . 39 (111!), 155.
July, 1018
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
557
Fig. IV is a photograph of the instrument, with solutions, or,
better said, suspensions, viewed from the front.
The cups and plungers for this instrument are shown in Fig. V.
The nephelometric cups have transparent sides and opaque
bottoms, while the colorimetric cups have opaque sides and trans-
parent bottoms.
In Fig. VI is shown the photograph of the instrument
used as a colorimeter, where the adjustable reflectors are in
position. The lamp switch may be seen in front, as well as the
doors of the lamp house, which when closed cut off any glare
from the source of light.
Before going over to the details of the applications, it may be
well to point out briefly the correct use of the nephelometer and
a few points on the production of nephelometric suspensions.
A large number of workers do not have favorable conditions
when they first apply the nephelometer. The work should be
conducted in the dark; glares from windows, doorways, and the
like, as well as artificial lights, being just as bad for photometric
work as for the moving picture show. Some laboratories have
permanent special dark rooms, others portable dark rooms,
while still others darken the regular laboratory with opaque
shades. A few workers forget that the eye is a sensitive instru-
ment, and by using it too much or too continuously, and not
allowing a period of rest, like the standard electric cell, it can
easily become polarized, or fatigued. When these precautions
are taken photometry or nephelometry can be practiced all day
without any special fatigue or eyestrain.
A few forget or overlook many of the following obvious de-
tails: They ignore the dust in the various parts of the optical
equipment and fail to fill the cups, so that the cups are clean on
the outside, which thus allows the light to be absorbed. They
overlook the fact that any air bubbles and dust underneath the
plungers reflect light. The zero point of the instrument, too,
as illustrated in Fig. VII, is not adjusted to represent zero light,
and other oversights are often present.
Probably the greatest source of error connected with nephel-
ometry or colorimetry is practically an instrumental one, pointed
out to me by Mr. Klett, head of the company1 manufacturing
this instrument. He found that most diaphragms or openings
at the top of the eyepieces, even in the best of instruments, are
too large. He found that by putting a small diaphragm of the
size of a pinhole over the eyepiece, he could make one or the
other side of the field of almost any intensity.
Only by putting the aperture over the optical center could he
obtain equal illumination of both sides of the field. When he
moved the pinhole 0.1 to 0.2 mm. to any side, as illustrated in
Fig. VIII, he obtained black spots and sides in the field. What
errors would be introduced by a nervous individual, who would
probably never have the eye twice in the same position, or by
a beginner doing the same, can easily be imagined. By the use
of such a diaphragm, not only will many discrepancies in readings,
such as an occasional off-reading, disappear, but the field will
become more flat; and only by its use it seems can the instru-
ment be accurately adjusted and used.
Time does not permit us to dwell on the production of colored
solutions suitable for colorimetry, however interesting and im-
portant from both theoretical and practical standpoints. As
we have pointed out elsewhere,2 the chief requisite for making
nephelometric clouds or colloidal suspensions, and for keeping
them as such for a definite time, is that the substance be in a
dilute solution, usually not stronger than 100 mg. per liter
Therefore, to apply the method to large amounts of substance
it is only necessary to dilute suitably. Clouds, produced by
one part in 500,000 of liquid, may be determined quantitatively.
In some cases one part in 2,000,000 can be easily determined.
Since the amount of substance may vary greatly it is important
to know whether the nature of the precipitate imposes any
limitations on the method. It is necessary to consider, there-
fore :
1. color — If the precipitate is highly colored and remains
in suspension, it is best determined colorimetrically ; if slightly
colored, it is best determined nephelometrically.
2. form OF precipitate — It must be colloidal in the form of
a suspension. A large number of precipitates found in practical
work are colloids, a number are partly so, while some are so en-
tirely crystalloidal, such as barium sulfate, that they settle
immediately. According to previous work published, certain
solutions of protective colloids can be used, such as egg albumin
and soluble starch, which cause crystalloids like barium sulfate
and other partly colloidal precipitates to remain in suspension
long enough for the application of this method.
The new nephelo
adjustable verniers, als
through which dust
eter-colorirueter. showing screw arrangement with
50 (he double milled head. There are no open spaces
y enter and light escape when fitted to the lamp house.
' Klett Mam
1 P. A. Kobe
» (1914), 121.
facturing Co., Inc., 202 E. 46th St., New
• and Sara S. Graves, "International Clin
York City,
cs," 24th Ser
While the application of nephelometry is comparatively simple,
the correct condition for producing and keeping the colloidal
suspension, the Fundamental condition of nephelometry, is by
no means a simple matter, in spite of Harry Jones' statement'
that "the colloidal solution or at most the colloidal suspension
is the natural condition of solid matter when first formed as the
result of a reaction."
1 "New Era of Chemistry," p. 248. Published by D. Van Nostrand
Co., New York City.
558
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 7
Although lime does not permit us to consider the details of
producing suspensions and the theory of nephelometry, which
I hope to present in a special future communication, a few words
and an illustration will help to make clear and emphasize the
difference between theory and practice, and give an example of
the unexpected difficulties encountered in developing nephelo-
metric methods.
Silver chloride has been estimated as a suspension for a cor-
rection in atomic weight work since Mulder's time in 1859,
yet the production of nephelometric suspensions of silver chloride
is as yet far from satisfactory.
Fro IV
The instrument used :is i nephelometer viewed from in front, in the
direction of li^ht. showing standard solution on the ri^ht, unknown
reads to be m itched on the left.
if has been assumed by the i'-u adverse critics of nephelometric
work, that when chlorides and an excess of silver nitrate arc pres-
ent itf dilute solution, silvei chloride must be formed, and, being
one of the most insoluble substances, it must be in the form of
i precipitate, and, therefore, impart reflected light. If the
amount of light was changed or was not up to what was
from previous experiments, the critics ol nephelometry assumed
that the light reflecting properties of silvei chloride changed.
On this assumption they have made the sweeping conclusion
that unless both the standard and the unknown were treated
exactly the same and in the same medium, a difficult condition
to realize, the nephelometric results would be inaccurate, if not
valueless. The simpler assumption that a change in the amount
of light indicated a change in the amount of precipitate seems
not to have been considered at all.
But the following experiment will show that the nephelometric
production of silver chloride is not as simple as the formula
would indicate it to be. If we take a dilute solution of sodium
chloride (0.0005 N = 0.030 mg. X) and add silver nitrate in
gradationed amounts, keeping the volume constant, as shown
in Fig. IX, we get silver chloride precipitate in all experi-
ments.
But. as may be seen, the maximum cloud is obtained with one
equivalent and the amount of precipitate decreases as the ex-
cess of silver nitrate is increased. Our experiments indicate
that silver chloride in solution, before it precipitates, forms with
silver nitrate an unstable, soluble complex, which slowly hy-
drolyzes, or decomposes, with the production of silver chloride.
By adding the same excess of silver nitrate as in the weakest one,
slowly, with stirring, the silver chloride is precipitated before
it can form the soluble complex with silver nitrate, and, therefore,
the maximum suspension is obtained even though the medium
is chemically the same in the end as in the weakest suspension.
In diluter solutions this phenomenon is still more marked.
It is interesting to note that Professor Richards, in his atomic
weight work, avoided this source of error intuitively by allowing
his silver chloride suspensions to come to an equilibrium by
standing from 24 to 48 hrs. If our explanation of this phe-
nomenon is maintained by further work, as these experiments
would indicate, the adverse critics of nephelometry are without
much, if any, experimental basis for their criticism. This ex-
periment, like all heretofore, seems to show that the amount of
light reflected by colloidal suspensions within moderate limits,
*. e., from the time the particles are formed until they are almost
visible to the unaided eye, is a function of the amount of pre-
cipitate in suspension.
n — APPLICATION
The number of possible applications of nephelometry is too
large for consideration here, and, therefore, a few representative
estimations have been chosen, i. e.. three inorganic and three
organic determinations: the estimation, respectively, of ammonia,
phosphorus, calcium, acetone, oils and fats, and, finally, pro-
teins. This choice was made not only to cover as broad a field
as possible, but also to bring out the nephelometric peculiarities
as well, especially the use of protective colloids.
While the "colloidal solution or at most the colloidal suspen-
sion is the natural condition of solid matter when first formed
as the result of a reaction," as Harry Jones gives it in his book,
yet it rarely, if ever, stays in that condition. In most cases
it quickly agglutinates and settles, a condition unfavorable
to accurate nephelometry. By adding a protective colloid we
can delay the agglutination, or, to be more exact, decrease its
speed sufficiently to make uniform and constant nephelometric
conditions. The protective colloids vary considerably, not only
in nature, but also in amount, as will be pointed out in detail
in the rest of the paper.
Not all the details of making the reagents and solutions will
be given in this paper, as recourse can be had to the original
articles on the subject; but for these six analyses, all the steps.
more or less, will be mentioned, su that from the six different
analyses a clearer judgment may be formed of the value of
nephelometric estimaf
[MONIA ESTIMATIONS Nessler's reagent for ammonia.
developed in the early part of the last century, was applied to
watei analyses in 1867. It has -food the test of time and has
come to be used extensively; but with the development of color-
July.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
559
imetry its disadvantages as well as its value have become ap-
parent and innumerable modifications of the reagent have
resulted. Its instability and tendency to produce a cloud in
dilute solutions are the chief difficulties.
Recently efforts have been made to apply the reagent in micro-
Kjeldahl work, without previous distillation, with varying de-
grees of success; the precipitate due to salts makes the matching
of colors, however, extremely difficult.
A probable explanation of why the colored solution produced
by Nessler's reagent becomes cloudy, especially in the presence
of salts, may be found in the following considerations:
i — Only the iodide complex of mercury and ammonia is
highly colored.
2— The other complexes of mercury and ammonia, like the
chloride described in this paper, are colorless insoluble com-
pounds.
Therefore, in the presence of the other salts the colored iodide
complex is probably partially changed to and in equilibrium with
the colorless complexes such as the chloride or sulfate.
On this basis Sara S. Graves' developed a sensitive nephel-
ometric reagent for ammonia as follows:
80.0 g. Sodium Chloride
130.0 g. Water
100.0 cc. Saturated Solution of Mercuric Chloride
Shaking until NaCl is dissolved, then add
70.0 cc. Saturated Solution of Lithium Carbonate (1.0
per cent)
Filter
Fio. V
Showing construction and optical clearness of plungers on the left),
of the nephelometric cups (in the center), and colorimetric cups (on the
right). The bottoms of all are fused on, though of glass having different
coefficients of expansion.
To show the sensitiveness some reagent was added to a liter
of water containing 0.006 mg. of ammonia. The cloud which
was obtained means that we can detect one part of ammonia
in 160 million parts of water.
For the purpose of illustrating how the instrument is used and
how the results are calculated, suppose some precipitated stand-
ard solutions of ammonia were placed in the instrument. If we
had simply added reagent to the known solution of ammonium
sulfate, the precipitate would have become agglutinated before
the observations were finished. Therefore, just before adding
reagent a protective colloid is added. In this case for every
10 cc. of ammonium sulfate solution, 15 cc. of a 0.003 per cent
solution of starch will keep the suspension from agglutinating
and settling for about an hour. The standard solution contains
9.43 mg. ammonium sulfate, which is equivalent to 2.43 mg.
ammonia, or 2.00 mg. nitrogen, per liter. Wlun precipitated
with 5 CC. of reagent the resulting suspension is put into I
of the instrument.
If we put the left cup at any convenient height, sa
2.5 nun., ami move tin other cup up or down until the light in the
. coming from both tubes, 1 equal, we find thai the
I Chtm 37 I VIS I. I 171.
Fig VI
Showing the instrument with lamp house used as a colorimeter; the
adjustable reflectors are reflecting the light to the round instrument reflec-
tors, which in turn transmit the light to the cups and instrument. The
light switch can barely be seen on the front of the base.
height on the right is rarely, if ever, equal to the height set
on the left side. It is in this respect like the zero point of the
analytical balance ; it must be determined from time to time, and
is seldom constant for a long time. The reading on the right side
we will denote as the standard reading, S, but the actual value
on the left is of no consequence and may be considered as a tare,
so long as it is constant. If in place of the standard on the
right we now put another solution of ammonium sulfate, say
0.900 as strong as S, we find a higher reading. If we then put in
0.800, 0.700, 0.600 and 0.500 standard strength, we obtain,
respectively, a series of corresponding readings. All of these
readings except that from the standard S are indicated as Y
in the curve and formula.
If we plot these readings on cross-section paper we obtain a
curve which will be very useful in practical work. In Fig. X
we have plotted the readings obtained from such a series of
gradationed known solutions of ammonium sulfate solutions
and drawn a cum through these points. Algebraically the
S (1 — x)Sk
curve is expressed by the formula Y = — ,
X X2
where k = 0.052 and S = 20.0. The lower curve, shown here,
is the colorimetric curve where the readings are inversely pro-
portional to the concentrations.
When the instrument changes so that a restaudardization is
necessary, the nephelometric formula obviates considerable
work, especially the readings for and the drawing of a new curve.
.Since the formula is complicated and many prefer to do with-
out mathematical calculations, the following scheme can be used:
The instrument is standardized as before, but the curve is used
alone in getting the amount of substance equivalent to the
readings. When the value of the standard readings changes.
Mi. instrument, the height of the solution
,,„ the I. it idi . ill' on. used as i tare, is adjusted 30 that the
original readin btained and, therefore, the original
curve is applicable ( al to changing the zero point
of a iia! ' tment so as to avoid calculation,
560
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 7
In Fig. XI, the same curve is used for practical work,
i. e., in expressing the results in per cent of nitrogen, obtained
in Kjehlahl nitrogen estimations, using 0.1000 g. of substance
or sample.
JEffi
in
r
1 1
9 I
Fig. VII— Showing Scale and Adjustable Verniers
The one on the right shows the plunger touching hottora of cup, thereby
giving more zero or color, with vernier in right position, i. «., exactly on
zero. The verniers c:in be put on zero by loosening the screw of vernier
and moving vernier to right position after plunger touches the bottom of
the cup, or its equivalent.
Suppose we had a Kjeldahl flask containing 20 cc. concen-
trated sulfuric acid, a little mercury or mercuric oxide as catalyzer
and 0.1000 g. ammonium sulfate. As far as the nephelometric
method is concerned, this could as well be the result of digesting
an equal weight of almost any nitrogenous substance, such as
a sample of fertilizer, leather, rubber, food, beer; any synthetic
or natural organic substance, as aniline, dyes, drugs, etc. The
melt is now dissolved in water and made up to 500 cc. Although
the heat of dilution of sulfuric acid is sufficient to warm the
solution considerably, we do not need to bring it to room tempera-
ture, provided, of course, we pipette an aliquot portion off at
once at the same temperature. Any error due to high tempera-
ture in the flask will then be compensated by the same error in
pipette and thereby automatically eliminated.
To 5 cc. of this solution are then added 5 cc. of TV NaOH and
then drop by drop of the same solution until it is neutral to
litmus paper. The solution is then diluted to 200 cc. with am-
monia-free water, and a 10 cc. portion is treated with 15 cc. of
0.003 per cent starch solution, precipitated with Graves' reagent
(5 cc), and matched against 10 cc. of standard solution (con-
taining 2.0 nig. of nitrogen per liter) similarly treated. From
the reading and the curve we can find out at once the exact
per cent of nitrogen. In the first step we diluted to 500 cc. ;
and in the second step, when we took 5 cc. for a 200 cc. final
volume, we diluted 40 times, thus giving a total volume of 20,000
cc, or 20 liters. If the standard reading S were 20.0 mm.
we would get for the unknown 39.10 mm., which would give us
21.36 per cent nitrogen1 in ammonium sulfate
1 If the reagents contain ammonia a control estimation, using about
V10 the dilution of above, will give a correction. I, *., a certain fraction of
per cent to be deducted from the per cent of total nitrogen.
Not only will this method save considerable time, but it will
eliminate the expense, attention and errors connected with
a bank of Kjeldahl stills
IOSFHORUS — The estimation of phosphorus in biological
and industrial fields, especially of small amounts, is becoming of
increasing importance. A large number of volumetric and
colorimetric methods have been proposed but thus far none
have been satisfactory for micro-quantitative work While
looking for a suitable nephelometric precipitant for phosphorus.
Kober and Egerer's attention was called to the reagent developed
by Pouget' and Chouchak. This reagent consists of a nitric
acid solution of strychnine and molybdic acid and produces a
very sensitive reaction with phosphates. Pouget and Chouchak
found that it will detect one part of phosphorus in 20 million
parts of water. As the precipitate is slightly yellow and remains
in suspension for a long time, the authors have recommended
it for a colorimetric reagent, but really the estimations were
turbidimetric, i. e , they measured the absorbed light of the
suspension.
On studying the reaction carefully, Egerer and Kober found
that (1) it was not constant and quantitative, and (2) the re-
agent gradually became yellow and deteriorated, probably be-
cause of the action of nitric acid. Pouget and Chouchak realized
this since their directions state that the mixing of constituents
must be made only just before using. After making many
variations of all constituents, no marked improvement was ob-
tained, but on substituting hydrochloric for nitric acid, the solu-
tion not only remained practically colorless for an indefinite
length of time, but was stable and gave quantitative and constant
results.
Variations in Diaphragms of Colorimeters and Nephblombtbrs
Showing a wide aperture as found in most instruments (on the left),
next a pinhole aperture off optical center. The pinhole aperture ,to_the
right) in correct position.
The directions for making Kober and Egerer's nephelometric
reagent for phosphorus2 are as follows:
150.0 g. Sodium Molybdate
250.0 cc. Water
100.0 cc. Hydrochloric Acid (1-1)
Add slowly with shaking
150.0 cc. Strychnine Sulfate Solution (2.0 per cent)
Filter
Protective action in addition to any produced by the strych-
qoI seem to be necessary. The reagent is so sensitive
that ordinary filter paper cannot be used for filtering the reagent,
as it extracts from it a substance which seems to be a phos-
phorus compound, gradually giving a very marked phosphorus
reaction
An idea of its sensitiveness may be obtained by the following
5 909), 104 9 tl91l>. 649.
•■J Am ( lun: - 37 1915 2375.
July, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
;6i
experiment: A solution of potassium phosphate, containing
0.0125 mg. of phosphates, 0.003 nag. phosphorus per liter, still
shows the reaction very plainly which means one part in 333
million parts.
As an example of its usefulness for technical purposes the de-
termination of phosphorus in a sample of cast iron will be de-
scribed briefly. The weighing of the sample, its solution in
nitric acid, and the elimination of the nitric acid by boiling a
few minutes with an equal volume of sulfuric acid require but a
few minutes for completion.
The actual details are as follows :
Two (2.00) g. of cast iron borings were dissolved in 100 cc.
of l/s nitric acid by boiling. After cooling under the tap the
solution was brought up to 100 cc. and 5 cc. taken and boiled
for 2 min. with 5 cc. of concentrated sulfuric acid. This mix-
ture is then diluted to 100 cc. and filtered through a dry, acid-
washed filter paper and 25 cc. are again diluted to 100 cc. 10 cc.
are now treated with 35 cc. of 0.5 N HC1 and precipitated with
5 cc. of reagent. On matching in the instrument with a standard
containing 5 mg. of KH2PO4 per liter the percentage1 of phos-
phorus can be obtained from a curve made similarly to one shown
with ammonia.
(c) calcium — The estimation of calcium, owing to its wide
distribution, is of considerable importance, and, therefore, simple
and rapid methods of estimation would be very valuable. Lyman
first sought to solve this problem by the nephelometric estima-
tion of calcium oxalate, but was not able to obtain satisfactory
results. He then tried, after a preliminary separation of the
magnesium, to precipitate the calcium as a calcium soap. This
method gave excellent results. It reduced the time required
in certain calcium estimations from 3 days to 2 hours for a set
of four estimations.
Lyman's nephelometric reagent for calcium2 is made up as
follows :
4.0 g. Stearic Acid
0.5 cc. Oleic Acid
400.0 cc. Alcohol (95 per cent)
Boil, add
20.0 g. Ammonium Carbonate in
100.0 cc. Hot Water
Boil, cool, add
400.0 cc. Alcohol (95 per cent)
100.0 cc. Water
2.0 cc. Ammonium Hydroxide (sp. gr. 0.90)
Filter
To show its sensitiveness the following experiment is made:
A solution of calcium oxalate in nitric acid containing 0.2
mg. of calcium per liter still gives a decided reaction, which is
one part in 5 million.
For the estimation of calcium in milk, 10 cc. are diluted to
100 cc. with distilled wfater. Five cc. of this mixture are then
treated with 15.0 cc. of 6.5 per cent trichloracetic acid, which
precipitates the proteins, and filtered. The calcium is now pre-
cipitated as oxalate by McCrudden's method,3 redissolved, and
the calcium determined after precipitation as soap, nephelo-
metrically.
Twenty cc. of standard calcium oxalate solution (dissolved
in nitric acid) containing 0.4 mg. of calcium are poured into
50 cc. of Lyman's reagent and gently shaken. This cloud is
used for matching an unknown treated in a similar manner.
Here, as in the other estimations, only a few circumventions
are necessary to eliminate interfering substances.
In this precipitation oleic acid acts as a protective colloid,
a small amount delays the agglutination for hours. •
id) acetone- — Marriott has applied the extremely sensitive
Scott-Wilson reagent for the nephelometric estimation of ace-
1 A check on the purity of reagents should also be made by a blank esti
maUon and corrections made if necessary.
■ J. Biol. Chem.. «9 (1917), 172.
• Ibid , 10 (1911), 187.
tone. The acetone in each case may be distilled from the original
solution into the reagent or may be aerated1 at room tempera-
ture into sodium bisulfite solution, and then estimated nephelo-
metrically.
The composition of Marriott's nephelometric reagent for
acetone2 is given as :
10.0 g. Mercuric Cyanide
180.0 g. Sodium Hydroxide
1200.0 cc. Water, shaking, slowly add
400.0 cc. Silver Nitrate (0.73 per cent)
Filter
To show the sensitiveness of the reagent, a solution of freshly
distilled acetone containing o.oio mg. per liter still gives a marked
reaction, which is one part in 100 million.
The standard and unknown solutions are precipitated by
distilling into 50 cc. water and 15 cc. of Marriott's reagent,
0.5 mg. of acetone and finally making the solution or suspension
up to 100 cc.
Standard solution if made with N/4 sulfuric acid so that it
contains 0.5 mg. of acetone in 10 cc. will keep for a few weeks
at least. Without N/4 acid the acetone solutions quickly
polymerize.
Fig. IX — Silver Chloride Suspensions
The one on the left made by slowly adding 5 Eq. AgNOa solution with
shaking or stirring. All the other equivalents were added at once. Un-
fortunately, the large volumes photographed, which are more or less
opaque, make it difficult to see the differences, except where it shows the
curvature of the bottoms.
As may be observed no additional protective colloid is added,
as the organic nature of the complex is sufficient protection
or, to be exact, makes the speed of agglutination low.
(e) fats and oixs — In quantitative work where the precipi-
tate is easily thrown down, easily washed, and easily dried and
weighed, gravimetric analysis imposes no difficulty, although
it may fail to estimate small amounts. Fats and oils are difficult
to filter and to free from solvent and, therefore, Bloor devised
a nephelometric method which overcomes these obstacles. The
fat or oil is extracted with an alcohol-ether mixture and then
poured into water, when the fats or the oil separate out in fine
globules or suspensions. Bloor's nephelometric reagent for
fats3 is made up as follows:
250 cc. Redistilled Kther
750 cc. Redistilled Alcohol
As accessory
500 cc. Normal Sodium Ethylate
Five-hundredths of a milligram (0.05 mg.) of fat can be easily
determined quantitatively, and a marked cloud is produced by
one part in a million.
The usual standard and unknown are precipitated by running
5 cc. alcohol-ether solution containing 2.0 mg. of fat or oleic
acid into 100 cc. of water and, after adding 10 cc. of 1 : 4 HC1
and gently stirring or shaking and allowing to stand for 5 min.,
are read in the nephelometer.
Murlin and Riche1 have modified tliis method by pouring the
fat solution into 0.05 per cent gelatin solution.' These authors
1 Polio, J. Biol. Chem., 18 (1914), 263.
'Ibid.. 16 (1913), 289.
>J. Am. Chem. Soc, S6 (1914), 1300; J. Biol. Chem.. IT (1914), 377
* Private communication.
J 1 g. gelatin in 2 liters of water with 5 cc. glacial acetic acid.
562
THE JOURNAL OF INDUSTRIAL AND ENGINEERING I HEMISTRY Vol. 10, No. 7
3
>_e-fiT\m"
Fig X
Showing a nephelometric curve (upper) and a colorimetric curve
(lower). The abscissas give the concentrations of substance, in this case
of ammonia, coordinates give the readings. I. e.. the heights of solutions.
Greater accuracy can be obtained by drawing curve to a larger scale.
found that the addition of this small amount of protein as
protective colloid delayed the coalescence of the fat globules and
thereby enabled them to keep the suspensions photometrically
constant for hours.
Woodman, Gookin and Heath1 have worked out a similar
method for the essential oils.
The solvent and extracting medium for essential oils is alcohol
.done and 5 cc. of the standard solution — containing 100 mg.
in 1 • 95 i"i cent redistilled) alcohol — are precipitated by
pouring into 25 cc of water, or better 25 cc. of 1 : 4 HC1.
By adding acid as used in the Bloor method, I found that
one could use a much weaker standard than the authors recom-
mended and Mill get suitable nephelometric clouds. They were
able to estimate the oils of roses, peppermint, anise, and nutmeg
uepheloinetricallv with ease and accuracy.
ROTEINS Proteins like other colloidal substances are
extremely difficult to filter, and when filtered arc rarely free-
enough from adsorbed substances to be useful for gravimetric
work. Also they are dried only with difficulty. The applica-
tion of nephelometrj to protein estimations has been found to
be fortunate for two reasons: 1 It enables us to estimate
small amounts of proteins easily since nephelometry fits protein
suspensions as 1 key does a loi tuse protein suspensions
were so easily produced and maintained that the possibility of
nephelometry as an accurate method of analysis became ap-
parent, just as the difficulties mentioned with silver chloride
prevented, without much doubt, the adoption of nephelometry
for twenty or more years Tin former give a true picture and
the latter a false picture of its possible accuracy and general
1 This Journal. 8 (1916). 128.
usefulness. Kober's nephelometric reagent for coagulable pro-
teins' consists of:
2,000.0 cc. Sulfosalicylic Acid
For Casein, 0.3 per cent
For Globulins. 0.6 per cent
Time does not permit me to go into all the details of protein
estimations, so only a test of its sensitiveness will be given.
A protein solution containing i.o mg. of protein per liter still
gives a marked test which is equivalent to I part in a million.
In milk the fat is first removed, by adding to the diluted milk
(5 cc. of milk in about 200 cc. of water) 10 cc. .V 10 sodium
hydroxide, making it up to 250 cc. and shaking with ether. As
further details will be found in the original communication,*
nothing more will be said except that the nephelometric method
reduced the time for the estimation of casein, globulin, and
albumin in milk. It requires from 2 to 3 days, if it is done ac-
cording to the usual technic, whereas with the nephelometric
method it can be done in 20 to 30 min.
m GENERAL DISCUSSION
There are many more applications which have not been
touched upon, but their development and their application to
analyses do not differ essentially from those just given.
It will be observed that practically all of them are of the
nature of an organic complex, ;'. e., the precipitate has an organic
constituent in its composition. In gravimetric analysis this
would not be an advantage, since it is necessary as far as possi-
ble to have the precipitate in relatively large masses for filtering
and in a condition easy to dry. In many cases the occlusion
and adsorption in gravimetric precipitates is very appreciable.
Show ing a similar
the per cent of nitrogti
be obtained bv drawing
Flo. XI
nephelometric curve but
per 0.1000 g. of sample,
curve to a larger scale.
. giving
:er accuracy can
.' Im I hem. Sot, 35 (1913). 290.
! Ibiii., SB (1913), 1589.
July, 1 9 1 8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
563
In nephelometry, however, occlusions are of no consequence
as the standard, having practically the same occlusion or ad-
sorption, would cancel the error. Of course, it does not follow
that occlusion or adsorption in nephelometric precipitates causes
any difference in the amount of reflected light, as the occlusion
may be in a dissolved phase, and, therefore, would not reflect
light. Furthermore, as organic reactions as a rule are more
specific, and, therefore, more accurate, nephelometry and color-
imetry enable us to make use of organic substances, which means
that our sources of reagents and possible methods are unlimited.
The great advantage of nephelometric analysis over gravi-
metric, outside of the enormous saving in time and labor as well
as in material, is in its more complete control over the media of
precipitation. By the great dilution necessary ordinarily in
nephelometry, color and other interfering substances are so
reduced that they seldom play a role.
The accuracy obtainable in nephelometry, as the instruments
and methods steadily improve in efficiency, is growing rapidly.
With the instrument, as it now is, when properly adjusted and
used, it is not difficult to obtain an accuracy of 0.25-0.50 per cent
in a single reading, and with two to three readings 0.1-0.2 per
cent. Not all nephelometric suspensions have been developed,
however, so that the maximum accuracy of the instrument is
utilized. As in gravimetric work, the accuracy obtainable in
final results depends on the particular method and precipitant,
as well as on the balance. As we have become so accustomed
to gravimetric work, to agglutinate or crystallize our precipi-
tates, it is difficult for most of us to consider doing our work in
an exactly reverse way. Like all other methods it takes time
to get accustomed to a new way of doing things, no matter
how good or convenient it is. Much more progress is made
when the new way is the only way an experiment can be done
at all. We all know when once an old method has been en-
trenched, as it were, by custom, it takes considerable time for
the new to find its way into favor, irrespective of its merits.
Much more work remains to be done, especially the study,
from as many angles as possible of the quantitative production
of suspensions.
Almost all colloidal chemistry, heretofore, the theoretical
or practical study, especially that of colloidal suspensions, has
been qualitative and not quantitative. We need a great deal
more information about quantitative colloidal chemistry for
nephelometry to find its greatest usefulness.
How many more applications nephelometry will find in ap-
plied and quantitative chemistry the future alone will tell.
This much we are sure of: the nephelometric method must be
used for colorless colloidal suspension and for the accurate de-
termination of amounts of material which give no delicate color
reaction and are too minute to filter, but which are daily com-
manding our interest and attention. The use of the method has
already been extended to all classes of substances and since, by
careful work, considerable accuracy can be obtained, its applica-
tion promises to be general in the different branches of chemistry.
SUMMARY
To sum up, attention has been called to the following :
I — A few erroneous conceptions about nephelometry and the
pitfalls of many beginners in nephelometry.
II — The great sensitivity of:
(a) Graves' nephelometric reagent for ammonia, which is
able to detect 1.0 part of ammonia in 160 million of water and
its usefulness in various tests and Kjcldahl estimations.
(b) Kober and Kgercr's nephelometric reagent for phosphorus
which will detect 1.0 part in 333 million of water and its use-
fulness in various tests and in phosphorus estimations applied
to iron and steel as illustrated by an experiment
(c) Lyman's nephelometric reagent for calcium which will
detect 1.0 part in 5 million of water and its usefulness in various
tests and calcium estimations applied to water and milk.
(d) Marriott's nephelometric reagent for acetone which will
detect 1.0 part in 100 million of water and its usefulness in de-
termining acetone quantitatively applied to various distillates.
(e) Bloor's method for estimating fats and oils with which
0.05 mg. of fat can be estimated quantitatively and the presence
shown of 1.0 part of fat in a million of water, its usefulness in
nephelometric fat estimation in milks, and its application in
Woodman, Gookin, and Heath's nephelometric estimation of
essential oils.
(/) Kober's nephelometric method of estimating proteins
which will show the presence of 1.0 part of protein in a million
parts of water.
JII — The advantage of nephelometry, its possible accuracy,,
its enormous field, and its possible future.
Division of Laboratories and Research
State Department of Health
Albany, New York
MUNICIPAL CONTRIBUTION TO CONSERVATION
THROUGH GARBAGE UTILIZATION1
By Edward D. Very
The word "garbage" is commonly used indiscriminately to
define any kind of refuse and is generally considered as a synonym
for "offal," but for the purpose of this paper it is used to define
the waste of both animal and vegetable matter which results
from the preparation of food for human consumption. It is
further limited to that portion of this class of waste which is
collected and disposed of as a municipal function.
When we take into consideration the fact that this material
results from action governed by no set rule or regulation and is,
in fact, subject only to the whim of the individual, there would
seem to be no general statement possible as to the constituents
of garbage, and yet it is found that this class of material, as it
is collected in different parts of the country, does not vary widely
in quantity per capita, weight per unit of volume, or in mechan-
ical or chemical analysis, and it is possible, within reasonable
limits, to make a statement of the average content of garbage.
The average quantity of garbage produced per capita per day
is one-half pound.
The average weight of garbage is 1 100 lbs. per cu. yd.
The average sample of garbage contains:
16 per cent animal matter
79 per cent vegetable mutter
5 per cent rubbish
and it analyzes, approximately:
70 per cent moisture
20 per cent tankage
3.5 per cent grease
1 .5 per cent bones
5 per cent rubbish
Published analyses from the cities of New York, Cleveland,
and Washington show this comparison as follows:
New York Cleveland Washington
Pounds per capita per annum... . 181 193 286
1'ounds per cu. ft 41 4') 47
Moisture, per cent 67 76 74
Laboratory Analyses
Per cent Per cent Per cent
Ether extract 4.85 4.00 5.00
Phosphoric acid as PjOj 0.59 0.24 0.39
Nitrogen, Kjeldahl method.... 0.94 0.64 0.71
Potash as K,<> 0.33 0.30 0.28
The figure lure given for the pounds per capita per annum
for Washington steins at variance with the others, but it must be
remembered that this city has an enormous floating population
which produces garbage but is not considered in the census.
Then, too, in Washington practically all of the hotels and res-
1 Read before New York Section, American Chemical Society.
May 10, 1918.
564
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No.
taurants have their garbage collected by the municipality,
whereas in some cities the garbage is not so collected, but is
taken by private collectors, under an arrangement with the pro-
prietors of these establishments.
The quantity of garbage produced varies by seasons very
materially, the maximum daily a lount being collected during
the summer months when vegetables and fruits constitute the
principal diet, and the minimum amount being collected during
the winter months. Usually August is the highest month,
with about 1 1 per cent of the total annual amount, and February
the lowest month, with about 6 per cent. The moisture content
is ln:s'li in percentage in the su inner months and low in winter,
whereas the grease content and the chemical plant food values
are low in the summer and high in winter, for obvious reasons.
Fresh garbage, as it reaches the can, will remain, in ordinary
weather, at a temperature of about 700 F. for from 12 to 14
hrs. before any change takes place From that time alcoholic
fermentation sets in and this will continue for another period
of, approximately, 12 to 14 hrs. If the can is loosely covered,
acetic acid fermentation develops, but if cans are fairly well
closed, the alcoholic fermentation continues for about 36 hrs.,
when there is practically no further action. There is no de-
composition of the animal matter, as that is inhibited by the
alcoholic fermentation. By test it has been found that in
garbage which has remained in the can under ordinary tempera-
tures for from 3 to 4 days, and even as long as 2 1 days, the free
fatty acids of the grease are not more than fro 1 5 to 7 per cent,
whereas where matter of a like nature is subjected to putrefactive
action, the grease analyzes from 30 to 40 per cent of free fatty
acids, which indicates the absence of decomposition in ordinary-
garbage as it is contained in the can.
The fermentation noted develops small amounts of alcohol
and acetic acid, with slight changes in the vegetable oils, but
none in the animal oils.
The sour odor of garbage is the result of this fermentation
developing acetic acid, together with certain fruit esters, alde-
hydes, and alcohol.
We have then a material made up of a combination of moisture,
fat, starch, sugar, albuminoid and nitrogeneous bodies, cellulose,
and ash. The problem is to recover from this mass whatever
may be of value, in the most economical manner, having at the
same time due regard for the sanitary requirements.
Disregarding the method of final disposition of municipal
wastes which attempt no reclamation of by-products, we find
the methods which have been adopted for the treatment of
garbage, as herein defined, are pig feeding, or some mechanical
treatment commonly known as reduction.
According to the latest statistics, there are in the United
States, 75 cities of 90,000 population and upwards; of these,
13 resort to dumping or burial, 21 have incinerators, 11 feed to
pigs, 6 sell or give to farmers,' probably to be used for pig feeding,
and .'4 use a reduction process.
Those who have reduction plants are:
Boston, Mass. Baltimore, .Mil.
New Bedford, Mass. Washington, D. C.
Bridgeport, Conn. Akron, Ohio
Buffalo, N. Y. Cincinnati, Ohio
New York, N. Y. Cleveland, Ohio
Rochester, N. Y. Columbus. Ohio
Syracuse, N. Y. Dayton, Ohio
Utica, N. Y Toledo. Ohio
Philadelphia, Pa, Indianapolis, Ind.
Pittsburgh, Pa. Chicago, 111
Reading, Pa. Detroit, Mich
Wilmington, Del. Los Angeles, Cal
The feeding of garbage to pigs is a matter which caused cou-
siderable discussion, both as to its economical phase and also
as to its propriety from the standpoint of sanitation.
Tersely, the advantages of pig feeding have been stated as
"using the pig as a middle-man. we find that 25 per cent of the
protein and 45 per cent of the total energy is returned to the
consumer as pork. The pig charges 55 per cent brokerage for
converting vegetable protein and fat into animal protein and
fat."
Of course, we must remember that there is a considerable
portion of the garbage that the pig will not consume, such as
fish scrap, fruit skins, coffee grounds, and miscellaneous rubbish.
Then, too, the garbage must come to the piggery' fresh, especially
in the summer time.
Again, there is the menace of hog cholera, or the foot and
mouth disease, which may cause the total loss of "plant."
To be sure, modern science is ready with methods of prophylaxis,
which may prove a safeguard, but there is always the peril of
slip-shod methods, which result in a partial or complete loss.
The United States Food Administration, in a booklet entitled
"Garbage Utilization," issued in February 1918, says:
"We have indicated that the reduction process is hardly suit-
able for cities of under 100,000 population. A proper question
would be, is pig feeding more applicable to cities now reducing
than the reduction process?
"In so far as the monetary return applies, the two methods are
practically identical. The reduction process possibly has the
advantage of improvement to a greater extent than pig feeding.
By improving the breed of the hog, gains might be made more
economically, but the reduction process requires only simplified
machinery, or additional recovery to make a ton of garbage
more valuable.
"It also seems that the larger the city the less adapted its gar-
bage to pig feeding. One might say that smaller cities were
better managed, but it is obvious that the difficulties of con-
trolling materials placed in the garbage increase more rapidly
than does the population. Although a pig is blessed with a
digestive system capable of assimilating almost anything, its
efficiency cannot be compared with the mechanical digestors of
the reduction plants.
"While from a purely conservation standpoint, pork produc-
tion may seem more important than the production of grease
and fertilizer tankage, the use of the grease recovered releases
an equivalent amount of edible oils, while our stock of agricultural
fertilizers is so depleted, at the present time, that fertilizer tankage
is a national resource not to be overlooked.
"The test of the practicability of the feeding method of disposal
is the selling possibilities of the pork produced. There is no
benefit in feeding if the pork is unfit for food, or if a popular
prejudice will prohibit it from selling freely.
"We have not been able to find any market where garbage-fed
hogs are being sold at a lower price than grain-fed animals.
"There is at present a mistaken idea throughout the country
as to the value of garbage. In a large number of cases it is a
question whether the value will be sufficient to pay the cost of
collection and transportation. Where collection and disposal
both are to be made by the contractor, we doubt if the work
will be done without cost to the city, unless the quality of the
garbage is exceptional, and there is keen competition for the
material.
"The ratio of 1 lb. of marketable pork to 50 lbs. of garbage has
already been established. With pork on the hoof at 15' j
cents, this would give a gross feed value of $6.20 to a ton of
garbage. In a general way, it is safe to assume that the cost of
disposal, after the farm is reached, including overhead charges
at the farm, would not exceed S3. 00 per ton."
Reduction processes now in use in this country are of three
types, the drying method, the cooking method, and the Cobwell
process.
In the drying method the green garbage is first deposited on
a floor or belt to facilitate the picking out of the bottles, tin cans,
and similar refuse. The material is then fed into a disintegrator,
either of the chopping or the crushing type, wherein the garbage
July, 1018 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
565
is ground to a fairly uniform size throughout, to allow of efficient
drying and percolating action. From the disintegrator the
material passes through a direct heat dryer so that the moisture
content may be reduced. It is then fed into a percolator, in
which, by the action of a solvent, grease is taken out and re-
claimed, leaving a resultant tankage fairly free from both grease
and moisture.
The dryer consists of a revolving cylindrical steel shell, fitted
with lifting vanes, which keep the material moving toward the
discharge end and at the same time draw it to the top of the
cylinder and drop it in a film through the hot gases, which are
passing through the dryer from a furnace to the stack.
The percolator may be either of two styles, a stationary vertical
or a horizontal rotary.
The former consists of a cylindrical tank, into which the
garbage is fed through an opening at the top. When filled
sufficiently, a heated solvent is introduced through perforated
pipes at the top, and this solvent percolates through the mass
and is withdrawn at the bottom, taking with it the grease which
it has absorbed in its passage. This introduction of solvent is
repeated until the outgoing liquid appears to carry too little
grease to warrant further attempt at recovery. Live steam is
then introduced into the percolator at the bottom, in order to
drive off, so far as possible, the solvent which has been taken
up by the tankage. The tankage is then taken out of the per-
colator, through a door near the bottom, by means of a hoe,
rake, or some similar tool.
Results from the stationary vertical percolator are unsatis-
factory, principally because the solvent jets usually form channels
through the material by which the remaining solvent finds its
way to the bottom without having been in contact with a con-
siderable portion of the material being treated, thus resulting
in an incomplete recovery of the grease. Similar channels
are formed by the steam, thus giving an equally incomplete
result in the driving off of the retained solvent.
The horizontal rotary percolator consists of a cylinder, having
three openings on one side for receiving and discharging the
tankage. There are three pipe sections running the full length
of the cylinder inside, perforated for the spraying of the heated
solvent on to the material being treated. There is also a burlap-
covered strainer-plate, made of brass cloth, extending the full
length, and so supported as to form a chamber beneath, into
which the saturated solvent, after passing the strainer, passes
to an outlet at one end of the cylinder. There are vapor lines
for the introduction of the steam.
The operation of this percolator is as follows :
The percolator is charged by feeding the material to be treated
through the three charging openings. The covers of these open-
ings are then put in place and securely bolted. The cylinder
is then revolved a one-quarter turn, thus bringing the solvent
pipes to the upper side and the strainer chamber to the lower
side. Heated solvent is then pumped into the cylinder in suffi-
cient quantity to fill all the voids and to completely submerge
the material. This solvent is allowed to stand for about 10
min. and is then withdrawn by pumps, after passing through
the material, becoming thoroughly saturated, and passing through
the strainer. This operation is repeated until the outflowing
saturated solvent appears to carry insufficient grease to warrant
further attempt at reclamation. After the final washing and
after all solvent possible has been withdrawn by the pumps,
live steam is introduced into the cylinder under a pressure of
from 15 to 20 lbs. per sq. in. This pressure forces out the major
portion of the remaining solvent through the strainer. The
cylinder is then revolved so that the three openings are at the
bottom and the tankage is emptied through them onto the floor
01 into a conveyor.
The saturated solvent from the percolator, in either case, is
piped to a still, wherein, by the application of heat, the solvent
is driven off as a gas, leaving the grease to be withdrawn, sepa-
rated from any water present by gravity, and then barreled for
shipment. The vaporized solvent is then condensed and re-used.
The last two washings are usually used for primary washing
in succeeding treatments because they are imperfectly saturated
The tankage from the percolator' is passed through a dryer
and thence to a screen and that portion which fails to pass
through the screen is taken to a grinder and pulverized and again
sent to the screen.
This method is practically the first used in this country and
is still in use in Chicago, Allegheny City, and Buffalo. It is
the cheapest when first cost is considered, but the results are
in proportion to its cost of installation, and so, while as an in-
vestment it may prove satisfactory, it still does not give the
full possible recovery of grease. In the drying of the material,
carbonization takes place, which affects the quality of the grease
and tankage adversely, and also in this part of the process there
is a very considerable loss of ammonia.
, This method is operated with a considerable resultant nuisance
from odors because of the great volume of gases passing off from
the dryers, which cannot be economically deodorized.
According to test made in Chicago, which is probably repre-
sentative, by this process, 46 lbs. of grease per ton were recovered.
In the cooking method the garbage is picked over for the re-
moval of the glass, tin cans, etc., and is then fed into large
vertical tanks, known as digestors or autoclaves.
These tanks, when filled, are sealed by a bolted cap, a small
quantity of water is added, live steam is introduced and the
mass is cooked, under pressure, until the whole has become a
pulpy mass, with the grease sacs ruptured and the entrained
grease released. The material is then pressed to express what
moisture can be mechanically released, the material then passes
to the dryer, thence to the percolator, to the redryer, the screen,
and then to storage.
The expressed moisture is piped to a settling tank or basin,
wherein the grease separates by gravity, is skimmed or pumped
off and placed in tanks to allow the final separation of the grease
from whatever slight amount of water is present, and then the
grease is drawn off and barreled.
These types vary usually and only in the manner of pressing.
In one type the pressing is done in the tank, there being a
perforated plate fitted just above the bottom, and pressure is
obtained by the introduction of five steam at the top, resulting
in the material being compressed and the expressed liquid being
forced through the perforations to the pipes leading to the settling
tanks or basin.
Another uses a roller press, having an endless perforated metal
belt, which, after receiving the material, passes between rollers,
causing the fluid to pass through the perforations to the pipes
leading to the settling device.
Another uses the old cider press, wherein the mass is fed into
forms made up of slats covered with burlap, which are built
upon a car and are then placed under a hydraulic ram, causing
the expression of the liquid through the burlap.
Then there is the curb press, wherein the material is fed into
a latticed steel basket, which later is run under a hydraulic ram.
The steam cone press is also used. This press is in the form
of two bottomless cones, lying horizontally, with their bases
meeting, and fitted with a bottom of perforated plates. After
the material has been fed into this form, steam is applied and
the liquid is forced through the perforations.
The operations of this method, which follow the pressing, arc
similar to those described for the drying method after the dis-
integration, except that some operators attempt the reclamation
of valuable portions of the tankage which are carried away in
suspension by the expressed liquid. This reclamation is made
up by the use of triple-effect evaporators and results in a gelat-
inous material, known as "stick." which is added to the tankage
drying and adds something to the fertilizing value,
In the cooking method, the materia] 1 1 ing objected to pres
in. and high temperatures gi ultant grease wherein the
free fatty acids and glycerin are split to a great extent, causing
erable loss of glycerin, and unsaponifiable bodies arc
566
////. Jul RA I/. i'l- INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 7
formed to an undesirable extent. Then, too, the starches and
sugars arc changed to glucose and dextrin and are more or less
caramelized and even carbonized, leaving them indigestible and
of small nutritive value. The albuminoids are broken up and
rendered difficult of digestion. The final product is made up
principally of cellulose fiber with small amounts of nitrogen and
bone phosphates. This material is under suspicion as a fer-
tilizer as to its availability because of the length of time neces-
sary for the chemicals to be released in the soil.
This method is in use in all of the cities of the country using
reduction methods, except those noted above and New York,
Los Angeles, and New Bedford.
The operation of this method is usually the cause of con-
siderable complaint because of the odors which arise from the
emission of gases, fumes, and liquids consequent to the different
processes, but there are reasonable means for the elimination
of those noxious features which can be used, although their use
entails a consequent reduction of the value of the reclamations.
Reclamation of grease by this method varies from 50 to 80
lbs. per ton, depending upon the efficiency of the individual
plant.
We now come to the Cobwell process, and while I desire to
avoid any appearance of taking advantage of your courtesy by
introducing a trade argument, I am forced to use this trade name
as there is no other means of differentiating this method from
the others, because in theory and practice it differs materially
from them. In order to carry out my intention to present facts
to you without any prejudice, I take the liberty of quoting
verbatim from a paper read before Section D, Engineering, of
the American Association for the Advancement of Science,
in December 1916, by C. R. Tuska, consulting engineer and also
lecturer on municipal waste disposal at Columbia University,
who is in no way connected with the company which controls
this process.
After describing the other methods and their results, Mr.
Tuska said:
The operation of this process is as follows :
The raw garbage is placed in a closed tank which is sealed
air-tight. This tank or reducer is constructed with jacketed
walls and jacketed bottom. Into these jackets the steam,
which is used in the reduction of the garbage, is delivered,
these jackets being so designed that it is impossible, under
proper operation, for the steam to enter the tank or come in
contact with the garbage. In the interior of this tank there is
an agitating device operated by power from the exterior. When
the proper charge of garbage has been placed in the reducer
and the covers placed thereon, the tanks are sealed and the
solvent is pumped into the reducer and steam admitted to the
jacketed walls. The heat from the steam which is transmitted
to the garbage through the walls of the reducer, causes the
evaporation of the solvent and the water in the garbage.
Garbage is usually composed of over 75 per cent by weight
of water. The steam heat vaporizes the solvent and the water
from the garbage and these mixed vapors are drawn off from
the reducer to the condenser. The economy in this method of
evaporation rests in the fact that water is vaporized at a lower
temperature when evaporated with a solvent having a low boiling
point than when evaporated without such solvent.
The mixed vapors of the solvent and water, while in the con-
densei together, are conveyed to a closed tank. < twing to the
solvent being of lighter specific gravity than the water, the
solvent and the water are separated by gravity, the solvent
rising to the top from which it is drawn back to the storage
tanks from which it is pumped back to the reducers and used
over and over again. The condensed water which has been
largely (hinted, owing to the- jet condensers used, is discharged
into sewers or waterways
When the garbage has been thoroughly dried by this method,
the solvent is pumped into the reducer and dissolves the grease.
The solvent With the grease is drawn off into a closed tank or
evaporator where the same is heated by steam pipes, where the
steam is kept separated from the grease. The solvent therein
is vaporized and Carried to a condenser where the same is again
liquefied and carried to storage tanks to be Used
After tile grease has been extracted from the garbage in the
reducer, tin garbagi is further dried by means ol the steam in
the jacketed walls and is now in the form of degreased garbage
tankage, which is used for fertilizer purposes, after being ground
and scp
It will be seen from the above description of the process that
if there are any leakages or vents in any of the tanks or piping
where the solvent is handled, more or less solvent is lost, and
thereby a substantial additional expense is imposed upon the
operation of the system. It is evident, therefore, that it is to
the financial interest of the owner of the plant to see that the
same is properly operated.
Furthermore, under this system, the garbage is at no time
brought in contact with the atmosphere, from the time of its
original entrance into the reducer until, after 12 hrs. of cooking,
it is finally discharged therefrom as finished products, dried,
sterile, and practically odorless. These finished products are
grease and the tankage above referred to.
It will be seen by the description that the process is one of
straight dehydration, and from the time the material is at the
boiling point, no further chemical action takes place. Xo process
of "digestion" occurs, and, therefore, the odors and gases in-
cidental to such process are not created. Only the volume of
gas contained in the raw material is driven out and only the
essential oils of an extremely volatile nature are carried over in
the current of steam and soh ent vapor evolved. That little
or no conversion takes place in the operation is shown by the
fact that in the dehydrated material, at the end of the operation,
there exists practically the same amount of unconverted starchy
bodies as existed in the garbage at the time of its entrance into
the reducer
The water condensed contains all the gases evolved and has,
when fresh, a slight odor of the mixed essential oils. Some
traces of alcohol are detected in the effluent and a very small
quantity of fixed oils is carried o\'er. Any ammonia evolved,
if it has escaped the acid in the garbage, is neutralized by acid
carried over in the vapor. Whatever albuminoid ammonia
exists in the effluent is carried over by mechanical entrainment,
as dust particles, during tin straining out of the solvent.
The effluent from this process consists of almost pure water,
this water being the condensed moisture drawn from the re-
ducer while the garbage is being treated and from which the
solvent has been extracted as completely as possible. The
effluent is cold and gives forth no steam or vapor and is prac-
tically odorless, and, as a result, can have no effect when run
into a large body of water
Mr. Tuska's paper continues to give some very excellent data
on this subject, but I will refrain from quoting further because
my time is limited.
The grease, which is the principal by-product from garbage
treatment, is a combination of glycerol and fatty acids, the
principal fatty acids being palmitic, stearic, and oleic. At the
pres< ut time this is sold as recovered and the purchaser refines
it and obtains glycerin, stearin, stearic acid, red oil, candle tar,
and soap fats.
The glycerin content of grease from the reduction methods,
other than Cobwell. runs from 5 to 6 per cent, the
free fatty acids from 18 to 40 per cent. In Cobwell the glycerin
runs from 7 to 8 per cent and the free fatty acids not to exceed
10 per cent. The purchaser demands that saponifiable shall
run about 97 per cent
While there are many solvents which might prove available
in this work, economy has reduced the numl>er to gasoline or
kerosene distillate, and engine distillate has been used In
Using an economical solvent due regard must be given to the
practicability of freeing the grease and tankage from any residue
from it at the end of the process
U to the cost of a reduction plant, it is impossible to make
a general statement, as SO much depends upon local conditions,
and also the cost of machinery vanes as the market price of
July, 191!
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
S67
steel fluctuates. However, it is usually estimated that a cooking
method plant will cost, approximately, $1,500 per rated ton with
steel at 3 cents per lb., while the cost of a Cobwell plant will
be about one-third more than this. In net recovery values it
is generally stated that for the cooking method $2 .00 per ton is
a fair average, while Cobwell gives, approximately, $1.00 more
per ton. The only safe method of estimating is to analyze
the material in each case. I have no definite figures as to the
drying method.
While in most of the cities the disposal of garbage is done by
contract, and in the majority of cases a bonus is paid to the con-
tractor, the following cities receive payment from the contractor:
New York At the rate of about 45 cents per ton
Los Angeles At 5 1 cents per ton
Minneapolis has just closed a contract for pig feeding at a
revenue of $1.26 per ton, and Richmond, Va., under the same
system, expects to receive $2.00 per ton. Denver was the first
to adopt pig feeding under contract, without the payment, and
is doing so at no cost to the city nor is anything paid to it.
These figures appear very attractive, but it is well to be con-
servative as to the expected revenues from this source, as this
system is, as yet, under trial and the result of the experiment
will only be assured when a renewal of such contracts show that
the contractor has been successful in operating under such a
method of payment. An inspection of successive reports from
the cities which operate municipal reduction plants gives a very
good idea of the uncertainty of the revenue derived from year to
year.
I am very much impressed with the patriotic purpose
evidenced by this association in giving so much of its
valuable time to the study of the subject of municipal waste
disposal, with the intention of performing a civic duty in en-
deavoring to promote more efficient methods and better financial
results, if possible, through the employment of the high pro-
fessional skill of its members, and I, therefore, take the liberty
of calling your attention to the fact that the United States
Food Administration recommends that at this time such energy
be used in obtaining more efficient operation of existing methods
rather than the evolution of new methods.
Cobwell Corporation
50 Church Street
New York City
AMERICAN GARBAGE DISPOSAL INDUSTRY AND ITS
CHEMICAL RELATION1
By Raymond Wells
It is undoubtedly true that before the world war there were
chemists in this country and that they were doing most wonderful
and useful work, but we were so bewitched by the work done by
German copyists and grinds, that when the awakening came, we
were astonished to find that the animals at home were likewise
endowed with horns and of no inconsiderable magnitude.
At once every industry that had ever thought of the possi-
bility of chemical assistance obtained three of this rare species,
and those that had never thought of it at all clamored for at
least one. Every business, industry, and manufacture wished
for this strange new thing — "scientific control," obtained it
as best it might, and found it good. Of course there may be
some things the chemist cannot do, but they do not exist in the
popular mind.
An industry at this date without a chemical advisor, director,
or, at least, a plain ordinary "lab. man" is in the same class
with the great auk, and yet there have been explorers who
have claimed to have seen specimens of this rare bird, even a1
the present time. It does not take an explorer to locate the
1 Remarks following Mr. Very's paper, New York Section, American
Chemical Society, May 10, 1918.
"garbage industry," but it might prove a stiff task for anyone
without the natural instincts of the lowly ferret to find more
than one or two even "lab. men" in the business, leaving out of
consideration a "regular chemist."
An industry has grown up in this country, taking care of the
household table and kitchen waste of 17,000,000 people, serving
twenty-nine large cities and returning an annual revenue from
the by-products of this service amounting to $11,500,000. At
the same time disposition is made of 1,200,000 tons of raw
garbage, from which, disregarding the monetary return, the
nation is the richer by producing from its own so-called waste
70,000,000 lbs. of grease and 175,000 tons of valuable fertilizer.
And such an industry is practically without a chemist or without
even being given recognition by chemists as being one of the
few unexplored fields, for their efforts, at the present day.
The disposition of garbage with recovery of the by-products
is essentially a chemical problem and its neglect has been due
to several causes. The attitude of all or of practically all men
or corporations engaged in the business, has been one of antagon-
ism toward chemists, either as individuals or as representatives
of science. They were not very unreasonable in this, since all
of those chemists attempting to work or to improve the garbage
business, did so by long range treatment of garbage as it ought
to be from a theoretical standpoint, and from their knowledge
of some other business in their mind similar to it. It is not like
any other business under the sun, so they fell down most lamen-
tably and the so-called "practical swill man" stood off and scoffed.
The "swill man," satisfied with partial success, with sometimes
profit and sometimes loss, but with the profit just enough in the
right pan of the balance to keep the attraction always there,
did not like the idea of disturbing things which had been done,
and was thus prevented from asking anything of science. His
whole attitude has been one of secrecy about the simplest of
operations and one of horror at the idea of starting anything
which might or might not turn out to their pecuniary advantage.
Don't blame the swill man for his attitude. He set out to
make something out of nothing, out of something which every-
one turned away from, about which no one knew anything, and
in approximately thirty years built up a real industry, without
assistance from anyone. It was all "try it and see," and after
a period of several years something was arrived at, which was
moderately satisfactory and sometimes made a little money.
After that, why change? Changes meant increased invest-
ment, possible big financial failure — better to jog along and keep
quiet, taking all that could be obtained and when not obtained,
slip it over quietly to the next chap.
Seeing this attitude and not looking into what promised only
to be a dirty, disgusting hot, sweaty business, where things
were accomplished by rather circuitous methods at times, viewed
from political and engineering standpoints, the chemist with-
drew to more savory and apparently more promising fields.
As a matter of fact he chose, as usual, the line of least resistance.
In spite of this neglect from the chemist, the business has
prospered and is doing very excellent work for the city and for
the nation. A short time ago the city and the nation woke up
to the garbage situation and were surprised to find that a real
industry existed. Immediately propaganda started and con-
tinue to start, which is well, for out of them may grow an in-
terest both popular and scientific, valuable to the industry and
to the nation.
Before venturing too far in denouncing our nation as a nation
of wasters and as a nation neglectful of its waste materials,
it is well to consider all of the facts in the case.
For instance, the largest city in the United States has the
largest garbage plant in the world and the most up-to-date
one from the chemical and engineering standpoints, representing
thi effort and financial hazard of many men. This plant possesses
the fine qua «»» "f the swill business, it is sanitary and does not
568
THE JOURS l/. OF tNDUSTRJAL AND ENGINEERING CHEMISTRY Vol. to, No. i
commit a nuisance either in the legal sense or actually. It
takes care of the waste food material from 6,000,000 people,
amounting even at the present time of conservation, to an average
of 800 tons daily or 320,000 tons per annum Xot one particle
nf this material is wasted. Only the water is eliminated and
that as distilled water. In one operation the garbage is trans
formed or separated into 19,200,000 lbs. of grease of a value of
S2, 200,000 and at the same time 64,000 tons of tankage of a
value of Si, 000,000 are produced. Several other items, as rags,
bones, etc., give an additional value of several hundred thousand
dollars. Aside from the money value, this grease recovery
means to the nation 1,344.000 lbs. of "dynamite glycerin"
and over 150,000,000 cakes of soap. The fertilizer value of
64,000 tons of tankage makes fertile many acres, at a time when
the nation is starving for fertilizer. This grease all enters the
soap, candle, and glycerin industry and constitutes no small
source of supply, and the fertilizer manufacturer regards garbage
tankage as a most valuable "base goods." These materials
are in no sense low grade and they find a ready market. This
one plant employs several hundred men and consumes daily
200 to 250 tons of coal and 3000 to 4000 gal. of kerosene. ■ Kero-
sene is used for percolation on a huge scale, an innovation in
the percolating line which no other industry conceived of or
dared to try on a large scale. When it is noted that in the regu-
lar course of operation 300,000 to 400,000 gallons of solvent
are in constant use, and that still capacity for solvent recovery
of 500 000 gal. actual operating capacity per 24 hrs. is required,
then one can realize what the industry in one plant means.
This is the largest of 29 garbage reduction plants in the country.
All of our largest cities have them, only a few of the medium-
sized cities still being unenlightened and sticking to the pre-
historic and very7 European method of expensively burning
valuable material. These twenty-nine cities produce the quan-
tities of material mentioned in a preceding paragraph. Xot all
of them have perfect plants, not all of them utilize all of the
values in the garbage, but they are performing a public duty
and doing it efficiently, as far as their equipment makes it
possible.
It is hoped that the preceding statements may lead to the
realization that a big industry of great value, not only from the
conservation standpoint, but from that of public service and
health, has been built up quietly and without attracting, till
this time, any public notice or any notice from the scientific
world.
The industry' is doing very well, it has improved much after
a sleep of twenty-five years, it has at last a real method, now
operating four years, which is the best yet and promises to be
better in the near future, but even now the whole business is
nothing more than a healthy embryo, which will require many
years of patient work on the part of many patient chemists to
incubate to a real live animal and then it will have to grow.
Analysis op Sample of Average Household Garbage
Per cent
Moisture . . , 71 .00
Grease 4.54
Protein 4 . 24
Ash.. 2 17(a)
Fiber 3.21
Cane Sugar 0.77
Invert Sugai ... 0.50
St.ir.-h Dextrin et< 10 46
Alcohol ii ;•-
Acid as Acetic 0.17
Essential Oils
Ethers, etc Oil
a Potash, bone phosphate, lime, silica, etc.
That it is a chemist's problem the foregoing analysis will
demonstrate Garbage is a conglomerate of all the odds and
ends of all the things which men eat, a mixture of every
naturally occurring organic material Think of it in terms of
this typical analysis and see if it does not suggest oppor-
tunities.
This analysis does not total ioo per cent, since none of the
determinations were made "by difference."
The opportunities suggested by such a mixture offer for re-
search almost virgin soil. And this field has never been touched
by our erstwhile German rivals. A nation which is lucky to
get garbage to eat, has no garbage problem to solve. Many
urge that we too should have no garbage cans. It may be so
some day, but not for several generations and jt is a very nice
question, whether with proper methods of utilization, it may
not be as economically profitable to so utilize it and not attempt
to force on the human anatomy that which is unattractive and
unpalatable. It may be better to let a mechanical digestive
tract turn less easily digested materials into substances of greater
value for other purposes than for food. Maybe it is better to
throw away rancid fat, tough sinews, and potato parings and
have the same come back as soap, fertilizer, and alcohol and
eat the vegetable oils, animal fats, and the grain released by such
an exchange Nothing is ever destroyed. It can be badly
mixed up and out of place, that's garbage. It is the duty of
science to put it back into place, and chemistry is the one science
most urgently called upon.
Homer. X. V.
THE POTTERIES AT SHEK WAAN, NEAR CANTON,
CHINA
By Clinton N. Laird
Received March 12, 1918
The prevalence of white ants in South China restricts the use
of wood as a building material to a minimum, and therefore all
but the most temporary' structures are built of brick with tUe
roofs. The bricks used range from sun-dried, in the poorest
villages, to well-burned gray or red of various dimensions. They
are made at many different places. The tile are of two kinds, a
pan tile, 9 in. square, curved like a shallow trough, and a round
tile, approximately half of a truncated cone. The latter are
laid in rows over the joint between the vertical rows of overlap-
ping pan tile. These round tile are often glazed but the pan tile
very rarely Most of the common unglazed tile, of different
grades, used in and near Canton, are made in Fa Uen district,
about 30 miles north of Canton. The only place where any
glazed roof or fancy tile or other glazed earthenware articles are
made in South China is at the village of Shek Waan, about 20
miles west of Canton.
The pottery industry there is said to be over 700 years old.
When the process for glazing earthenware was developed is not
recorded, but as one of the temples in Canton has a glazed tile
roof (never relaid and still in good condition .1 known to have been
laid 400 years ago, the process is not one of recent origin. At
this village are made earthenware jars and dishes of all kinds,
clay idols and figures of men and animals, and, in recent years,
tile pipe, as well as the glazed ware of many kinds, in color chiefly
brown, green, blue and yellow.
For some unknown reason or reasons, possibly through con-
sideration of both beauty and expense, the use of colored glazed
roof tile was restricted long ago to temples and imperial buildings.
Other blue and green articles made of the same materials in the
same way have had a wide use in private buildings, and after the
First Revolution (191 1) the restriction on the use of glazed roof
tiles was removed General use, except by foreigners, will
probably not become common for many years, however, because
of the strong association between the tiles and temples. I have
been told by one who has travelled widely in the interior of China,
that the only place he has seen the green roof tile used on build-
ings other than temples is at Peking where they are used on the
tombs of the imperial concubines. The imperial buildings in
July, 1918
THE JOURNAL OF IX DUST RIAL AND ENGINEERING CHEMISTRY
56Q
Peking and the imperial temples throughout China were the only
buildings having yellow tiled roofs.
The original deposits of clay at Shek Waan were exhausted
long ago, and now all the materials are imported. The clay,
Fig. 1 — The Mi
Machine1
which varies in color from a cream, streaked with red, to a dark
gray, comes from two places, the more plastic from Tung Koon
district, about 40 miles east of Canton, and the stiffer from Fa
Uen district where the ordinary' tiles are made. It is all bought
at Shek Waan of the people who bring it there in boats from the
districts named. The fuel used is wood, which comes down the
river in rafts from the province to the west. It is cut to size and
dried across the river from the village of Shek Waan. The pot-
teries are low, one story structures, cheaply built and poorly
lighted, but the workers are protected from the heat and glare of
the tropical sun.
The article to be made will determine the relative proportions
of the two kinds of clay used in any batch. Sand is mixed with
the clay in the proportions of one part sand to four parts clay to
lessen the danger of cracking in the firing. Nearly 2300 pounds
of clay and sand are mixed at a time by one man who mixes it
with his feet, by tramping on it, adding a little water from time
to time to make it work easier. This is said to be the original
method, and the workmen claim that it can be done more thor-
oughly this way than by machinery. Two batches are mixed
by each man in a day, working 4 hrs. on each batch. Large
lumps of clay, when mixed, are stuck up against a wall to dry
for a day or two, depending on the weather, before being ready
for use.
Three methods are used at these potteries for making the various
articles : some are formed on the wheel, others in a mold, and sonic
are modeled by hand. They are glazed in practically the same
way and all are burned in the same kind of kiln. The chief
articles made on the wheel are earthenware dishes, pots used in
cooking, and covers for certain kinds of jars. The clay comes to
the potter wet. His wheel, nearly 2 ft. in diameter, is mounted
on a pin which rotates in a block set in the ground so that the
upper surface of the wheel is only a few inches from the ground.
The potter sits on a low stool. At his left, close to the wheel,
1 Because of the Chii esc superstition that a man will never be able to
do a kind of work different from that which hi- was doing when his
picture was taken, it is very difficult to net satisfactory pictures of the men
at work
is a flat dish about 10 in. in diameter, partly filled with rice straw
ashes, and at his right, also close to the wheel, is a vessel contain-
ing water. With his left hand he picks up a ball of clay from the
dish and with his right hand dips up a little water to moisten
the clay. The wet clay is then put on the wheel which is turned
by his assistant. Working from the center out he shapes the
vessel, holding his thumbs in and his fingers out. The assistant,
generally a boy, propels the wheel by striking its upper surface
with his right foot as he swings it back, a running motion. Be-
fore giving the first impulse to the wheel he picks up a lump of
clay which he rolls into a ball while kicking the wheel. He then
throws the ball into the dish at the potter's left on to the gritty
ashes which make the bottom of the vessel, when finished, a
little rough so that it will not stick to the wheel. The boy then
takes a piece of flexible bamboo which he holds between his hands
in the shape of a U. This acts as a spring to help keep his hands
far enough apart so that he will not deform the dish as he picks
it up from the wheel and sets it on a board. When the ^heel is
empty the potter puts on another lump of clay and begins work-
ing it. As soon as the boy has put down one dish he picks up
another lump of clay and begins kicking the wheel again. The
performance is repeated until the board is full, when work stops
while the boy puts the board up into a rack over head where the
dishes dry until the next day. They are then put out into the
sun. I have seen the simplest form of dish, about i>/« in. deep
and 6 in. in diameter made in 8 sec, though this would be under
the average time. A day's work for the pair would be 1500 or
more of these dishes. Larger vessels take more time, and more
kicking by the boy who has no chance to kick with his left leg
occasionally for a change.
These earthenware dishes, used chiefly in the household, are
glazed only on the inside. The glazing material is wood or rice
straw ashes, mud from the river bottom (the fouler, the better,
according to the workmen), and water, forming a muddy cream.
Some of this is poured into the sun-dried dish, and, with a short
turning motion, most of the inside of the dish is covered with the
cream. The rest is poured out. The dish is allowed to dry be-
fore being taken to the kiln to be fired. The final color, after
burning, is a dark brown.
All the jars, roof and window tiles, tile pipe, etc., are formed in
molds. A wooden model is first made and from it the clay mold.
This is burned from 4 to 6 hrs. in a moderate fire; too hot a fire
will ruin the mold. The clay is worked stiff and shaped into a
large lump with straight sides of such a shape that a slice cut
) sely through the lump for use in the mold will be of the
right shape and dimensions for the particular article to be made.
This lump is placed on a smooth table and cut into slices from
1 ', in. to */t in. thick. The workman then selects two flat bam-
boo sticks, notched on the sides at the proper intervals, and,
57°
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 7
holding in those notches a wire kept tight by a bow, pulls the
whole towards him through the lump of clay, the bottom ends
of the guides sliding along the table. He then drops the wire
down a notch and cuts another slice, thus working from top to
bottom through the lump.
Fio. 3— Ct
Slices of Cl
The slice of clay is placed in the mold and pressed into position
with the fingers. Then it is taken from the mold and sun-dried
for 2 hrs. If the article is, say, a lattice work tile to be used
in windows instead of glass, the two complementary pieces are
then put carefully together and all joints made smooth and tight
with a little clay put on with the fingers or a bamboo tool. Jars,
smaller at the top and bottom than in the middle are made of
five pieces of clay. The lower half is made in one mold of a bot-
tom and two side pieces, the edges being pressed together with
the fingers; the upper half is formed in another mold. The two
sections, after partially drying in the sun are put together and
the joint made tight. These articles are then ready to be glazed
and burned.
Glazes of three colors are common: green, blue, and yellow.
Copper is used to get the green and cobalt for the blue. One of
the leading tile manufacturers in the village told me that they
add lead to get the yellow. The same man informed me that
they had always made their own copper oxide by roasting copper,
but I have never been permitted to see how they do it. The
cobalt is imported under the name "English green" and costs
more than the copper, but the yellow is the most expensive color
of all, which probably explains why the only yellow articles made
are roof tile for imperial buildings and burial urns.
The glazing mixture is made of powdered glass, ashes of either
mulberry bushes or rice straw, and the coloring matter, all stirred
up in water to form a thick, black cream. This is kept in large
jars near the kilns and the articles to be glazed are dipped a
short time before being stacked in the kilns. The coating is not
uniform in thickness, as the glaze runs somewhat, giving a differ-
ence of shade, if the color is green, in the final product. This is
not noticeable in the roof tile when laid, but is objectionable in
other articles. Some of the green tile will show spots or streaks
of blue if the firing is not done properly, but generally the color
is nearly uniform in the green and quite satisfactory in both the
blue and the yellow. Salt is not used in any of the glazes.
The articles modeled by hand are of three classes. Small
birds, animals, figures of people, teapots, etc., are modeled by
hand, some of solid lumps of clay, and are burned at the bottom
of the kiln used for all the other articles. The fancy glazed tile
of unusual shape or size are made by hand without a mold but
often forms for curves, etc., are used. These are then treated
the same as the regular tile. The third kind are the figures and
grotesque decorations used on buildings. Some of these are
sun-dried, painted, and then burned like the ordinary tile; others
are burned without being glazed and then painted or otherwise
decorated. They do not have the life of the glazed articles, but
the purpose for which they are intended, or the style of decora-
tion, prevents firing after the decoration has been put on.
The most novel feature of the whole process is the kiln. There
are seventy of these in the village. They are long tube-like
structures, up to 200 ft. long, built on the sides of the hills in
the village. As the hills slope at an angle of from 15 ° to 20°,
(the angle may not be the same all the way up), the kilns are
really long inclined chimneys. At any place a cross section will
be an inverted U. Each kiln is protected from the sun and
weather by a low roof, built in a series of steps to allow of better
ventilation, supported on pillars without walls. Thatched palm
leaf awnings are hung at the sides in summer time for further
protection from the sun.
One long kiln was only 3 ft. 4 in. wide and 3 ft. 4 in. high, in-
side measurements, at the bottom. The dimensions gradually
increase towards the top where the kiln was 6 ft. wide and 7
ft. high in the center, also inside measurements. The walls
are 8 in. thick, made of vitrified brick locally burned for the pur-
pose. Access to the kiln is secured through openings in the sides,
20 to 24 in. wide by 3 ft. high at the lowest opening, gradually
increasing in height to 5 ft. at the opening nearest the upper end.
The openings are bricked up when the kiln is being fired. The
articles to be burned are stacked on the sloping floor, boys doing
the work where the kiln is small, each pile having some old
broken burned pieces on top. At every 30 in. up the top of the
kiln are transverse rows of holes, each not over 2 in. in diameter,
through the top wall into the kiln. There are 3 holes in each
row near the bottom and 5 holes in each row at the top. The
holes are generally closed with pieces of brick set in loosely.
The fuel used is wood. A fire is built at the bottom and the
smoke goes up through the kiln, warming the ware therein.
Fig. 4— Tin; Yard OuTSTDS a Pottbry. Note Lcmps op Clay Dry-
ing on the Wall, and Molds for Lattice Work Tilb above
Them; Also Drying in thk Son, Halves of the Lattice
Wore Tile. Large Tile for a Ridge Pole, and
Small Imitation Bamboo Tile
When the fire is hot enough and sufficient draft has been created,
no more fuel is added to the tire at the bottom, but the burners
take their places at the first row of transverse holes and feed the
fire by dropping in pieces of wood about 15 in. long. When the
master burner thinks the lire is hot enough the burners move to
the next row and add more fuel. The fire is thus fed through
July. 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
57i
each row of holes all the way to the top. It takes 2700 lbs. of
wood and 12 hrs. work to fire a long kiln. As the fire at the bot-
tom goes out before long, the cheaper articles which do not re-
quire much heat, or these that would be spoiled by too much heat,
are packed near the bottom. The top of the kiln heats more
slowly, becomes much hotter, and cools more slowly so the better
grades, like the colored glazed ware, are burned in the upper part
of the kiln, and only in a long kiln.
Following the burners and their helpers, the woodcarriers,
come another set of men who put the articles for the next run on
top of and beside the kiln to be dried out thoroughly before being
fired. (When the accompanying picture (Fig. 6) was taken the
packers, working from one side, had taken off half of the articles to
put them in the kiln.) A kiln is packed on the first day, fired on
the second, allowed to cool over the third, and is unpacked on the
fourth day; but ordinarily the packers for the next run are follow-
ing close on the heels of those who are unpacking the previous
run, both crews beginning at the bottom and working up the kiln.
A large kiln will hold up to 10,000 articles at a time. If 80 per
Fig. 5 — Roof over a Kiln Showing over the Housetops
cent of the articles fired are marketable, the yield is said to be
good. The kilns are not owned by the shops which employ the
labor and make the goods, but must be rented at the rate of $5.00
for each run, renter to furnish fuel and labor.
The population of the village is said to be 15,000. As is usual
at industrial centers, most of the men have left their families
back in the country villages, so the statement that two-thirds
of the people there are men and boys is not an exaggeration.
The only industry in the village is the potteries, with the necessary
shops that supply food, clothing, etc. There are a few women
working in the potteries, chiefly at tasks like luting together the
halves of a fancy tile. They also make most of the small figures,
but this modeling work is done in their homes.
The workmen are well organized, there being at least sixteen
guilds or local unions of the men. The men doing the same kind
of work belong to the same guild — there are four guilds of men
working on the wheel, the members of each guild making a dif-
ferent article. It is difficult to get accurate general information
as no one can speak with authority about conditions in other
guilds, and he does not care to tell much about his own. A man
must serve an apprenticeship of six years, during which time he
is said not to receive any wages (this may mean no cash, though
he may get both food and lodging), before he is admitted to the
guild. A fee of $75 must be paid the guild at the time of joining,
but this is generally paid by the shop or employing company.
The wages run up to 40 cents a day for skilled potters (a good
carpenter in Canton will get only 25 to 30 cents a day), most of
whom are paid by piece work. A semi-skilled workman gets
$4 .'xi a month and his food, and the boys about a dollar a month
and food. Any of the workmen can rise to be an employer if he
can get a little capital. The employers, too, have their guild
house, said to be a very fine one.
These potteries are typical of most of the native industries
of China in state of development, ingenuity and skill of her ar-
tisans, and labor conditions. This description should also sug-
gest the opportunity in China for American goods. At the pres-
ent time those interested in reaching this market will probably
do best to deal through the foreign (chiefly European) firms
established in the port cities, who may, or may not, be interested
in pushing American lines.
The future growth of the industries of China may be along one
of two lines: either the native industries may be de-
veloped along modern scientific lines, or the effort may be made
to completely ignore the native industry and establish a foreign
industry using a foreign process, foreign machinery, and foreign
methods. The latter method will almost certainly fail when
applied to most industries at most places because of cheap labor,
the close relationship between the guilds of both workmen and
merchants, and the fact that the market is conservative and
I
H
11
-**JUv^v*k
*-*'<• JfeULlttiM
■% i :"
■
■H^H
^H^HHH
H^H
Fig. 6 — Lower End of a Kiln, Showing Fire Pit, Holes in Top
through Which Fuel is Fed, and Vessels Drving
Out for the Next Run
demands, in general, a low-priced article. In lines where there
has been no native industry it will be necessary to introduce
foreign methods, but full recognition must be paid to economic,
social, and labor conditions in adapting the foreign process to
the local situation.
Those Chinese who have been educated either in the United
States, Europe, or the few modern schools in China will be the
ones best fitted to develop China's industries. Being conversant
with both local conditions and western science and practice
they will be able to so remodel the industries that the good points
will be conserved, no prejudices aroused, and scientific results
obtained. British firms have equipped the engineering labora-
tories at the University of Hongkong with British machinery,
thus training the students at that institution to prefer British
goods in future years. So far-sighted Americans, looking for
future business in China, should sec that American institutions
in China lack no facilities for advancing American methods and
products, and that at least those Chinese who are studying chem-
istry in the United States are persuaded to join the American
Chemical Society. Those who join will be kept in latei years
conversant with scientific developments in America and be able,
through the advertisements, to know where to get the supplies
ih. v need in their own work. The advantages to both countries
are unlimited in having an enthusiastic body of Chinese who ad-
mire tin- United States and turn first to Americans when in
need.
Canton Christian College
Canton, China
THE JOURNAL OF INDUSTRIAL AND ENGINEERING i HEMISTRY Vol. 10, No. 7
CURRENT INDUSTRIAL NLW5
By A. McMillan, 24 Wtstend Park St, Glasgow, Scotland
NITER CAKE
An interesting discussion on niter cake is reported in the
Journal of Chemical Industry for December 15, 1917. Various
uses for the substance were given, among which the following
may be quoted: (1) The utilization of the niter cake as a sub-
stitute for sulfuric acid in the manufacture of hydrochloric acid
and the salt cake from salt; (2) for obtaining ferric sulfate for
sewage precipitation by furnacing burnt pyrites with niter cake,
grinding and leaching the product with water; (3) as a diluent
for sulfuric acid in the manufacture of superphosphate. Dr.
Terlinck stated that he had used niter cake as a substitute for
sulfuric acid in the recovery of fats from wool waters and he
further proposed to use it in the purification of ammonium salts.
In the Nottingham district niter cake was used for lace bleach-
ing, grease extraction from wool, pickling of metals, and mineral
water manufacture. Dr. E. Naef proposed utilizing the sodium
sulfate which, on reduction, gives sodium sulfide by grinding with
anthracite, charcoal or boiler coal and heating at 500 to 6oo° C,
the yield obtained being 95 to 98 per cent. The free acid may
be neutralized by adding soda during the grinding. No less
than 50,000 tons of sodium sulfide are used for the preparation
of sulfur dyes alone per annum. By treating niter cake at 300
to 350° C. with superheated steam, 90 per cent of the free acid
is driven off but the product is too dilute to concentrate.
PETROLEUM IN THE BRITISH EMPIRE
The Bulletin of the Imperial Institute states: "In 1903, at
the request of the Admiralty, the Imperial Institute prepared
a memorandum describing the known and prospective sources
of supply of petroleum within the Empire. Since that time
continuous attention has been given to this subject and a large
number of samples of crude petroleum, oil shales, asphalt, etc.,
have been reported on from British Guiana, Trinidad, Barbados,
New Brunswick, Gold Coast, Newfoundland, Somaliland,
Nigeria, Australia, Papua, etc. In certain of these cases, im-
portant developments have since taken place, notably in Trini-
dad, while in others, investigations are still in progress, in some
instances with considerable promise of success It cannot be
claimed that any source of supply of petroleum of first-class
importance has yet been found within the empire, but sufficient
has been done to show that including deposits of oil-shale, there
is a considerable possibility of further oil production within the
Empire.
POTASH LYE
The manufacture of potash lye from vegetable ashes and its
application for boiling straw in the paper industry is the sub-
ject of an article by Mr S. Tanaka in a Japanese technical
journal. It shows that ashes from vegetable materials have
been investigated from the point of view of the manufacture of
caustic potash for the digestion of straw for paper making
Ashes from soy-bean pods contained 16.19 per cent potassium
carbonate, and from chestnut. 13.96 per cent For the manu-
facture of caustic potash it is necessary that the ashes should
contain liion- than io per cent potassium carbonate Lime
may be added directly to the solution of ash in water without
separating the insoluble residue. The yield of caustic potash
depends very largely 011 the perfection of the filtration and lixivia
tion processes. The potash obtained is quite efficient for the
manufacture of straw pulp, and its substitution for caustic soda
is a question of cost. A constant and sufficient supply of potash
from these souiees is hardly to lie expected and the difficulties
of the filtration process increase the cost
OH. CLARIFLER
According to a German patent, a cylindrical vessel fitted with
a removable cover is provided with a false bottom, perforated,
and covered with corrugated wire gauze which, in turn, is
covered with a layer of felt secured to the false bottom by a
metal ring and bolts so as to make a tight joint all round. This
arrangement also keeps the felt from pressing tightly against
the false bottom and by means of the corrugations in the gauze
the filtering surface. Above the filter bed, the vessel
is charged about '-' j full with shavings to remove coarse impuri-
ties and the oil is kept fluid by a heating coil embedded in the
shavings. Taps are provided at different levels to draw off the
oil and any separated waters
CANADA'S EXPORT TRADE
The expansion of Canada's export trade, says the Times
Trade Supplement, during 1917, was even more remarkable than
during the preceding year. The latest available figures are
those for the twelve months ending November last. These
show that the total value of the trade for that period in mer-
chandise alone was 81,575,233,006, which was an increase over
19 1 6 of 46 per cent and over 19 15 of 160 per cent. The increase
extended to all general classifications except forest products in
which there was a slight decrease. The most remarkable in-
crease was in manufactured goods. The total under this classi-
fication was $703,147,168, which was an increase over 19 16
and 1915 of 72 and 410 per cent, respectively. The value of the
manufactured goods exported becomes all the more remarkable
when the fact is taken into account that it exceeds by the sub-
stantial sum of $104,405,262 the total export trade of all kinds
of merchandise in 1915. As a result of this remarkable devel-
opment in the export trade, there was a favorable balance over
merchandise imported of $563,832,904, whereas the year be-
fore the war broke out, there was an adverse balance of $300,000,-
000. The total trade balance for three years ending November
amounts to the sum of $1,056,538,845.
IRRIGATION PLANT
According to the Board of Trade Journal, there are very promis-
ing prospects for business to be done in irrigation plants in
Yunnan Province, South China. At present, four irrigation
sets, owned by a private company, are in operation within a
few hours' journey of the city of Yunnanfu, and it would be
comparatively easy to install 100 such sets if the business were
followed up and cared for, as there are immense tracts within
easy reach of water, but at an elevation of some 15 ft. above the
water level. There are also great opportunities for trade in
machinery at the tin mines. Innumerable small pumps are
needed and mining machinery in general would find a ready
market.
RECOVERY OF SOLVENT NAPHTHA
According to a recent German patent, the resinous mass left
behind in the still after refining solvent naphtha and benzol
with sulfuric acid is subjected to dry distillation and decomposes
at 3300 to 385° C, leaving a pitchy residue. On redistilling the
distillate, two fractions are obtained, the bulk consisting of heavy
naphtha with boiling point 160 to 2200 C. The second frac-
tion is a heavy oil of mineral character which does not gum even
in warm air and does not corrode metals or give any deposit in
the cold. It may, therefore, be used as a lubricant and as a
rosin oil substitute
July, 1018 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
573
PURE BISMUTH
M. Mylins and E- Groschuff describe a satisfactory method
for preparing pure bismuth suitable for electric and magnetic
measuring instruments. Bismuth of 99 per cent purity may
be obtained fairly easily but the 1 per cent of impurities is
difficult to remove. By heating the nitrate of bismuth, the
oxide is formed and this can be reduced by hydrogen. The
I residue is melted and crystallized. The method of purifying
bismuth by distillation does not work out in practice as most
1 of the impurities remaining after the ordinary refining process
1 boil at a temperature of less than 15000 C. which is the tempera-
ture of boiling bismuth. The method given above is stated to
yield a metal which does not contain more than 0.0 1 per cent
impurities and which melts at 271 ° C. Wire of 1 mm. diameter
has an electric resistance of 1.20 ohms at 22° C. If the per-
centage of impurity amounts to 0.1 per cent, the resistance
value is 3 ohms.
RUSSIAN MONAZITE SAND DEPOSITS
VARIOUS CLASSES OF ENGINES
The following average weights per brake horse power for
various classes of engines were given in a paper recently pub-
lished by Mr. P. N. Everett: Triple expansion steam engines
for cargo-boats (no boilers or auxiliaries), 130; triple expansion
including boilers and auxiliaries, 450; Diesel engines for cargo-
boats (no auxiliaries), 250; Diesel engines with all auxiliaries,
400; turbines for cross channel boats with boilers and auxiliaries,
200; Diesel engines for submarines, 50; steam reciprocating en-
.gines for destroyers, 3.5; turbines for destroyers with boilers,
etc., 30; petrol engines for motor cars, 15; petrol engines for
racing boats, 7V2; aero engines, 2l/V
REGISTER OF OVERSEAS BUYERS
The first edition of this register, which measures 10 in. X 7 in.
and contains close on to 400 pages, has been compiled with the
assistance of chambers of commerce and the consuls abroad
and is issued at the price of $5 by Messrs. Bemrose and Sons,
London. Besides containing a list of the principal imports in
allied and neutral countries, arranged geographically under the
class of goods they import, the volume includes articles on over-
seas trade, written under the authority of the chamber of com-
merce abroad. The requirements of the colonies and foreign
countries and how to extend trade with them are dealt with
thoroughly, as also are the causes which have hitherto impeded
British trade development. A large amount of information
is also given on the coinage of various countries, lighthouse,
quay and other duties, Government officials, chambers of com-
merce, banking facilities, newspapers, local trading conditions,
etc., all of which will prove useful for the development of trade.
INDUSTRIAL USES OF BISMUTH
The most important use of bismuth at present is as a component
of fusible alloys. An alloy of bismuth, lead, tin and cadmium
melts below the boiling point of water. It may also be used
as a component of the alloy used for silvering mirrors. Safety-
plugs for boilers are made of an alloy containing bismuth which
fuses at a temperature just above the boiling point of water.
Automatic sprinklers or fire extinguishers placed in the ceilings
of buildings are also sealed with an alloy containing bismuth,
the rise of temperature caused by a lire fuses the plugs and jets
of water fall over the lire. Bolivia produces the largest quantity
of bismuth, the output in 19 15 being 559 tons valued at $1,1 15,755.
In Queensland the product in 1915 was valued at $67,445,
including some wolfram In New South Wales, the output in
1916 was 29V2 tons valued at $27,365. Smaller quantities
are produced in Tasmania, South and West Australia.
It is stated that in Nizhi Tagil district there are deposits of
monazite sand with a large cerium content up to 23 per cent.
Hitherto little interest has been shown in Russia in the pro-
duction of cerium which certainly does not exist in large quanti-
ties in the ground in any of its combinations, in fact, only mon-
azite and orthite have been found in the country. The latter
is sold in small quantities from the mines of the Transbaikal
territory, while the former is found in many parts of the Urals
where it was known long ago by the natives. It has also been
found in the Cabinet lands of Transbaikalia. It is proposed
to send the monazite sand to Petrograd for the extraction of
the' rare metals.
MINERAL OUTPUT OF GREAT BRITAIN
The report of the Inspector of Mines for the year 1916 has
just been issued. The total output of coal for the year was
256,375,366 tons which is an increase of 3,169,285 tons over
the year 191 5. The value of the output was $1,000,073,130,
being no less than $210,919,780 more than 1915. The total
value of the output of minerals in 1916 was $1,070,072,620,
an increase of $217,881,330 over 1915. The quantity of coal
exported was 55,001,113 tons against 59,951,925 tons in 1915.
The coal was used as follows :
Tons
Exported 55,001,1 13
Used for gas coke 39,384,819
Manufacture of pig iron 19,780,690
Domestic purposes 142,208,684
The other principal minerals of value are:
Tons Value
Chalk 12,786,321 $ 727,520
Clay and shale 6,500,388 6,236,690
Gold ore 1,338 3,250
Copper ore 787 31,170
Iron ore 13,494,658 27,725,360
Lead ore 17,107 1,695,845
Limestone 11,115,909 6,979,150
Oil shale 3,009,232 5,161,470
Salt 1 ,960,448 4,520,665
Tin ore 7,892 3,560,710
Tungsten 394 248,495
Uranium ore 51 5,005
Zinc ore 8,476 326,520
Some of the figures show an increase and some a decrease
over the figures for the preceding year.
The following table gives the amount and value of the metals
obtained by smelting from the ores given above:
Antimony 4 tons $ 1,700
Copper 278 tons 188,970
Gold 273 oz. 4,420
Iron 4,319,096 tons 175,226,055
Lead 1 2,573 tons 1 ,947,245
Silver 86,483 oz. 56,420
Tin 4,697 tons 4,278,280
Zinc 3,000 tons 1,026,750
The total value was $182,729,840, an increase of nearly
$45,000,000 over the year 191 5.
EFFECT OF INSULATION ON STEAM DRUMS
The Electrical World describes an interesting test for determin-
ing the loss of heat by radiation from boiler settings and steam
drums. The 560 h. p. Babcock and Wilcox boiler tested had
steam drums covered with one course of common brick. A
rectangular can containing a measured amount of water was
placed on the top of one drum and the boiler was run at its rated
capacity for three days, the rise in temperature of the water
being noted. A course of Armstrong nonpareil insulating
brick 2'/i in thick was then placed on the top of the common
brick covering and the readings repeated. The result showed
that the saving in heat radiated, if converted into the equivalent
consumption of fuel per year, would be more than enough to
pay for the cost of the insulation brick and the labor required for
its insulation.
574
THE JOURNAL OF INDUSTRIAL AND ENGINEERING ( HEMISTRY VoL
10. No.
HARDENING CARBON STEEL
An automatic detector fitted by Automatic and Electric
Furnaces, Ltd., Westminster, London, to tlu-ir electric furnace
for use in connection with the hardening of carbon steel depends
on the principle that carbon steel at its non-magnetic point is
at the best temperature for quenching. The furnace chamber
consists of an inner pot, which contains a special mixture of
salts having a comparatively low melting point but a high
vaporizing point. The pot is wound with a heating coil, and is
provided with a special heat-resisting lagging. Round the
outside case of the furnace is wound an insulated copper coil,
the ends of which are connected to a special galvanometer. A
current of electricity passed through the heating coil quickly
heats the furnace and renders the salt mixture molten and also
magnetizes any steel article that is placed in the pot. When
the steel has been heated to the non-magnetic point a small
current is induced in the outer winding and the consequent de-
flection of the galvanometer needle informs the attendant that
the best temperature for quenching has been reached. A 4 in
furnace will, it is stated, harden 10 lbs. of tools, gauges, or other
articles in an hour.
TUNGSTEN FILAMENTS
A new German process for making tungsten filaments is
based upon the idea of forming the lamp filament out of one
long crystal. Tungsten crystals can be made to form gradually
out of a mixture of tungsten powder and thorium oxide. The
mixture is squirted through diamond dies into a filament of
0.02 mm. to 1 mm. in diameter. This filament is then drawn
through a chamber in which it is rapidly heated to a temperature
of 2400 ° to 2600 ° C. and with a velocity of 2.5 miles per hour,
which is rather slower than the crystallization velocity of tung-
sten, so that a single crystal of indefinite length is formed. The
chamber is filled with a neutral gas and the heating is performed
in two stages by a pair of electrically heated coils, through the
center of which the filament is passed. The filament in this
state is ready for use in a lamp without further treatment. It
is softer than drawn tungsten wire at low temperatures and
hard at high temperatures, making it particularly suitable for
use in lamps. According to the Electrician, filaments consisting
of a single crystal of 25 in. length have been produced in this
manner.
TAR-STILL CORROSION BY CHLORINE
Some particulars have been communicated to us, says the
Chemical Trade Journal, 62 (1918), 360, of a useful investiga-
tion carried out by Mr. L. Crawford, late of Littburn Colliery
Tar Works. Durham, with reference to the chlorine content of
tars and the consequent corrosion of tar stills and particularly
of the domes. In seven different tars from varying types of
by-product coke ovens and from vertical and horizontal gas
retorts, Mr. Crawford found the chlorine percentage varying
from 00053 to 0.148 and, in one case, though the bulk showed
only 0.111 per cent, as much as 0.226 per cent was found in a
sample from the coolers. The investigator states that his ex-
perience with the different tars does not enable him to draw
conclusions but, in regard to one showing chlorine content of
o.m per cent, he has been concerned in the distillation of large
quantities for a year and he thinks that a chlorine content above
o.i per cent is above the limit compatible with longevity in still
domes. The results are put forward, he states, in the hope that
others with experience in individual tars will contribute theirs,
so that by correlation of chlorine content with corrosion effects
a maximum permissible percentage might be established. It is
recognized that other factors may have an influence on still
corrosion, but Mr. Crawford believes chlorine to be the predom-
inant factor.
COTTON-SAMPLING MACHINE
In the course of a paper on some instances of applied science
in tin cotton trade, read before the Royal Society of Arts, Lon-
don, I >i W. I. awn no Halls described a machine for sorting
cotton hairs according to length. It consists primarily of a
pair of rollers which, as they revolve, are transversed or trans-
lated bodily along a path at right angles to their axis of rotation.
The cotton to be examined is first run through ordinary drafting
mechanism so as to cause the hairs to lie parallel and straight
and this "sliver" is presented to the rollers at the beginning of
a traverse until they have seized a millimeter or so of the front
ends of the hairs. The sliver is then drawn away, leaving in
the nip of the rollers a tuft of hairs which are all held by their
front ends. The rollers continue to revolve and obviously the
first hairs to be delivered from them on the other side will be
the shortest ones, while the longest ones (since all started with
their front ends level ) will be the last to escape. But since
this feeding action of the rollers is combined with and positively
geared to the motion which causes the traverse, it follows that
the short hairs will escape on a suitable collecting device at the
beginning of the traverse, the long ones at its completion and
intermediate lengths at intermediate points. Thus, the cotton
is fractionated by a continuous cycle of repeated operations,
as many times as is convenient not merely into separate parcels
of hairs but into a graduated series which may be subdivided
to any degree desired. The device provides a technique by which
it is possible to take a sample of raw cotton, make it into a sliver,
treat that sliver for 2 min. only in an automatic machine,
weigh the graduated produce of the machine's activity, and, at
the end of half an hour, plot frequency curves of a reasonable
and measurable degree of precision, showing the variation of
length of staple within a sample.
THE LONG-RANGE GUN
In the issue of Le Genie Civil for April 20, Mr. N'icolas Flamel,
a French authority, continues the discussion of the German
long-range gun. Interesting information is given regarding the
type of gun, powder, shell, etc. It appears that the Germans
have taken one of their 15-in. naval guns and, by means of the
technical process known as refining, reduced the caliber to 8.2
in. The powder is probably an ordinary slow-burning powder,
the weight of the charge being increased to give the desired
muzzle velocity to the gun. The shell is in two parts: the special
fine-pointed head and the body. The shell has special driving
bands turned on projecting portions of the body, in addition to
the usual copper bands. The burster is either T. X. T. or tri-
nitroanisol (an explosive similar to T. N. T. but having a lower
melting point). The writer of the article does not incline to
the theory of a special propellant shell, but the gun has been
produced in accordance with the usual practice, with necessary
modifications in charge, shape of shell, and other minor details.
BRITISH BOARD OF TRADE
During the month of April the British Board of Trade re-
ceived inquiries from firms in the United Kingdom and abroad
regarding sources of supply for the following articles. Firms
which may be able to supply information regarding the things
an requested to communicate with the Director of the Com-
mercial Intelligence Branch, Hoard of Trade, 73 Basingnall St.,
London, E. C.
lull paper covered Machinery ami Plant fi>r
Manufacture of fasteners for
Cider vinegar
Eyelets, small, colored, black
Ink powderf! writing .md print-
ing)
Tmi cut tine machines
Vegetable ivory discs for export)
Watchlkeys (manufacturers only)
Production of fish products
(canned)
Making electric blankets
July, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
SCIENTIFIC SOCIETIES
FRENCH SECTION, AMERICAN CHEMICAL SOCIETY
Paris, lE 15 Mai
Major Hamor
Gas Service, A. E. F.
Dear Major Hamor:
Please find enclosed copy of the letter sent to Dr. Nichols,
requesting the foundation of a French section of the American
Chemical Society. This has been greatly delayed in order
to obtain the signature of Mrs. Curie, who is the first French
honorary member and of whom it was necessary to ask her com-
pliance.
It took me nearly a month to find the occasion of getting in
touch with her, mainly due to my lack of time.
Very sincerely yours,
Rene Engel
Dr. W. H. Nichols
President American Chemical Society
Washington, D. C.
Dear Dr. Nichols:
According to the constitution of the American Chemical So-
ciety and the privileges granted by Article IX for the formation
of local sections, the following undersigned members have the
honor of requesting the permission of the Council to found in
Paris a French section of the Society covering the entire terri-
tory of France.
A more propitious time could not be chosen for such a move-
ment, as it would contribute to the formation of an American
chemical home for our members belonging to the Expeditionary
Forces and bring into closer fellowship the chemists of the two
sister Republics.
With our best wishes, we are
Very sincerely yours,
V. Grignard
Edward Bartow
s. s.,
Reston Stevenson
George Seatchard
W. F Durand
Elienne Meen
Major, C. S S., U. S.
I. V Walker, 1st I.t., C. S. S., U. S.
Raymond F. Bacon
Ben H. Nicolet, Capt
U. S. N. A.
G. N. Lewis, Major, C. S. S.,
U. S. N. A.
Joel H. Hildebrand, Capt., O. R. C.
A. R. Norton, 1st Lt., C. S. S..
U. S. N. A.
A. R. Olson, 2nd Lt., C. S. S.,
U. S. N. A.
D. H. McMurtrie, 2nd Lt., C. S. S.,
U. S. N. A.
Leonard H Cretcher, 1st Lt..
C. S. S., U. S. N. A.
G. S. Skinner. 2nd Lt., C. S. S.,
U. S. N. A.
P. R. Parmelee, 1st Lt., C. S. S.,
U. S. N. A.
Jos. W. MacNaugher, 2nd Lt.,
C. S. S., U. S. N. A.
Louis C. Whiton, 1st Lt ., San,
Cps., U. S. N. A.
C. W. Crowell, Sgt., C. S. S.,
S.N. A.
E. B. Peck, 2nd Lt.. C, S. S ..
V. S. N. A.
May 14. 1918
THE GERMAN UNION OF TECHNICAL AND SCIENTIFIC
SOCIETIES'
A short account of this important movement is as Follows
On March 4, 1917, at a meeting of the Verein Deutsche*
Eisenliiittenleute (German Iron and Steel Institute), held at
lorf, I>r. Fr. Springorum said the war had intensified
1 The following statement and translations have been prep red b
the need for closer cooperation of the German Technical Societies.
Preliminary negotiations had therefore led to a combination
of such Societies, and the Verein Deutscher Eisenhvittenleute
had gladly joined such Union and promised their support.
On April 19, in an article published in a German newspaper,
it was stated that the Managing Committee of the LTnion has
decided to create an Intermediary Agency between the technical
world and scientific institutions for the carrying out of scientific
and technical research work, so that industry not equipped for
experimental work, specially smaller concerns, might be afforded
an opportunity of having problems solved through the aid of the
Union.
In November the Union held its first General Meeting at the
premises of the Association of German Engineers in Sommer-
strasse under the Chairmanship of Privy Councillor Busley,
at which the Imperial Government Offices, Federal Council, and
Legislative Bodies were represented. The purposes and aims
of the Union were explained. Herr Busley said their object
was to establish a balance between science and practice, and
that the technical world ought to be represented more than was
hitherto the case in the Legislative Bodies.
Professor Dr. Wiedenfeld, of Halle, speaking on "Economics
and Technics During and After the War," stated the blockade
of the sea had necessitated the remodelling of the foundations
of German economic life, the production from her own resources
of raw materials and food, the utilization of waste materials
and the production of substitutes. Technical science could only
meet these new requirements by disregarding the question of
cost price and all considerations as to the possibilities of markets
and the risks involved.
The above meetings and the objects of this important German
Union of Technical and Scientific Societies are described more
fully in the accompanying statements:
Statement I
Meeting of the German Iron and Steel Institute held at Dusseldorf,
March 4, 1917.
GERMAN UNION OF TECHNICAL-SCIENTIFIC SOCIETIES
Dr. Fr. Springorum, during the course of his address, stated:
The war has intensified the need, already felt before, of closer
cooperation of the German Technical Societies, and preliminary
negotiations on this question have led to a combination of the
Technical Societies into a German Union of Technical-Scientific
Associations. We have gladly joined this Union and promised
our cooperation, feeling sure that the purposes and aims of the
Union are the right ones. The Union leaves to its individual
members complete liberty in the special domain which each
Association has hitherto been dealing with, but wishes to ensure
joint action of the Associations (whose number has now risen to
eleven) on all important questions.
Statement II
This is a precis of the full Statement III, which describes the objects
of the German Union of Technical and Scientific Societies acting as Inter-
mediary for scientific technical research work.
INTERMEDIARY AGENCY FOR SCIENTIFIC-TECHNICAL
RESEARCH WORK
i — Managing Committee of German Union of Technical
Scientific Associations decided to create department to act as
diary between technical world and scientific societies
of universities and technical academies for carrying out scientific-
b . hnical research work.
ol departments of work so highly spei
and so ninny problems at present, thai sometimi
available for dealing with a certain question in scientific in-
3 — It can direct all such problems i" suitable operators,
ige with minimum of labor.
576
THE JOURNAL OF INDUSTRIAL AND ENGINEERING < HEMISTRY Vol. 10, No. 7
4 — Great intellectual and material resources of scientific
institutions of universities and technical academies, and knowl-
edge and experience of their heads, might be rendered service-
able to German industry more than hitherto.
5 — Industry, where not equipped for carrying out the task by
means of its own arrangements and staff (particularly smaller
concerns less equipped for experimental research), will be
afforded opportunity of having questions otherwise left unsolved
conducted into proper channels for solution through aid of
Union.
6 — Sometimes even not undesirable for large industria
establishments to come into touch in this way with academicians
to judge on complicated questions from scientific standpoint,
yet in cohesion with technics.
7 Large number of heads of institutions in departments of
(o) applied and physical chemistry, (6) physics, (c) electro-
technics, (</) engineering science willing to undertake such work
through Intermediary Agency.
8 — Further, men of special experience in each of above-
named departments have placed themselves at disposal of
Agency to assist in selecting suitable operators.
9 — -German Union and heads of scientific institutions hope
Agency will be valuable and useful not only during war but in
economic life afterwards.
10 — Union asks industrial works engaged in departments of
(a) applied physics, (b) electro-technics, (c) machinery con-
struction, (d) engineering science in general to address inquiries
to them
Statement III
The following statement describes the objects of the German Union of
Technical and Scientific Societies, acting as Intermediary for scientific-
technical research work, April 19. 1917.
This is shown as a precis in Statement II.
GERMAN UNION OF TECHNICAL SCIENTIFIC SOCIETIES
INTERMEDIARY AGENCY FOR TECHNICAL-SCIENTIFIC RESEARCH
WORK
The Managing Committee of the German Union of Technical
Scientific Associations has decided to create, at its offices, a
department which is to act as an intermediary between the
technical world and the scientific institutions of the universities
and the technical academies for the carrying out of scientific-
technical research work.
Very many problems, and likewise the special knowledge
of the departments of work, are nowadays so highly specialized
that sometimes there are but few suitable operators available
for dealing with a certain question in the scientific institutes.
If now it were possible to direct all such problems to suitable
operators in each instance, a very material advantage might be
gained with a minimum expenditure of labor.
On the one hand the great intellectual and material resources
which are extant in the equipment of the scientific institutions
of universities and technical academies and in the knowledge
and experience of their heads, might be rendered serviceable to
German industry to a greater extent than hitherto. On the other
hand, industry — as far as it is not itself equipped for carrying
out the task by means of its own arrangements and staff or other
connections, hence in particular medium sized and small concerns
are less amply equipped with experimental research arrange-
ments— will be afforded the possibility of having questions
which would otherwise have to be left unsolved, conducted into
proper channels for effecting their solution, through the aid of
Union. Even to large industrial establishments it might some-
times be not undesirable to come in this way into touch with
academicians who are willing to judge as to complicated ques
tions from the scientific standpoint, yet in cohesion with technics.
A large number of heads of institutions in the departments o(
applied and physical chemistry, physics, electro technics and
engineering science have declared themselves willing to under-
take such work introduced to them through the Intermediary
Agency Further, those of special experience in each of the
departments named have placed themselves at the disposal
of tins Urn* \ with a view to assisting it in the selection of suit-
able operators for the purpose in question
The German I oion and the heads of the scientific institutions
hope that this i-gency will be of value and prove very useful
not only foi the duration of the war but also in the sub
economic life ol peace time
The Union therefore requests industrial works engaged in the
departments ol (a) chemistry, (6) applied physics, (e) electro-
(il) machinery construction, and (e) engineering
science in general, to address inquiries to "Vermittlungsstelle
des Deutschen Verbandes, 40 Sommerstr., Berlin, N. W., ' care
the Secretary 'he committee in charge of the
secretarial offii
Statement IV
This i Full Statement V, showing the latent information
with regard to the work being done by the German Union of Technical
itific Societies.
TECHNICS DURING AND AFTER THE WAR
1 — German Union of some 13 technical scientific societies
recently held its first General Meeting in Berlin.
2 — Those present included Privy Councillor Busley (Chair-
man), Representatives of Imperial Government Offices, Federal
Council, and Legislative Bodies.
3 — Object — -to establish balance between science and practice.
4 — Many technical tasks could not be carried through
without collaboration of several branches of science; metallurgist
required cooperation of technician, architect that of engineer, etc.
5 Influence to be exerted on technical education towards
admitting academically trained technicians to all administrative
departments of Federal States.
6 — Technical world should be more represented in Legislative
Bodies.
7 — Union should be consulted in preparatory' work of draft-
ing regulations or enactments. Imperial Treasury alone had
availed itself of their advice in preparatory work, namely,
taxation of coal and sources of energy.
8 — Desire expressed for an Austrian and Hungarian Section
of Union.
9 — Professor Wiedenfeld said Germany managed with her
own production formerly, then more dependent on foreign
countries owing to her increased population; afterwards owing
to sea blockade, having to produce her own war materials and
food.
10 — Technical science could only meet new requirements by
disregarding question of cost price, which formerly was one of
chief consideration in competing with other countries.
1 1 All considerations relating to market and risk involved
disregarded, and substitutes produced by new methods.
12— Though cannot carry over all new conditions and products
into peace times, cannot revert to old economic conditions.
"What has been will never return."
13 — Technical science had tried to help economic life in three
ways :
(a) Procuring raw materials formerly obtained from
abroad partly by re-establishing unremunerative industries, e. g.,
manganese production, increasing iron production, sulfur pro-
duction, agricultural intensification.
Increasing use of waste products (term "non-utilizable
substance" eliminated by war) such as obtaining lubricants from
coal tar, supply of enough clothing by using waste material.
(c) Producing substitutes, e. g., nitrogen from the air,
substances by synthetic processes where natural way not avail-
able, such as cattle food from straw.
14 — The speaker recalled the dictum of His Excellency
Professor Fischer: "I cannot imagine any substance for which a
substitute could not be found." Too much regard paid to
quality during early part of the war. This impossible as war
continues.
15 — Deprecated multiplicity of Government authorities con-
trolling construction. This had prejudiced German production
in peace time.
16 — -Ought to aim, even after war, at reduced use of certain
raw materials Owing to high expense for industrial war in-
stallations, production would have an unfavorable aspect in
certain departments.
17 — Amortization necessary in this respect during war of war
installation expi
1S Monopolies (not necessarily State ones) for materials
produced wholesale.
19 — Could only establish steady movement of prices by
strictly regulated syndicates, then obtain sure remunerativeness,
favorable to technical science, and consequent brisk investment.
Statement V
The following statement shows the latest information with regard
to the work being done by the German Union of Technical and Scientific
Societies, November 1917.
This is shown as a precis in Statement IV.
TECHNICS DURING AND AFTER THE WAR
The "German 1 uion ol Technical Scientific Societies," which
has recently been formed by the combining of thirteen associa-
July, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
tions and unions, held its first General Meeting this morning
on the premises of the Association of German Engineers in
Sommerstrasse, where the Chairman, Privy Councillor Busley,
after welcoming those present — among whom the Imperial
Government Offices, the Federal Council and Legislative Bodies
were represented by members — explained the purposes and aims
of the Union.
Herr Busley said that their object was to establish a balance
between science and practice. Many a technical task could not
be carried through without participation and collaboration of
several branches of science: the metallurgist required the coopera-
tion of the technician, the architect that of the engineer, etc.
An influence was also to be exerted on technical instruction and
education, and towards ensuring that the academically trained
technician should be admitted to all administrative departments
of the Federal States. The technical world ought to be rep-
resented, more than was hitherto the case, in the Legislative
Bodies. The Union had also applied to the authorities with a
view to being consulted in the preparatory work of drafting
regulations or enactments. Unfortunately, hitherto, the Im-
perial Treasury alone had availed itself of their advice, in the
preparatory work for the taxation of coal and sources of energy.
Finally, the speaker stated that a desire had been expressed
that an Austrian and Hungarian Section should be attached to
the Union, as to which resolutions were still to be passed.
Professor Dr. Wiedenfeld (Halle) then spoke on "Economics
and Technics During and After the War." The speaker showed,
in a very exhaustive manner, how, in former days, Germany
could manage well with her own production, how subsequently
she became more and more dependent on foreign countries owing
to the increase of her population, and was then subjected, by the
blockade of the sea, to the necessity of remodelling all the
foundations of her economic life, of producing from her own
resources, raw materials and food. Technical science could only
meet these new requirements by fundamentally disregarding the
question of cost price, which formerly, in competing with other
countries, was necessarily one of the foremost considerations.
Disregarding all considerations as to the possibilities of the
market and the risk involved, substitutes were produced by
calling in the aid of new modes of production and devoting
thereto all human powers. Although not all of these new
conditions and products can be carried over into times of peace,
nevertheless the old economic conditions cannot be reverted to.
"What has been will never return," nor would this be even
desirable. He said that technical science had been endeavoring
to come to the aid of economic life in a threefold manner.
1 — By procuring the raw materials formerly obtained from
abroad partly by the re-establishment of industries which had
become unremunerative (production of manganese, increase of
the production of iron, production of sulfur, intensification of
agriculture).
2 — By promoting the technical tendency, already existing
in pre-war times, towards increased utilization of waste products.
The term "non-utilizable substance" has been eliminated by
the war. The speaker emphasized in this respect obtaining
lubricants from coal tar and supplying clothing requirements
by utilization of waste material.
3 — By producing substitutes, such as for instance nitrogen
from the air, and the production of substances by synthetic
processes, where the natural way is no longer available, as for
instance the cattle food produced from straw.
The speaker recalled a dictum of His Excellency Professor
Fischer: "I cannot imagine any substance for which a sub-
stitute could not somehow be found." In the speaker's opinion
too much regard had been paid during the early part of the war,
to the quality of the production, which however became im-
possible with the continued duration of the war. The speaker
also found fault with the multiplicity of Government authorities
controlling construction, which had already manifested itself
in peace times to the prejudice of German production. With a
view to the projects, the speaker demanded that even after the
war we ought to aim at a reduced utilization of certain raw
materials. Production would assume an unfavorable aspect
in certain departments owing to the high expense for industrial
war installations. In this respect amortization during the war
of these expenses for war installations would be necessary.
Further, wherever materials produced wholesale are in question,
the speaker would be in favor of monopolies, though not neces-
sarily state monopolies. He held that it would only be by
strictly regulated syndicates that steadiness in the movement
of prices could be established, and an assurance of remunerative-
ness, favorable to the display of technical science, and conse-
quent brisk investment of capital, obtained. The speaker
concluded by attempting to lay down guiding principles for the
577
collaboration of technical science and enterprise, which cannot
do without each other.
Finally Dr. Taaks, Dr. Eng., spoke on "Technical Academic
Study After the War."
RESEARCH WORK ON IRON AND STEEL IN GERMANY'
The following is an account of an important movement now
going on in Germany relative to research work upon iron and
steel. This does not appear to have yet been noticed in this
country.
The German proposition is to found and establish a special
institution and research laboratory to be entirely devoted to
researches on iron and steel. Surely we in this country will not
allow this action of the enemy to go unchallenged. While Great
Britain has several important laboratories devoted to research
on iron and steel, there is certainly required a general building
and common meeting place for the following important In-
stitutions.
(A) Iron and Steel Institute
(B) Institute of Metals
(C) Institution of Mining and Metallurgy
(D) Institution of Mining Engineers
(Ej Faraday Society
(F) Society of Chemical Industry
(G) And others
On March 4, 191 7, at a General Meeting of the Verein
Deutscher Eisenhuttenleute (German Iron and Steel Institute)
held at Diisseldorf (see the accompanying Statement I), Dr.
Fr. Springorum, during the course of his address, said the com-
mittee appointed by the Board of that Institute had recently
discussed the subject and recognized the necessity of promoting
progress in metallurgy by the establishemnt of a special research
institute probably to be attached to the Kaiser Wilhelm Society.
This was followed on June 19, 191 7, by a further meeting of
the same Institution (see Statement II) at which a resolution
was unanimously passed with regard to the establishment of
such an institution and research laboratory to be devoted to
research on iron and to be attached to or affiliated with the
Kaiser Wilhelm Society, an important new German association.
On July 6, 191 7, at a meeting of the Senate of the Kaiser
Wilhelm Society, held under the presidency of Professor Von
Harnack (see Statement IV) the Senate declared itself in agree-
ment with the proposal of the Verein Deutscher Eisenhutten-
leute to establish this institute and laboratory for research on
iron and steel.
On July 28, 1917 (see Statement V), reference was made to the
meeting of the Verein Deutscher Eisenhuttenleute held on June
19, and after discussing the foundation and site of the building
the writer stated that "the means for building and maintaining
the Institute, except a small contribution from the Kaiser
Wilhelm Society, will be raised by the iron and steel industry of
Germany."
Finally, from the latest information in the possession of the
compiler of this present statement there was held on November
!3» IQI7, the nrst meeting of the "Curatorium" (Trustees
Committee) of the Kaiser Wilhelm Institute with regard to the
establishment of the research institute and laboratory for re-
search on iron and steel in the "Stahl und Eisen" Building in
Diisseldorf, when Dr. Springorum was elected Chairman.
(See Statement VII.)
It may be added that the Kaiser Wilhelm Society was founded
by the initiative of Emperor William II in January 191 1 for
establishing and maintaining in a scientific manner independent
institutes for research in the sphere of physical science. It has
assisted in the foundation of the Institute for Chemistry; In-
stitute for Experimental Therapy; Institute for Coal Research;
Institute for Labor Physiology; and now the Institute for Re-
search on Irou and Steel; also (1914) projected the Biological
Institute and the Institute for Aerodynamics and Hydro-
dynamics.
The president is Dr. Harnack and the first vice president is
Dr. Krupp von Bohlen und Halbach. Half the members are
elected, the other half nominated by the Emperor and the
Committee of Management. The election by the Senate and
confirmation by the Emperor carries with it the obligation of a
contribution of £1,000 with an annual contribution of £50.
Statement I
Meeting of the German Iron and Steel Institute, held at DQsseldorf,
March 4, 1917.
INSTITUTION POE METALLURGICAL RESEARCH
l>r. Fr. Springorum, during the course of his address, stated:
> Statement and translation! prepared bj Sir Robert Hadfield
S7»
THE JOURNAL OB INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. $
"The titanic struggle "I '<■< '• • nfronted our iron in-
dustrj in every direction with particularly great difficulties,
and I hope that some day, when the war time records of our
works and our associations maj be re fri elj disi losed, not only
the full tribute of recognition will be paid Foi the great things
which have been achieved, but that it will also in- possible, im-
mediately, to find ways ami means of Further pursuing, in the
-.I' the Fatherland, tin- thou in i which,
arising from the emergencies of war, could perhaps be solved
only in part during the war. We shall, after the war. far more
than hitherto, have to depend on i i to rely on our
own strength. According!; on us will be enormous.
Industry will only be able to meet th m bj itrenuous work, and
will, above all, have to study better utilization of in Is and the
further perfecting of metallurgical processes. Coordination
between metallurgical practice and metallurgical research,
which has always been insisted on and promoted by us, will in
future be imperatively needed.
"The weightiness of thes Fa< I ha revived among our Board
an old idea which, to our gratification, lias once more been
brought forward, of late, by Prof. Oscar Simmersbach, viz., to
prepare the soil in order to call into life as quickly as possible,
and to promote by financial assistance, an increased activity of
research in the domain of the metallurgy of iron and its alloys.
For the study of this question the Hoard has appointed a com-
mittee which has recently held an exhaustive discussion on this
subject. They were unanimous in recognizing the necessity of
promoting with all energy, by scientific research, the progress
of metallurgy, with an eye to the exceedingly keen competition
in the world's markets, to be anticipated after the war. The
only divergency of opinions still existing is as to how such
promotion can be effected in the best and most effectual manner;
whether by the establishment of a special research institute,
possibly attached to the Kaiser Wilhelm Society, or by the
expansion of an already existing similar institution, or by study-
ing the problems of research, as they arise, in one or the other
scientific laboratory, but always while maintaining the requisite
relations with the practical working establishment.
"We may leave the decision as to the course to be adopted to be
quietly matured, but the Board recognized that it seemed
appropriate just now, in view of the present General Meeting,
to acquaint the members with this far-reaching and weighty
project, and to gain for it adherents in the widest circles of our
works and members. No doubt, funds to a considerable amount
will be required for carrying it through; the Board has therefore
approved the proposal of its committee that steps should be taken
for collecting a nucleus of funds, which should for the present
remain at the disposal of the Board of the German Iron and
Steel Institute. This fund is to serve in the first place to assist
towards turning to account, in practical working, the results
of the hitherto purely theoretical labors of the special branch
committees of the Institute in the manner appearing most
suitable in each case, if a research committee, to be specially
appointed for this purpose, endorses the proposal of the respective
special branch committee, and if the Board, on its part, considers
the granting of funds for the respective purpose appropriate.
In this way it would be possible, by enlisting suitable experts
or institutions, to take in hand, with the least possible delay,
the study of scientific questions important to the iron industry,
and at the same time we should, in this way, collect reliable
data to serve as a basis for the establishment of a special in
stitution.
"In thus submitting, for the first linn- in public, the idea of the
creation of a fund for an 'Institution for Metallurgical Re-
search,' I feel convinced that, when hereafter the works are
called upon to contribute towards the creation of the fund, we
may also rely on general and liberal support in the shape of
contributions. The German iron industry would thereby erect
to itself a worthy war memorial, a cradle for the solution of the
manifold problems, still confronting us, and which are of great
importance, not only as regards the iron industry, but also as
regards the common weal of our Fatherland."
Statement II
Meeting of tin- German Iron and Steel Institute, held at Diisseldorf,
June 19, 1917.
ESTABLISHMENT OF A GERMAN INSTITUTION FOR RESEARCH
ON IRON AND STEEL
In the midst of the war. (he German iron and steel industry
has laid the foundation stone of an important work of peace
At a meeting of leading men ol the German iron and steel in
.In .i i j i mill .ill pai is ul the Empire, which was held on June 19,
Diisseldorf, the establishment of an institution for re-
search on iron and steel was discussed. The invitations to the
meeting were issued by the Yerein Deutscher Kisenhiittenleute
(German Iron and St . whose president, A. Vogler,
General Manager of Dortmund, took the chair at the meeting.
Dr. 0 ' Eng., secretary of the association, gave
an exhaustive exposition of what had hitherto been done in the
ttific advancement of the metallurgy of
iron in the various countries. He pointed out the necessity of
rendering foundry technical research more and more profound,
in order that we may be well armed in every respect in the
inevitable economical struggle of the after-war period. He
could only refer briefly to the great and important tasks de-
volving on a research institution, especially as they are shortly
to be dealt with more explicitly in an exhaustive commemorative
publication. 'II pointed out, however, that only a
research institution free from any one-sided direction or delimita-
tion of its purpose would be capable of taking these in hand with
any prospect of success. The speaker further explained how
such an institution should be arranged, developed, and main-
tained, in detail, thus sketching to the meeting the main outlines
of the new research institution itself as well as of th
uisites of its fruitful working.
The subsequent expression of opinions on the part of those
present led, we are glad to say, to the momentous resolution,
passed unanimously, that the German iron and steel industry
w.is willing to establish a special scientific institution for ironand
steel research, to be attached to (or affiliated with) the Kaiser
Wilhelm Society. The preparatory work will be set on foot at
once by the Yerein Deutscher Eisenhiittenleute, and the associa-
tion will also be subsequently afforded the opportunity of
ensuring, in conjunction with the administrative committee of
the institution and a scientific advisory council, the indispensable
cohesion between the iron industry and the new research in-
stitute.
The locality of the new foundation has not yet been definitely
decided upon; the decision hereon has been left to the Yerein
Deutscher Kisenhiittenleute. But. according to the views
expressed in this respect at the meeting, the research institution
will be located in the Rhenish- West phalian industrial region.
The Southwestern and Silesian iron industries have unselfishly
renounced from the outset, in the interest of the great cause,
all claims in this direction.
The considerable funds required for the construction and main-
tenance of its research institution will be provided by the iron
and steel industry alone, apart from a small contribution from
the Kaiser Wilhelm Society, while the town in which the in-
stitution will be established will have to undertake to provide,
in addition to a subsidy towards the building expenses, the
requisite ground for its site, and its connection with the railway
by a siding, etc. The possibility is not precluded that, later
on, other industries engaged in the further elaboration of iron and
steel, may themselves take a share in the new research institution.
Thus it seems that all prerequisites are provided for to enable
this new creation to exercise a highly momentous and beneficent
influence on the further technical development of German
metallurgy of iron. It must be considered a high merit of the
German iron and steel industry that the project submitted by
Dr. F. Springorum, Doc. Eng., Councillor of Commerce, of
Dortmund, at the last General Meeting of the Verein Deutscher
Eisenhiittenleute, has so speedily been realized.
Statement III
This is a precis of the full Statement IV. report of meeting of the
Senate of the Kaiser Wilhelm Society agreeing to proposal to establish an
institute for research on iron and steel.
KAISER WILHELM INSTITUTE FOR RESEARCH ON IRON
KAISER WILHELM INSTITUTE FOR PHYSICAL SCIENCE
1 Meeting of Senate of Kaiser Wilhelm Society (founded
191 1) held on July 6, 1917, under presidency of Professor von
Harnack.
j Also present. Dr. Schmidt, Ministerial Director, and
Richter, Privy Councillor, on behalf of Ministry of Public
Health and Education.
Senators :
Dr. Fischer Dr. Planck von Rath
von Gwiuncr Dr. von Scbj
Koppel Dr. von Schnitzlex
Dr. Krupp von Bohlen und Dr. von Siemens
Halbach Count Ticle-Wmcklcr
Fran/, von Mendelssohn von Waldthausen
vonMoller Dr. Trendelenburg, District
von Passavant Gontard Judge. Gen. Sec
July, 1 918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
579
3 — Senate agreed with proposal of Verein Deutscher Eisen-
hiittenleute to establish the "Research Institute for Steel and
Iron," in form of a "Kaiser Wilhelm Institute."
4 — Intend to establish jointly with "Leopold Koppel Founda-
tion" an "Institute for Physical Research."
5 — To promote investigations of promising problems of
theoretical and experimental physics by monetary grants to
individual investigators.
6 — Professor Einstein, Member of Academy of Sciences,
proposed for appointment as Director of Institute.
7 — Scientific management to be entrusted to Directorate of
eminent physicists; administration to a body of Curators.
Statement IV
The following statement is a report of the meeting of the Kaiser Wilhelm
Society held on July 6, 1917, at which they agreed to the proposal of the
German Iron and Steel Institute to establish an institute for research on
iron and steel.
This is shown as a prens in Statement III.
KAISER WILHELM INSTITUTE FOR RESEARCH ON IRON
KAISER WILHELM INSTITUTE FOR PHYSICAL SCIENCE
On the 6th inst. a meeting of the Senate of the Kaiser Wilhelm
Society (founded 191 1) was held under the presidency of Pro-
fessor von Harnack.
Dr. Schmidt, Ministerial Director, and Richter, Privy Council-
lor, had appeared on behalf of the Ministry of Public Worship
and Education.
There were present the Senators Dr. Fischer, von Gwinner,
Koppel, Dr. Krupp von Bohlen und Halbach, Franz von
Mendelssohn, von Moller, von Passavant-Gontard, Dr. Planck
von Rath, Dr. von Sehjerning, Dr. von Schnitzler, Dr. von
Siemens, Count Tiele-Winckler, von Waldthausen, and Dr.
Trendelenburg, District Judge, General Secretary.
The Senate declared itself in agreement with the proposal
of the Verein Deutscher Eisenhuttenleute to establish the "Re-
search Institute for Steel and Iron," projected by them in the
form of a "Kaiser Wilhelm Institute."
It is intended to establish, jointly with the "Leopold Koppel
Foundation" an "Institute for Physical Research." The In-
stitute is to promote the investigation of promising problems of
theoretical and experimental physics by monetary grants to
individual investigators.
Professor Einstein, Member of the Academy of Sciences, has
been proposed for appointment as Director of the Institute.
The scientific management is to be entrusted to a Directorate
of eminent physicists, and the administration of the Institute
to a body of Curators.
Statement V
nhuttenleute (G>
Deutscher Eisenhiittenleute (German Iron and Steel Institute),
July 28, 1917.
FOUNDATION OF A BUILDING FOR IRON AND STEEL
RESEARCH
In the midst of the War, the German iron and steel industry
has laid the foundation of a significant peace work. At a
meeting of leading men of the industry from all parts of the
Empire, which took place at Diisseldorf on June 19, 1917, the
foundation of a building for research was discussed. The meet-
ing was convened by the German Iron and Steel Institute, the
president of which, General- Director A. Vogler, Dortmund, gave
an introductory address.
The business manager of the Institute, Dr. Engineer O.
Petersen, gave a detailed account of what has already been done
in the way of scientific research for the iron and steel industry
in various countries. He showed the necessity which will be
increasingly greater for technical research in all directions in
order to arm for the business struggle which will follow the War.
He could only deal shortly with the great and important tasks
which will fall on a research institute, especially as a detailed
memoir will shortly be published on the subject. The speaker
called attention, however, to the fact that the one aim of such
a technical research institute should be to attain success in every
task coming before it. How such an establishment is founded,
built, and maintained, was the subject of the speaker's further
discussion, who unfolded to the meeting in outline a picture
of the research building and the requirements for its profitable
working.
Tin concluding speeches of the meeting produced a satisfactol J
and unanimous resolution that the German iron and steel
industry is willing to erect, in conjunction with the Kaiser
Wilhelm Society, a special Technical Institute for Ferrous
Research. The preliminary work will be put in hand by the
German Iron and Steel Union, as then the Union will be able
later, in conjunction with the Governing Board of the Institute
and a technical assistant counsel, to guarantee proper connection
between the steel industry and the research institute.
The site of the new buildings has not yet been settled. The
decision has been left to the Committee of the German Iron and
Steel Institute. But it is apparent from the views expressed
at the meeting that the research building will be established
in the Rhenish-Westphalian locality. The Southwest and
Silesian industry have renounced their claims in this direction.
The means for building and maintaining the Institute, ex-
cepting a small contribution from the Kaiser Wilhelm Society,
will be raised by the iron and steel industry, while the town in
which it will be situated will be responsible, in addition to a
building subsidy, for the necessary land and its connection
to the railway, etc. It is not impossible that later other in-
dustries will participate in the new research institute.
All appearances show that the new institution will exert a
significant and valuable influence on the technical development
of the German steel industry. That the plan has matured must
be largely attributed to the speech of Dr. Engineer F. Springorum
before the last General Meeting of the Iron and Steel Institute
(see "Stahl und Eisen," March 15 and April 19, 1917).
Statement VI
a precis of the full Stati
of Kaiser Wilhelm Instit
ent VII, report of first meeting of
: foi Research on Iron.
KAISER WILHELM INSTITUTE FOR RESEARCH ON IRON
I — On June 19, 1917, German iron and steel industry adopted
a resolution to found an institution for free scientific research in
the domain of iron.
2 — -On November 13, 1917, a first meeting of "Curatorium"
(Trustee Committee) was held in "Stahl und Eisen" Building,
Diisseldorf.
3 — This research institution will carry on its activity under
the title of "Kaiser Wilhelm Institute for Research on Iron."
4 — -Curatorium consists of:
NAME
QUALIFICATIONS
REPRESENTATIVE OF
Dr. Schmidt
Minister of Education
Ministry of Education
(Substitute : Prof. *
and Public Worship
and Public Worship
Kruss)
.
Prof. D. A. von
Royal Privy Council- 1
Harnack
lor. President of the
(Sub.: Dr. Trendei- | Kaiser Wilhelm So-
enburg, Sec-Gen.)
ciety
Kaiser Wilhelm Society
Prof. Emil Fischer
Royal Privy Council-
Dr. G. Krupp von
lor
Bohlen und Halbach
Dr. Eng. '
General Manager
Councillor of Corn-
Dr. F. Springorum
Member Prussian Up-
per Chamber (Dort-
, German Iron and Steel
mund)
Institute
Dr. Eng.
General Manager
Dr. O. Niedt
Councillor of Com-
merce (Gleiwitz)
A. Vogler
Gen. Manager (Dort-
mundj
5 — The meeting, at which all above were present, except Prof.
Fischer, was also attended by the Secretary of the German
Iron and Steel Institute, Dr. O. Petersen, Dr. Eng.
6 — Dr. Springorum was elected Chairman of the Curatorium.
7 — On November 24, iyi~. a second meeting of the Curatorium
is to be held.
Statement VII
The following statement is B report of the first meeting of the Cura-
torium of the Kaiser Wilhelm Institute for Research on Iron, November
13, 1917. This is sh ow.i is a precis in Statement VI
Verein Deutscher Eisenhuttenleute (German Iron and Steel Institute.)
KAISER WILHELM INSTITUTE FOR RESEARCH ON IRON
Since the German iron and steel industry, on June ig last,
adopted the momentous resolution to found an institution for
free scientific research in the domain of iron, the preparatory
work infc ndi d to afford to this new centre of research an assured
itorj and financial basis has been advanced by the
Verein Deutscher Eisenhuttenleute sufficiently far to admit of
1 meeting of the Curatorium (Trustee Committee)
58°
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol.
10, No. 7
being held on the 13th inst. in the- "Stahl und Risen" Building
in Dusseldorf. The Curatorium of the research institution
which will carry on its activity under the style and title of
"Kaiser Wilhelrn Institute for Research on Iron" consists of
His Kxc. Dr. Schmidt. Minister of Education and Public Wor-
ship (Substitute: Prof. Kriiss) as representative of the Ministry
of Education and Public Worship; His Kxc. Prof. D A. v.
Harnack, Royal Privy Councillor, President of the Kaiser Wil-
helrn Society (Substitute: Dr. Trendelenbui ;, Secretary General) ;
His Exc. Prof I*iTiil Fischer, Royal Privy Councillor, and Dr.
Gustav Krupp von Bohlen und Halbach, as representatives
of the Kaiser Wilhelrn Society; and Dr.'F. Springorum, Dr.
Eng., General Manager, Councillor of Commerce, Member
of the Prussian Upper Chamber (Dortmund), Dr. 0. Niedt,
Dr. Eng., General Manager, Councillor of Commerce (Gleiwitz),
and A. Vogler, General Manager (Dortmund), as representatives
of the Verein Deutscher Eisenhuttenleute. The meeting, at
which all the above-mentioned gentlemen except His Exc.
Prof. Fischer were present, was also attended by the Secretary
of the Verein Deutscher Kisenhiittenleute, Dr. O. Petersen,
Dr. Eng. ; Dr. Springorum, Councillor of Commerce, was
elected Chairman of the Curatorium. The subject to be dealt
with at the meeting was the rules and regulations of the new
research institution. A second meeting of the Curatorium, for
the discussion of further questions concerning the organization
is to be held on November 24, 1917, in Berlin.
AMERICAN PHARMACEUTICAL ASSOCIATION
The Annual Convention of the American Pharmaceutical
Association will be held in Chicago, August 12 to 17, 1918.
Following is a brief outline of the program:
August 12: Meeting of the National Association Boards of
Pharmacy and American Conference of Pharma-
ceutical Faculties.
AUGUST 13: Second Session N. A. B. P. and A. G. Pb F.
Trip to Municipal Pier and Luncheon.
Card Party for Ladies.
Address of President of A. Ph. A.
Nomination of Officers.
August 14: Session of A. Ph. A.
Section Sessions.
Dinner of Alumni Organizations.
Theatre Party for Ladies.
President's Reception and Ball.
August 15: Sessions of A. Ph. A.
Section Sessions.
Automobile Ride.
Banquet.
August 16: Sessions of A. Ph. A
Section Sessions.
Election of Officers.
August 17: Closing Sessions.
CALENDAR OF MEETINGS
National Fertilizer Association — Annual Convention. Atlantic
City, N. J., week of July 15, 1918.
American Pharmaceutical Association — Annual Convention,
Chicago, 111., August 12 to 17, 1918.
American Chemical Society — Fifty-sixth Annual Meeting,
Cleveland, Ohio, September 10 to 13, 1918.
National Exposition of Chemical Industries Fourth' — Grand
Central Palace, New York City, September 23 to 28, 1918.
NOTL5 AND CORRESPONDENCE,
IMPORTANCE OF CHEMISTS RECOGNIZED BY SECRE-
TARY OF WAR
War Department
The Adjutant General's Office
Washington
May 28, 1918
From: The Adjutant General of the Army.
To: Department Commanders, Commanding Officers of
Replacement Training Camps, Depot Brigades and
Recruiting Depots, and to the heads of Bureaus
and Staff Corps.
Subject: Chemists.
1 — Owing to the needs of the military service for a great
many men trained in chemistry, it is considered most impor-
tant that all enlisted men who are graduate chemists should be
assigned to duty where their special knowledge and training can
be fully utilized.
2 — Enlisted chemists now in divisions serving in this country .
have been ordered transferred to the nearest depot brigade.
3 — You will make careful inquiry into the nu lber of graduate
chemists now on duty in your co imand and report their names
to this office. The report will include a statement as to their
special qualifications for a particular class of chemical work,
and whether they are now employed on chemical duties.
tlisted graduate chemists now in depot brigades, or
hereafter received by them, will be assigned to organizations
or service by instructions issued from this office. The report
called for in paragraph 3 herein will be submitted whenever men
having qualifications for chemical duties are received by depot
brigades, or replacement training camps, or by the training camps
organized by the various staff corps.
5 — Enlisted men who are graduate chemists will not be sent
overseas unless they are to be employed on chemical duties.
Prior to the departure of their organization for overseas duties,
they will be transferred to the nearest detachment or organiza-
tion of their particular corps.
6 — The Chief of the Chemical Service Section will be charged
with the duty of listing all American graduate chemists, including
those in the Army and those in civil life.
7 — Whenever chemists are needed by one of the bureaus
or staff corps, requests will be made on the Chief of the Chemical
Service Section for reco nmendation of a man having the quali-
fications necessary for the particular class of work for which he
is desired. If men having chemical qualifications are wanted
for only a short period of duty, they will be temporarily attached
to the bureau or staff corps; where the duty is of a permanent
nature, instructions covering their transfer will be issued. When-
ever the chemists thus attached or transferred are no longer
needed for purely chemical duties a report will be made to the
Chief of the Chemical Service Section in order that they may
be assigned to chemical duties at other places.
By order of the Secretary of War-
Roy A. Hiul
Adjutant General
War Department, A. G. C, May 29, 1918. To the Chief,
Chemical Service Section. 7th and B Streets. X W.. Washing-
ton, D. C, for his information and guidance. When reports
showing the number of chemists now at recruit depots, depot
brigades, and other places are received, they will be furnished
you, in order that proper notation may be made in your
register of chemists and for consideration in connection with
recommendations for assignment of chemists which you may,
from time to time, be called upon to make.
By order of the Secretary of War.
Roy A. Hnx
Adjutant General
July, 101S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
58i
COOPERATION OF AMERICAN CHEMICAL SOCIETY
WITH THE CHEMICAL SERVICE SECTION
The following letter to Secretary Parsons, of the American
Chemical Society, has been placed in our hands by Lt. Col.
Bogert, of the Chemical Service Section, N. A., with a request
for its publication in the belief that it will be of interest to
the members of the American Chemical Society. — [Editor]
War Department
Chemical Service Section, N. A.
Unit F, Corridor 3, Floor 3,
7th and B Streets, N. W.
Washington, D. C.
May 24, 1918
Dr. Charles L. Parsons, Secretary
American Chemical Society
Washington, D. C.
Dear Parsons:
There has just been placed on my desk a memorandum of a
conference between you, representing the American Chemical
Society, and Major Victor Lenher and Captain Frederick E.
Breithut, representing the Chemical Service Section of the Na-
tional Army. From this memorandum I note that a routine
mode of procedure has been agreed upon whereby the American
Chemical Society and the Chemical Service Section will cooperate
in order to keep in touch with every available chemist in the
country.
May I take this opportunity to express to you my sincerest
appreciation of all that you have done to aid the Chemical Ser-
vice Section. When, in February 1917, before the United
States entered the war, you, with rare foresight, sensed the
future course of events, and began the taking of a census of our
chemists, few of us realized how speedily such a census would
be needed nor how dependent we would be on your records for
the successful prosecution of our work.
The experiences and mistakes of France and England were
known to us all. The sending of chemists to the line in a war
which can be most accurately described as a chemical war, was a
suicidal blunder which we all hoped would not be repeated in
this country But this feeling on our part could have meant
but little when translated into action, had we not had the
necessary facts regarding the chemical man power of our coun-
try. These facts you gathered, card-catalogued, and indexed in
a manner which made immediately available precisely the data
which were needed.
In thanking you for this latest offer of cordial cooperation,
I desire also to express my great pleasure in being able to be
associated with you in an undertaking which must mean much,
not only for the winning of the war but also for the elevation
of the chemical profession to its true status.
One of our aims in the Chemical Service Section is the
organization and maximum utilization of the chemical man
power of the country for the general good. In endeavoring to
realize this, your work is going to count more than any other
single factor.
Cordially yours,
Marston T. Bogert
Lt. Col., Chem. Serv. Sect., N. A.
DU PONT FELLOWSHIPS
The situation in regard to the supply of chemists and chemical
engineers both for the present and for the future has been giv-
ing many industrial concerns a great deal of uneasiness. It is
a well-known fact that the number of men studying chemistry
and engineering in the advanced classes of all the colleges and
universities is on tin- decline, due to the inroads made by tin-
draft and by enlistments The du Pont Powder Company,
one of the largest employers of chemists in this country, has
been finding very great difficulty in obtaining a sufficient num-
ber of experienced chemists to meet the requirements involved
in the enormous expansion required to meet the situation brought
about by the war. As one means of inducing young men to
continue the study of chemistry, the du Pont Company has
recently set aside a sum of money to establish fellowships and
scholarships in a number of colleges and universities throughout
the United States. The fellowships are intended for graduate
students and have been offered to a number of the larger uni-
versities which have strong and well-developed graduate schools
of chemistry. The scholarships may be granted either to seniors
or to graduate students and have been offered to a number of
the best of the smaller schools which have the reputation of
doing high-grade undergraduate work. The fellowships amount
to $750 each and the scholarships from S300 to $350. The
money appropriated for the scholastic year 1918-19 has been
offered to a list of forty-eight of the representative institutions
of higher learning.
The object of this plan is to promote the study of chemistry
and to assist deserving students who have shown special apti-
tude for chemistry to pursue further work. The scholarships
and fellowships have been granted entirely without restriction
except that they are to be awarded by the college authorities
to advanced students of chemistry and it is hoped that the plan
may prove an initial step toward the true spirit of cooperation
between American educational institutions and industrial
concerns. The du Pont Company feels that the accomplish-
ment of these objects should materially assist in placing the
manufacturing and commercial interests of the United States
on a firmer basis.
FOUR HUNDRED THOUSAND DOLLAR GIFT TO THE
MASSACHUSETTS INSTITUTE OF TECHNOLOGY
At a recent meeting of the Corporation of the Institute,
President Maclaurin announced a gift of $400,000 from an
anonymous benefactor. The income of this fund is to be avail-
able for the general purposes of the Institute during the war
and thereafter is to be applied to the development of courses
in chemistry and physics.
It is a matter of the first importance in a school of applied
science to develop the fundamental sciences of physics and
chemistry as thoroughly as possible. The Institute has already
a strong staff in these departments.
A great group of the graduates of the chemistry department
are now serving the country in the development of its chemical
industries and in the prosecution of research with reference to
war problems, among this number being ten of the professors
of chemistry who have been wholly relieved from regular aca-
demic duties to devote themselves to the national cause.
The building up of strong departments of physics and chem-
istry at a school like the Institute of Technology which draws
men in large numbers from all parts of the country is a matter
of national importance. There is not only a great need for
well-trained chemists and physicists to solve the vital problems
of the war, but there will be a similar need in the industrial
struggle that will come when peace is declared. The oppor-
tunities presented by the war are being seized upon by alert
Americans, and great chemical industries are being built up
which will need the support of the most highly trained experts
to carry them on successfully under the conditions that will
later prevail. It is interesting t.> note that the rising genera-
tion also recognizes the opportunitj a 1 videnced among other
things by the fact that out of 620 freshmen at the Institute of
Technology tin-- year, 160 "! '• • • lined For the profession
of the chemist.
582
THE JOURNAL 01 INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 7
COAL-TAR PRODUCTS FOR 1917
The- United States Tariff Commission announces the comple-
tion of its census of coal tar produi 1 foi 1017. This group of
products includes not only the coal-tar dyes and the crude and
intermediate materials required for their manufacture, but
also all of the medicinal and ; chemicals, explosives,
synthetic resins, synthetic perfume materials, and flavors which
are in any way derived from coal-tar products. There were
produced in the United States (not inclusive of explosives and
synthetic phenolic resins) 54,367,994 lbs of fives and other
finished products, which have a total value of §68,711,228.
The production of the materials known as intermediates amounted
to 322,650,531 lbs., with a value of $106,942,918.
The annual production was reported for the following groups
of products made in whole or in part from materials derived
from coal tar: 45,977,246 lbs. of dyes valued at $57,796,027;
5,o92>558 lbs. of color lakes valued at $2,764,064; 2,236,161 lbs.
of medicinal chemicals valued at $5,560,237; 779,416 lbs. of
flavors valued at $1,862,456; 263,068 lbs. of photographic chem-
icals valued at $602,281; and 19,545 lbs. of perfume materials
valued at $125,960.
There were 81 establishments engaged in the manufacture of
coal-tar dyes in 191 7 and their production during that year
was practically identical with the amounts annually imported
before the war. The imports for the fiscal year 191 4 amounted
to 45,840,866 lbs. and the production in the United States in
1917 was 45,977,246 lbs. However, an analysis of this total
reveals that the domestic production, though equal in quantity
to the preceding imports, differs in the relative amounts of the
various classes of dyes. Only a small production was reported
for indigo, and the alizarin and vat dyes derived from anthra-
cene and carbazol — classes of dyes which include some of the
best and fastest colors known to the textile trade. The United
States produced only 2,166,887 lbs. of these dyes in 1917; and
the elimination of 1,876,787 lbs. of extract made from imported
indigo, reduces the output of these dyes to less than 3 per cent
of the pre-war imports. Dyes of this class are dutiable at 30
per cent in the Tariff Act of 1916. The lack of development
in the manufacture of these particular dyes promises to be reme-
died to a considerable extent in 1918, for a number of firms
have begun their manufacture and a large increase in produc-
tion can clearly be foreseen.
In the classes of dyes which if imported would be dutiable at.
30 per cent plus 5 cents per lb., the American manufacturers
have shown remarkable progress, producing 43,810,359 lbs.
at a total value of $57,639,990. That this represents something
of an excess over the American needs is evidenced by the fact
that during the fiscal year 1917, American-made dyes to the
value of Si 1,109,287 were exported to other countries. Thus
the exports exceeded the pre-war imports in total value although
not in tonnage nor in the variety of the dyes.
The development of the manufacture of intermediates is
equally marked, for before the war almost all of these necessary
materials were imported from Germany. The Tariff Commis-
sion finds that intermediates were manufactured by 117 firms
in 1917 and that the production amounted to 322.650,531
lbs. valued at $106,942,918. These figures, however, are some-
what misleading as there is inevitable duplication in the totals.
It is well known that many of the intermediates are derived from
other products of the same class. Thus starting with benzol
the following succession of products is obtained : nitrobenzol,
anilin, acetanilid, nitroacetanilid, and nitranilin. Each of these
products had to be reported by the manufacturer and hence
there has been some cumulative counting.
The totals for all of the coal-tar products will be pub-
lished in the final report which may well be expected to offer
accurate evidence on the progress of the American dyestuff
industry.
WASHINGTON LLTTLR
By Paul Wooton, Union Trust Building, Washington, D. C.
Revenue legislation, industrial curtailment, restriction of
imports, stimulations of domestic production and freight rates
have vied with each other during the past month in their bids
for public attention. Representatives of the chemical indus-
tries have been prominently associated with these activities.
Hdgar Gilbert, the general manager of the Lyster Chemical
Works of New York, brought to the attention of the Ways and
Means Committee some interesting facts with regard to the
taxation of capital invested in secret processes. While Mr.
Gilbert appeared primarily in his own behalf, he stated that the
matter was one of peculiar importance to the chemical industry.
In part, Mr. Gilbert said:
"The process patent is of such a nature very frequently that when it is
disclosed it makes it very difficult to protect the inventor. I might cite an
illustration that is old and familiar to all of us, that of the nitration of cotton.
"We will go hack to the time when nitrocellulose was first introduced;
it is au unknown thing; and we will to be used in this n
product, because il bad 1 se as nitrocellulose, but in a solvent form it
was used as a nitrocellulate. Now, the inventor, if he discloses it to the
he nature of his patent and of his process. But he
maintains hi: secret il and puts his nitrocellulose in another
1 II I Such as celluloid. Now if lie patents that, he has no m
himself against infringements because nitrocellulose appears
on the market and someone is producing it, but it would be difficult to know
■ other patent In that case the
inventor would naturally kn-|i secret the nature of his invention and find a
markel Foi it in the finished form ol some other product. There is an
ly, in tlu act of Congress in recognizing the in-
ventor of this subsl ml recognizing in
the inventor the right of protection, The nature of the thing may be such
rel process ,
he disclosure wo in of the product.
So I think the right of protection [i bed thai tl is only a step
ire identical from the in-
u .'i view, 11, takes whatever course seems to give him the
curity.
for
"Now, about his assignee. The inventor discovers a proce
doing a certain work. In one case he patents it and in another case he
keeps it secret. Now, he sells to a corporation for a certain consideration
and then that becomes an item of invested capital for the corporation.
Now, in the last bill secret processes were not mentioned at all, and my
point simply is that in the redraft of the new bill secret processes should be
classified as such, because they form, in the chemical industry especially,
a considerable item in the assets of the corporation.
"I had this matter up with Mr. Roper's committee for rulings, and they
felt that it was proper, they were identical, but they had no power to reach
it, they thought, to reach a secret process, to classify it; it had to go into
the patent proces
Industrial curtailment is still in an uncertain stage. To re-
lieve this undesirable condition, official promise has been given
that announcement will lie made of the amount of curtailment
it is necessary to make just as soon as the matter can be weighed
sufficiently to permit of an intelligent ruling. Careful surveys
have been made by the War Industries Board and theFueland
Railroad Administrations. It is shown conclusively that the fuel
supply is not adequate for all purposes. At the same time, steel
and other materials cannot be manufactured in sufficient volume
to meet all requirements. In deciding which industries should
be curtailed, great difficulties have been experienced. The Fuel
Administration has a lisl ol som< j6o industries which are classed
as non-war activities. The list has not been, made public and the
amount of curtailment that will be expected from each has not
been determined, with the exception of .1 few cases The m.inu-
1 pleasure cats lias been reduced to 25 per cent of the
volume of last year. 1 Uher restrictions are expected to follow
promptly.
By heavier loading this year, the fertilizer manufacturers of
the country havt ce equivalent to 87.000 cars. The
loading this year was 30.02 tuns, as compared with
21 ..si tons in 1017. This shows an increased loading efficiency
of 40. 8 per cent.
July, io if
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
5S3
Hearings on the War Minerals bill continued throughout the
month of April, but delay in the consideration of the bill by the
committee was occasioned by the enforced absence of Senator
Henderson, the chairman of the Committee on Mines and Min-
ing. Great uncertainty exists among members of the committee
as to this legislation. Some of the most capable men in the
country appeared before the committee and urged that no legis-
lation be enacted which would permit governmental interfer-
ence with delicately poised industries which handle the war
minerals. The power to fix prices and to regulate the industry
otherwise might have such far-reaching consequences that some
of the members of the committee, at least, are of the opinion
that such measure of control as is needed can be exerted under
existing law by the War Industries Board.
Additional restriction on imports have been announced by the
War Trade Board. They include castor beans, castor oil,
caffeine, and gypsum. All outstanding licenses allowing ocean
shipment of castor oil and castor beans have been revoked.
Imports may be made only on the approval of the Bureau of
Aircrafts Production.
Imports of caffeine, theine, and trimethylxanthine have been
cut off entirely.
Importation of gypsum from overseas has been stopped, with
the exception of that which can be carried on sailing vessels or
barges, which may be designated for that purpose.
Announcement was made by the War Industries Board
of/a schedule of manganese prices, which ran from 86 cents per
unit for 35 per cent metallic manganese to $1 .30 per unit for
54 per cent metallic manganese. While the schedule did not
cover the chemical ores, it has direct bearing on them.
Daniel C. Jackling, director of the Explosive Plants Division
of the War Department, announced on June 1 1 the completion,
two months ahead of schedule, of the big plants at Charleston,
W. Va., and at Nashville, Tenn. Sulfuric and nitric acid produc-
tion at these plants began early in June.
In the trade agreement recently consummated with Norway,
the War Trade Board was particularly liberal in allowing the
exportation to that country of chemicals. Among the chemical
substances which may be exported under this agreement are:
linseed oil; turpentine; palmitic acid; stearic acid; paraffin
wax; varnishes; rapeseed oil; ceresine and carnauba wax; rosin;
animal and vegetable oils; fats and fatty acids; Chinese wood oil;
small quantities of starch, chalk, pyrites, copper, borax, nitrate of
soda, bleaching powder, sulfuric acid, and silicate of soda;
alum; sulfur; lead; and Solvay soda. Most of the chemicals
are to be shipped into Norway consigned to the Oil and Color
Merchants' Association and to the Norwegian Papermakers'
Association.
Nitrate plant No. 3 is to be constructed and operated by the
Air Nitrate Corporation. The plant is to consist of two units,
one to be built near Cincinnati and one near Toledo. In each
instance, construction work has started. Each of the plants
will require the services of 1700 operators.
Exports of chemicals during Aprii fell off decidedly, as com-
pared with forwardings abroad during the corresponding month
of last year. According to preliminary figures, based on returns
to the Department of Commerce, chemical exports in April
of this year were valued at $12,646,505. This compares with
$16,159,506, the value of chemical exports in April of last year.
F. J. Goodfellow, Secretary of the National Wood Chemical
Association, has been appointed charcoal representative of the
Fuel Administration.
PERSONAL NOTLS
John Harper Long, dean of the Northwestern University
School of Pharmacy and a member for many years of the
American Chemical Society, died at his home in Evanston,
111., June 14, 1918, after an illness of nine months. He had been
making definite progress toward recovery and was looking
forward to complete restoration of his health when a sudden
attack of the heart trouble from which he had been suffering
caused his death.
Funeral services were held on June 17. Professor Long's
sons and son-in-law, Dr. Holgate, president of Northwestern
University, and Dr. Ira Remsen, past president of the American
Chemical Society and a close friend of Dr. Long, were the
active pallbearers. The colleagues of Professor Long on the
University staff and Dr. Julius Stieglitz, past president of the
American Chemical Society, who had been closely associated
with Dr. Long in many scientific undertakings, were the honorary
pallbearers.
John Harper Long was born near Steubenville, Ohio, in
December 1856. In 1877 he received the degree of B.S. at the
University of Kansas; during the years 1877-1880 he studied
at Tubingen, Wiirzburg, and Breslau, receiving the degree of
Sc.D. at Tubingen in 1879. In 1881 he became professor of
chemistry at Northwestern University Medical School and in
1913 was made dean of the School of Pharmacy at the same
institution.
Professor Long was a member of the referee board of consult-
ing scientific experts for the U. S. Department of Agriculture,
the revision committee for the U. S. Pharmacopoeia, the council
on pharmacy and chemistry of the American Medical Associa-
tion. He belonged to the Deutsche chemische Gesellschaft,
the Washington Academy of Sciences, the Society of Biological
Chemists, the American Association for the Advancement of
of which he was a Fellow, and the American Chemical
Society of which he was a past president
Charks Christopher Trowbridge, assistant professor of physics
in Columbia University and a noted ornithologist, died suddenly
on June 2 in Roosevelt Hospital, New York City, of blood poison-
ing Professor Trowbridge had been a member of the teaching
Staff of Columbia since iK<>2. He was in his forty-ninth year.
Mr Lester F. Weeks, assistant professor of chemistry in the
University of Maine, has been appointed assistant pi
of chemistry at Colby College to succeed Dr. Robert G. Caswell,
who has resigned.
Mr. S. H. Diehl was killed in the explosion at the Aetna Chem-
ical Works in Oakdale, Pa., on May 18, 1918.
At the annual meeting of the American Academy of Arts and
Sciences held on May 8, 1918, acting on the recommendation
of the Rumford Committee, it was unanimously voted to award
the Rumford Premium to Theodore Lyman for his researches
on light of very short wave-length.
Mr. Frank Maltauer, formerly employed as bacteriologist
in charge of research work on biological chemistry problems
at the New York State Laboratories and Research Division of
the Heath Department, is at present serving as a private at
General Hospital No. 14, Fort Oglethorpe, Ga.
The name of Dr. A. B. Lamb, who has given generously of
his time and energy to the work of the Bureau of Mines Experi-
ment Station in Washington, was inadvertently omitted from
the list of representative leaders in that work mentioned in the
editorial "America in Safe Hands" in the June issue of This
Journal.
Mr. John H. Card, teacher of chemistry at the High School,
Brockton, Mass., has joined the Chemical Service Section, N. A.
He has been assigned to the Offensive Research Investigations at
the American University Experiment Station, Washington, D. C.
Dr. Geo. R. Bancroft has resigned the professorship of chem-
istry and physics in Transylvania College, Lexington, Ky., to
accept a position in the University of Kentucky as assistant
professor of organic and physical chemistry.
The honorary degree of Doctor of Chemistry was conferred
upon Mr. Arthur D. Little, of Cambridge, Mass., by the Uni-
versity of Pittsburgh at the commencement exercises on May
31, 1918.
Mr. A. Gordon Spencer, consulting chemist and metal-
lurgist, 619 Transportation Building, Montreal, P. Q., is giving
up his consulting practice to devote all his time to the munition
and other work of the Peter Lyall and Sons Construction Co.,
Montreal, as their consulting metallurgist.
Mr. C. A. Clemens, formerly instructor of chemistry at Rens-
selaer Polytechnic Institute, Troy, New York, who is now with
the Gas Defense Service, Sanitary Corps, has been sent to the
Lakehurst Experimental Grounds, Lakehurst, N. J.
Mi. C'has. B. Waller, formerly with the Pennsylvania Trojan
Dtown, Pa., is now with the Non-Freezing High
Explosive Corporation at Kingston, N. Y.
Mr William A, Waldie, formerly chemist for the 1
Varnish Company, bul more recently with the Thibaut and
Walker Company, has again returned to the Glidden Company
as chief chemist.
--C'J
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10 No. 7
In Science for May 10 Associate Director Kdward R. Weidlein of the Mellon Institute, who is Acting Director in the absence of
Director Bacon, gives the following summary of the industrial fellowships in operation at the Institute on March 1, 1918.
Names op
Industrial Fellowships
No. in Operation
92 Leather Belting
95 Magnesia
99 Glyceryl Phosphates
Indtstrial Fellows. Names and Decrees
. D. Wilson (Ph.D., University of Chicago)
. D. ISagley (Eli.. University of Illinois)
F. Rupert (Ph.D., Massachusetts Institute of Technology)
10:
Fruit Juice
Enameling
Bread
Window Glass
Leather Soling
Iron Ore
Dental Products
129 Illuminating Gla
137 Toilet Articles
138 Silicate
139-A Organic Synthesis
139-B Organic Synthesis
Insecticides
By-products Recovery
Coke
R. R. Shively (Ph.D., University of Pittsburgh)
ivcrsity of Wisconsin)
H. A. Kohman (Ph.D., University of Kansas), Senior Fellow
R. R. Irvin (M.S., University of Kansas) (Vacancy)
R. M. Howe (M.S.. University of Pittsburgh), Senior Fellow (Vacancy)
A. C. Nothstine (B.S., Ohio State University)
C. B. Carter (Ph.D., University of North Carolina)
P. M. McClenahan (M.A., Yale University)
C. C. VoKt (Ph.D., Ohio State University)
C. L. Perkins (B.S., New Hampshire College)
J. W. Schwab (B.S., University of Kansas)
C W t lark (Ph.D., University of Pittsburgh)
Harry Ivssex (Ph.D., University of Gottingen)
I. W. Humphrey (M.S.. University of Kansas) (Vacancy)
E. O. Rhodes (M.S., University of Kansas)
B. A. Stagner (Ph.D., University of Chicago)
H. D. Clayton (B.A.. Ohio State University)
C. W. Trigg (B.S., University of Pittsburgh)
A. H. Stewart (A.B., Washington and Jefferson College) (On leave of ab-
sence)
F. W. Stockton (A.B., University of Kansas)
J. B- Garner (Ph.D., University of Chicago), Senior Fellow (Vacancy)
F. A. McDermott (M.S., University of Pittsburgh)
Ruth Glasgow (M.S., University of Illinois)
T. A. Frazier (B. Chem., University of Pittsburgh)
P. H. Brattain
I. S. Hocker (B.S., University of Pennsylvania)
E. E- Bartlett (Pet.E., University of Pittsburgh)
J. E. Schott (M.A., University of Nebraska)
J. D. Malcolmson (B.S., University of Kansas)
G. A. Bragg (B.S., University of Kansas), Senior Fellow of all Copper
Fellowships (Vacancy)
L. M. Liddle (Ph.D., Yale University)
M. G. Babcock (M.S., Iowa State College)
G. O. Curme, Jr. (Ph.D., University of Chicago), Senior Fellow
J. N. Compton (M.S., Columbia University)
H. R. Curme (B.S., Northwestern University)
E. W Reid (M.S., University of Pittsburgh)
H. A. Morton (Ph.D., University of Pittsburgh), Senior Fellow
C. J. Herrly (B.S., Pennsylvania State College)
H. E. Peck (B.S., Clarkson Memorial College of Technology)
O. F. Hedenburg (Ph.D., University of Chicago)
Walther Riddle (Ph.D., University of Heidelberg)
F. W. Sperr, Jr. (B.A., Ohio State University), Advisorv Fellow
Marc Darrin (M.S., University of Washington)
O. O. Malleis, (M. S.. University of Kansas)
L. R. Office (B.S., Ohio State University)
H. H. Meyers (B.S., University of Pennsylvania)
(Fellow to be appointed)
R. H. Bogue (M.S., Massachusetts Agricultural College)
David Drogin (B.A., College of the City of New York)
H. F. Perkins
W B. Pattison (M.A., University of Nebraska)
H. G. EUedge (M.S., University of Pittsburgh), Senior Fellow
K. R. Beach (A.B., Southwestern College)
(3,800 a year. April 1, 1918
$4,750 a year. November 1, 1918
$1,500 a year. Bonus, 10 per cent
of profits. October 1, 1918
$5,000 a year. April 1, 1918
$2,200 a year. April 1. 1918
$7,500 a year. Bonus, $10,000.
March 1, 1919
May
1918.
$6,000 a year.
Bonus, $500
$3,000 a year. Bonus. $2,000.
June 1, 1918
$3,500 a year. June 4. 1918
$3,000 a year. June 15. 1918
$2,400 a year. Bonus, royalty
on sales. Julv 1. 1918
$5,400 a year. July 1, 1918
$3,500 a year. September 1. 1918
$10,000 a year. Bonus. $10,000.
September 1, 1918
$4,000 a year. Bonus, $3,500.
August 1, 1918
$3,000 a year. October 1, 1918
$2,800 a year. October 1, 1918
$1,800 a year. Bonus, 2 per cent
of gross receipts. October I.
1918
$900 a year. October I. 1919
$5,000 a year. October 16, 1918
$7,500 a year. September 15,
1918
$12,700 a year. Bonus. Novem-
ber 1. 1918
$3,000 a year. November 1, 1918
$3,000 a year. November 15,
1918
$2,500 a year. November 15,
1918
$5,000 a year. November 1. 1918
$3,500 a year. December 1, 1918
$2,500 a year. December 1. 1918
$10,000 a year. Bonus. $5,000.
January 1, 1919
$5,000 a year. Bonus, $5,000.
January 1, 1919
$2,500 a year. December 1 1 .
1918
January 1, 1919
January 1, 1919
January I. 1919
$3,000 :
$3,000
$7,000
year,
year,
year.
$5,000.
$3,000 a year. Bonus.
January 5, 1919
$2,000 a year. January 5, 1919
S2.500 a vear. January 5. 1919
$5,300 a year. January 18. 1919
$2,100 a year. Bonus. $2,000.
February 1, 1919
$5,000 a vear. February 15, 1919
Kenneth D. Kahn, research chemist and metallurgist for the
Cleveland Brass Manufacturing Company, Cleveland, Ohio,
has been appointed assistant chemical engineer at the Bureau of
Mines Experiment Station, American University, Washington,
D. C, engaged in the manufacture of war chemicals.
Mr. William Rhafferty, who was formerly chief chemist at
the Camden Works, General Chemical Company, and was later
transferred to the Bayonne Works, has resigned his position to
take up work as assistant to the superintendent of Chas. Lennig
and Company, located at Bridesburgh, Pa.
Mr. M. E. Jennings, formerly with the Central Pharmaeal
Co., Seymour, Indiana, is now a Sergeant in Company E, 30th
Engineers, and is located at Fort Meyer, Ya.
Mr. I'. A. Fererer has left Eli Lilly and Company and is in
the Medical Department of the Army, located at Newport News
Mr. C. M. Sharp, formerly an instructor at Shortridgc High
School, is in the chemical service of the Medical Corps, located
at St. Louis.
Mr. V P. McManus, well known in drug and chemical circles
and for many years associated with McKesson and Robbins,
has severed his connection with that house and is now with
H. W. Hcnning & Son, 80 Maiden Lane. New York City.
Henry Coit MacLean, for two years assistant manager of
the Foreign Trade Bureau of the Merchants' Association of
New York, has assumed his new duties as manager of the New
York Office of the United States Bureau of Foreign and Domestic
Commerce. Mr. MacLean is thoroughly familiar with the work
of the Bureau of Foreign and Domestic Commerce and has been
in close touch with questions confronting exporters and importers
arising from war conditions.
Mr. Howard A. Winn, formerly of H. H. Hay Sons, manu-
facturing pharmacists, Portland, Me., is now with the United
Drug Co. in the pharmaceutical department.
Dr. A. S. Eastman has given up his position as professor of
chemistry at the L'niversity of the South, Sewanee, Tenn., and
is now connected with the research laboratory of the Hercules
Powder Co., Kenvil. X. T , in charge of the research work on
T. X. T.
Dr. Robert G. Caswell has resigned as assistant professor of
chemistry at Colby College, to accept a position as one of the
research chemists for E. I. du Pont de Nemours & Co Wil-
mington, Del.
Prof. Herman I. Schlesinger has been promoted to assistant
professor of chemistry at the University of Chicago.
July, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
S8S
INDUSTRIAL NOTES
Statistics compiled by the Bureau of Foreign and Domestic
Commerce show that nearly twice as much sulfuric acid was
produced in the United States in 191 7 as 1913, which is taken
as a normal before-the-war-period.
Contracts have been awarded by the Ordnance Department
for the establishment of two large picric acid plants at Little
Rock, Ark., and Brunswick, Ga. It is expected that the
Little Rock plant will be in operation in September 1918.
These will be the first Government-controlled picric acid plants
to be established in this country.
How 2,000,000 gallons a year of cymene which is now going
to waste in the manufacture of paper pulp can be used to pro-
duce a line of dye colors very close in their properties to aniline
dyes has been worked out in the Color Investigations Laboratory
of the Bureau of Chemistry, United States Department of
Agriculture. This is the first and very important result of ex-
tensive research, investigation, and experimentation conducted
in this laboratory under the direction of Dr. H. D. Gibbs.
Paul Wengerand Co., 35 Nassau Street, New York City, well
known in the metal trade, have opened a chemical branch in
which they will act as buyers, sellers, exporters, and importers.
They intend eventually to enter into the manufacture of chem-
icals and drugs. Charles W. Buck, who up to now has been
manager of the Cooperative Drug Company, at South Norwalk,
Conn., has been appointed manager of the new plant.
The Cobwell Corporation will have completed in Cleveland
within the next 35 days a plant of 25 to 35 tons' daily capacity
handling garbage, butcher's offal, and dead animals. This
will be of most modern construction and will incorporate all
of the newest features covered by the patents of Raymond
Wells including a complete equipment for the manufacture of
alcohol as an additional product. This plant has been under-
taken as a large scale demonstration and experimental plant
and will be open at any time to those interested in the business
or its development.
On June 2 the J. K. Mosser Tanning Company's plant
at Noxen, twenty-five miles from Wilkes-Barre, Pa., was de-
stroyed by fire. The loss is estimated at $3,000,000. The
cause of the fire is believed to have been due to crossed wires in the
hair-drying room. The plant was controlled by Armourand Co.
For the first quarter of 19 18 the metalliferous production of
the Province of Ontario was $17,909,000, a gain of $2,315,000
over the same period last year. Gold production amounted to
"3,387 ounces, and of that amount the Hollinger mines contrib-
uted 68,804 ounces, or a little more than half of the total. The
increase was principally silver, owing to the higher price obtained.
Gold, on the other hand, in the aggregate fell off, owing to
labor difficulties. The three months' silver total was $3,740,000,
against $2,831,000 in 1917. Total gold production fell from
$2,601 ,000 to $2,265,000. Nickel and copper show a small decrease.
Hollinger is now producing gold at the rate of approximately
$6,000,000 annually.
H. Koppers Company announce that they have been awarded
a contract by the Jones and Laughlin Steel Company for the
construction of a by-product coke plant of 300 ovens. This
plant will have a carbonizing capacity of approximately 2,000,000
tons per year, and will replace beehive coking capacity to that
amount. The plant will be complete in every respect, and will
be equipped for the recovery of ammonia in the form of ammo-
nium sulfate, of tar, and of benzol and toluol as pure products.
The ammonium sulfate and pure toluol from this plant will be
sold to the Government for war purposes. The steel company
proposes to use the gas in its steel plant operations. It has
also been announced recently that H. Koppers Company are
to build two more batteries of by-product ovens for the plant
of the Steel Corporation at Clairton, Pa. This will give the
Steel Corporation a plant of 748 ovens which, when completed,
will be the largest by-product coke plant in the world. The
plant of the Illinois Steel Co., Gary, Ind., which has recently
added 140 Koppers ovens to its original installation of 560 ovens,
is at present the largest by-product coke oven plant in the world.
The War Industries Board has announced that a commodity
section on medicines and medical supplies has been created, with
Lieut. Col. F. F. Simpson as its chief. The work of this section
will be closely coordinated with that of the Chemical Division.
This new section will deal incidently with chemicals as they enter
into medical compounds, preparations, etc., and will work in
conjunction with the section of the Chemical Division dealing
with fine chemicals and bulk medicinal chemicals.
Any doubt about the status of the steel industry in relation
to the Government was cleared away Friday, May 24, at the
annual meeting and banquet of the American Iron and Steel
Institute. A good index to the situation was furnished by Judge
E. H. Gary, representing the steel interests; Charles M. Schwab,
representing the Emergency Fleet Corporation; and J. Leonard
Replogle, director of steel supplies for the Government. The
steel manufacturers pledged their support to the Government
to the extent of 100 per cent of their respective outputs. They
also agreed that steel would be allotted to consumers in order
of the importance of its use for national purposes, the judge
being the director of the steel supply. Preference is now given
to' shipbuilding steel, following which in importance comes shell
steel, and then steel rails. Mr. Replogle has announced that to
fill the Government's demands will require the entire capacity
of the steel mills for at least a year. The prospects of manufac-
turers engaged upon other than Government work keep growing
dimmer, though producers are anxious to aid them so far as
possible. Steel for Japan has begun to go forward. Already
20,000 tons have been shipped from the Pacific Coast, and the
balance, 155,000 tons still due, will follow later.
The Independent Filter Press Company has removed from
47 West 34th Street, New York City, to 418 Third Avenue,
Brooklyn, N. Y.
Like most other countries Japan has suffered from the shortage
of dyes and chemicals due to the European War. Prior to the
war, Japan imported annually dyes valued at $3,500,000, nearly
all of which came from Germany. As most of these dyes were
used in the important textile industries of Japan and prices had
been advancing by leaps and bounds, the Government passed
a law in 1915 providing for the grant of subsidies to companies
engaged in the manufacture of dyes (including aniline salt, aniline
dyes, alizarine dyes, and synthetic indigo,) and chemicals in
Japan, and requiring that more than half of the capital
of any such company be subscribed by Japanese subjects.
The amount of the subsidy to be granted is sufficient to en-
able the companies to pay a dividend of 8 per cent per annum
on their paid-up capital. The subsidies are for a period of
ten years from the date of the promulgation of the law.
Medicines or perfumery specified by Imperial Ordinance,
manufactured from by-products of coal tar, are regarded as
manufactured dyes and chemicals. The manufacture of the
materials of gunpowder and explosives and of certain medicines,
to be determined by Imperial Ordinance, are also regarded as
the manufacture of dyes and chemicals. One of the results
which attended the efforts made by the Japanese Government
to solve the dyestuff problem was the formation of the Japan
Dyestuff Manufacturing Company, Ltd., with a capital of
8,000,000 yen (about $4,900,000), subsidized by the Government.
The War Department authorizes the statement that opera-
tions in the Government's new powder plants near Charleston,
W. Va., and Nashville, Tenn., have begun two months ahead
of schedule. The Nashville plant started June 5, and the
Charleston plant started June 12. These plants will produce
sulfuric and nitric acids. The capacity of these two plants is ex-
pected to equal that of all the other American smokeless powder
plants combined.
At a meeting of the Iron and Steel Institute on May 3,
awards of $500 from the Carnegie Research Fund were made to
Mr. George Patchin, of London, an associate of the Royal School
of Mines, and formerly head of the metallurgical department
of Birkbeck College, to enable him to pursue research on "Semi-
steel and its heat treatment;" to Mr. Samuel L. Hoyt, U. S. A.,
to enable him to study "The foreign inclusions in steel, their
occurrence and identification;" and to Professor J. A. Van den
Broek, of the University of Michigan, for research work on "The
elastic properties of steel and alloys."
During May nine new companies were organized for the manu-
facture of drugs, chemicals, and dyestuffs. The aggregate for
the entire war period now stands at $378,987,000. The figures
for May compare with eighteen concerns formed in April for
an aggregate capitalization of $3,980,000. The average in-
corporation per company in May was $133,333. This figure
compares with $221,111 in April and $439,838 in March. Two
war companies were created during May. They were the Swift
Aircraft Manufacturing Company with an authorized capital
of $50,000, and the United States Ammunition Company,
with a capitalization of $2,500,000. The addition of these two
concerns brings the total of investments in this industry up to
$269,625,000.
586
THE JOURNAL OF INDUSTRIAL AND ENGINEERING ( HEMISTRY Vol. io, No. 7
GOVERNMENT PUBLICATIONS
By R. S. McBride, Bureau of Standards. Washington
NOTICE — Publications for which price is indicated can be
purchased from the Superintendent of Documents, Government
Printing Office, Washington, L). C. Other publications can
usually be supplied from the Bureau or Department from which
they originate. Commerce Reports are received by all large
libraries and may be consulted there, or single numbers can be
secured by application to the Bureau of Foreign and Domestic
Commerce, Department of Commerce, Washington. The regu-
lar subscription rate for these Commerce Reports mailed daily is
$2.50 per year, payable in advance, to the Superintendent of
Documents.
COUNCIL OF NATIONAL DEFENSE
List of Staple Surgical and Medical Supplies. Reprint
with revisions of the lists of medicines, antiseptics, disinfectants,
chemicals, etc., selected to meet war conditions by the Com-
mittee on Standardization. 27 pp.
Laboratory Supplies. Reprint of list selected by the Com-
mittee on Standardization. 26 pp.
PAN AMERICAN UNION
Some Andean Sulfur Deposits. B. I,. Miller and J. T.
Singewald, Jr. Reprint from January 1918 number of Bull,
of the Pan American Union. 16 pp.
PUBLIC HEALTH SERVICE
A New Disinfectant Testing Machine. A. M. Stimson and
M. H. Xeill. Public Health Reports, 33, 529-39 (April 12).
Arsphenamine (Salvarsan) and Neo-Arsphenamine (Neo-
Salvarsan). Public Health Reports, 33, 540-2 (April 12).
Licenses ordered and rules and standards prescribed for their
manufacture.
The Dietary Deficiency of Cereal Foods with Reference to
Their Content in "Antineuritic Vitamine." G. Yoegtlin, G. C.
Lake and C. N. Myers. Public Health Reports, 33, 647-66
(May 3).
The Present Status of Our Knowledge of Fatigue Products.
E. L. Scott. Public Health Reports, 33, 605-610 (April 26).
1 — Substances carrying hydrogen ions, as lactic and /3-oxy-
butyric acids, potassium dihydrogen phosphate, and carbon
dioxide Maud as causal agents of fatigue.
2 — Certain products of protein disintegration, as indol, skatol,
and phenol may produce fatigue Symptoms and may be active
agents in producing normal fa1
,\- — There is some evidence that the negative ion of lactic and
0-Oxy-butyric acids and that certain positive ions, especially
that of potassium, are callable of producing certain fatigue
phenomena.
4 — There is no evidence that the negative ions of carbonic,
phosphoric, or sulfuric acids are fatigue substances.
5 — There is no evidence at present for the existence of specific
fatigue substances as proposed by Wciehardt.
6 — There is very little probability that creatin or creatinine
have any relation to fatigue or to muscle work in general.
7 — There are no doubt numerous bodies, as purine bases, uric
acid, etc . which may Ik- increased by work, but which have no
!.. aring on fatigue.
GEOLOGICAL SURVEY
The Lake Clark-Central Kuskokwim Region, Alaska. P. S.
Smith. Bulletin 655. 147 pp. and _• maps. With special
ion to mineral resources.
Cannel Coal in the United States. G. H Ashley. Bulletin
659. 116 pp. Paper, 15 cents. The present paper is not in-
tended as an original contribution to the subject, though the
writer has drawn on his own notes in describing many of the
deposits mentioned, particularly those in Pennsylvania. Indiana,
and parts of West Virginia and Kentucky. It consists of a
preliminary review of well-known facts about the character,
uses, and value of caimel coal and brief descriptions of workable
deposits of cannel coal, including cross sections of the beds, and
it give> such analyses of the coal as are available.
The Structural and Ornamental Stones of Minnesota. O.
Bowles Bulletin 663. 199 pp. Prepared in cooperation
with the Minnesota State Geological Survey.
Manganese at Butte, Montana. J. T. Pardee. Bulletin
690-E. From Contributions to Economic Geology, 1918. Part I.
20 pp. Published April 9. A search through the published
reports describing the ore deposits of Butte, supplemented by a
brief field examination in August 191 7, revealed the fact, per-
haps not generally appreciated heretofore, that the amount of
material in the lodes that is sufficiently rich in manganese to
be considered a possible source of that metal is very large. The
smaller part of this material, which is found in the outcrops and
upper parts of the lodes, consists of manganese oxides associated
with more or less quartz.
By far the most of the manganiferous material below the oxi-
dized zone at Butte consists of rhodochrosite and rhodonite,
the carbonate and silicate of manganese, respectively, associated
in different proportions with quartz and sulfides. The most
interesting and promising feature concerning the occurrence of
manganese at Butte is the fact that portions of this unoxidized
material consist of fairly pure rhodochrosite and are, therefore,
very valuable as a source of the metal. Reported analyses of
material of this character in the Emma mine run from 34 to 41
per cent manganese and as low as 1 per cent silica. According
to reports this material when lightly roasted gives off its carbon
dioxide, and as a result the percentage of manganese is increased
in the product. The known workable bodies of this ore aggre-
gate several thousand tons, and there is reason to expect that
future developments will disclose large additional amounts.
Whether the general run of the unoxidized manganiferous
material can be considered under any conditions as a possible
source of manganese is a question for metallurgists t>'
The amount of material that contains 15 per cent or more man-
ganese and occurs within the depths ordinarily reached in mining
is indicated, by the evidence available, to be millions of tons.
Because they lie at the surface the oxide ores can be mined as
rapidly as desired, and the extensiveness of the underground
workings, of which many that are temporarily abandoned could
probably be made usable in a short time, will permit the car-
bonate and silicate ore also to be rapidly extracted. Therefore,
whether Butte can be counted upon without delay for a con-
siderable production of manganese depends on the solution of
problems concerning the metallurgy rather than the mining of
its manganiferous deposits.
The Structure of Parts of the Central Great Plains. X H.
DarTON. Bulletin 691-A. From Contributions to Economic
101S, Part II. 26 pp. Published April 2 Mainly
of geologic interest.
Gold, Silver, Copper, Lead, and Zinc in Idaho and Washington
in 1916. C X. GERRY. From Mineral Resources of the United
States. Hiid. Part 1. 5; pp. Published March 14. Mines.
reporl ; general report later.
July, 191S
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
NLW PUBLICATIONS
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I Agriculture: The Teaching of Agriculture. A. W. Nolan. 12mo. 277
pp. Price, $1.30. Houghton, Mifflin Co., Boston.
Blast Furnace: Principles, Operation and Products of the Blast Furnace.
J. E. Johnson, Jr. 8vo. 551 pp. Price, $5.00. McGraw-Hill Co.,
New York.
I Carbon and Its Allies. R. M. Craven. 8vo. 468 pp. Price, $5.00.
J. B. Lippincott Co., Philadelphia.
Chemical French. M. L. Dolt. 8vo. 398 pp. Price, $3.00. Chemical
Publishing Co., Easton, Pa.
Chemistry: What Industry Owes to Chemical Science. R. B. Pilcher.
8vo. 164 pp. Price, 3s. Archibald Constable & Co., London.
Chemistry of Food and Nutrition. H. C. Sherman. 2nd Ed. 12mo.
545 pp. Price, $2.00. The Macmillan Co., New York.
Concrete and Cement; a List of Books. 12 pp. Gratis. The Public
Library, Brooklyn, N. Y.
Enamels. R. D. Landrum. 8vo. 106 pp. Gratis. The Harshaw,
Fuller & Goodwin Co., Cleveland.
Fuel Oil: Elements of Fuel Oil and Steam Engineering. Robert Sibley
Beveridge. Paper,
20 pp.
$3.00. Technical Vu
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and C. H. Delany.
San Francisco.
Gear Cutting, In Theory and Practice. J. G. Horner. 8vo. 404 pp.
Price, 8s. 6d. Emmott & Co., London.
Kiln Drying of Lumber. H. D. Tiemann. 8vo. Price
Lippincott Co., Philadelphia.
Lubricants: American Lubricants. L. B. Lockhart.
Price, $2.00. Chemical Pub. Co., Easton, Pa.
Measurement of Gas by Orifice Meter. H. P. Westcott. 12mo. 408 pp
Price, $3.50. Electric Metal Works, Erie, Pa.
Mechanics: Cours de mecanique professe a l'ecole polytechnique. Leon
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Metallurgical Study of the Steel Base as Related to Galvanizing. G. A.
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Metallurgy of the Non-Ferrous Metals. Wm. Gowland. 2nd Ed. 8vo.
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Oil: A Short Hand-book of Oil Analysis. A. H. Gill. 8th Ed. 12mo.
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588
MARKET REPORT— JUNE, 1918
WHOLESALE PRICES PREVAILING IN THE NEW YORK MARKET ON JUNE 17, 1918
INORGANIC CHEMICALS
Acetate of Lime 100 Lbs.
Alum, ammonia, lump 100 Lbs.
Aluminum Sulfate, (iron free) Lb.
Ammonium Carbonate, domestic Lb.
Ammonium Chloride, white Lb.
Aqua Ammonia, 26°, drums Lb.
Arsenic, white Lb.
Barium Chloride Ton
Barium Nitrate Lb.
Barytes, prime white, foreign Ton
Bleaching Powder, 35 per cent 100 Lbs.
Blue Vitriol Lb.
Borax, crystals, in bags Lb.
Boric Acid, powdered crystals Lb.
Brimstone, crude, domestic Long Ton
Bromine, technical, bulk Lb.
Calcium Chloride, lump. 70 to 75% fused.... Too
Caustic Soda, 76 per cent 100 Lbs.
Chalk, light precipitated Lb.
China Clay, imported Ton
Feldspar Ton
Fuller's Earth, foreign, powdered Ton
Fuller's Earth, domestic Ton
Glauber's Salt, in bbls 100 Lbs.
Green Vitriol, bulk 100 Lbs.
Hydrochloric Acid, commercial, 20° Lb.
Iodine, resublimed Lb.
Lead Acetate, white crystals Lb.
Lead Nitrate Lb.
Litharge, American Lb.
Lithium Carbonate Lb.
Magnesium Carbonate. U. S. P Lb.
Magnesite, "Calcined" Ton
Nitric Acid, 40° Lb.
Nitric Acid, 42° Lb.
Phosphoric Acid. 48/50% Lb.
Phosphorus, yellow Lb.
Plaster of Paris Bbl.
Potassium Bichromate, casks Lb.
Potassium Bromide, granular Lb.
Potassium Carbonate, calcined, 80 @ 85%.. .Lb.
Potassium Chlorate, crystals, spot Lb.
Potassium Cyanide, bulk, 98-99 per cent Lb.
Potassium Hydroxide, 88 ©92% Lb.
Potassium Iodide, bulk Lb.
Potassium Nitrate Lb.
Potassium Permanganate, bulk Lb.
Quicksilver, flask 75 Lbs.
Red Lead, American, dry 100 Lbs.
Salt Cake, glass makers' Ton
Silver Nitrate Ox.
Soapstone, in bags Ton
Soda Ash, 58%. in bags 100 Lbs.
Sodium Acetate Lb.
Sodium Bicarbonate, domestic 100 Lbs.
Sodium Bichromate Lb.
Sodium Chlorate Lb.
Sodium Cyanide Lb.
Sodium Fluoride, commercial Lb.
Sodium Hyposulfite 100 Lbs.
Sodium Nitrate, 95 per cent, spot 100 Lbs.
1 Silicate, liquid, 40° B* 100 Lbs.
. Sulfide. 60%, fused in bbls Lb.
1 Bisulfite, powdered Lb.
Strontium Nitrate Lb.
Sulfur, flowers, sublimed 100 Lbs.
Sulfur, roll 100 Lbs.
Sulfuric Acid, chamber 66° Bi Ton
Sulfuric Acid, oleum (fuming) Ton
Talc. American white Ton
Terra Alba, American. No. 1 100 Lbs.
Tin Bichloride, 50° Lb.
Tin Oxide. Lb.
White Lead, American, dry Lb.
Zinc Carbonate Lb.
Zinc Chloride, commercial Lb.
Zinc Oxide. American process XX Lb.
ORGANIC CHEMICALS
Acetanilid, C. P.. in bbls Lb.
Acetic Acid, 56 per cent, in bbls Lb.
Acetic Acid, glacial, 99lA%. in carboys Lb.
Acetone, drums Lb.
Alcohol, denatured, 180 proof Gal.
Sodi.
Sodii
Sodii
4.00 @
4.50
3'/. @
3'A
nominal
19'/s @
20
nominal
9'A @
16>/i
65.00 @
85.00
11 @
12
30.00 @
35.00
1.80 @
2.00
8.80 @
9.00
7 '/« @
8'A
13'A @
15
nominal
75 @
85
22.00 @
25.00
4.35 @
4.40
4'A @
5
20.00 @
30.00
8.00 @
15.00
nominal
20.00 @
30.00
1.25 @
2.50
1.15 @
1.25
2 @
2 'A
4.25 @
4.30
17 @
18
nomina
7'A @
8
1.50
1.05
2.00
1.30
2.50
nomina
80
@
82 'A
3.75
@
4.00
27
@
30
2.50
8
3.00
119.00
@
22.00
10.79
8
12.75
22.00
@
25.00
62 'A @
65
10.00
@
12.50
2.25
a
2.45
nominal
3.00
@
3.25
2.50
8
2.60
4.75
@
5.00
2.50
@
3.00
nominal
11
8
12
22
8
28
4.05
8
4.50
3.70
@
4.10
37.00
@
40.00
60.00
@
65.00
18.00
1
8
.17'A
20.00
28
8
30
1.00
8
1.10
9'A
8
107.
Alcohol, sugar cane, 188 proof
Alcohol, wood, 95 per cent, refined
Amyl Acetate
Aniline Oil, drums extra
Benzoic Acid, ex-toluol
Benzol, pure
Camphor, refined in bulk, bbls
Carbolic Acid, U. S. P., crystals, drums
Carbon Bisulfide
Carbon Tetrachloride, drums, 100 gals
Chloroform
Citric Acid, domestic, crystals
Creosote, beech wood
Creaol, U. S. P
Dextrine, corn (carloads, bags)
Dextrine, imported potato
Ether, U. S. P. 1900
Formaldehyde, 40 per cent
Glycerine, dynamite, drums included
Oxalic Acid, in casks
Pyrogallic Acid, resublimed, bulk
Salicylic Acid, U. S. P
Starch, cassava
Starch, corn (carloads, bags) pearl 100
Starch, potato, Japanese
Starch, rice
Starch, sago flour
Starch, wheat
Tannic Acid, commercial
Tartaric Acid, crystals
OILS, WAXES, ETC.
Beeswax, pure, white Lb.
Black Mineral Oil, 29 gravity Gal.
Castor Oil, No. 3 Lb.
Ceresin , yellow Lb.
Corn Oil, crude 100 Lbs.
Cottonseed Oil, crude, f. o. b. mill Lb.
Cottonseed Oil, p. s. y 100 Lbs.
Menhaden Oil. crude (southern) Gal.
Neat's-foot Oil, 20° Gal.
Paraffin, crude, 118 to 120 m. p Lb.
Paraffin Oil, high viscosity Gal.
Rosin, "F" Grade, 280 lbs Bbl.
Rosin Oil, first run Gal.
Shellac, T. N Lb.
Spermaceti, cake Lb.
Sperm Oil, bleached winter, 38° Gal.
Spindle Oil. No. 200 Gal.
Stearic Acid, double-pressed Lb.
Tallow, acidless Gal.
Tar Oil. distilled Gal.
Turpentine, spirits of Gal.
METALS
, No. 1 , ingots Lb.
Antimony, ordinary Lb.
Bismuth. N. Y Lb.
Copper, electrolytic Lb.
Copper, lake Lb.
Lead, N. Y Lb.
Nickel, electrolytic Lb.
Platinum, refined, soft Ox.
Silver Or.
Tin, Straits Lb.
Tungsten (WOi) Per Unit
Zinc. N. Y Lb.
Gal.
4.87
a
4.92
Gal.
90'A
a
91
Gal.
5.25
a
5.30
Lb.
26
a
28
Lb.
3.30
a
3.50
Gal.
23
a
28
Lb.
1.12
Lb.
48
a
50
Lb.
8'A
a
9
Lb.
15 'A
a
16
Lb.
63
a
65
Lb.
82
a
83
Lb.
2.00
a
2.10
Lb.
18
a
20
Lb.
8 a
Lb.
9'A a
Lb.
5 a
6.75
8
17.00
17 'A
e
—
1.00
a
22.00
95
a
1.00
3.45
e
3.55
7.25
55
i
13»/«
3.65
.50
56
nominal
99 Vi
nominal
20.00 % 23.50
7V» % 8
FERTILIZER MATERIALS
Ammonium Sulfate 100 Lbs.
Blood, dried, f. o. b. Chicago Unit
Bone, 3 and 50, ground, raw Ton
Calcium Cyanamide Unit of Ammonia
Calcium Nitrate, Norwegian 100 Lbs.
Castor Meal Unit
Fish Scrap, domestic, dried, f. o b. works.. . .Unit
Phosphate, acid, 1 6 per cent Ton
Phosphate rock. f. o. b. mine: Ton
Florida land pebble, 68 per cent Ton
Tennessee. 78-80 per cent Ton
Potassium "muriate," basis 80 per cent Ton
Pyrites, furnace size, imported Unit
Tankage, high-grade, f . o. b. Chicago Unit
7
JO
8
7
13
6
-o
a
6
73
37
00
a
40.00
nominal
7
n
a
10
M
16
00
a
nominal
17
00
3
so
a
3
»
5
so
a
nom.ual
nominal
6.60
6
n
The Journal of Industrial
and Engineering Ghemistry
Published by THE AMERICAN CHEMICAL SOCIETY
AT BA3TON. PA.
Volume X
AUGUST 1, 1918
No. 8
Editor: CHARLES H. HERTY
Assistant Editor: Grace MacLeod
Advertising Manager: G. W. Nott
APVISORY BOARD
H.E.Barnard H.K.Benson F.K.Cameron B.C.Hesse A. D. Little A. V. H. Mory
Published monthly. Subscription price to non-members of the American Chemical Society, $6.00 yearly; single copy, 60 cents
per single copy to American Chemical Society members, 50 cents. Foreign postage, seventy-five cents, Canada, Cuba and Mexico excepted
Entered as Second-class Matter December 19, 1908, at the Post-Ofiice at Easton, Pa., under the Act of March 3, 1879
All communications should be sent to The Journal ot Industrial and Engineering Chemistry.
Telephone: Vanderbilt 1930 35 East 41st Street, New York City
Subscriptions and claims for lost copies should be relerred to Charles L. Parsons, Box 505, Washington, D. C.
ESCHENBACH PRINTING COMPANY. EASTON, Pa.
TABLE OF CONTENTS
Editorials:
Political, but Not Politics 590
By Order of the President 590
The Demise of the "Garabed" 590
The Cleveland Meeting 591
Living from Hand to Mouth 591
The Approaching Exposition 59-
Original Papers:
Recovery of Solvents from Air- Vapor Mixtures. E. L.
Knoedler and C. A. Dodge 593
Determining the Comparative Melting Points of Glues
as a Measure of the Jelly Strength. C. Frank
Sammet 595
On the Influence of the Temperature of Burning on the
Rate of Hydration of Magnesium Oxide. Edward
De Mille Campbell 595
The Determination of Phthalic Anhydride in Crude
Phthalic Acid. Charles R. Downs and Charles G.
Stupp 596
An Improved Distillation Method for the Determina-
tion of Water in Soap. Ralph Hart 598
The Use of Sodium Sulfate in the Kjeldahl-Gunning
Method. C. T. Dowell and W. G. Friedeman 599
The Structure of Scarlet S3R (B) and Ponceau 3R(By).
H. W. Stiegler 600
Ammonia and Nitric Nitrogen Determinations in Soil
Extracts and Physiological Solutions. B. S. Davis-
son 600
Studies in Synthetic Drug Analysis. V — Estimation of
Theobromine. W. O. Emery and G. C. Spencer. . . . 605
Studies in Synthetic Drug Analysis. VI — Evaluation of
Hexamethylenetetramine Tablets. W. O. Emery and
IC. D. Wright • 606
An Improved Method for Determining Citral — A
Modification of the Hiltner Method. C. E. Parker
and R. S. Hiltner 608
The Identification and Determination of Potassium
Guaiacol Sulfonate. Samuel Palkin 610
The Occurrence of Carotin in Oils and Vegetables.
Augustus H. Gill 612
Determination of Loosely Bound Nitrogen as Ammonia
in Eggs. N. Hendrickson and G. C. Swan 614
A Method for the Detection of Foreign Fats in Butter
Fat. Armin Seidenbcrg 617
Comparison of Percentages of Nitrogen in Tops and
Roots of Head Lettuce Plants. H. A. Noyes 621
An Anaerobic Culture Volumeter. Zae Northrup 624
Laboratory and Plant:
An Electrical Conductivity Recorder for Salinity
Measurements. E. E. Weibel and A. L. Thuras. . 626
An Alinement Chart for the Evaluation of Coal. A. F.
Blake 627
Note on the Use of the Dipping Refractometer.
Wyatt W. Randall 629
Decanting. H. Tillisch 631
A Device to Insure Tight Connections between Glass
and Rubber Tubing. C. C. Kiplinger 631
A Simple and Entirely Adjustable Rack for Kjeldahl
Digestion Flasks. Frank E. Rice 631
Relative Viscosity of Oils at Room Temperature. C.
Frank Sammet 632
An Aspirator. J. M. Johlin 632
Pipette Used in Titration of Oils for Acidity. J.Jacobscn 633
A Safety Valve. E. Rittenhouse 633
A Test for Wool. Harry LeB. Gray 633
Addresses:
Gilman Hall: The Research Unit of the Chemistry
Group at the University of California. Merle
Randall 634
Dyeing of Khaki in the United States. John C.
Hebden 640
The Status of Chemical Engineering in Our Uni-
versities and Colleges Immediately Prior to the
Declaration of War. Harper F. Zoller 644
College Courses for Industrial Chemists. Charles W.
Hill 646
Current Industrial News 648
Scientific Societies:
Fourth National Exposition of Chemical Industries;
American Institute of Chemical Engineers; Cleve-
land Meeting, American Chemical Society; Northern
Ohio Section, American Ceramic Society; Calendar
of Meetings 651
Notes and Correspondence 653
Washington Letter 656
Personal Notes 658
Industrial Notes 659
Government Publications 662
Book Reviews 666
New Publications 669
Market Report - ■ ■ 670
I III. JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. Xo. 8
EDITORIALS
POLITICAL, BUT NOT POLITICS
The joyous news from France of the transformation
of the allied defensive into a crushing offensive,
and especially of the part played by American
troops in this great movement, thrills the hearts
of Americans who are devoting their every energy and
talenl to furnishing adequate supplies to these men
whose fresh spirit and dashing attack has proved so
great an inspiration to all.
It is a long way to Berlin, however, and doubtless
a long time before th( ha1 full victory for the
ideals so nobly expressed by President Wilson which
guide us in this bloody strife. During the coming
days many grave questions of most serious import
must be rightly determined by those who represent
us in our national legislative body; many pitfalls in
, the form of plausible peace proposals must be avoided
' if we are to secure that righteous peace which con-
stitutes the justification of lives laid down and sacrifices
made.
As a citizen, every chemist must contribute his best
judgment of men in the selection by vote of those who
are so to represent us. Study the record, the character
and ability of ^ach man whose name is presented for
office and see to it, so far as we are able to affect the
choice, that only such as are thoroughly loyal at heart
to the principles for which we are contending gain
place in the councils of the nation.
BY ORDER OF THE PRESIDENT
President Wilson, acting under the authority dele-
gated to him by Congress in the recently enacted
Overman bill, has issued an executive order transfer-
ring the Experiment Station at American University
(gas warfare research) from the Interior Department
to the War Department. Accompanying the order of
transfer (page 654 , this issue) the President sent to
Director Van. H. Manning, of the Bureau of Mines, a
letter of unstinted commendation of thj splendid
results achieved under his guiding hand. Equally
generous in its praise was a letter to the President from
the Secretary of War.
The action was based solely upon the ground of
organization need in the formation of the new Chemical
Warfare Service, directly in charge of Major General
William I.. Sibert, one of the most distinguished
ers in the Wai Dep That the Pt
felt convincingly the need of such reorganization is
evidenced by the fad thai the transfer was ordered
in the face of a unanimous recommendation to the
contrary by the body of eminent chemists comprising
the Committee Advisory to the War Work of the
Drs. Wm. 11. Nichols. Chairman,
E. C. Franklin, William Hoskins, C. L. Parsons. Ira
Rem; n. T. W. Richards, H. P. Talbot and P. P.
Venable
Frankly, we had hoped thai the President would
to leave this organization in the congenial
atmosphere in which it began and which had con-
tributed so much to its rapid growth. This hope
based upon the conviction that its unlimited
service stood freely at the disposal of General Sibert,
regardless of departmental connections. We be-
1 also that the spirit of the Bureau of Mines
was through its very nature more conducive to re-
search than that of the War Department, the strictly
military division of the Government. Then, too. we
feared- the numbing effect of the much discussed "red!
tape" of War Department methods upon the spirit
of originality, daring and speed in following new
trails, so essential to the successful prosecution of
research.
We sincerely hope that these fears will prove entirely
groundless, that no slowing up of this fast machine
will be permitted, for otherwise a national disaster
would result. On the other hand, we hope with equal
sincerity that under General Sibert's leadership the
pace will even be accelerated, for intensive research
is the sure foundation of this new development in war-
fare.
A side from all this, the one outstanding feature of
this situation is the fact that the President, the Com-
mander-in-Chief of the Army, has under due authoriza-
tion from Congress ordered this transfer, and it is
needless to say that all American chemists, soldiers and
civilians alike, will continue to give to this work
patriotic support and service to the very limit of their
abilities.
THE DEMISE OF THE "GARABED"
The Garabed's completely dead. "Twas put to
sleep through just one peep by a bloomin' committee
that had no pity — Xo. this is not poetry but merely
the reflex action on a hot summer night from reading
one of the speeches in Congress advocating the
guarantee of special government protection to the free
energy machine which was to revolutionize the world,
if a committee of five distinguished scientists should
give its O. K. after a demonstration.
Unfortunately the committee reported "We do not
believe its principles are sound, that his devices are
operative, or that they can result in the practical de-
velopment or utilization of free energy." But this
here nor there. The machine did
Free energy even in advance of inspection.
the proof in the form of quotations from the
introduction of the speech above referred to. printed
in the Congressional Record of December 15, IQ17. page
370, reproduced for the benefit of the scoffers who insist
that the Record is dry reading.
Mr. Speaker, tin- miracle of yesterday is the commonplace of
to-day There was a time when man was perfect in all his parts
ami elements. He was complete physically. The poet, the
painter, the sculptor, the dreamer, in the wildest ftif
superb fancy, never caught more than a fleeting vision of that
beauty which was given by the Lord to the first man and first
woman
Aug., 191S
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Not only was man complete physically at one time, but he
was perfect mentally. He knew all philosophy and all science.
Mathematical exactness was instinctive with him. He knew
and could interpret bird song. He knew where the flower
bloom came from, and why. He understood the passions of the
tiger. He saw all problems with clear and unmistakable vision.
He was complete spiritually. He discussed with the Divine
the themes of the divinity. He communed with the angels.
He was so complete in his structure that he possessed the
power to destroy his own perfection, and he exercised this power.
He sinned. That is to say, he violated some law of harmony.
What it was we do not know. Perhaps we never shall know .
But we know that it was the exercise of a power by which the
integrity of his triple structure was destroyed.
There was some power by the exercise of which the integrity
of the triple structure was destroyed. I think that touched his
every phase and characteristic. It devitalized him physically.
The majestic brow receded; the form became bent. Warts and
vile protruberances grew upon the skin. The nerves lost con-
trol over the muscles, and these, uncontrolled, fell to hideous
expression.
All of which and much more was apropos of the
Garabed.
On the day of the demonstration Mr. Finney of the
Department of Justice was on hand to corral the
committee and to insure a demonstration by the in-
ventor, but he was not allowed to witness the test.
We venture the statement that that was the first
time this alert branch of the Government ever failed
to "get a look in."
THE CLEVELAND MEETING
By unanimous vote of the Directors the Annual
Meeting of the Society will be held in Cleveland,
September 10 to 13, 191S. Many important matters
await the action of the Council, while the lapse of a
year since a general meeting w^as held insures a program
of unusual interest.
Cleveland's central location and accessibility, and
its reputation for unbounded hospitality, should bring
together a great gathering of chemists whose delibera-
tions will have notable bearing upon the welfare of the
country and upon the advancement of chemistry in
our midst.
LIVING FROM HAND TO MOUTH
25,000 ounces of platinum in hand, 15,000 ounces
more under control, and Government needs for the
year beginning March 1, 1918, 60,000 ounces — these
were the figures set forth in the testimony of Messrs.
L. L. Summers and C. H. Conner of the War In-
dustries Board, Platinum Section, before the Ways
and Means Committee on July 17, 191S. This im-
pending shortage of 20,000 ounces is admitted within
earshot of the remarkable order which immediately
released to the jewelers twenty-five per cent of their
commandeered unmanufactured platinum, in order
not to disturb too greatly this individual item of the
jewelry trade. Xo stronger testimony' could be
- to the foresight of those who have been advoca-
eparedness in this all-important matter.
During the past month the question of our platinum
resources has received much consideration. R
Congress has enacted legislation placing platinum under
equiring the Bureau of Mines to
issue licenses governing the sale, possession and use of
platinum. The rules and regulations for the operation
of this statute have not yet been issued.
The Ways and Means Committee has held Hearings
on the subject of taxation of jewelry. On July 10
representatives of the jewelry trade appeared before
the Committee ostensibly to discuss taxation but, as
events proved, chiefly to defend' their trade against
charges which they considered had been unjustly
lodged. Some of the statements made by the jewelers
involved the American Chemical Society so in-
correctly and unfairly that we received permission to
correct these misstatements. This was done. At-
tention was also called to a section of the brief read
by Mr. Rothschild, the representative of the jewelers,
setting forth a letter written early this year by the
Chairman of the War Industries Board, stating "it
is necessary for the Government to have command of
every bit of platinum that can possibly be had" and
expressing the desire that "no further use of platinum
should be made in the manufacture of jewelry." In
response to this letter the jewelers' representatives
had visited the War Industries Board, and had "rec-
ommended that all the unmanufactured platinum
held by jewelers be commandeered," but the objection
had been made by the War Industries Board that it
did not wish to disturb the jewelry industry to such an
extent. This revelation was so surprising that we
went on record as gladly willing to make editorial
apology to the jewelers for past criticisms of their
attitude toward the commandeering orders, in case
the statements were confirmed by the War Industries
Board. A transcript of the statement was forwarded
to the Chairman of the War Industries Board for his
confirmation. Later we wired asking a reply to our
letter, but up to the present no answer has been
received. Meanwhile representatives of that Board
testified before the Ways and Means Committee on
July 17, and although the printed testimony is not
yet available we learn from a correspondent present
at the Hearings that a denial was made of the com-
mandeering recommendation of the jewelers. In
view of this denial the apology is withheld.
A new turn was given to the discussion by the in-
teresting testimony of Mr. Louis J. Weinstein, Director
of Advanced Courses in Dentistry, Columbia Uni-
versity, concerning the substitution of certain alloys
for pure platinum in dentistry. By such substitution
the practice of dentistry would in no wise be injured,
while some 15,000 ounces of platinum annually would
be conserved for munitions manufacture. Mr. Weic
stein's testimony, and the patriotic spirit which
prompted it, made an evident impression upon the
Committee.
The most surprising statement throughout the
Hearings was to the effect that platinum is not neces-
sary in the manufacture of explosives. This state-
:, . ascribed by some of tin- newsp
Summers (an electrical and by oth
Mr. Conner (a banker). Telegrams were immediately
-.nil to each, asking if he had been correctly reported.
Mr. Conner replied referring us to the full te
592
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 8
before the Committee (which by the way was not to
appear for several days), while Mr. Summers not only
referred us to the same source of authoritative in-
formation but added the entirely irrelevant sentence
"Do not feel that War Industries Board platinum
section should be party to controversy between
chemists and jewelers."
Of course, from a'n academic standpoint, explosives
can be manufactured without the use of platinum.
Sulfuric acid was manufactured many, many years
before the contact process was known. So too is the
oxidation of ammonia to nitric acid by the catalyzing
action of platinum a very recent matter, on which
process, however, our Government is now spending
millions of dollars for plants in Alabama, Ohio and
Maryland. That is not the point. We are not
raising an army to quell a revolution in the island of
Guam, but an army already more than a million
strong, and soon to be two millions. Ex-President
Taft advocates five millions, and President Wilson
says 'Why limit it to five millions?" In other words,
this country is determined to win the war, no matter
how many of our men are required, and therefore an
indefinite expansion of the munitions program must be
provided for. The forceful editor of the Manufacturers
Record ably states the case in a recent editorial
condemning the use of platinum in jewelry.
There are two ways of battering through Germany's en-
trenched army and carrying our flag across the Rhine. One is
through a tremendous amount of explosives sufficient to blow
out everything ahead of our men. The other way is through
using the bodies of millions of American soldiers against the
tremendous fighting ability of the German army.
Which will America choose?
Preparedness of even the most elemental type demands
that an ample reserve of platinum be provided, and we
repeat the conviction that the immediate place for
such a reserve is in the vaults of the Treasury De-
partment, absolutely under the control of our Govern-
ment, rather than distributed throughout the country
in the show cases of 36,000 jewelers, offered freely for
sale to any purchaser, loyal or disloyal.
The blood of American soldiers weighs too heavily
in the balance against the hand-to-mouth policy now
being pursued.
THE APPROACHING EXPOSITION
As the summer advances the question is often asked,
and happily always in a sympathetic tone, "What
kind of an Exposition are we going to have in Septem-
ber?'' To such a question there is only one answer —
"Excellent." The list of exhibitors shows a marked
increase over previous years, exhibitors are being
urged to ship exhibits amply in advance to avoid
present shipping delays, and the management has
arranged for storage of shipments which may through
some perversity of transportation ways come through
on the schedules usually allotted for shipments.
For the first time an approach will be noticed
toward at least some slight coordination of the
multifarious exhibits, a matter fraught with many
and perplexing problems. A better auditorium is
promised for the many speakers of national prominence
whose addresses contribute so much to the permanent
value of the Exposition.
Again, following unvarying precedent, the Exposi-
tion will be devoted not to popular entertainment
of the idly curious, but to the serious function of a
clearing house of information as to progress in all lines
of the chemical industries, thereby enabling still greater
progress in the year ahead of us. If the Exposition
did not have this solid background of patriotic purpose
its continued existence at such a time as we are now
passing through could not be justified. Xo matter
how great the progress made in the past three years,
we need to speed up more, and still more. The rapid
increase, present and prospective, of our army in
France entails a similar expansion of the chemical
industries at home if that army is to fight with the
material all Americans would have them furnished.
There is only one fly in the Exposition ointment —
the action of the Railroad Administration in forbidding
the use of railroad funds for exhibiting the unde-
veloped resources along the several railway lines which
await the touch of the chemist to change these lowly
products into national assets of far greater value at a
time when the nation's resources should be mustered
to the highest possible limits. It was the unanimous
testimony of all at the last Exposition that the rail-
roads', exhibits of resources in contiguous territory
pointed the way to a great and rapid industrial ex-
pansion. Plans were immediately set on foot to per-
fect and enlarge these exhibits, when suddenly the
command "Halt'' was given, and so in the midst of
an era of chemical expansion the chemists of the rail-
roads engaged in this work of development were told
to seek other fields for their talents, even with the
prospective passage of a bill by Congress appropriating
millions of dollars for encouraging domestic production
of many lines of mineral wealth in order to save snip-
ing space, hitherto devoted to importations, for the
transport of men and supplies to European battle-
fields. We could better afford to take pattern of our
neighbor, Canada, who, in spite of the great drain
upon her resources from four years of participation
in the war, is making increased effort to enlist the in-
terest of the chemists in her development.
Only a few days ago we were visited by a chemist
from the laboratory of a railroad in the South, whose
exhibit last year attracted the attention of every
chemist, and were told of the chemical library and
the modern laboratory equipment, which are soon
to be packed away or sold, as a result of the new order
of things. Such a step backward seems to be incom-
prehensible in this day, yet such is the fact. Surely
this matter of the chemists' aid in development work
must have been overlooked among the great problems
incident to the reorganization of the railroad operation
under government control. We are not yet willing
to believe that a false sense of economy is responsible
for this amazing situation. We appeal to Mr. McAdoo
to correct this error of executive policy which is fraught
with certainty of national loss.
Aug., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
ORIGINAL PAPERS
RECOVERY OF SOLVENTS FROM AIR-VAPOR MIXTURES
By E. L. Knoedler and C. A. Dodge
Received March 29, 1918
At the present time the great scarcity of solvents
and the enormous demand for them for military pur-
poses makes necessary the highest possible degree
of conservation by those industries in which they are
used. Furthermore, the high prices which these
solvents now command add to the other reasons for
conservation the important inducement of large manu-
facturing economies.
This conservation may be effected either by a re-
duction in consumption or by the recovery of the
solvent vapors from those processes in which they are
driven off. The first method in many cases would
involve a reduction in volume of business, unthinkable
except in cases of dire necessity; the second, on the
other hand, actually adds to the available supply and
holds out the prospect of increased business, at the
same time making possible substantial economies
in manufacturing cost.
their very low concentration; and this led to the de-
velopment of tightly closed, steam-heated, drying
chambers, efficiently insulated with asbestos and
equipped with quick-acting, close-fitting, sliding doors,
through which are fed the wheeled carts carrying the
product. Tracks running completely through the
box make it possible to feed the goods in at one end
of the box and remove them from the other end. In this
way a steady stream of wet materials is fed to the
drying chambers, maintaining a reasonably uniform
air-vapor mixture.
The temperature of each one of the fourteen drying
boxes is controlled by a thermostat which regulates
the steam supply, and upon each box is mounted an
air compressor of such capacity as to remove the
vapors as generated. This arrangement of inde-
pendent units permits any dry-box not in use to be
cut out of the system, so as to deliver to the recovery
equipment at all times an air-vapor mixture uniform
in composition and of a constant temperature.
Ge
al layout of recovery plant showing course of vapors from box
through pre-cooler and towers, then back to pre-cooler and to atmosphere;
also of scrubbing liquors from pump to towers, then to cooling basins
where the pump takes its suction
To those who may have considerable quantities of
solvent vapors available, the description of a successful
recovery plant may be of interest. The plant has
been in operation several years and has recovered
many thousand gallons of these precious materials.
The solvents which are being recovered are mixed
vapors of methyl alcohol, ethyl alcohol, acetone, and
camphor, which are driven off in drying the collodions
used in coating gas mantles. The proportions of the
several solvents have varied from time to time, but
the outfit has operated with success on any mixture
so far attempted.
The drying of the collodions was first carried on
in the open air, then in chambers with open ends,
through which the collodionized mantles were passed
as they dried. Under these conditions it was found
difficult to recover much of the vapors because of
i^r^-J^.
imwaSSSfSSsSI
1
L Lfl W\ I
Fig. II
Bank of four drying chambers showing delivery end. Individual
compressors, temperature regulators and steam supply for each chamber
are in plain view, also tracks and wheeled carriages for transporting the
product
As delivered by the compressor to the recovery
plant the mixture of vapors shows about the following:
Volume about 450 cu. ft. per M.
Pressure 1 lb. per sq. in.
Concentration 4 per cent solvents (by vol.)
Temperature 80° C.
After the solvents are removed from the air vapoi
mixture, the air, which is discharged to the atmos-
phere, shows about the following:
Vapor concentration 0.9 per cent solvents (by vol.)
Temperature 14° C.
It will be seen from these figures that approximately
80 per cent of the vapors passing through the plant
are recovered and these figures are confirmed by the
actual output.
The plant consists of a large surface condenser
used as a pre-cooler; a group of scrubbing towers,
594
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. IO, No. 8
in which the vapors arc scrubbed; receiving vessels
in which the liquors from the lowers are caught and
kept cold by means of brine 'mis; pumps for re-circu-
lating this liquor until it attains a concentration suit-
able for distillation; an ice machine; and a column still.
Fir.. Ill
and catch basins
solvent recovery
plant
As the vapors enter the recovery plant they pass
through the tubes of a surface condenser where they
are lowered from 8o° C. to nearly the temperature of
the washed waste gases (about io° C). They then
pass into a header and are distributed to a group of
"bell-and-seal" scrubbing towers where they bubble
through water of a temperature of 50 C. Here the
vapors are removed from the mixture, and the air,
lowered to a temperature of about 6° to 70 C. from
its contact with the refrigerated wash solutions,
passes out of the tower and back to the surface con-
denser where it serves to cool the vapors just entering
the plant. After passing through the pre-cooler,
the air, deprived of its vapors and warmed up by the
heat absorbed from the entering vapors, is discharged
to the atmosphere. Of course, any solvents left
in this air are completely lost and it is quite possible
that in some industrial operations it would pay to
return this air to the drying chambers for re-use.
The washing of the gases in the towers is carried
out by means of cold water which is re-circulated
by pumps. Prom the towers the water returns to
catch basins containing brine coils for keeping it at
a low temperature, the pumps taking their suction
from the catch basins. The re-circulation continues
for some hours until the solution reaches a concen-
nit 1 j per cent solvents, when it is pumped
to the storage tank and held until required by the
still. After passing through the still, where the
solvents arc driven off, these waters are permitted
to cool and are then returned to the scrubbing system.
In this way small losses in the tail-liquors are avoided.
Each tower, like each drying chamber, is a com-
plete unit, with its individual pump and catch basin.
and can be operated regardless of the other units.
The still is a copper, fractionating column, composed
of a steam-heating section, 36 in. in diameter.
3 distilling sections, 24 in. in diameter, and 7 dis-
tilling sections, iS in. in diameter, divided into
20 distilling chambers. The 18-in. sections are
provided with internal cooling coils, connected in
series and regulated by a throttle valve. The vapors
from the .24-in. sections are by-passed through a
tubular condenser, preheating the feed liquors, then
back into the 18-in. sections, and from there through
the condenser. The steam is supplied by a closed
coil and controlled by a differential steam pressure
regulator. The still produces a 97 to 99 per cent
product, according to the varying percentages of
acetone, ethyl and methyl alcohols in the vapor
mixture being worked.
The camphor remains in the sections of the still
where the temperature ranges between 95 ° C. and
750 C. Periodically, these trays are drained through
a header to a copper condenser, consisting of a series
of trays, where the liquor is cooled and some of the
camphor separates out on the trays. The remaining
camphor passes on to a sump where it is precipitated
and filtered. The camphor press cake is preserved
for further purification, and the filtrate is combined
with the still liquors and used over again in the scrub-
bing towers.
— AL.O
Fig. IV
Elevation of still showing urangemi
its operation
of all elements required
The cost of operation per 8s 4-hr. day. with a pro-
duction of from 65 to 75 gal. of solvents, runs ■ap-
proximately as follows:
Aug.. 19 1 8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Direct labor — one man at 35 cts. per hr $ 3.07
Indirect labor and supervision 0.50
Expense and repairs 0.60
Steam (pumps and still) 5 . 20
Fixed charges 8. 75
Product — 70 gals. $18.12
Total cost per gal. — $0.26 (making no allowance for camphor)
The accompanying cuts give a good idea of the
general layout of the plant, also of the appearance
of drying chambers, scrubbing towers, and distilling
column.
Welsbach Company
Gloucester City, New Jersey
DETERMINING THE COMPARATIVE MELTING POINTS
OF GLUES AS A MEASURE OF THE JELLY STRENGTH
By C. Frank Sammet
Received March 22, 1918
Methods for testing the comparative jelly strengths
of glues have never been entirely satisfactory. Criti-
cisms of the various methods are extensively written
into the literature of glue testing, and it would seem
that a simple, rapid, and yet accurate method is de-
sirable, as the jelly strength is an important factor
in the quality of glue for paper making and other
purposes.
These features are involved in the following method,
which is a comparison of the melting points of either
the ground glues or their jellies. The melting points
may be taken as a measure of the jelly strength as
the two bear a close relation to each other.
The dried glues are brought to a ground condition
in a hand mill and sieved between 20 and 40 mesh
screens, and that portion remaining on the 40 mesh
sieve is retained for the test. Although in many cases
glues are mixtures of several qualities, with different
melting points, yet the mixture of ground particles
has never caused inaccuracies in the comparative
melting-point tests. The grades determined by the
melting-point test have corresponded exactly with
grades determined by testing the actual jelly strength
by other methods. About 1 g. samples of the glues,
so prepared, are placed in small beakers and each
stirred with 10 cc. to 15 cc. of cold water, not above
ic° C. They are allowed to soak one minute, then
a portion of each glue is withdrawn by a spatula and
placed on a thin, smooth surface of metal. This
metal should be preferably of brass, having an ap-
proximate length of 6 in., a width of 1.5 in., and a
thickness of l/« in. The long edges may be
turned over to give the strip rigidity. The glue
particles should be placed about 3 in. from the end
of the strip, and then a portion, about the area of
five pin heads, is separated with the spatula and
pushed to within 2 in. of the end, thereby draining
off a certain excess of water which adheres to the
surface of the metal.
The little heaps of glue particles are now aligned
equally distant from the end of the strip, which is
then dipped to a depth of V2 in. in a beaker half full
of water at 40 ° C. The heating should be fairly slow,
that the initial sign of melting of the glue particles
may be noticed, as this is the determining factor.
Glues that are a grade apart in jelly strength show
a very marked difference in their initial melting points.
The poorer grades even slide rapidly down the metal
surface, while the better grades melt considerably
before a sliding effect occurs.
This same procedure may be followed, using the
jellies of definite concentrations which have been
chilled for at least 12 hrs. Sometimes it is preferable
in the case of jellies to squash them flat on the metal
strip with pieces of thin copper, each about l/, in.
square, leaving a layer of jelly about ' 3. in. The
copper adds weight, and slides quickly at the first
indication of the jelly melting.
In these comparisons, it is essential for accurate
results to keep the operations on each glue identical,
and conditions uniform as to time, temperature, con-
centration, etc. The method has proved most satis-
factory when conducted with due care. It has the
advantage of ease of manipulation, rapidity of de-
termination with ground glues at least, and only small
samples need be used. It is more positive in its
accuracy of the determination of jelly strength than
other methods.
In furthering the value of this method for testing
jelly strength of glues, it is possible to utilize other
standards than known grades of glue. Mixtures of
petrolatum with paraffin wax having definite initial
melting points can be established for glues of higher
jelly strength, while mixtures' of petrolatum and
paraffin oil can be used in the case of lower grade glues.
With these mixtures having definite initial melting
points, the grades of glue could be more exactly de-
fined as far as their jelly strengths are concerned, and
conditions and concentrations standardized for testing,
so that results from any analyst would have the same
significance.
This work should be conducted with enthusiastic
cooperation by glue chemists, for the good of all con-
cerned.
Crane and Company
Dalton, Massachusetts
ON TILE INFLUENCE OF THE TEMPERATURE OF
BURNING ON THE RATE OF HYDRATION
OF MAGNESIUM OXIDE
[second paper)
By Edward De Mille Campbell
Received April 9, 1918
In the first paper under the above title1 a series of
experiments was described giving the method of burn-
ing, at different temperatures between 500 ° C. and
1450° C, a sample of pure magnesite and of deter-
mining the degree of hydration of the resulting mag-
nesium oxide after treatment witli water for periods
ranging from 1 day to 18 mos. The magnesium
oxide resulting from the burning of magnesite had
the following composition: Silica, 2.53 per cent;
alumina and ferric oxide. 2. 70 per cent; calcium oxide,
3.96 per cent; magnesium oxide, 90.78 per cent.
This burned magnesium oxide required an average
of 44.50 per cent of its own weight of water to com-
' This Journal, 1 (1909), 665-68.
596
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 8
pletely hydrate the magnesium oxide and the basic
silicates, aluminates, and ferrites derived from the
combinations of the basic and acidic oxides.
The results reported in the first paper were summa-
rized as follows:
i — That magnesite is not completely dissociated at 500 ° C.
in 1 hr. under the conditions used in the experiments.
2 — That dissociation of the magnesium carbonate is com-
plete at 6oo° C, while that of calcium carbonate is not.
3 — That the hydration of magnesium oxide burned at 600 °,
7000, or 8oo° C. is practically complete in 3 days.
4 — That between 8oo° and 9000 C. the calcium carbonate is
dissociated, and that combination takes place between basic
and acidic oxides, resulting in the formation of silicates or
aluminates. The silicates or aluminates so formed combined
with more water than would be required for the complete hydra-
tion of the basic oxides alone.
5 — That a change in the constitution of the magnesium oxide
sets in between 1000° and noo°C, resulting in a marked
decrease in the rate of hydration, and that this change becomes
more marked with rise of temperature of burning, until at
1450 ° C, or nearly the temperature required for burning Port-
land cement, the magnesium oxide after 18 mos. immersion in
water has combined with only 61.4 per cent of the water
required for complete hydration.
}
< 80
■4)
IZOO"
1
y
I30O"
l40Cf
MSO'
1
:
1
-)
f 6
I
vo -
Time /n Years
Fig. I — Curves Showing the Influence op Burning at Tempera-
tures above 1000° C. on the Rate of Hydration op MgO
The object of this second paper is to record the re-
sults obtained after continuing the hydration of the
samples described in the first paper up to a period
of 6 yrs.
A study of the data reported in the first paper
shows that all samples burned at temperatures not
exceeding 11000 C. were completely hydrated within
3 mos., very slow hydration taking place only in the
case of samples burned at 12000 C. or above. Dur-
ing the first 4 yrs. the desiccator, in which were placed
the crucibles with the samples just covered with
water, was partially filled with distilled water, but it
was noted at the end of the 4 yrs. that there had been
a slight, but steady, increase in weight of the samples,
due to absorption of carbon dioxide. This increase
in weight amounted in the course of 4 yrs. to about
3 per cent in the cases of all those samples which had
been completely hydrated. Further increase in weight
due to absorption of carbon dioxide after 4 yrs. was
prevented by replacing the distilled water in the
desiccator with a dilute solution of potassium hy-
droxide.
The total percentage gain of weight of the samples
burned at 9000 C. or above at the end of each year
between 1 and 6 yrs. is given in Table I.
Table I — Percentage Gain op Weight
Hydration *-
—Temperature ol
Burning-
Years
900°
1000"
1100°
1200°
1300°
1400°
1450°
I
44.88
44.92
45.33
41 .34
28.99
28.12
23.31
2
4S.25
45.18
46.20
42.75
32.75
32.05
26.31
3
46.27
46.27
47.25
45.13
34.43
34.08
27.97
4
47.88
47.45
47.90
47.33
36.90
35.26
30.25
5
47.50
47.49
47.77
47.61
37.36
35.94
30.99
6
47 .13
47.54
47.77
47.67
37.71
36.58
31.82
Since all samples burned at or below 11000 C.
were completely hydrated within 3 mos., the per-
centage of complete hydration after long time periods
has been computed only for those samples burned at
or above 1200° C. In computing the percentages
of complete hydration of these latter samples, correc-
tion has been made for the increase in weight due to
the slight absorption of carbon dioxide. The per-
centages of complete hydration of these latter sam-
ples computed in this way are given in Table II.
Table II — Percentage op Complete Hydration
Temperature
of Burning . Time of Hydration in Years .
Degrees 12 3 4 5 6
1200 91.8 94.9 100.0
1300 64.0 72.4 76.2 81.7 82.7 83.5
1400 62.0 70.8 75.3 78.0 79.5 81.0
1450 51.2 58.0 61.7 66.8 66.9 70.3
The results given in Table II are shown graphically
in Fig. I, in which the ordinates give the percentage
of total hydration and the abscissae the length of time
the samples were kept in water. These results show
clearly why materials containing frc magnesium
oxide, if burned at temperatures approaching that
used for the production of Portland cement, will not
become completely hydrated, even when continuously
immersed in water, until the lapse of probably 20
yrs. or more.
Chemical Laboratory
University op Michigan
THE DETERMINATION OF PHTHALIC ANHYDRIDE IN
CRUDE PHTHALIC ACID
By Charlbs R. Downs and Charles G. Stuff
Received February 28, 1918
In connection with the control of a plant producing
phthalic anhydride it became necessary to develop
a method whereby the crude phthalic acid, contain-
ing mineral impurities, sulfur compounds, and other
organic acids, might be assayed for the amount of
phthalic anhydride present.
A search of the literature was made, but the methods
described, with the exception of that given by Bos-
well (noted below), were not applicable to the crude
acid resulting from the manufacture of phthalic acid.
Aug., 1018
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
597
Several attempts were made to sublime a mix-
ture of pure phthalic acid and anhydride, in such
ordinary laboratory subliming apparatus as is used
in investigating other materials. The apparatus was
made up of heated dishes, inverted funnels, etc.,
with the object of weighing the sublimate, thus ob-
taining quantitative results. In most of these trials
a current of air was passed over the subliming sur-
face, heated to a temperature of 200° to 220° C . Various
types of condensing chambers were used.
In all cases it was found that either the sublimed
crystals, built up on the condensing surface, fell
back from their own weight onto a hot portion of the
apparatus and remelted, or else they were carried
through into the collecting chamber in the form of
a fine suspended dust, which was hard to collect
quantitatively.
A detachable tube appa-
ratus was then made up as
shown in Fig. I.
A weighed amount of the
phthalic acid to be tested
was placed in the weighed
glass capsule D and the
tube C was inserted, as per
sketch, after it came to con-
stant weight in a steam
oven. Air was drawn
through the tube C by
connecting to a suction
pump at the point B, the
air entering the apparatus
through the annular space
E. The apparatus was
then immersed to the point
A in a low-melting metal-
lic bath kept at a temper-
ature from 200° to 2200 C.
Any vapors formed during
sublimation were drawn
through the cotton and held
there instead of escaping through the annular space E.
Using this apparatus it was expected that the weight
of the residue could be obtained, that this residue
would be in a convenient form for testing for the
presence of unsublimed phthalic left behind, and
that after drying the cotton tube to constant weight,
i. e., when the water of decomposition had been evap-
orated, the weight of the sublimed material or phthalic
anhydride would be given.
Results Obtained on, a Sample op Crude Phthalic
Time Weight Per
W
perature Immer- of cent of Per
of Bath sion Sample Subli- cent of
° C. Hours Gram mate Residue
200-220 1/2 0.2574 72.9 10.4
200-220 P/t 0.2453 72.0 10.2
The difference of o. 2 per cent in the weight of the
residue represents an actual weight in the case of
only 0.0005 S-i which shows that practically all of
the sublimable material was off after V2 hr. immer-
sion. The speed of the air drawn through was ap-
proximately 3 bubbles per sec. from a 'A in. glass
tube through a 3-in. layer of water in a Woulff bot-
tle. This rate of air was found to be satisfactory.
A higher rate tended to carry some phthalic through
the cotton plug.
In connection with weighing the sublimate in the
cotton tube, the following tests were made on pure
"commercial" anhydride.
Weighed portions of the anhydride were placed on
watch glasses, moistened with water, and placed in
an oven.
Temperature Time
of Oven of Heating Weight Taken Loss
0 C. Hours Gram Per cent
88 15 0.2500 97
88 18 0.2500 96
100 3 0.2500 24
From these results it was evident that a direct de-
termination by weighing the sublimate, after reach-
ing constant weight in a steam oven, could not be
used as a method of analysis.
Colorimetric tests were attempted on the residue,
using phenol or resorcinol with a dehydrating agent,
but dark green solutions were obtained that did
not at all resemble the colors of phenolphthalein or
fluorescein. In fact they were so dark that small
amounts of phthalic could not be detected. Attempts
were also made to determine phthalic anhydride present
in the crude phthalic acid by colorimetric tests, but
this method was found to be inapplicable. Atten-
tion was then turned to the titration method described
by C. Boswell1 and this method was used with the
substitution of the detachable tube described above.
The details of the method finally adopted by us
are given as follows:
0.250 g. of the sample to be analyzed shall be weighed into
the glass capsule, and 1.5 g. of the prepared cotton boiled in
10 per cent NaOH and then washed and dried, shall be packed
not too tightly in the inner tube. The length of this tube
shall be about 5V2 in. and the column of cotton shall extend
to within ■/< m- of the bottom. The tube itself shall be inserted
into the capsule to within '/> m- °f the bottom of the latter.
Suction is then applied to the top of the inner tube and air
drawn through as described before, so that it bubbles through
a '/« in. glass tube in a suction bottle at the rate of three bub-
bles per second. This apparatus shall be then transferred to
the heating bath of melted Rose metal and adjusted so that the
capsule is immersed to a depth of about '/i in. It is impor-
tant that the apparatus should be assembled and the air be
passing through it, and that the bath temperature be regulated
to 2000 to 2200 C. before the immersion occurs. Only in this
way can accuracy of results be assured. The heating shall
then be continued 45 min., during which time the phthalic acid
is completely decomposed and the sublimed anhydride col-
lected in the cotton tower. The tube is then removed from the
bath, the outside of the capsule cleaned of adhering metal and the
weight of residue determined. The cotton plug containing the
sublimate is pushed out into a beaker containing 45 cc. of stand-
ard N/10 NaOH. About 50 cc. of water are added and the solu-
tion boiled '/» hr. In case some anhydride adheres to the glass
tube, the latter may be left in the caustic solution during the
boiling. After '/j hr. the anhydride is completely dissolved
in the alkali, and a small amount of solid phenolphthalein
(alcoholic solution of phenolphthalein cannot be used) shall
then be added for an indicator and a known excess of standard
acid added. This excess must be at least 5 cc. Boiling shall
then be continued 15 min. longer and the titration completed
by adding alkali in the hot until the end-point is reached. The
1 /. Am. Chem. Soc, »9 (1907), 235.
598
I III JOl RNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol.
10, No. 8
phthalic anhydride tit. actly N to NaOH solution
is 0.0074.
It will be found that the cotton plugs can be used
again and again provided they be washed carefully
with neutralized water after each run. Occasional
titrations must be made on the cotton blanks to be
sure of their uniformity and their acid equivalent.
New cotton must be thoroughly boiled with .Y 10
caustic soda and washed well with neutral water.
Where there are a number of determinations to be
run daily it will be found that this method using the
detachable tube considerably simplifies the method
as described by Boswell and in addition the weight of
the unsublimable residue is obtained. This is an
important feature in connection with plant control.
It is important to note that when a crude phthalic
is obtained containing sulfuric and sulfurous acids
it must be washed free of these compounds be-
fore testing. The presence of sulfuric acid in the
crude is generally indicated by a charring of the cot-
ton and, if this happens, the test must be repeated.
This method has been thoroughly checked by
analyses of pure phthalic anhydride.
A further proof that this method is correct, when
applied to crude phthalic acid, is that the actual
sublimation in the plant, where there are small known
losses, has given, at the lowest. 95 per cent of the ana-
lytical figure for phthalic anhydride as determined by
the above method.
Rbsearch Department
The Barrett Company, 17 Battery Place
New York City
AN IMPROVED DISTILLATION METHOD FOR THE
DETERMINATION OF WATER IN SOAP
By Ralph Hart
Received May 20, 1918
Water in soap is usually calculated after determin-
ing all the other ingredients. In many instances,
however, it is found directly by drying the soap to
constant weight in an oven at 105° C. This pro-
cedure, of course, takes considerable time and the
result indicates not only water but also any other
volatile constituents that may be present. A quicker
method is to heat the sample over a free flame until a
watch glass held over it for a moment shows no con-
densation of vapor, or until the odor of acrolein is just
noted. This method, evidently, depends a good
deal upon the personal equation.
A method occasionally employed and originally
suggested by Marcusson1 is to distill with xylene.
The distillate containing the water is received in a
ipecial flask having a graduated leg in which the
water settles, and the reading of the lower layer is
taken as the water content of the sample. In the
case of soaps containing alcohol or ammonia, these
I' i"und partly in the water layer; corrections are
made by taking the specific gravity in the case of alco-
hol, or by titrating with standard acid in the case of
ammonia.
The distillation method has been employed quite
1 Mill. t. MatrrialprHfuntsoml, 23 (1905), 58.
ests
Oven Tests
at 100° C
t
Per cent
II
I
II
15.35
15.70
29.90
29.25
29.51
11.88
12.25
13.22
5.90
5.83
5.72
11.80
9.85
16.50
successfully for the determination of moisture in such
materials as foods, oils, tars,1 creosoted wood,2 etc. A
comparison of this method with that of drying to con-
stant weight is given in the following table taken from
S. S. Sadtler:3
Distillation Tests
Per cent
Analyses I
Egg Alljumen 15.90
Cheese 2<>.7S
Buttei 11.48
Linseed Ml:i1 A 5.90
Linseed Meal B. 12.00
Sawdust 17.20
In the case of soaps, however, the distillation method
gives considerable trouble on account of excessive
foaming during the heating. The operation becomes
tedious and slow, and considerable care is necessary
to prevent the foam from entering the condenser tube.
Another objection to this method is the very viscous
condition of the xylene-soap solution towards the end
of the distillation, thereby hindering the free escape
of the vapor. The solution at the end of the distilla-
tion usually gelatinizes on cooling.
These obstacles, the writer found, are very satis-
factorily overcome by the addition of red oil or oleic
acid before distilling. The foaming is entirely elim-
inated and the solution remains very fluid even at
low temperatures. The addition of red oil presents
another advantage in that the xylene-red oil mixture
is a much better solvent for soap than xylene alone;
under like conditions it takes considerably less time
to dissolve a sample of soap in the mixture than in
pure xylene.
The quantity of red oil required is about the same
as the weight of the soap taken for analysis. In
that case, the soap is quickly and completely dissolved
by the xylene, and the foaming is entirely eliminated,
allowing the distillation to be carried out at any de-
sired rate. The results compare favorably with the
oven method for soap as recommended by the D. S.
Bureau of Standards.4 The two methods are com-
pared in the following table:
Distillation Test Oven Test
with Red Oil at 105° C
Per cent Per cent
Soft Soap 42.5 42.7
Degumming Soap 69.5 70.6
Fulling Soap 16.2 17.1
3 cc. 0.5 N NaOH 96.4 98.0(a)
(a) Theoretical.
Michel5 finds it necessary in the determination of
water in foods to apply a correction of 0.125 cc. to
the water reading to allow for the shape of the menis-
cus. This correction is not necessary in soap anal-
ysis as the meniscus is very nearly flat, probably due
to traces of soap mechanically carried over; for it
was noticed that the meniscus between fresh water
and xylene became flat on adding a few drops of a
liquid soap. However, a correction of 0.05 cc. may
be allowed for moisture left in the condenser, since
the results in the table are uniformly lower than by
the oven test.
' J. A m. Chcm. Soc. 25 (1903), 814.
> U. S. Dcpt. Agr., Forest Service. Circ. 134 (1908).
> This Journal, 2 (1910), 66.
« Circular 62 (1916), 21.
»/. Sot. Chtm.Ind., 32 ( 1Q1. ») 44S.
Aug., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY 590
In this connection, it may be of interest to note that that sodium sulfate had been substituted for potassium
on shaking the water and xylene layers in the receiver sulfate since the appearance of Latshaw's article, but
after the distillation, the water formed a permanent instead of using 7 to 8 g. of the anhydrous salt as was
emulsion with some of the xylene, but on adding done by Latshaw, 10 g. of the hydrated salt were being
sufficient red oil, the emulsion was destroyed and the used. This is equivalent to 4.4 g. of the anhydrous
layers separated completely in a short time. No salt. It was thought that it should be determined
emulsion, however, was formed on shaking pure water whether or not the addition of water (as the water of
with fresh xylene. This emulsion is probably also crystallization of the sodium sulfate) would affect
due to traces of soap. Those familiar with the manu- the result and the time required for the completion
facture of soluble mineral oils, which consist mostly of the digestion following the Kjeldahl-Gunning
of mineral oil, red oil, and soap, or other emulsifiers, are method.
probably aware with what care the red oil must be Table i
incorporated; only a slight excess of the latter to the per cent Nitrogen
compounded oil is sufficient to destroy its property clear Naiso! foHiO
of emulsifvinp in water after (equivalent to
01 emuisnymg in wdtei. Material Used Hours 4.076 g Na;SO, 4.076 of Na.SO.)
The method, as carried out in our laboratory, is to Cottonseed feed l'A ' 3.032 3.054
weigh into a 500 cc. Erlenmeyer flask enough of the S^nTt shorts I'.So loo?
soap to vield about % cc. of water. An equal quantity Wheat white shorts jy. 2.606 2. 603
r - ° -x -a j Molasses feed I1/: 1.707 1.702
of red oil and 1 ;o cc. of water-saturated xylene are standard wheat shorts. . . l'A 2.918 2.918
, , , , , ,..,,, , , Standard wheat shorts. .. l'/i 2.841 2.824
added and the contents distilled at the rate ot 1 to 2
drops per second. The receiver at the start is filled Table l shows the results of analyses made to decide
with 5 cc. of the water-saturated xylene and the dis- this Point- There was little or no difference in the
tillation is stopped when about 85 cc. are collected. time required for digestion, about 10 mm. longer time
The inside of the condenser tube is finally rinsed out beinS required where the hydrated salt was used. It
with the xylene and the washings added to the distillate; should be noted that 4-°7 g. of the anhydrous salt were
this rinsing is best accomplished by distilling rather used and not 4-4 g. This was because we wished to
vigorously 15 cc. more of xylene. The receiver1 compare the results obtained when 5 g. of potassium
consists of a cylinder holding about 120 cc. and is sulfate were used wlth the results when lts molecular
constricted at the bottom to a tube which is about equivalent of sodium sulfate was used. Table II
4 cm. long, graduated in tenths of a cc, and holds about shows the results of analyses made for this comparison.
4 CC. Of water. Table II
The reading may be taken at room temperature or Clear Number Per Cent Nitrogen
, . . . , , , Material after of K2SO. NajSOi
brought to any desired temperature m a water bath, used Hours Analyses 5 g. 4.076 g.
Any drops of water adhering to the glass of the ves- Poultry mash 2 3.163 3.230
/ \ ,. , , , , 6 , 8 ... Mill run bran 2 2.760 2.760
sel may be dislodged by means of a very thin wire Rice bran 2 1.891 1.986
." , . , . , m, , , - Standard wheat shorts .. 2 2.858 2.851
twisted at one end into a circle. The xylene layer is Mill run bran i>/, 2 2.491 2.485
usually somewhat emulsified. On standing over ^m run bran...... . iy. 2 2.690 2.715
night, however, the layers get clear, but the reading ...
.> ,, A-a 4. 4.. -c i„i „ u„u- !,„„,. The sulfuric acid cleared up in about the same time
is practicallv no different than it taken a halt hour r
r* j- »-n V using the above salts.
after distillation. & .... . , , , , .
„,, , .... t 1 ■ -j j 1 *„ m« „,,i„„Q The time of digestion was independent ot the salt
The addition of oleic acid or red oil to the xylene b ^
in the distillation method for the determination of used-
j j • „,.„,- tu^ It should be noted that in our comparisons we used
moisture in soap, as recommended, increases the . r
..... 1 ' v -a ™„ra t K- of potassium sulfate instead of 10 g. as called tor
accuracv bv keeping the soap-xylene liquid more J & * ,
fluid and 'shortens the time of the distillation by in the official method
hastening the solution of the soap in the xylene, and lt might be said that this would give wrong results
, .. . , and that the time of digestion would be different trom
by eliminating foaming. , ... ... , ,
that obtained and the time required when 10 g. are
Laboratory L. Sonneborn Sons, Inc. m..TTT, , , - - ,
Nsw vork City used. Table III shows the results ot tour analyses
made to answer this question.
THE USE OF SODIUM SULFATE IN THE KJELDAHL- Table hi
GUNNING METHOD Number Per Cent Nitr SN
„ „ „ „ ^ Material of K!SO. C1SO1
By C. T. Dowbll and W. G. Friedeman tsED Analyses 5 g. JO g
Received February 2. 1918 Oat feed 2 0.787 0 792
_,,_,. „ T o , ,x Cottonseed meal 2 6.072 5.909
W. G. Latshaw gave in This Journal, 8 (1910), Dried blood 2 14.032 13.880
a, .. .. ,B . ,. , , , MUlrunbran 2 2.943 2 896
386, the results of some analyses which showed very
conclusively that sodium sulfate could be substituted The time required to clear was the same, about 60
for potassium sulfate in nitrogen determinations by mill., in each analysis. It should be pointed out that
the Gunning modifications of the Kjeldahl method. a slightly higher per cent of nitrogen was obtained
One of the writers found on coming to this laboratory in each analysis where 5 g- of potassium sulfate, were
... „ . J . , , ,„,, .. used instead of 10. This might be due to a slight
1 Graefe s Oil Cylinder. Eimer & Amend Catalogue for 1911. No. ■ , ,
4;m oxidation ot the ammonia by the great amount of
6oo
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 8
sulfur trioxide present when 10 g. were used, but no
conclusion can be drawn from so few analyses, and in
fact the results obtained by Fieldner and Taylor1
show apparently that the per cent of nitrogen is in-
dependent of the amount of potassium sulfate, provided
the ratio of grams of potassium sulfate to cubic centi-
meters of sulfuric acid is not greater than 0.5.
Thirty cubic centimeters of acid were used in all of
the analyses reported in this paper. Mercury equiva-
lent to 0.7 g. of mercuric oxide was added and per-
manganate was added at the end of the digestion.
It is shown by our analyses that either the anhydrous
or the hydrated sodium sulfate may be used in the
Kjeldahl-Gunning method, that the time of clearing
is not affected appreciably by the water of crystalliza-
tion of the sodium sulfate, and that as little as 5 g.
of potassium sulfate is sufficient in the analysis of sub-
stances such as we used. No analyses were made with
greater amounts of sodium sulfate than 4.07, since that
amount gave the same result as 5 g. of potassium
sulfate, and 5 g. of the potassium sulfate gave the same
result as 10 g., which is the amount used in the official
method. It is realized that our reasoning is not quite
conclusive because of the lack of a sufficient number of
analyses to compare the results when 5 g. of potassium
sulfate are used with these when 10 g. are used, but
the analyses of Fieldner and Taylor2 seem to leave no
question on this point.
Oklahoma Experiment Station
Stillwater, Oklahoma
THE STRUCTURE OF SCARLET S3R (B) AND
PONCEAU 3R(By)
By H. W. Stieglbr
Received May 21, 1918
Scarlet S3R (B. A. S. F.) is one of the more im-
portant of the unclassified azo dyestuffs (U. S. Dye-
stuff Census), some 80,000 lbs. being imported in
1913. It was thought that a determination of its
structure would be of interest.
The sample of Scarlet S3R was decomposed by
means of SnCl2-HCl solution and the cleavage products
separated and purified.
The azo component was identified as amido R-salt
(1 : 2-amido-naphthol-3 : 6 di-sodium-sulfonate).
Steam distillation of the alkaline reduction liquid
yielded a brownish oil of no definite boiling point. On
standing for some time (cold), traces of crystalliza-
tion were noted. Separation by further cooling yielded
a white crystalline solid, identified as pseudo-cumidine
(1:2: 4-trimethyl-5-amido-licnzcnc; melting point,
63° C).
The presence of an oil with the pseudo-cumidine
crystals probably indicates the use of crude cumidine,
which contains a considerable amount of one of its
isomers, mesidine.
Scarlet S3R then, being a monazo dyestuff, has the
following structural formula:
1 Bureau of Mines, Technical Paper, M, 10.
3 Loc. cit.
NaSO
y\ — N =
-OH
CH,'
-NaSO,
CH,
CH,
R-salt + pseudo-cumidine
Scarlet S3R
This investigation therefore classes the Badische
Scarlet S3R as Ponceau 3R, No. 83 Schultz Farbstoff-
tabellen.
In making comparative tests of the Scarlet S3R
with several classified Ponceaus, slight discrepancies
were noted in the case of Bayer's Ponceau 3R. This
dyestuff is listed by Schultz under No. 83 as being of
the same structure as that determined for Scarlet S3R.
An investigation established the interesting fact
that Ponceau 3R is entirely different in structure
from that given by Schultz. Both cleavage products
were found to be naphtholsulfonic acid derivatives.
Difficulty was encountered at this point in obtaining
either product free enough of the other to proceed
with their identification, as both were only slightly
soluble in water, neutral sodium sulfite, etc.
Small quantities of both components were finally
obtained in a pure state. Further investigation es-
tablished the rather unusual use of amido Bayer acid
(1 : 2-amido-naphthol-8-sulfonic acid) as the diazo
component, and gamma acid (2 : 8-amido-naphthol-6-
sulfonic acid) as the azo component, thus giving
Bayer's Ponceau 3R the structure:
OH
NaSO:
-NH,
Amido Bayer acid -f- gamma acid
Ponceau 3R (Bayer)
This investigation indicates an error in Schultz, in
that Bayer's Ponceau 3R is not crude cumidine + R-
salt as stated there, but amido Bayer acid + gamma
acid. It also classifies Scarlet S3R (Badische) as
Ponceau 3R, Xo. 83 Schultz.
Lowell Textile Organic Laboratories
Lowell, Massachusetts
AMMONIA AND NITRIC NITROGEN DETERMINATIONS
IN SOIL EXTRACTS AND PHYSIOLOGICAL SOLUTIONS'
By B. S. Davtsson
Received January 8, 1918
INTRODUCTION
Studies in soil biology dealing with the transforma-
tions of the soil nitrogen require frequent and exact
determinations of ammonia and nitric nitrogen. The
unreliability of the methods in vogue among soil
biologists renders necessary a study of the means by
which the true value for ammonia and nitric nitrogen
can be obtained. The error due to the hydrolyss of
nitrogenous organic compounds is quite appreciable,
and should be reduced to a minimum. The often
I An abstract of a dissertation presented in partial fulfilment of the
requirements for the degree of Doctor of Philosophy in the Graduate School
of the Ohio State University.
Aug., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
601
limited amount of material available for analysis
renders it desirable to obtain both ammonia and nitric
nitrogen upon the same sample. The method should
be applicable for both large and small quantities of
the two forms of nitrogen and the error should be of
the order of magnitude of 2 per cent or less.
HISTORICAL
The determination of ammonia in urine and in other
animal fluids has received the attention of many bio-
logical chemists. The aim of the proposed methods
has been to obtain the true ammonia value by re-
ducing to a minimum the error due to the hydrolysis
of the nitrogenous organic matter.
The methods employed in determining ammonia in
soils are more or less modifications of those used by
biological chemists for determining ammonia in urine.
These methods, until recently, have been adopted by
soil investigators without any study having been
made of their applicability to soil investigations.
In 1 90 11 Folin offered objections to the Schlosing
method of determining ammonia in urine because of
the uncertainty of the time necessary for the trans-
ference of the ammonia to the standard acid. He
proposed diluting the urine sample with 400 to 500
•cc. of water, distilling the solution with MgO, col-
lecting the ammonia in standard acid and titrating.
The urine solution was then diluted back to the original
volume, distilled for a second period, and the ammonia
collected in a new portion of standard acid. The
ammonia obtained during the second distillation repre-
sents the urea which was decomposed. The decom-
position for this period is assumed to be the same as
that for the first distillation and the difference between
the two values represents the preformed ammonia
•of the urine.
Shaffer2 made a critical study of the methods used
t>y biological chemists for determining ammonia in
■urine and found that the earlier method of Schlosing
(consisting in allowing the urine and the alkali to
stand under a bell jar with standard acid for absorb-
ing the ammonia) and the Boussingault method (dis-
tilling with an alkali to dryness in a vacuum at 30 °
to 40 °) gave dependable results when the directions
of the original workers were carefully followed. With
certain modifications, satisfactory results were ob-
tained. Folin's3 method was found to be unreliable
because the ammonia from the second distillation
•did not represent the decomposition of urea during the
first distillation. More urea was decomposed during
the first distillation than was represented by the am-
monia recovered, consequently the second boiling
.gave results which were too high, thus reducing the
value for the preformed ammonia.
Folin4 outlined a second method which, with a few
modifications, is now largely used for determining am-
monia in urine and in other animal fluids. This
method consists in the transference of the ammonia
from 25 to 50 cc. of urine into standard acid by means
■ Z. physiot. Chem . 32 (1901), SIS.
',1m. J.Phytiol., 8 (1903), 330.
>Loc. cil.
* Z. Physiol. Chtm., 37 (1902-3), 161.
of a rapid air current. The ammonia is liberated by
i to 2 g. of sodium carbonate and 8 to 16 g. of sodium
chloride. An air current of 600 liters per hr. for a
period of 1 to i'/2 hrs. is necessary for the complete
removal of the ammonia at room temperature. The
author found that an appreciable amount of alkali
is carried by a rapid air current and a trap, inserted
between the aeration cylinder and the standard acid,
is necessary to arrest this alkali. A special absorption
tube was devised to insure complete absorption of
the ammonia. This method was modified by Steel,1
who used 0.5 g. of sodium hydroxide as the alkali.
The hydroxide decomposes any triple phosphate
present in the urine but does not decompose such
nitrogenous organic compounds as urea, leucine,
tyrosine, glycocoll, uric acid, hippuric acid, creatine,
creatinine, and taurine.
Russell2 investigated the Schlosing method for de-
termining ammonia in soils by allowing the latter to
stand in contact with a strong alkali. To remove
the danger of re-adsorption of ammonia by the soil, he
prepared a hydrochloric acid extract of the soil. Russell
found that distillation with magnesium oxide and alco-
holic potash gave reliable results and did not decom-
pose the nitrogenous organic compounds. The most
reliable results were obtained when the soil was dis-
tilled under reduced pressure with either of these
alkalies. Only 50 to 70 per cent of the ammonia
added to a soil could be recovered.
In 1915 Potter and Snyder3 employed Folin's4
aeration method for determining ammonia in soils.
The sample of 25 g. of soil was suspended in 50 cc. of
water and aerated with 2 g. of sodium carbonate for
a period of 19 hrs. at a rate of 250 liters of air per hr.
The apparatus is essentially the same as that used by
Folin with the exception that no trap was employed
to stop any entrained alkali. Remarkably con-
cordant results were obtained and in nearly all cases
the added ammonia was recovered.
The work of Potter and Snyder is a step toward
obtaining more reliable methods for determining am-
monia in soils. The method of attack in this labora-
tory differs somewhat in that we are working with
solutions instead of with the soil direct. A serious
objection to the method as used by Potter and Snyder
is the time necessary for the removal of the ammonia.
The employment of large volumes of solution and the
reduction of the time of aeration present difficulties
not encountered by these authors. Increasing the
rate of aeration increases the error from entrained
alkali and lack of absorption of the ammonia.
It has been shown in this laboratory5 that amounts
of ammonia up to 25 mg. can be recovered from 250
cc. of solution by aerating with magnesium oxide for
a period of 3 hrs. at a rate of 1080 liters of air per hr.
With such a rapid air current it was found that com-
plete absorption could not be obtained without the
use of a scrubbing tower to thoroughly wash the
■ J. Biol. Chcm., 8 (1910), 36S.
' J.Agr. Sci.. 3 (1910), 233.
• TmB Journal, 7 (1915), 221.
« Loc. cil.
' Tina Journal, 8 (1916), 896.
6oj
THE JOURNAL Of INDUSTRIAL AXD EXGIXEER1XG CHEMISTRY Vol. 10. No. 8
passing air. After aeration is complete the absorbing
acid is washed from the tower into a 500 cc. Kjeldahl
flask and the ammonia determined by distillation
with magnesium oxide. This distillation overcomes
the error from entrained alkali.
nitric NITROGEN
A method has been developed in this laboratory1
for determining nitric nitrogen in soil extracts. The
reduction methods were studied and the combination
of the best features of the Devarda, Valmari-Devarda,
and Mitscherlich-Devarda methods resulted in a
method designated as the Valmari- Mitscherlich-De-
varda method. The nitrates are reduced in a N/10
sodium hydroxide solution with 1 g. of Devarda's
alloy. By using a minor modification of the Mitscher-
llch2 distilling apparatus very accurate results are
easily obtained. The reduction is carried on for a
period of 40 min. after the solution begins boiling. It
has been found that the hydrogen evolved at the
boiling temperature is much more effective for reducing
nitric nitrogen than that evolved at a lower temperature.
Solutions containing decomposable nitrogenous or-
ganic matter are boiled for 30 min. with the alkali,
previous to the reduction of the nitrates. This pre-
liminary boiling was intended to destroy such nitrog-
enous compounds, but it has since been found that
this is not of universal application, as some of these
organic compounds continue to yield ammonia for
several distillations.
The methods for determining ammonia and nitric
nitrogen have been developed to give reliable results
under conditions admittedly extreme, that is, large
volumes of solutions and small quantities of nitrogen.
However, a further study, refinement, and modifica-
tion of the methods seemed desirable in order that
both these forms of nitrogen might be determined
> This Jim kn.m., 7 (191
'Landu-. Jahrb . 38 (1909), 279.
upon the same sample. Also, an examination of the
hydrolysis of nitrogenous organic matter under vary-
ing conditions is necessary to establish the justifica-
tion of such methods.
EXPERIMENTAL
ammonia-free water — The water used in this
work was distilled over sulfuric acid and potassium
dichromate and the steam scrubbed before condensa-
tion.
ammonia-free reagents — All the reagen'
made ammonia-free before using.
indicator — Methyl red, prepared by dissolving
0.02 g. of methyl red in too cc. of double-distilled
alcohol , was used. The solutions were carbon dioxide-
free when titrated.
ammonia SOLUTIONS- Standard ammonium sulfate
solutions were made from chemically pure ammonium
sulfate and standardized by distilling with magnesium
oxide.
nitrate solutions — Standard nitrate solutions were
prepared from pure sodium nitrate and standardized
by the Valmari-Mitscherlich-Devarda method under
ideal conditions.
standard acids and alkalies — The standard acids
were prepared from chemically pure sulfuric acid and
carbon dioxide-free water. The solutions were stand-
ardized by the sodium carbonate method, which, ac-
cording to Mitscherlich,1 is the most accurate. Twenty-
five cc. burettes provided with 3-way stopcocks
and connected with reservoir bottles were used.
These burettes are of regular 50 cc. burette length
with a correspondingly smaller internal diameter and
graduated to 0.05 cc. These burettes were standard-
ized by the U. S. Bureau of Standards for 20° C.
and the temperature was maintained as nearly as
possible at that point. Slight deviations from this
temperature were neglected as they were found to
cause no appreciable change in the volume of the
liquid. When portions of the solutions had stood
in the burettes for 12 hrs. or more they were discarded.
For small quantities of nitrogen N 50 acid was used,
and for larger quantities N/10 acid.
Artificial light, having been found more satisfac-
tory than daylight because of its being constant at all
times, was used for all titrations. Large electric
bulbs were used as a source of light. These bulbs
were enclosed outside of the laboratory window
with three panes of glass separating them from
the titrating table. Thin paper was then placed
over the window- to shade the eyes while the full
light from the bulbs fell upon the table.
distilling apparatus — The apparatus used for
distilling over magnesium oxide is shown in Fig. I,
in which A is a quartz or Pyrex glass tube, B contains
the ammonia solution and C is the Erlenmeyer flask
containing the standard acid. Quartz Erlenmeyer
flasks and quartz tubes were first used for the distil-
lations. Later it was found that the Pyrex glass could
be substituted for the expensive quartz.
Nitrate reductions were made in the apparatus
'Landw. Jahrb.. 39 (191<
Aug., 191S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
shown in Fig. II. Flask A contains the nitrate solu-
tion, B a pinch of magnesium sulfate and one of mag-
nesium oxide with a small amount of water, and C
contains the standard acid.
The aeration apparatus is shown in. Fig. III. The
two towers, I and J, are used as scrubbers, one contain-
ing sulfuric acid and the other sodium hydroxide,
when aeration is made over magnesium oxide. If
sodium carbonate is used as the alkali both towers
may be filled with acid.
rate of aeration — The rate of aeration was 1080
liters of air per hr. measured as previously described.1
A Crowell pump was used for drawing air through
the solutions.
SEPARATION OF AMMONIA AND ORGANIC NITROGEN
Before a positive method for separating ammonia
and organic nitrogen can be developed it is necessary
that we have some knowledge of the hydrolytic action
of the alkalies upon some pure nitrogenous organic
compounds somewhat similar to those found in the
soil. The action of magnesium oxide and sodium
carbonate was studied upon some pure compounds.
The averages of several determinations on each sub-
stance are reported in Table I. These substances
were dissolved in water and aerated with magnesium
oxide and with sodium carbonate. Data are also given
for boiling with magnesium oxide for a period of 20
min. Substances containing an amide group show
considerable hydrolysis on boiling with magnesium
oxide while the amino groups have not been apprecia-
bly attacked.
Wt. of Sub
stance Usci
Substance Mg
Formamide 200.0
Acetamide 100.0
Urea 100.0
Asparaginc 100.0
Aspartic acid 50.0
Tyrosine 41.7
Leucine 33.3
1 Lot, cil.
Table I
Nitrogen Obtained
Boiling Aeration Aeration
I with MgO with MgO with Na:CO>
Mg
Mg
Mg
5.933
2.726
l K,i,
0.127
0.008
0.032
1.094
0.022
0.017
il _'4<
0.012
0.008
0.023
0.013
ii inn
0.027
0.034
ii 039
U.0H
ii o "'
ii ii' ■
603
Formamide has undergone decomposition on aera-
tion with the alkalies but the other substances do not
show an appreciable decomposition when one con-
siders the large sample of substance taken. It is
doubtful if as easily decomposable a substance as
formamide can exist in the soil as such for any length
of time. Consistent results could not be obtained
by hot distillation with MgO. The results were in-
consistent when the same gas burner or electric heater
was used for all distillations.
A soil extract rich in organic matter after standing
inoculated with Aspergillus niger for several days
was subjected to analysis. Two hundred cc. of the
extract were used. The results in Table II show the
justification of aeration methods for determining am-
monia nitrogen in soil extracts. Boiling with magne-
sium oxide has given an error of 21.8 per cent.
Table II
1 Soil Extract
ation over MgO
0.948
0.945
0.948
0.871
The application of the methods for determining
ammonia and nitric nitrogen was studied upon an ex-
tract prepared from a greenhouse soil which had been
heavily manured for several years. The extract was
prepared by extracting one part of soil with five parts
of water. After agitation for 4 hrs. the extract was
clarified with a laboratory centrifuge, some dextrose
added, and, when nitrate-free, the extract was ster-
ilized with chloroform and preserved in a closed bottle.
Soil extracts rich in organic matter offer some diffi-
culty in determining nitrates by reduction with De-
varda's alloy in an alkaline solution. The preliminary
boiling in N/10 alkali was found not to destroy all
decomposable nitrogenous compounds. The nitrate
determination under such conditions has, therefore,
a plus error. A volume of 250 cc. of the extract con-
tinued to give ammonia after two distillations of 30
min. each with 2 cc. of a 50 per cent sodium hydroxide
solution. It was found that much of this decom-
posable organic matter could be removed by using 2
cc. of a saturated lead acetate solution and subse-
quently boiling the filtrate with 4 cc. of so per cent
sodium hydroxide. Table III contains results on
the soil extract, one with organic matter removed and
•In- other having it present. The amounts 0.028
ami 0.017 illy negligible
604 THE JOURNAL Of INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 8
Table in .pj^ probable error obtained by calculation, using
Organic Matter Organic Matter the method of least squares, is satisfactorily low.
Dis£oation 1Mg':nt RMg°.ved N° determinations were made using larger quantities
1 Not determined Not determined of the two forms of nitrogen. The order and maeni-
2 0.109 0.028 , , . . ,, 5
3 0.057 o.oi7 tude of the error remains practically constant while
..,.., the percentage error decreases with increasing amounts
Alter boiling 50 min. the solution is diluted back to r .. , t _ r _..
s ° , , ,, . ... of the two forms of nitrogen.
250 cc, and 0.9 cc. of concentrated sulfuric acid is
added, leaving approximately a N/10 alkaline solu- discussion
tion for reducing nitrates. The data presented in this paper show that the
When sodium carbonate is used as the alkali it is aeration method for determining ammonia in small
necessary to use some substance other than lead ace- volumes of urine can be successfully used for deter-
tate for removing the organic matter. Stutzer's1 mining ammonia in large volumes of soil extracts
reagent was prepared and found very satisfactory. and physiological solutions. Some modifications of
At the outset of the work with the' greenhouse soil, the method as ong^lly used bX Folin' w"e neces-
it was found that added nitric nitrogen could be re- sarv for lts application to conditions encountered in
covered by reduction with Devarda's alloy, but in SQl1 blolog>' studies.
no case could all of the added ammonia be recovered The hydrolytic action of magnesium oxide and
by aeration with magnesium oxide or sodium car- sodium carbonate upon such nitrogenous organic
bonate. The amount of ammonia remaining in the compounds as occur in the soil is very small when
solution was usually less than o. 5 mg. the soil extract is aerated ln the cold wlth elther of the
„ . , , . , . ., . , alkalies. The organic and ammonia nitrogen of the
I his retention of the ammonia has been attributed ., . , .. .
, , ,.„. , , ... . soil extract are easily separated by aeration in the
to the formation of the difficultly soluble magnesium ... . . . .,
, .. cold with sodium carbonate or magnesium oxide.
ammonium phosphate- or to the presence 01 a consid- „ . ,. ... .. c ., ., ...
Z , , . f , • Hot distillation of soils or soil extracts with magnesium
erable number of calcium and magnesium3 ions. .... . „, . ,
, , ,.„ . . * . . oxide gives unreliable results. This procedure has
Although the cause of the difficult v in this case was B., , . . . Jz . , c
6 , , , , ,. . ' ,. . . . been widely used and the results obtained are of
not exactlv clear the addition of sodium oxalate . / , „T, , , . , , , ,. ....
'...«., , n. ,, T,r , questionable value. When blank and check distilla-
overeame the difficulty, as shown in Table IV. A "*. .. ,, . ,
,,.•".. ... tions are made the results are unreliable because of
very heavy crystalline precipitate was obtained upon , , . , .
' , /. . . the unequal hydrolysis,
adding the sodium oxalate. The ^^ decomposable protein-like substances
Table iv which yield ammonia when making nitric nitrogen
Reagent a^ent u«d NTak°egnn Recovered determinations are easily removed by using basic
u*d G- Ms- Mg- Error lead acetate or Stutzer's reagent. The subsequent
MeO 0.5 11.27 11.02 — 0.05 , *»
11.27 10.94 —0.33 boiling with N <i sodium hydroxide destroys the re-
11 .27 10.97 —0.30 . .& , . . .. , ... . ,
11.27 10.71 —0.56 mainmg simpler substances which are likely to de-
Na,CQ' I0 J } ; I7 {0;s5 ^0^72 compose during the reduction of the nitric nitrogen.
'.'. 11.27 11.08 — 0.19
11.27 11.08 —O J? PROCEDURE FOR DETERillNING NITRIC AND AMMONIA
MgO 0.5 5.57 5.24 — 0.33
5.57 5.29 — 0.28 NITROGEN ON THE SAME SAMPLE
5 57 5.38 —0.19 . ■ - j c >-
s.57 5.16 —0.41 In the absorbing towers are placed 25 cc. of N/2
Natc:o... :::: '° HI III ^o:ot sulfuric acid. Two hundred to 250 cc. of the ammonia
II] If" iS;o4 and nitrate solutions are placed in the aeration flask,
a few drops of oil, 2 g. of ammonia-free sodium oxalate,
A number of determinations were next made using and 10 g. of pure sodium carbonate added, and the
250 cc. volumes of the extract with added ammonia flask connected with the aerating apparatus. The
and nitric nitrogen. The extract was free from am- solutions are then aerated for 3 hrs. at a rate of 1080
monia and nitric nitrogen. The results of the de- liters of air per hr.
terminations are found in Table V, and the recovery After aeration is complete the ammonia is deter-
of both forms of nitrogen is complete. mined by washing the acid from the towers with 3 or 4
Table v portions of 50 cc. each of distilled water and distilling
Ammonia Nitrogen Nitric Nitrogen with magnesium oxide in the apparatus shown in
4.73 Mg. token 4.03 Mg. taken 6 rr
Mg. found Error Mg. found Error Fig. I.
\]\ +0,;g5 \ 99 Z^:o4 The aeration flasks are removed and the aerating
■» Is ■" ": 1 ™ +g:JE tubes washed with distilled water. The tube is washed
4 . 0 U. 03 4 .U3 U.UU . .
4 72 *.04 +0.01 on tile inside by forcing water into it by means ot jet
+o!o2 4 oi — o!o2 from a wash bottle and allowing the water to drain into
o oo 4^07 +o!o3 the aeration flask. The sodium carbonate is destroyed
^.o°2 4*:S 7°o:o2 by adding 5 cc. of concentrated sulfuric acid. The
Probable error .. ±0.02 solution is heated to boiling and 5 cc. of the copper
I'er cent error 0.42 .. 0.49 ,, , « .. i_ ••■
hydroxide suspension are added and the boiling con-
B,«.uof^stry.B^«107(1909)r38 tjnued for abouf Qnc minute. The solution is then
Steel, -' . litoi. C hem., 8 (1910), 365.
» Kober, J. Am C hem S«„ SO (1908), 1279. 1 Loc. cit.
Aug., 1918
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
605
filtered, while hot, through a coarse 15 cm. filter
paper into another Kjeldahl flask. The aeration
flasks are washed with hot water and the washings
poured into the other flasks without filtration, since
practically all the residue has been transferred to the
filter paper. The residue is washed 4 or 5 times
with small quantities of boiling water. A small piece
of paraffin and an ebullition tube are placed in the
flask to prevent frothing and bumping, 4 cc. of a 50
per cent sodium hydroxide solution added, and the
solution boiled for 30 min. The solution is diluted back
to 250 cc, and 0.9 cc. of concentrated sulfuric acid
added to reduce the alkalinity of the solution to about
N 10. The nitric nitrogen is then determined by re-
ducing with 1 g. of Devarda's alloy and boiling the
solution for 40 min. after bringing it to boiling in
minimum time. When the solution reaches the boil-
ing point it is advisable to reduce the flame. The re-
action is quite vigorous and may result in foaming
over if this precaution is not taken. As soon as the
vigorous action ceases, the flames are turned up and
boiling continued.
SUMMARY
The work reported in this paper justifies the fol-
lowing conclusions:
I — Organic and ammonia nitrogen can be separated
by aerating the solutions in the cold over magnesium
oxide or sodium carbonate.
II — Ammonia determinations obtained by boiling
soil suspensions or soil extracts rich in organic matter
with magnesium oxide are unreliable.
Ill — Ammonia and nitric nitrogen can be accurately
determined upon the same sample by the method re-
ported in this paper.
The author takes this opportunity to thank Dr.
E. R. Allen for his helpful criticisms in this investiga-
tion.
Laboratory of Soil Biology
Ohio Agricultural Experiment Station
STUDIES IN SYNTHETIC DRUG ANALYSIS'
V— ESTIMTION OF THEOBROMINE
By W. O. Emery and G. C. Spencer
Received April 25, 1918
INTRODUCTION
Questions having quite recently arisen relative to
the actual therapeutic strength of certain diuretic
combinations of theobromine and theophylline, nota-
bly with sodium acetate and sodium salicylate, an
investigation of such products seemed desirable. In
the present paper, however, consideration will be
given only to experiments involving theobromine and
looking to the utilization of its periodide as a basis
for evaluation. A description of very similar work
on theophylline and its combinations is reserved for
a future communication.
The quantitative estimation of theobromine in ad-
mixture with other agents of medicinal value, or with
materials of a more or less inert nature, is complicated
by the great insolubility of this compound in the more
1 This Journal. 6 (1914), 665.
common organic reagents. A somewhat similar diffi-
culty, encountered in developing a procedure for the
estimation of acetanilide and phenacetin (acetpheneti-
dine) in admixture, was met by the employment of
glacial acetic acid. A number of preliminary trials
soon demonstrated the adaptability of this solvent
also for theobromine when applied to periodide forma-
tion. It was further found that the solubility is favor-
ably affected by the presence of sodium acetate.
While it is by no means difficult to prepare several
periodides of theobromine, its quantitative separa-
tion in the form of an iodine addition-product of un-
varying composition, suited to the purposes of titri-
metric control, is manifestly beset with difficulties
naturally inherent in operations of this character,
such as homogeneity, freedom from other periodides
and salts, losses by decomposition, evaporation, etc.
In the method presently to be described, advantage
is taken of the fact that, when an acetous solution of
theobromine containing sufficient iodized potassium
iodide is treated with a mineral acid, a grayish black
crystalline precipitate separates, which, judged by
its iodine content, has the composition C7H8N4O2.-
HI.I4. The separation of this hydriodo-tetriodide
becomes quantitative if the iodine solution is reen-
forced with a small quantity of sodium chloride. If,
therefore, the precipitation is effected in a measured
volume of standard iodine and the insoluble addition-
product removed by filtration, the volumetric de-
termination of the unconsumed iodine is readily ac-
complished, and therefrom the quantity of theobro-
mine involved as readily calculated by means of the
appropriate factor.
EXPERIMENTAL
For purposes of identification, the above-mentioned
periodide was prepared by dissolving theobromine
in a few cubic centimeters of hot glacial acetic acid,
transferring the clear liquid to a flask containing suffi-
cient iodized potassium iodide, adding a little con-
centrated hydrochloric acid with constant agitation,
and then shaking the mixture vigorously. After
standing some hours, the periodide was isolated by
pouring the product onto a small suction plate pro-
vided with a suitable filter, washing the mass several
times with a saturated aqueous iodine solution, and
exposing the crystals in the open air until apparently
dry. Protracted exposure of the substance to atmos-
pheric influences, however, is inadvisable, such treat-
ment inducing an appreciable lightening in the color
of the crystals with consequent loss of chemically
combined iodine. The "exterior" iodine was deter-
mined by titration with sodium thiosulfate in alco-
holic solution, and in the presence of sodium bicar-
bonate. Total iodine, on the other hand, was esti-
mated by first treating the substance in acetic acid
with a saturated solution of sulfur dioxide in water,
followed by precipitation with silver nitrate.
Colcd. for CtIIaN4O1.HI.I1: I«, 62.2; I», 77.8.
Found: It. 59.9, 61.7, 62.2; Ii, 76.5, 77.0, 77.2.
Thus it appears that, even with the greatest care,
the operations of washing and drying arc likely to be
6o6
THE JOURNAL Of INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 8
attended with some loss in iodine, which is reflected
in the above analytical findings obtained on different
samples. In order to determine experimentally the
conditions best suited to the iodometric estimation of
theobromine in commercial samples, it was necessary
to carry through several hundred analyses on con-
trols involving this substance, both alone and in various
combinations. As typical of these experiments, the
following tabulated results show the percentage re-
covery from precipitates prepared with varying amounts
of hydrochloric acid, as also with and without the
add.i1 ion of brine.
Theobromine
Theo- Glacial 0. 1 .V Coned. Said N'aCl Found
bromine AcOH Iodine HC1 Soln. Per
No. G. Cc. Cc. Cc. Cc. G. cent
1 0.1000 2 50 1 None 0.0958 95.8
-> 0.1000 2 50 1 None 0.0951 95.1
3 . 0.1000 2 50 3 None 0.0982 98.2
4 0.1000 2 50 3 None 0.0978 97.8
5 . 0.1000 2 'SO 5 None 0.0981 98.1
6 0.1000 2 50 5 None 0.0987 98.7
0.1000 2 50 2 None 0.0977 97.7
8 0.1000 2 50 2 None 0.0976 97.6
y' 0 1000 2 50 2 10 0.0981 98.1
10' 0.1000 2 50 2 10 0.0986 98.6
11 0.1000 2 50 2 20 0.0995 99.5
12 0 1000 2 50 2 20 0.0996 99.6
13 0 1000 2 50 2 20 0.0999 99.9
!4 0.1000 2 "50 2 20 0.0997 99.7
The influence of other factors like sodium acetate,
sodium salicylate, sodium benzoate, and sodium
formate on the estimation of theobromine is shown
in the following series, this substance and the com-
ponent salt being applied in molecular proportions:
Satd. Theobromine
Theo- Glacial 0 1 .V Coned N'aCl Found
bromine AcOH Iodine HC1 Soln. Org. Per
No. G. Cc. Cc. Cc. Cc. Salt G. cent
1 0.1000 2 50 2 20 NaAc 0.0981 98.1
2. .. 0.1000 2 50 2 20 NaAc 0.0990 99.0
3 0.1000 2 50 2 20 NaAc 0.0993 99.3
♦.... 0 1000 2 50 2 20 NaAc 0.0995 99.5
5 0.1000 2 50 2 20 NaAc 0.0994 99.4
6 . 0.1000 2 50 2 20 Na Sal. 0.1002 100.2
7 0.1000 2 50 2 20 Na Sal. 0.1004 100.4
8... 0.1000 2 50 2 20 Na Sal. 0.0997 99 7
9 0.1000 2 50 2 20 Na Sal. 0.0998 99.8
10 0.1000 2 50 2 4 Na Sal. 0.0974 97.4
11 0.1000 2 50 2 8 Na Sal. 0.0990 99.0
12 0.1000 2 50 2 15 Na Sal. 0.0998 99.8
13 0.1000 2 50 2 20 Na Sal. 0.0994 99.4
14... 0.1000 2 50 2 20 Na Sal. 0.0996 99.6
15 0.1000 2 50 2 20 Na Form. 0.1078 107.8
16 0.1000 2 50 2 20 Na Form. 0.1064 106.4
17 0.1000 2 50 2 5 Na Form. 0.1054 105.4
18 0.1000 2 50 2 5 Na Form. 0.1064 106.4
19 0.1000 2 50 2 20 Na Benz. 0.0997 99.7
20 0.1111 2 50 2 20 Na Benz. 0.1105 99.5
21 0.0555 2 50 2 20 Na Benz. 0.0554 99.9
From these experiments it is evident that the per-
iodide method may be safely applied in the quantita-
tive estimation of theobromine, both alone and in
admixture with sodium acetate, sodium salicylate,
and sodium benzoate. The abnormal results ob-
tain* .1 in the presence of sodium formate, however,
for which no satisfactory explanation based upon
experimental data is as yet available, clearly indicate
that some special treatment would be necessary in
combinations of that character.
METHi'l)
In a small (50 cc.) lipped Krlcnmeyer flask dissolve 0.1 g.
of tilt- sample (with about the molecular equivalent of sodium
acetate, in the case of theobromine alone) in 2 cc. glacial acetic
acid by gentle heat on a wire gauze. Dilute with 3 to 5 cc. hot
water. Transfer the perfectly clear solution to a 100 cc. grad-
uated glass-stoppered flask containing 50 cc. standard 0.1 iV
iodine, using warm water for rinsing, Next add 20 cc. saturated
sodium chloride solution, and finally 2 cc. concentrated hydro-
chloric acid while rotating the Bask. Stopper the latter and
allow to stand at room temperature over night. Make up to
the mark with water and mix thoroughly. Pass the liquid
through a small (5.5 cm.) filter previously fitted to funnel
by wetting and drying, reject the first 15 cc. and collect 50 cc.
in a graduated 50 cc flask Transfer this aliquot by pouring
and rinsing to an Erlenmeyer flask of about 250 cc. capacity,
and titrate the excess of iodine with standard o . 1 A" sodium
thiosulfate The quantity of theobromine involved in the sam-
ple under examination is thereupon readily calculated from the
expression :
Theobromine = I (0 0045026 X normality of thiosulfate
used), in which I represents the number of cubic centimeters
of thiosulfate equivalent to the iodine expended in periodide
formation.
The foregoing method has been successfully ap-
plied to several commercial mixtures or combinations
of theobromine, or its sodium salt, with sodium ace-
tate and sodium salicylate. Thus, in the case of a
well-known brand alleged to consist of theobromine
and sodium acetate, with a calculated theobromine
content of 63.9 per cent, the following values were
obtained: 57.4, 58.6, 58.7 and 59.0 per cent. An-
other brand of a similar mixture gave 32. 19 and 31.87
per cent. A sample alleged to be the double salt of
sodium salicylate and sodium theobromine was found
to contain 49.78 and 49.73 per cent (calculated
49-73 per cent theobromine).
SUMMARY
A method has been developed for estimating theo
bromine, both alone and in combination with sodium
acetate and sodium salicylate, based on the formation
of its periodide, C7HsN4O2.HI.I1.
Synthetic Products Laboratory
Bureau op Chemistry
Washington. D. C.
STUDIES IN SYNTHETIC DRUG ANALYSIS. VI— EVALU-
ATION OF HEXAMETHYLENETETRAMINE TABLETS
By W. O. Emery and C. D. Wright
Received May 15. 1918
INTRODUCTION
The present study had its inception in certain pre-
liminary experiments connected with cooperative
work on synthetic drugs, and instituted with a view
to adapt a known or devise a new procedure for the
estimation of hexamethylenetetramine as it ordi-
narily occurs in tablet preparations. A series of tests
looking to its quantitative isolation by the use of im-
miscible solvents early demonstrated the futility of
attempting a solution of the problem in this \vay.
In operations with like volumes of water and chloro-
form, for example, only about 3 to 4 per cent of the
substance are taken up by the latter solvent in one
extraction. Attempts to utilize the condensation
product of hexamethylenetetramine with antipyrine
as a basis for the quantitative determination met with
scarcely better success. After several other equally
fruitless trials, recourse was finally had to a procedure
substantially identical with a method proposed by
Stuewe,1 primarily for formaldehyde and formalin,
but quite as applicable to hexamethylenetetramine.
1 Arch. Pharm., 161 (1914). 430; Phorm. Ztg.. 59 (19:-
Aug., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
607
Stuewe's method, however, while essentially a reversal
of the procedure first employed by Rupp1 in the evalua-
tion of mercuric chloride tablets, was unfortunately
so formulated as to leave the operator very much in
the dark respecting the influence of certain, presumably
determining, factors like time, temperature, and con-
centration on the quantitative outcome.
In the original, as also in the amplified and amended
procedure presently to be described, advantage is
taken of the fact that, when an aqueous solution of
formaldehyde is treated with alkalized potassium
mercuric iodide, the former is converted into a formate
with a corresponding separation of slaty gray colloidal
mercury, in accordance with the equation:
CH20 + K2HgI4 + 3KOH =
Hg + HC02K + 4KI + 2H20
If now the acidified mixture is treated with standard
iodine, solution of the precipitated mercury results,
and by subsequent titration with thiosulfate the quan-
tity of iodine thus entering into combination with the
mercury is easily ascertained. The procedure, there-
fore, resolves itself into five principal operations,
namely:
1 — Hydrolysis of hexamethylenetetramine to for-
maldehyde and ammonia.
2 — Interaction of formaldehyde with potassium mer-
curic iodide.
3 — Acidification with acetic acid.
4 — Solution of the precipitated mercury in standard
iodine.
5 — Titration of the unexpended iodine with sodium
thiosulfate. From the data thus gained, the quantity
of hexamethylenetetramine is readily calculated.
EXPERIMENTAL
In the preliminary survey, the findings obtained with
apparently pure samples were in part so contradictory
as to indicate that a more detailed study of the method
was indispensable to its successful operation. Ac-
cordingly, numerous experiments were carried out on
controls with a view to ascertain, if possible, the more
predominating factors, and to eliminate any such cal-
culated to unfavorably affect the quantitative results.
Thus, it was found that, while precipitation of the
mercury is practically instantaneous and hence com-
plete after the lapse of one minute from the time the
mixture has attained homogeneity, there can be no
objection to allowing the product to stand for a longer
period, if desired, before the addition of acetic acid.
In order to determine to what extent, if any, the
final result may be influenced by varying the time during
which the precipitated mercury is in actual contact
with acetic acid, and as a consequence subjected to
its solvent action, the following tests were made.
The data show conclusively, first, that pro-
tracted contact of the separated mercury with the
acid is detrimental, invariably leading to a correspond-
ing diminution in the quantity of substance sought,
and, second, that any considerable excess of acctii acid
above that required to produce distinct acidity in the
1 Arch. Pharm., 243 (1905), 300; 244 (1906), 540.
reacting menstruum is likewise calculated to impair
the efficiency of the method.
Glacial AcOH I added after CeHiiNt found
No. Cc. Min. Per cent
1 4 i/< 100. 1
2 4 1 99 . 5
3 4 2 98.9
4 4 3 98.5
5 4 4 97.9
6 4 5 97.7
^ 4 10 97.3
8 4 20 96.7
9 4 30 96.3
10 3 y, 99.8
11 4 V« 99.9
12 3 5 98.5
13 4 5 97.9
14 5 5 97.4
15 10 5 96.1
That the presence of vehicles or diluents like starch.
lactose, and acacia has no appreciable effect on the
quantitative findings is clearly shown in experiments:
on controls involving the materials in question, whereby
recoveries of 99.8, 99.9, and 100.2 per cent, respectively,
of hexamethylenetetramine were effected. In the fol-
lowing series will be found the results obtained with the
perfected method on three samples: Nos. 1 to 6,
a well-known commercial brand of pure granulated
hexamethylenetetramine; Nos. 7 to 12, a com-
mercial brand of hexamethylenetetramine tablets
containing about 10 per cent of a vehfcle or diluent;
and Nos. 13 to 18, a laboratory product consisting
of a triturated mixture of equal parts of pure hexa-
methylenetetramine and air-dried talc.
40 Per cent AcOH I added after CiHi-N, found
No. Cc. Min. Per cent
1 10 >/< 99.9
2 10 '/, 99.7
3 10 '/> 99.8
4 10 'A 99.8
5 10 >/, 99.7
6 10 >/t 99.8
7 10 V, 90.7
8 10 '/, 90.6
9 10 '/, 90.8
10 10 V. 90.7
11 10 '/, 90.6
12 10 >/, 90.7
13 10 V 50.8
14 10 '/< 50.8
15 10 '/< 50.9
16 10 'A 50.7
17 10 '/< 50.9
18 10 Vi 50.7
The entire procedure as developed on numerous con-
trols contemplates the following:
REAGENTS
A — Modified Nessler's reagent, involving:
(a) Solution of 10 g. HgCl2, 30 g. KI, and 5 g. acacia
dissolved in 200 cc. H20 and filtered through a pledget
of cotton wool.
(b) Solution of 15 g. NaOH in 100 cc. H20.
B — Tenth normal iodine.
C — Twentieth normal thiosulfate.
PRELIMINARY TREATMINI
Ascertain the weight of 20 or more tablets, triturate
in a mortar to a fine powder, and keep in a small capsule
tightly closed with a cork or glass stopper. Weigh
out 0.5 g. of the powdered sample on a metal scoop or
watch glass, transfer with sufficient water to a round
bottom Mask, add additional water to a total volume of
100 CC, and finally 25 CC. of 10 per cent hydrochloric
acid. ( 'onneet witli a re I 1 .1 ily ol
the worm type) and hoi] gently 15 min.; then, aftei
cooling, wash out the condenser tube witli a little v iti I
6o8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. Xo. 8
and transfer the contents of flask quantitatively to a
graduated 250 cc. flask, finally diluting to the mark
with water.
METHOD
With a pipette withdraw 10 cc. (containing in the
case of a pure product the elements of 0.02 g. of hexa-
methylenetetramine) of the solution so prepared to a
200 cc. Erlenmeyer flask containing a mixture (pre-
viously chilled in ice water if available) of 20 cc. of re-
agent A (a) and 10 cc. of A (b), wash down neck of
container with a fine jet of water, and allow the mixture
to stand at least one minute after gentle rotation of
the flask. Now add 10 cc. of 40 per cent acetic acid
in such manner that the inside of neck is completely
washed by the reagent, mix quickly and thoroughly
by gently rotating and tilting the flask, and immedi-
ately run in from a burette 20 cc. of reagent B, then
titrate with reagent C (adding 5 to 10 drops of starch
solution toward the end of the operation) to the dis-
appearance of the blue coloration. The final color
of the solution is a pale straw-green. If preferred,
the end-point may be determined by the reformation
of a faint blue coloration, induced by the addition of
a drop of iodine solution.
Since the standard iodine (reagent B) employed has
twice the titrimetric strength of the thiosulfate
(reagent C), and 1 cc. of iV/io' iodine is equivalent to
o. 001 167 g. of hexamethylenetetramine (O = 16),
the quantity of this product, as represented by its
elements formaldehyde and ammonia, in the aliquot
under examination may be readily calculated from the
expression
H— I XT
— NX 0.001 167
2
in which H = the number of cubic centimeters of re-
agent C equivalent to 20 cc. of reagent B, I = the
number of cubic centimeters of reagent C required to
offset the unexpended iodine, and N = the normality
of reagent C.
SUMMARY
A procedure is described for the estimation of hexa-
methylenetetramine, whereby advantage is taken of
the fact that, when an aqueous solution of formalde-
hyde is allowed to react with alkalized potassium mer-
curic iodide, the former by virtue of oxidation to a
formate effects a corresponding separation of mercury,
which latter on treatment with an excess of standard
iodized potassium iodide and subsequent titration with
thiosulfate affords all necessary data for calculating
the hexamethylenetetramine originally involved.
Synthbtic Products Laboratory
blirbau of cbbmistky
Washington, D. C.
AN IMPROVED METHOD FOR DETERMINING CITRAL
A MODIFICATION OF THE HILTNER METHOD
Hy C. I£. Parkbr and R. S. Hiltnbr
Received November 27, 1917
In the determination of citral by the Hiltner colori-
metric method1 with metaphenylenediamine hydro-
chloride, it not infrequently occurs that lemon and
orange "ils and extracts produce blue or green colors
1 U. S. Dept. Agr., Bureau of Chemistry, Bull. US, 34; 13S, 102-
1ST, 70.
instead of yellow. This abnormal behavior has some-
what restricted the applicability of the method.
An investigation having for its object the study and
removal of this difficulty proceeded upon the theory
that an oxidation phenomenon is involved therein.
In cases where the blue color develops slowly it appears
to spread downward from the surface of the mixture.
The metaphenylenediamine hydrochloride reagent
acquires a blue color by the action of hydrogen dioxide
solution, and the formation of peroxide compounds
by the action of air and moisture upon terpenes is
noted in the literature.1 Nevertheless, observations
of Mory,2 Hilts3 and the writers that it is not a matter
of indifference whether fullers' earth, or animal char-
coal, or nothing whatever be used for decolorizing the
reagent, suggested that oxidation of the citrus oil
might not be the sole cause of the phenomenon. It
has even been stated that by omitting the use of
fullers' earth the difficulty may be avoided. This is
not always the case.
INFLUENCE OF DECOLORIZING AGENTS
Experiments, unnecessary to detail here, with
fullers' earth, animal charcoal, talcum, pumice, zinc
powder, platinized asbestos, eponite and kaolin, led to
the conclusion that besides their obvious decolorizing
action upon the reagent, such substances affect it in
a more obscure way, rendering it more responsive to
the action of a citrus oil which has the property of
producing the blue color. It was possible, by washing
the powdered metaphenylenediamine hydrochloride
with small amounts of 94 per cent alcohol, to prepare
a reagent which had less tendency to produce the blue
color than a reagent made with the unpurified meta-
phenylenediamine hydrochloride. The purified re-
agent had a lighter color, but it is not supposed that
the substance producing dark reagent solutions is
identical with that causing the blue color.
THE CONSTITUENTS OF CITRUS OILS GIVING RISE TO THE
BLUE COLOR
A decided blue coloration was obtained with a
sample of </-limonene (carven) from Kahlbaum, with
one marked "Limonene, pure, Schimmel and Co."
which was quite yellow and sirupy, and with several
samples of commercial oil of turpentine "for technical
use." No blue color was obtained with available
samples of citral.
Orange oil which failed to give the blue coloration
was exposed to the air by standing over night in a
shallow receptacle, and also by bubbling air through
it for one-half to four hours, after which it gave a blue
color with the reagent in a short time.
These experiments are considered to favor the pre-
sumption that oxidation of the terpene is in part
responsible for production of the blue color.
EFFECT OF REDUCING AGENTS
Stannous chloride was found to prevent the forma-
tion of the blue color, whether added in the solid form
1 Bugler and Wcissberg, Ber., SI (1898), 3046; Roscoc and Schorlem-
mer, Chemistry, 1 U905), 257; Kingzett, /. Soc. Chcm. lid.. 1898, 691:
Thorpe, Diet. Appl. Chem., 3 0912), 68.
» U. S. Dept. Agr.. Bureau of Chemistry. Bull. 13S, 107.
' Ibid . 1SS, 32.
Aug., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
609
or in aqueous or alcoholic solution. It was hoped that
the use of an absolute alcohol solution of this salt, which
remains limpid for some days, would meet the require-
ments, but the necessary presence of at least a small per-
centage of water in the solutions to be compared and the
turbidity resulting from precipitation of basic tin com-
pounds were complications leading to its rejection. Hilt-
ner recommended 50 per cent alcohol as the solvent for
making the reagent. It was found impracticable to
make a 1 per cent solution with 94 per cent alcohol,
and 80 per cent was finally adopted as the concentra-
tion of the solvent, but even using this reagent stannous
chloride produced a turbidity.
Sulfurous acid and metaphenylenediamine sulfite
were tried, but with them citral produced no yellow
color or one which was rather transient according
to circumstances. The metaphenylenediamine base
likewise produced no yellow color with citral. Meta-
phenylenediamine oxalate, citrate and tartrate gave a
yellow color with citral, but produced no blue color
with citrus oils. The solubilities of these compounds,
compared with the solubility of the hydrochloride,
are such that a more dilute alcohol is required to make
a 1 per cent solution.
The addition of a proper amount of oxalic acid to the
original Hiltner reagent was found to accomplish the
desired object in the most simple and convenient
way, and was finally adopted for the proposed method.
The procedure detailed has been tried upon a
number of lemon and orange oils and extracts with
entirely satisfactory results, the only color aberration
so far observed being a slightly brownish tinge de-
veloped in some cases. If the various samples to be
compared are mixed with the reagent at the same time,
as many as a dozen can be compared with a single
standard within an hour without any substantial
error, so far as our experience indicates. In order to
do this it appears advantageous to employ always a
fixed amount of the citral standard, instead of ad-
justing this amount as in the original method. The
comparisons are then made by adjusting the dilution
of the unknown samples. In this manner the operator
will always work toward approximately the same
shade as an end-point. Each operator may choose a
concentration or amount of the citral standard appro-
priate to the conditions of his work, the shade of yellow
to which his vision appears most sensitive, the colorim-
eter used, etc.
So far as known, the presence of extraneous color-
ing substances would not introduce sufficient dis-
turbance to affect materially the determinations.
This possibility may well be considered, however,
especially in connection with orange extract, of which
a larger amount must be used in making the dilutions.
DETAILS OF THE METHOD
reagents — Alcohol — Practically colorless 94 to 95
per cent alcohol may be employed. It need not be
aldehyde-free.
Citral Standard Solutions — Weigh into a 50 cc.
graduated flask 0.5 g. citral. Make up to the mark
with 94 per cent alcohol at room temperature, stopper
and mix well. Pipette 10 cc. of this "1 per cent
solution" into a 100 cc. graduated flask, make up to
the mark with 94 per cent alcohol, stopper and mix.
Each cc. of this contains 0.001 g. of citral. These
solutions may be kept in the refrigerator but should be
measured at room temperature.
Metaphenylenediamine Hydrochloride-Oxalic Acid
Solution — Dissolve 1 g. of metaphenylenediamine
hydrochloride and 1 g. of crystallized oxalic acid each
in about 45 cc. of 80 per cent alcohol. Mix in a
stoppered 100 cc. graduated flask or cylinder and make
up to the mark with 80 per cent alcohol. Add 2 or 3
g. of fullers' earth, shake well, allow to settle nearly
clear and decant upon a double filter. When most
of the liquid has run through add the turbid residue
to the liquid in the filter.
apparatus — Any convenient form of colorimeter
may be used. (The conditions given herein are based
upon the use of the Campbell-Hurley instrument.)
manipulation — The operations may be carried out
at room temperature. Weigh into a 50 cc. graduated
flask about 0.5 g. of a normal lemon oil, or about 4 g.
of orange oil, or 10 g. of lemon extract, or 50 cc. of
orange extract (*. e., with orange extracts, the original
extract is used as a first dilution), respectively, make
up to the mark with 94 per cent alcohol, stopper and
thoroughly mix the contents. Pipette an exactly
measured amount (say 5 cc.) of these respective first
dilutions into 50 cc. graduated flasks. Pipette also
4 cc. of the standard "0.1 per cent" citral solution
into a 100 cc. graduated flask. As nearly as possible
at the same time add, from a small graduated cylinder,
to the 50 cc. flasks 10 cc, and to the 100 cc. flask
20 cc. of the metaphenylenediamine hydrochloride-
oxalic acid reagent, make all up to the mark with 94
per cent alcohol, stopper the flasks and mix well.
Empty the 100 cc. flask of citral dilution into the
plunger tube of the colorimeter and a 50 cc. flask
of the unknown dilution into a comparison tube.
Both comparison tubes are graduated in millimeters.
Adjust the plunger until both halves of the field have
the same intensity of color, and note the heights of the
columns compared. Calculate the average of 5 or
more observations. From these preliminary results
compute the amount of the first dilution of the un-
known which should be used in making the second
dilution to produce the same color as the standard
in the same height of column of liquid. Repeat the
determination preparing at the same time fresh dilu-
tions of the standard and unknown until columns of
liquid of equal intensity of color differ in length not
more than 5 or 10 per cent.
In cases where the quantity of material available is
scanty, it may be better to reverse this procedure by
varying the dilution of the standard instead of the
sample in developing comparable colors.
calculation — Let a = grams of citral (0.002) in
50 cc. (not 100 cc.) of diluted standard used for com-
parison.
b = grams of oil or extract weighed.
c - volume in cc. (50) of 1st dilution of unknown.
d = volume in cc. of same used for 2nd dilution.
6io
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 8
e = height of column (mm.) of standard used for
comparison.
/ = height of column (mm.) of unknown used for
comparison.
a X c X e X ioo
= per cent citral in oil or ex-
Then
b X d X f
tract.
example — Lemon oil weighed 0.5384 g.
Preliminary d — 5 cc, e = 86 mm.,/ = 77 mm.
0.002 X 50 X 86 X 100
" per cent, and
0.5384 X 5 X 77
77
= 4-25
5 cc. X = 4.47 cc. approximate amount of 1st dilu-
06
tion to be used in final determination.
Final d = 4.5 cc, e = 79 mm.,/
0.002 X 50 X 79 X 100
0.5384 X 4-5 X 77
mm.
4.23 + per cent.
U. S. Food and Drug Inspection Laboratory
Denver, Colorado
THE IDENTIFICATION AND DETERMINATION OF
POTASSIUM GUAIACOL SULFONATE
By Samuel Palkin
Received June 1, 1918
The sulfonic acid salt of guaiacol has been used in
medicine for a number of years. When so employed
it is practically never used by itself but in conjunction
with gums, resins, alkaloids, and other medicinal
agents to counteract various symptoms. This renders
its identification and determination much more difficult
than if the substance were used alone. Many well-
known qualitative tests for common elements are thus
rendered almost useless by the presence of ordinary
resins and other complicating substances that are
generally present in medicinal preparations.
The potassium guaiacol sulfonate1 used in medicine
is apparently the metasulfonic acid2 salt of guaiacol.
It is a colorless salt, very soluble in water, only slightly
soluble in alcohol and insoluble in ether, benzene, and
chloroform.
Two samples of potassium guaiacol sulfonate from
different manufacturers were obtained in the open
market. These samples are designated A and B in the
paper.
EXPERIMENTAL
As stated in the patent of Fabrik-Heyden,3 no
insoluble salts of the sulfonate were obtained with the
heavy metals, with the exception of lead subacetate
in the neutral or alkaline solution. As the compound
is most generally accompanied by resins and other
substances precipitable by lead subacetate, this reagent
could have but little value in this connection. Organic
bases gave no insoluble compounds. No good solvent
was found which would extract guaiacol sulfonic acid.
Amyl alcohol does so to some extent, but has not been
found of value.
Lg advantage of the phenolic properties of this
compound, the action of chlorine and bromine was
tried. Very little action occurs in the concentrations
i I), k. P 109,789, Friedlander, V U900), 738; D. R. P 188.506,
Friedlander, VIII (1907), 936.
' il. Bar., 39 (1906), 2773, 4093; A. Rising, Ibid., 39 (1906), 3685
*Loc. cil. (2).
of the compound generally used, but in higher con-
centrations the dibrom guaiacol sulfonate1 is formed.
This compound is extremely soluble in water and quite
insoluble in most organic solvents. As it has no
definite melting point or other easily identifiable
physical or chemical property, the formation of this
compound was not found to be of any use for the
purpose in hand.
In the presence of strong hydrochloric acid and with
heat, a rather unexpected reaction takes place. In-
stead of mere formation of a chlor- or brom-com-
pound, hydrolysis takes place, sulfuric acid being split
off almost completely and but a very small amount of
chlor- or brom-compound is precipitated, and that
apparently of guaiacol itself. That guaiacol is an
intermediate compound is made apparent by the fact
that it can readily be detected by its odor during
the process of heating. This is especially true when a
dilute chlorine solution is used. The amount of halogen
compound formed is very small and is furthermore
contaminated by other by-products, thus making
it useless for purposes of identification. So effective,
however, is the halogen (bromine in particular) in its
hydrolytic action on the sulfonate that nearly 97 per
cent of the theoretical amount of sulfuric acid is thus
obtainable. In fact, this procedure with some modi-
fication is actually made use of subsequently in the
quantitative determination of this compound.
Another and rather useful reaction depending on the
phenolic properties was found in the coupling of this
compound with diazotized amines. Among those
tried were aniline, toluidine, xylidine, tolidine, 0- and
p-mtvo aniline, p-amido phenol and naphthylamine,
and an azo dye was formed in practically every case;
but in nearly all cases, a dirty brown precipitate,
exceedingly voluminous and not particularly charac-
teristic, resulted, with the exception of that obtained
with />-nitro aniline. The diazotized ^-nitro aniline
gave, with the alkali guaiacol sulfonic acid, a dark
red, water-soluble dye, which behaved as an indicator.
A small quantity of the dye used as an indicator changes
very sharply from red in the alkaline solution to yellow
in the acid solution. The dye is only slightly solubl;
in chloroform and ether but very readily soluble in
amyl alcohol. In the presence of various contaminating
substances as mentioned above, this dye can be ex-
tracted from the water (acid) solution with amyl
alcohol and with alkali re-extracted from the amyl
alcohol, thus rendering it free from obscuring im-
purities and observing clearly the color changes.
It is necessary to eliminate or establish the absence
of phenols, or guaiacol itself, which also give red dyes
when applied as coupling agents to diazotized />-nitro
aniline. Since guaiacol sulfonic acid is nonvolatile
with steam and cannot ordinarily be shaken out by
organic solvents, preliminary treatment to insure the
■ if cither interfering phenols can readily be
resorted to before applying the reaction.
HYDRO) vsis — As pointed out in the discussion of the
action of halogen on this compound, instead of the
1 Kruuss and Krede. J. Am. Chrm. Soc, 39 (1917), 1432.
Aug., 191!
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
expected halogenation, there results the hydrolytic
action yielding sulfuric acid.
The usual procedure of heating with hydrochloric-
acid in a sealed tube was resorted to. About 100 mg.
substance was heated with concentrated HC1 in a
sealed tube to 200 ° C. for several hours. Some
charring took place but most of the sulfuric acid was
split off and some of the guaiacol was further attacked
to form pyrocatechol as indicated by a number of
corroborative tests. A quantitative determination
showed that about 88 per cant of tha guaiacol sul-
fonate was converted. The use of the sealed tube is,
of course, attended with some difficulty and quite
inapplicable to preparations that generally contain
guaiacol sulfonate. The experiment was made merely
to note approximate extent of hydrolysis and products
formed.
A procedure involving the same principles, vis.,
high temperature, strong acid, and at the same time
presence of moisture, was found in the use of high
boiling liquids as well as salt solutions. These accom-
plished the same results much more readily. Best
results were obtained with phosphoric acid (containing
some NaCl) and with a concentrated ZnCl2 and HC1
solution which ultimately boils at about 2000 C.
The characteristic odor of guaiacol is given off during
the boiling, if interfering substances are not present,
and the volatile phenol can be distilled over and tested
for in the usual manner. A color change to wine-red
and then to brown or charring is observed in the latter
stages of the boiling. Attempt was made to utilize
either phosphoric acid or zinc chloride for the quanti-
tative conversion of the sulfonic acid to sulfate. Nearly
quantitative results were obtained with ZnCU, but
the results were nearly always somewhat low, owing,
apparently, to the reduction of some of the sulfuric acid
during charring. Oxidation with a few drops of nitric
acid during boiling was tried but was found to cause
formation of nitro compounds (apparently picric acid),
which precipitated along with the barium sulfate and
invariably gave high results on ignition. Owing to
the tendency of phosphates to be dragged down with
the precipitates in the determination of sulfates, the
results, using phosphoric acid as the hydrolytic agent,
were always high. This procedure, while useful for
qualitative purposes, was, therefore, deemed un-
desirable for quantitative determinations.
A table follows which shows results obtained by the
various procedures described above.
The two samples of potassium guaiacol sulfonate
used were previously analyzed by the bomb ignition
methods as follows: A weighed amount of sample
not exceeding 150 mg. mixed with an equal amount of
sulfur-free benzoic acid was inserted in a Parr calorim-
eter bomb, about 5 g. C. P. sodium peroxide added, the
whole mixed and ignited, and the sulfates determined
in the usual manner, with the following results:
Per cent SOi
1 (b) 30.8
Sample A < (b) 30.5
I \e)
1(a) 31.6
Sample B \ CM 31.2
tic) 31.4
SOj
SOi by
Weigh
Sugar
found bomb method
Sample Mg.
Reagent used
syrup added
G.
G.
0.0316(a)
B 100
HNOi Cone.
None
0 . 0308
0.0312(o)
100
(No bromine)
None
0 0314(c)
100
(No bromine)
None
0.030+
0.0314'
100
(No bromine)
None
0.0302
0.0314
100
(No bromine)
0.0303
0.0314
100
(No bromine)
None
0 . 03 1 1
0.0314
100
(No bromine)
None
0.0308
0.0314
100
ZnCl;
None
0.0291
0.0314
100
ZnCl.
0.0280
0.0314
100
ZnCl:
0.0300
0.0314
100
ZnCl:
None
0.0301
0.0314
100
ZnCl:.
None
0.0294
0.0314
100
ZnClg
None
0.0284
0.0314
100
ZnCli + drops of
HNOi
None
0.0324
0.0314
100
ZnCb + drops of
HNOi
None
0.0336
0 0314
100
iBr+ HNOs + Br)
Proposed method
None
0.0314
0.0314
100
Proposed method
0.0315
0.0314
100
Proposed method
None
0.0318
0.0314
100
Proposed method
None
0 0315
0.0314
100
Proposed method
None
0.0319
0.0314
100
Proposed method
5 cc. Cone.
Syrup
0.0316
0.0314
100
Proposed method
5 cc. Cone.
100
Proposed method
Syrup
5 cc. Cone.
0.0315
0.0314
100
Proposed method
Syrup
5 cc. Cone.
Svrup
5 cc. Cone.
Svrup
5 cc. Cone.
Syrup
0.0318
0.0314
100
Proposed method
0.0315
0.0314
200
Proposed method
0.0622
0.0628'
250
Proposed method
0.07855
0.07852
5 cc. Cone.
200
Proposed method
Syrup
5 cc. Cone.
Syrup
0.0631
0.06282
A 100
Proposed method
0.03074
0.0307"
5 cc. Cone.
100
Proposed method
Svrup
5 cc. Cone.
Syrup
0.0306
0.0307J
225
Proposed method
0.0692
0.0691'
1 Average of 3 determinations of B.
- Calculated from average of B.
3 Average of 3 determinations of A.
* Calculated from ($).
The following method for the qualitative testing and
quantitative determination of potassium guaiacol
sulfonate is recommended, with the view to its adapta-
tion to the medicinal preparations in which it is most
likely to occur.
It must be borne in mind that other sulfur-bearing
compounds such as sulfonal, trional, saccharine, etc.,
must either be proven to be absent or, if present,
previously removed by extraction before applying the
method described. The author knows of no other
sulfonic acids employed in medicine except ichthyol
and the rarely used phenol sulfonates. The quantita-
tive procedure herein described will not be accurate
in the presence of those compounds. The qualitative
tests are not interfered with by ichthyol, as nearly all
of the ichthyol is precipitated on acidification with
hydrochloric acid as directed in the method, the
free sulfonic acid of that compound being very diffi-
cultly soluble in water. The phenol sulfonates are
readily converted into the insoluble tribrom phenol
by the action of bromine.
QUALITATIVE — (a) Some of the sample containing
potassium guaiacol sulfonate is diluted with water and
acidified with hydrochloric acid. If a resinous or other
precipitate comes down, it is filtered. A portion of the
filtrate is tested for sulfate. Another portion of the
is made more strongly acid with HC1 after the
addition of a few grams of sodium peroxide. The
solution is boiled and chlorine is generated in limited
quantities which attacks the guaiacol sulfonic acid.
In the presence of this compound, the characteristic
odor of guaiacol becomes perceptible. If, after boil-
6l 2
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 8
ing for about 15 to 20 min., a precipitate is formed, this
is filtered off and the nitrate nearly neutralized with
sodium hydroxide and tested for sulfates. Com-
mercial hydrogen peroxide contains sulfates and
naturally cannot be used for that test. In the absence
of sulfate in the original sample, and subsequent
formation of sulfate by the action of the chlorine, a
good indication is had of the presence of sulfonic acid-
guaiacol. In the presence of sulfate in the original,
determination of sulfates before and after have to be
resorted to in order to note increase due to sulfonic
acid.
(6) Some of the filtrate is made alkaline and to it is
added drop by drop a cold solution of diazotized
/>-nitro aniline. (The diazo salt is prepared by
dissolving 140 mg. />-nitro aniline in 8 cc. H»0 and 1
or 2 cc. concentrated HC1, cooling and adding 75 mg.
sodium nitrite dissolved in a few cc. of H20.) In the
presence of guaiacol sulfonate the solution will be
colored deep red. If substances are present which
obscure the color, the solution is made acid with HC1,
extracted in a separatory funnel with amyl alcohol,
the lower aqueous layer is tapped off, and the alcohol
layer re-extracted with NaOH solution, when the
azo dye will color the aqueous layer deep red. On
acidification, the solution changes very sharply to
yellow, the azo dye behaving like an indicator in that
respect. If guaiacol or other phenols are present
in the original solution, they should be removed be-
forehand by steam distillation or extraction with
organic solvent as the case may require. The guaiacol
sulfonic acid will remain behind and can subsequently
be tested for as indicated above.
(c) In the absence of much organic material or
possible removal of the same the following procedure
may be used. To a concentrated solution of the sample
(a few cc.) in a hard glass test tube are added about
5 cc. syrupy phosphoric acid containing a little NaCl,
and the mixture is boiled or preferably distilled over.
Distillate, which may be less than 1 cc, may then be
tested for the presence of guaiacol and pyrocatechol,
as both are generally formed. A few drops of a very
dilute ferric chloride solution will give with the dis-
tillate (in the absence of much HC1) a green coloration
which changes to yellowish and on addition of ammonia
changes to violet-blue. The neutral, or better,
ammoniacal solution causes marked reduction of silver
nitrate.
quantitative determination — (a) In the absence
of much contaminating material, a known amount
of the sample, which should not contain much more
than 200 mg. of potassium guaiacol sulfonate, is
diluted somewhat with water in a 150 to 200 cc. Erlen-
meyer flask and 10 to 20 cc. concentrated HC1 are added
and then a few cc. liquid bromine. The solution is
boiled gently and bromine added several times. It is
then evaporated down to a small volume on the steam
bath, using air blast, 10 cc. concentrated HN03 added,
and some more bromine and boiled. This is done to
convert the last traces of sulfonic acid guaiacol. The
process is repeated twice and the whole evaporated to
dryness on the steam bath. It is then diluted with
water and sulfates determined in the usual manner.
(6) In the presence of much organic material, which
is most often the case, a weighed quantity of the
sample in a 150 cc. Erlenmeyer flask is treated re-
peatedly with concentrated HN03, preferably fuming
HNO3, heating gently at first until nearly all of the
organic material has been oxidized. The same process
is then repeated, using bromine and concentrated
HNO3, several times. The whole solution is then
evaporated to dryness on the steam bath and the
sulfates determined as above.
Factor for conversion of BaSOi to SOi = 0.3428; factor for conver-
sion of BaSO* to potassium guaiacol sulfonate = 1.0376.
Bureau op Cs
Department op Agriculture
D. C.
THE OCCURRENCE OF CAROTIN IN OILS AND
VEGETABLES
By Augustus H. Gill
Received April 5, 1918
In a previous paper1 it was shown that the peculiar
bluish reaction of palm oil was due to carotin, and that
palm oil could not be detected in oleomargarine by
this test, because the animal fats also contained carotin.
At that time, the subject was being further studied,
as to what other fats and oils might contain it.
As the carotin is undoubtedly dissolved out from the
seeds by the oils they contain, and as it is present in
them in extremely small amounts, it was deemed best
to extract it from the seeds, rather than from the oils
themselves.
The substances investigated were:
(a) Seeds: Yellow corn, flax, mustard, black sesame,
rape, and white sunflower.
(b) Yellow colored vegetables or products: Carrots,
squash, turnip, orange peel, safflower, cottonseed meal,
turmeric, and neat's-foot and linseed oils.
The procedure used in isolating carotin from various
oils and vegetables consisted in extracting the finely
divided dried vegetable with carbon bisulfide at a
return flow condenser, evaporating off the solvent, and
saponifying the residue or oil with alcoholic sodium or
potassium hydroxide, leaving a slight excess of alkali;
to ensure the absence of free oil, the alcohol was evapo-
rated, keeping the temperature below 700 C. as much
as possible, and the residual soap was then dissolved
in water. The solution was shaken out with carbon
bisulfide, which, in the presence of carotin, assumed a
yellow or orange color, depending upon the amount of
carbon bisulfide used. The carbon bisulfide was
evaporated off, and the residue again treated with an
excess of sodium hydroxide to ensure the complete
removal of any oil which might possibly have escaped
saponification. The resulting soap solution was ex-
tracted with carbon bisulfide, as before, with similar
results. Those vegetables that were free from oils,
such as carrots, were extracted directly with carbon
bisulfide, after first drying the finely divided sample
at a low temperature.
> This Journal. 9 (1917), 136.
Aug., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
613
The carbon bisulfide solution, after the extraction
from sunflower seeds, was colorless, showing at once
the absence of carotin.
Turnip gave a pink solution, safflower, neat's-foot oil,
and cottonseed meal a yellow one, while turmeric gave
a yellow solution with a greenish fluorescence. All
the other solutions were blood-orange in color.
To prove the presence of carotin in these different
substances, advantage was taken of various chemical
and physical properties which carotin exhibits, being
the same tests as employed by Palmer and Eckles1
in their work.
These properties of carotin are:
(1) It absorbs bromine.
(2) It is not extracted from its petroleum ether solu-
tion by 80 to 90 per cent alcohol.
(3) It gives a deep red or blood-orange color in carbon
bisulfide solution.
(4) It is not adsorbed by precipitated chalk.
(5) It gives characteristic absorption bands when
tested in the spectroscope.
(6) It gives a blue color with the Crampton-Simons
test.
Test 6 was carried out by adding the carbon bisulfide
solution of the carotin to cottonseed oil — proved free
from carotin — evaporating the solvent and applying
the Crampton-Simons test to the oily solution in the
usual way.
The results of the tests, except the spectral analysis,
are tabulated in Table I ; the analysis follows in Tables
II and III.
Various
(6)
Cramp- Rela-
(4) ton- tive
(3) CaCOa Simons Amts.
Color of Ad- Color of
CS2 Soln. sorpn. Test Carotin
Blood-Orange Large Blue Small
Blood-Orange None Blue Small
Blood-Orange Large Blue Small
Blood-Orange None Blue Small
(2)
Alcohol
Seed or (1) Extrac-
Vegetable Bromine tion
Yellow Corn Absorbs None
Flaxseed Absorbs None
Mustard Absorbs None
Black Sesame.. . . Absorbs None
Rapeseed1 Absorbs Extracted Blood-Orange Some None None
White Sunflower. None Colorless None
Squash Absorbs None Blood-Orange Some Blue Some
Turnip1 Absorbs Trace Pink Some Brown None
Orange Peel Absorbs None Blood-Orange Large Blue Small
Safflower1 Absorbs Yellow .... None None
Cottonseed Meal1 .... Yellow .... None None
Turmeric' Yellow Large None
Neat's-foot Oil ... ? Yellow .... None Trace
Linseed Oil Absorbs None Blood -Orange None Blue Trace
1 Shows no evidence of carotin.
The fifth test, the spectroscopic test, is probably the
most reliable test for carotin. It depends upon the
fact that carotin cuts off the violet end of the spectrum
sharply, as if a card had been placed between the in-
strument and the test tube containing the solution.
The instrument used in this investigation was a Kruss
single-prism spectroscope and the solutions were tested
according to the method of Formanek.2 Carotin
from carrots was used as a standard. The carbon
bisulfide solution from this material was run through
CaC03 and then extracted with 80 to 90 per cent al-
cohol in order to remove other pigments, although if
xanthophylls were present they probably would not
interfere with the readings, as the bands of this sub-
stance are shifted further toward the blue end of the
spectrum from the corresponding bands of carotin.
1 J. Biol. Chem.. 17 (1914), 190-249.
1 Spectral-analytischcr Nachweis ktinstlichcr organischer Farbstoffe.
Phytosterol which might have been extracted along
with carotin gives no absorption spectrum.1 The
spectroscope was equipped with an arbitrary scale.
By setting this scale at a constant point, before taking
any measurements, it was possible to standardize the
absorption bands from carotin so that the bands of an
unknown pigment could be compared with them.
The solvents used were carbon bisulfide and ethyl
alcohol. The colors of all unknown solutions were
brought to the same tint as the solution by means of
the Lovibond tintometer. This was the only means
available of standardizing the strength of the solutions,
which is an important factor. This was not so pro-
nounced in the case of the carbon bisulfide solutions,
being mostly a question of clearness of reading, but
in the case of the alcoholic solutions a marked effect
was noted. The more the solutions were diluted the
greater was the shifting of the absorption bands toward
the blue end of the spectrum. So, in order to get
comparative results, it was necessary to have all solu-
tions as nearly as possible at the same concentration.
Palmer and Eckles, as well as other investigators,
noted and read three absorption bands for carotin.
In this investigation, an attempt was made to read
only the extremity of one band, the end of the band
toward the red, between the E and# F lines. This
line was particularly clear and distinct. The readings
obtained are given in the following table:
Table II — Carotin Absorption Spectra — CSi Solvent
Carrots 13.64 Rape Seed.
Palm Oil 15.64 Turnip'...
Corn (yellow) 13.46 Grass
Squash 13.65 Safflower1.
Flaxseed 13.87 Turmeric'.
14.02
13.09, 14.89. 16. 10
13.88
15.29
15.10
1 Shows no evidence of carotin.
Neat's-foot oil and cottonseed meal were too weak
to give readings, although both were colored yellow.
Neat's-foot oil responded to none of the other tests,
the color being so dilute. The amount of cottonseed
meal obtainable was so small that the failure to obtain
a reading of this substance cannot be taken seriously.
Turnip was interesting in the fact that it gave three
distinct absorption bands, none of which corresponded
to the carotin reading. Black sesame seed gave con-
siderable trouble as the carbon bisulfide solution dis-
solved resinous material which interfered with the
readings. By evaporating off the carbon bisulfide
and treating with alcohol the resins precipitated, and
on filtering it was possible to get readings both in
carbon bisulfide and alcohol. Safflower, rape seed,
and turmeric gave readings considerably further toward
the blue end of the spectrum than carotin. All read-
ings given in the tables are mean readings of a series
of nine observations.
Table III — Carotin Absorption Spectra — CiHiOH Solvent
Carrots 15.38
Palm Oil 15.38
Corn (yellow) 15.32
Squash 15.38
Flaxseed 15.46
Orange Peel 15.36
Sesame Seed .... 1 5 . 24
Rape Seed 15.99
Turnip 14.80
Grass 15.47
Mustard Seed. . 15.49
Neat's-foot oil, cottonseed meal, and linseed oil
were too weak to give readings, although a reading
could be obtained with the carbon bisulfide solution
' Gill. hoc. cit.
614
THE JOURNAL OF INDUSTRIAL AND ENGINEERING ( HEMISTRY Vol. 10, No. 8
from linseed oil where the absorption was more dis-
tinct. No reading was obtained with safflower, as
on the addition of alcohol to the coloring matter, a
white precipitate formed and the solution which re-
mained after filtering was too weak to read. It is
quite evident from this, its behavior towards bromine
and its high reading in carbon bisulfide solution, that
the coloring matter in this substance is not carotin.
Rape seed and turnip gave high and low readings,
respectively, which is not surprising in view of their
behavior in the previous tests.
SUMMARY
From this work it would seem that carotin is con-
tained in corn, squash, orange peel, flaxseed, mustard
seed, and black sesame seed. Palmer and Eckles
showed its presence in butter fat and beef tallow, Gill
in palm oil, and it has long been known to be in carrots
and grass. It does not seem to be present in rape seed,
white sunflower, turnip, safflower, cottonseed, or tur-
meric.
In conclusion the writer wishes here to acknowledge
his indebtedness to Messrs. James F. Maguire, Jr., and
In-shing Wan, by whom the experimental work was
performed.
Massachusetts Institute op Technology
Cambridge. Mass.
DETERMINATION OF LOOSELY BOUND NITROGEN AS
AMMONIA IN EGGS1
By N. Hendrickson and G. C. Swan
Received February 18, 1918
The chemical methods for the detection of incipient
decomposition in foods must be selected in accor-
dance with the character of the substance under ex-
amination. As is well known, ammonia is one of the
decomposition products of proteins, and the deter-
mination of loosely bound nitrogen as ammonia has
proved to be one of the best chemical methods in
general laboratory use for the grading of eggs.2-3
The principle is that of Folin,4 namely, of aerating
an alkaline fluid until all the loosely bound nitrogen
is driven off as ammonia. This is caught in a known
amount of standard acid for titration, or merely in
an excess of acid for a colorimetric determination.
The size of sample and the time in which it must be
run are the determining factors in the selection of
the method.
The apparatus used for this purpose has been
changed from time to time as improvements were de-
vised until it is now most satisfactory and may be of
interest to those who have to deal with the determina-
tion of loosely bound nitrogen in biological material.
Of the two optional methods of aeration (suction or
blowing), the latter is preferable, for it is easier to
keep the conditions of aeration constant, and this is
' Published by permission of the Secretarj of Agriculture
: M, E. Pennington and A, I) Greenlee. "An Application of the Folin
Method to the Determination of the Ammoniacal Nitrogen in Meat," J.
An, < hem Soi , 32 I 191 1), 561.
1 II. W Houghton and P. C. Weber. -.Methods Adapted for the De-
termination of Decompositicn m Eggs .uid m Other Protein Food Prod-
ucts," Biochem. Bull.. 1914, 447
« Z. phys. Chem., 37 (1902). 161.
important in determining the length of time neces-
sary for complete removal of the ammonia, as other
experimenters have shown1 and as has been our ex-
perience.
■ aration method is preferred wherever possi-
ble, but in case a large number of samples are to be
run in a short time, the colorimetric method can be
substituted. In the latter case the amounts of am-
monia to be determined are so small that great care
must be exercised to keep the apparatus free from
ammonium salts.
Fig. I — Apparatus for Titration Method
A — Pipe from air pump.
B — Wash bottle containing 35 per cent sulfuric acid.
C — Pipe to which aeration cylinders are connected.
D — Aeration cylinder (14'/< in. high X l'/j in. inside diameter)
containing sample. The glass tube for aeration extends to within l/i
in. of the bottom and is open at the end.
E — Trap.
F — Flask in which ammonia is caught, containing 10 cc. of .V/50 sul-
furic acid plus 2 drops of 0.2 per cent methyl red (dissolved in alcohol),
and 75 cc. of water.
G — Dispersion tube made according to method of Folin and Farmer
[J. Biol. Chem., 11 (1912). 493] to insure complete absorption.
Xote — It has been found by test that the ammonia is always com-
pletely absorbed in the one flask by this method.
H — Water gauge for keeping air pressure constant and thus ensuring
the passage of an equal volume of air through the cylinders in a given time.
DIRECTIONS FOR TITRATION METHOD
Mix samples well (preferably with one of the elec-
tric mixers in common use at soda fountains) and
weigh out 25 g. Pour the bulk of the egg into the
aeration cylinder D and transfer the remainder by
means of four 25 cc. portions of distilled water, stirring
each time with a rubber-tipped glass rod to remove
the egg adhering to the sides of the weighing vessel.
Add 75 cc. of alcohol, mix well, and let stand 15 min.
Now add about one gram of sodium fluoride, 2 cc. of
50 per cent potassium carbonate and 1 cc. of
kerosene. Connect the apparatus, blow air through
until no more ammonia comes over, and titrate solu-
1 P. A. Kober and S. S. Gra
by Aeration, for Kjeld.ihl Urea
.4m. Chem. Sot, S5 11913), 1594.
"Quantitative Ammonia Distillation
■ id c Ither Nitrogen Estimations," J.
Aug., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY 615
tion in flask F with N/50 sodium hydroxide to ascer- with the liberation of ammonia, and no definite stop-
tain how much of the 10 cc. of N/$o sulfuric acid, with ping place is reached. This holds even in the pres-
which the experiment started, has been neutralized. ence of sodium chloride to decrease the ionization,
The per cent of nitrogen is then calculated from and is well shown in the following table.
0.00028 X cc. of N/ so H2SO4 neutralized X 100 _ _ _ .. _ xr „, „ „„
= Per J able II— Comparison of NaOH and NaiCOj in the Presence op
25 NaiFi and NaCl. Sample Run in Triplicate
„,>„+ MJ+-«™=^ ' G- Na'COa 0.8 G. NaOH 1 G. NaOH 3 G NaOH
Cent Nitrogen. and and and and
Tests on standard ammonium sulfate solutions ' G NaiF° , % ' «• Nad?, 15 g. NaCl 15 g. NaCi
. Per cent N (a) Per cent N Per cent N Per cent N
and on egg, at 25 C. (the usual temperature 0.0032 0 0059 0.0054 0.0104
of the laboratory) and under 14 cm. water pressure, 0:0032 (kooIi o.'ooso 00112
showed that the ammonia Was all driven Over in 4 (") It should be mentioned at this point that all percentages given in this
, T, ., , ,.,.., , .. , paper are on the wet basis; that is, on the weight of egg fresh from the shell,
hrS. It the pressure under Which air IS forced through or in the case of frozen egg, immediately after thawing.
is altered to any extent, it is necessary to alter the -r>u c -j ■ ,
' the action 01 magnesium oxide as compared with
aeration time to correspond. ,. , . . ., . ,. . . , ,
_,, . . , . , ... potassium carbonate is shown in the following table,
lhe air is passed through ^ s per cent sulfuric acid -p, 1 1 • ^ • ,• , r
, , , . , , , . , , the sample was run as usual, in triplicate for each,
in wash bottles as a precaution, although it has been .. , . . . ., , ... .. .
b . the only variation being in the substitution of mag-
found that the amount of ammonia present is not • , „ ,
. r nesium oxide for potassium carbonate,
great enough to interfere. 35 per cent sulfuric acid
are used, because at this strength the volume of the a a
..... . ,, .... c Run as Usual Repeated after Standing 181/. Hours
liquid is nearest constant under the conditions of 1 g k2cos i g MgO k-coj Sample Mgo Sample
humidity ordinarily prevailing in Philadelphia, and P««° ^ p— ^ P«0lZ™ "Z.%\"
no attention is therefore required except to see that 0.0030 0.0031 . 0.0005 0.0014
4V A ■ 4. 4 I- A WUM t 4.1. 1 0003° O0032 00004 00014
the acid is not neutralized. While, of course, the vol-
ume will increase or decrease somewhat, depending It is seen that the differences on the first run are
upon a high or low humidity, the change is not great. within the limit of error, but after having allowed
By the use of a small concentration of potassium both portions to stand over night (18V2 hrs.), then
carbonate any perceptible hydrolysis of the egg adding 75 cc. alcohol and 25 cc. water, and again
protein is avoided. aerating 4 hrs., more ammonia was given off by the
At the end of 4 hrs.' aeration all loosely bound magnesium oxide sample, indicating that in this
nitrogen originally present has been freed, and the particular case the magnesium oxide is more active
quantity given off on aerating for 2 hrs. more is so than the potassium carbonate.
small that it cannot be determined by titration. The Table IV shows the result of using sodium hydroxide
potassium carbonate may be added in solid form, and sodium carbonate in place of potassium carbon-
but for convenience it is preferable to add 2 cc. ate. One gram of each was used and the sample run
of a 50 per cent solution, using a 10 cc. graduated in triplicate, otherwise as usual,
bacteriological pipette for measuring. Sodium carbon- Table iv
ate may be used in place of potassium carbonate, but k2cOj Na.coj NaOH
J . . Per cent N Per cent N Per cent N
as it is much less soluble, it is not quite so convenient 0 0029 0 0030 0 0044
to nsp as trip latter 00029 00029 °0048
10 use as T,ne laner. 0.0029 0.0029 0,0044
Eggs cannot be aerated satisfactorily without the
addition of something to prevent foaming, and alcohol It will be noted that potassium carbonate and sodium
has been found to be most effective. Kerosene must carbonate give the same results, whereas the results
be added also, as most of the alcohol evaporates after obtained by the use of sodium hydroxide are much
2 hrs.' aeration. Kerosene carried over into the col- higher. There is no definite end-point with sodium
lecting flask does not interfere with the titration. hydroxide; ammonia is given off continuously for a
The directions for adding 100 cc. of water to the egg long time.
before addition of the alcohol should be carefully To illustrate the practical application of this method,
followed; if the alcohol is added first, the egg is coagu- the following tables and explanations are given,
lated in a coarse, stringy condition, instead of finely Table V includes results obtained on whites, yolks,
divided, and is therefore not as efficiently aerated. and whole eggs, fresh, and after 10 mos. in cold storage.
It has not been found advisable to correct for a They were so-called "April Firsts," the besi
blank. The following table shows the reason, namely, for storage. The figures show clearly that no cha 1 -
that in many cases no blank at all is obtained; where takes place as regards the loosely bound nitrogen of
there is one, it is too small to be of practical impor- the white, the increase for the amount in whole 1 gg
tance being referable solely to the rise of loosely bound nitro-
(,,„, , 1 2 Blanks COMPOSED OP. G. N«CO,. 1 C-Na.F,. 75 IV. Alcohol gefl in the yolk. It also shoWS how closr ,HV the n<
and 125 Cc. of Water. Aerated l'/i H«8. Through 5 Cc. N/SO suits on individual egL'S of the same grade computed
Acid and then Titrated Against A//50 NaOH
tf/SO NaOH used — ra 4.95 5.00 5.04 4.96 4.95 5.02 on the moist basis.1
Blank— cc 0.05—0.00 0.04+0.04 — 0.05—0.02 +
AT/50 NaOH used— cc 4.95 4.95 4.95 5.00 4 90 4 95 li might be Stated here that determination of ammonia in dl
1 a 0.05 — 0.05—0.05—0 00 0.10—0.05— -5 of HuU. v,;l|,„. for it has been shown thai ammonia is driven „M , I, .tiny;
_ .. , , . ., „ .. commercial drying. See U. S. Dcpt of Agriculture. Bulletin SI, 'A
Sodium hydroxide cannot be used a th( alkaline Bacteriological and i rial Bgg> to tha Produdni
agent because continuous hydrolysis takes place Durtrict of the Central Wert," M. B. Pennington, el at.
6i6
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 8
Table V — Individual Egcs — "April Firsts"
— Frbsh-
After 10 Months in
Cold Stora
White
Yolk
Whole Egg
White
Yolk
Whole Egg
Per cent
Per cent
Per cent
Per cent
Per cent
Per cent
N
N
N
N
N
N
0.0005
0.0029
0.0013
0.0003
0,0060
0.0025
O 11(1114
0.0031
0.0013
0.0004
0.0056
0.0026
0.0003
0.0028
0.0011
0.0003
0.0062
0.0022
0.0004
0.0028
0.0012
0.0004
0.0065
0.0035
0.0005
0.0031
0.0014
M onus
0.0059
0.0031
0.0003
0.0034
0.0013
0.0004
0 0062
0.0030
Table VI shows results on liquid egg held frozen
for some months. No apparent increase of loosely
bound nitrogen is indicated in edible eggs held hard-
frozen for 9 mos. If the eggs are held in the
shell for that length of time at slightly above freezing,
a gradual increase does take place, however. This
is well shown in Table VII.
Table VI — Liquid Eog Held Frozen
When Put
in Freezer
Per cent N
After Coming
Months Held from Freezer
Frozen Per cent N
0.0026
0.0030
0.0024
0.0022
0.0025
3
3
9
9
9
0.0025
0.0031
0.0026
0.0024
0.0025
Table VII — Case Eggs Held in
Storage — "June Firsts"
(Eggs in each
sample — 2 dozen — about 1 kg.)
Months
Per cent N
0
2
3
4
5
6
7
8
9
0.0013
0.0011
0.0022
0.0021
0.0028
0.0032
0.0032
0.0030
0.0035
0.0040
MICROCHEMICAL METHOD
The principle of this method is the same as for the
titration method, but in operating, scrupulous cleanli-
ness is compulsory for even minute amounts of am-
monium salts in apparatus or reagents will, of course,
invalidate the results.
Five cubic centimeters of liquid egg are placed in
a 250 cc. Erlenmeyer flask and 45 cc. of phospho-
tungstic acid solution (made up in the ratio of 10
cc. of 1 per cent sulfuric acid, 20 cc. of 20 per cent
phosphotungstic acid, , and 420 cc. of water) added.
Shake well, and let stand 5 min.; then filter through
an ammonia-free folded filter.1
Ten cubic centimeters of the phosphotungstic acid
filtrate are transferred to the large test tube D, shown
in Fig. II; 1 cc. of 10 per cent sodium hydroxide and 2
drops of heavy white paraffin oil are added, then the
solution is aerated as fast as possible into 2.5 cc.
of 1 per cent sulfuric acid for one-half hour.
The dispersion tube is rinsed into the collector with
ammonia-free water, 1 cc. of Nessler- Winkler solu-
tion added, and the volume then made up to 10 cc.
with water. Comparison is made with pure standard
ammonium sulfate solution in a Duboscq or Schreiner
colorimeter.
Directions for making pure ammonium sulfate
may be found in the article by Folin and Farmer
previously referred to, and for Nessler- Winkler solu-
tion in Chem. Zcntr., 11 (1899), 320, or "Analytical
1 Test filter papers by soaking a packet of them in ammonia-free water.
If a portion of this water shows much ammonia when nesslerized, the
water is poured off and allowed to drain from the filter papers The soak-
ing and testing are repeated until the ammonia is removed; the papers are
then dried.
Chemistry," Treadwell-Hall, I, 46. Ammonia-free
water is prepared for use by the method of J. Barnes I
in which the water is boiled with enough bromine to
color it. Before using, test with starch-potassium
iodide solution to be sure all bromine has boiled off.
A comparison of results by the colori metric and
titration methods is given in Table VIII. They show
that with very minute amounts of ammonia the colori-
metric figures are a little high, but when dealing
with amounts of ammonia (expressed as nitrogen)
ranging from 0.0020 to 0.0040 per cent
(0.02 too.04 mg.) the agreement is good. If possi-
Fig. II — Apparatus for Microchemical Method
A — Acid wash bottles.
B — Air pipe leading from A, to which aeration tubes are attached.
C — Dispersion tube reaching to within '/« in. of the bottom of the
large test tube D.
D — Large test tube for holding sample — 10 in. high by l'/s in. inside
diameter.
E — Trap.
F — Dispersion tube for complete absorption. Tubes C and F
are made according to the directions of Folin and Farmer referred to in the
preceding method.
G — -Special form of test-tube for catching ammonia without splashing
liquid out of the tube. Its dimensions are — height. 6V1 in., inside
diameter Vs in., diameter of bulb l'/« in. A mark is placed on the
constriction at the 10 cc. point.
A V* h. p. motor is used to drive the air pump.
ble, it is well to use aliquots of the egg filtrate which
will bring the amount of ammonia within these limits.
When dealing with bad eggs there is often so much
ammonia present that a heavy brick-red precipitate
forms on adding the Nessler solution. This may be
overcome by adding just enough 5 per cent acetic
acid to dissolve it, diluting to about 45 cc, again
nesslerizing and making up to 50 cc. Of course it
is necessary to make a corresponding change in the
calculation.
Table VIII — Comparison of Results by Color and Titration
Wh
ite
Yolk
Whole Egg
Per cent
Per cent
Per cent Per cent
Per cent
Per cent
N by
N by
N by N by
N by
Nby
Color
Titration
Color Titration
Color
Titration
0.0010
i' i^
0.0033 0.0029
0.0018
0.0013
0.0009
0.0004
0.0030 0.0031
0.0016
0.0013
0.0010
0.0003
0.0030 0.0028
0.0017
0.0011
1) iinii'i
0.0004
0.0031 0.0031
0.0016
0.0012
0.0010
0.0005
0.0028 0.0034
0.0016
0.0014
Table IX shows the results obtained when sodium
hydroxide, potassium carbonate and a mixture of
potassium carbonate and potassium oxalate are used
in the colorimetric method as reagents for making
alkaline before aeration. It will be seen that there
is no difference which is not within the limit of ex-
perimental error.
' J. Soc. Chem. Itid., 16 U896), 254.
Aug., 1918 THE JOURNAL OF INDUSTRIAL
Table IX — Comparison of K2CO3, NaOH and a Mixture of K2CO1 and
KjCsOi IN THE COLORIMETRIC METHOD
4 Drops of
(8 Per cent
1 Cc. of KiCOi + 12 Per 3 Drops of
Sample 10 Per cent cent K2C2Oi 5 Per cent
No. NaOH in Equal Parts) KiCOa
1 0.0024 0.0022 0.0025
2 0.0023 0.0025 0.0021
3 0.0021 0.0026 0.0018
4 0.0027 '0.0025 0.0025
5 0.0026 0.0025 0.0027
6 0.0026 0.0026 0.0026
SUMMARY
I — Titration and colorimetric methods for the de-
termination of the small amounts of loosely bound
nitrogen in liquid eggs by aerating the alkaline material
(according to the principle of Folin) have been pre-
sented, with descriptions of the apparatus and pre -
cautions necessary.
II — The effect of various agents used to make the
material alkaline, some results on different grades of
eggs, and a comparison of results obtained by both
methods are shown in the tables.
Food Research Laboratory
Bureau op Chemistry
PHrLADELPHTA, Pa.
AND ENGINEERING CHEMISTRY
617
A METHOD FOR THE DETECTION OF FOREIGN
FATS IN BUTTER FAT
By Armin Seidenberg
Received May 22, 1918
The methods at present available for the detec-
tion of foreign fats in butter fat are such that in many
cases considerable difficulty is experienced in definitely
ascertaining the addition of limited quantities. The
constant which has been found to be of most signifi-
cance in the analysis of butter fat is the Reichert-
Meissl number. This constant is dependent upon
the soluble volatile acids which are particularly charac-
teristic of butter fat. While the other constants which
are usually depended upon in determining the purity
of fats and oils, such as the specific gravity, refractive
index, melting point, saponification number, iodine
number, etc., have in the case of butter fat well-
defined limits, sufficiently distinct to permit the iden-
tification of an unadulterated butter fat, they never-
theless in many instances lie so close to those of other
fats that considerable quantities of these can be
added to a butter fat without thereby transgressing
the limits for a known pure sample.
THE REICHERT-MEISSL NUMBER
Among the more commonly known edible fats and
oils none has a Reichert-Meissl number that approaches
the minimum and maximum limits of this constant
for butter fat. These range according to the numer-
ous authorities cited by Lewkowitsch1* from 17 to
36.3. According to Sherman2 the usual variations
in the Reichert-Meissl value for butter fat are be-
tween 24 and 34; cocoanut oil. with a Reichert-Meissl
number of 6 to 8, has the next highest value among the
more widely used edible fats and oils, while the other
edible fats and oils usually have numbers below 1.
According to Lewkowitsch3 the lowest Reichert-
Meissl value adopted by analysts in various countries,
although not officially, lies between 23 and 25. He
» Numbers refer to corresponding numbers in "References," p. 621.
states that values need not fall below this in a legitimate
sample of butter fat if proper precautions in feeding,
etc., are taken. In view of the fact, however, that a
large number of undoubtedly pure samples of butter
fat have been observed with Reichert-Meissl values
below these, it is evident that no butter can be ad-
judged legally adulterated unless its constants are all
decidedly below the lowest observed limits of a pure
sample.
The wide variation of the Reichert-Meissl number
makes it feasible to add considerable quantities of
foreign fats to a butter with a high value without
thereby causing it to fall below the lower limit. The
problem is further complicated according to Lewko-
witsch4 by the fact that glycerides or ethers of the
volatile fatty acids such as tributyrin or amyl acetate
may be added to an adulterated butter fat in order to
raise its Reichert-Meissl value. He states that even
without counteracting the effects of sophistication by
this means it is not possible to detect in every case
the presence of 10 or even 20 per cent of a foreign fat
in butter fat by means of the Reichert-Meissl value.
Indeed, it is quite evident that on a butter having a
Reichert-Meissl value of ^^ or above, adulteration
to the extent of 25 and 30 per cent may be practiced
without lowering the value below the lowest observed
limits. Thus the writer found on adding 30 per cent
of tallow to a butter fat having a Reichert-Meissl
number of 33.9 that the value was decreased to only
24.7. The refractive index of the sample contain-
ing the 30 per cent added tallow was 1.4588, which is
still within the limits that have been observed for a
pure sample. None of the other constants usually
determined would be affected to a greater extent.
Methods depending upon determining the amount
of stearic acid present are likely to prove uncertain,
particularly in view of the varying amounts of this
acid found in butter fat by different observers.
COMPOSITION OF BUTTER FAT
The constants of any fat or 'oil are of course de-
pendent upon the glycerides which it contains and
upon the fatty acids which constitute these glycerides.
The fatty acids generally considered to be present in
butter fat are butyric, caproic, caprylic, capric, lauric,
myristic, palmitic, and stearic. The compara-
tively large amount of the lower soluble volatile fatty
acids are peculiarly characteristic of butter fat and it is
upon these that the Reichert-Meissl number depends.
Their amount in proportion to the other fatty acids is,
however, not very large. According to Browne
the total amount of butyric and caproic acids present
in butter fat is 7 . 54 per cent. Duclaux6 found butter
"fat to contain 2 to 2.26 per cent caproic acid and
3.37 to 3.65 per cent butyric acid. Browne states
the amount of oleic acid to be 32.50 per cent, of pal-
mitic acid 38.61 per cent, and of stearic acid 1.83
per cent. According to a large number of butters of
varied composition examined by Siegfeld7 the volatile
soluble acids range from 5.60 to 7.09 per cent, the
volatile insoluble acids from 0.95 to 3.28 per
cent, the saturated nonvolatile acids from 40. 65
6i8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING I HEMISTRY Vol. 10, No. 8
to 52.01 per cent, and the unsaturated acid from
32.19 to 46.07 per cent. In a former investigation
he had found the oleic acid to vary between 23 . 53
and 53.28 per cent. Hehner and Mitchell8 using an
alcohol saturated at 0° C with stearic acid came
to the conclusion that butter did not contain any or
only very small amounts of stearic acid. However,
Holland, Reed, and Buckley9 secured considerable
amounts of stearic acid from butter fat, namely, from
7 to 22 per cent of the insoluble fatty acids present.
There are not many references in the literature with
respect to the glycerides formed by these acids. In
only a few instances have any attempts been made
to isolate them. Amberger10 succeeded in isolating
tristearin and palmito-distearin from butter fat al-
though in such slight amounts that he was not capable
of forming any conclusions as to the actual quanti-
ties of these glycerides present. However, in view
of the comparatively small amount of stearic acids
found to be present in butter fat by other investiga-
tors, the quantity of these glycerides must be com-
paratively slight.
GENERAL DISCL'SSIOX
From these facts the assumption seems fairly well
justified that butter fat does not contain any consid-
erable amount of glycerides consisting entirely of the
higher saturated and less soluble fatty acids. The
absence of any very large amount of tripalmitin is
indicated by the conclusion arrived at by many in-
vestigators such as Bell" and others that the largest
part of the glycerides in butter fat consists mainly
of mixed glycerides. It is evident that the compara-
tively small amount of insoluble glycerides which
seems to be present in butter fat may be sufficiently
characteristic to form the basis of a method for de-
tecting the addition of other fats and oils containing
larger proportions of the insoluble glycerides. With
this idea in mind Amberger1- undertook to develop a
method for detecting lard and tallow in butter fat.
The method consisted in dissolving 20 g. of sample
in ether to 65 cc. and allowing to stand at 150 to 180
C. for 24 hrs. In this way he found that from pure
butters, crystals weighing 0.009 to 0.4 g. separated
out while butters containing 15 per cent tallow gave
residues between 0.63 and 1.45 g. and those con-
taining 15 per cent lard gave residues between 0.11
and 0.40 g. In a later paper13 he added to 31 g. of
sample, ether to a combined volume of 100 cc. and
allowed it to stand for 1 hr. and then shook the solu-
tion. After another hour the solution was again shaken
and if it contained no deposit or only a trace the sam-
ple was shown to be pure butter or to contain less
than 12 per cent of tallow. If a deposit is formed it.
is filtered off and weighed. The addition of 15 per
cent tallow to butter fat can be definitely detected
by this method. Hydrogenated fats can also be de-
tected when the iodine number has been reduced to
less than one-half.
DISCUSSION OF PROPOSED METHOD
In a previous paper14 the writer outlined a method
for fractionating fats and oils. The method con-
sists essentially in dissolving the fat or oil in two or
more solvents, one or more of which has the greater
solvent action upon one or more groups of glycerides
and is at the same time more volatile. This more
volatile solvent is then removed by aspirating air
through the solution, the removal of the solvent be-
ing accompanied by a* very slow and finely graded
lowering of temperature and by a very thorough
agitation of the solution. In this way a progressive
condition of insolubility is attained with the greatest
possible refinement, making it possible to distinguish
to some extent between the nearly placed points of
comparative insolubility of the more nearly related
glycerides. It is possible to accomplish by this method
a separation of the glycerides into fairly well defined
groups. The writer pointed out in this paper how
this method might be applied to detect the addition
to butter fat of a foreign fat containing larger amounts
of the less soluble glycerides. In view of the previous
expei ience it was evident that the absolute quanti-
tative isolation of the pure glycerides of the higher
saturated fatty acids could only be accomplished
after making numerous fractionations. It was there-
fore determined to undertake to secure a series of
empirical constants, developed under well defined
conditions and which would serve to distinguish be-
tween a pure and an adulterated butter.
As on the previous occasion, it was found that a
mixture of alcohol and ether offered the most favora-
ble medium in which to dissolve the fat. The ether
has great solvent action on all the possible glycerides
of butter fat, this action decreasing, however, par-
ticularly with respect to the stearates and palmi-
tates, with decreasing temperature, and the alcohol is
readily miscible with ether and also has slight but
at the same time selective solvent action on the gly-
cerides of butter fat. The solvent action of alcohol
on most fats and oils according to Vandervelde"
amounts to only 2 per cent. It is, however, greatest
on those containing the glycerides of the lower fatty
acids or of the unsaturated fatty acids.
In the course of the experimental work it developed
that in order to get significant results the conditions
of operating the method would need to be exactly
defined and standardized. It was found that the con-
ditions which were most important were the quantity
of sample, quantity and proportion of solvents, speed
of suction, and temperature of suction. In order to
determine in what way these conditions could be com-
bined to give the most satisfactory results, consider-
able preliminary work was necessary. All the results
obtained refer to 10 g. of sample dissolved in ether-
alcohol to a total volume of 96 cc. While other
amounts were tried these seemed to give the most
favorable results and further experimental work was
confined to these quantities. The suctions were
carried on in a 150 cc. graduated cylinder. The tem-
perature was in each case controlled so as not to fall
below the points indicated. In the preliminary series of
determinations no time observations were taken and no
attempt made to keep the speed of the suction at a
uniform rate. To this may be ascribed a lack of uni-
Aug-, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
619
formity observed between some of the results. It
was therefore deemed necessary so to conduct the
process as to proceed within a specified time limit.
11; will be noticed that by observing this condition
quite satisfactory agreements were secured.
From a consideration of the preliminary results it
was seen that the proportion of 90 parts ether to 10
parts absolute alcohol with the temperature regulated
between 10° and 150 C. seemed most favorable,
both because it indicated most sharply the addition
of fats, such as lard and tallow, containing the more
insoluble glycerides, and also because it indicated
the presence of oleomargarine containing in this
case a lesser proportion than butter fat of the more
insoluble glycerides. Oleomargarine is usually made
from a fat such as tallow deprived of most of its con-
tent of glycerides of the higher fatty acids. It there-
fore consists mainly of the more soluble oleates and
has a larger proportion of these than butter fat. For
this reason a butter fat containing oleomargarine comes
down at a lower point than when pure; of course this
depends largely upon the type of oleomargarine
used.
OUTLINE OF PROPOSED METHOD
In order to get comparable results it is necessary
to adhere with the utmost precision to the method as
adopted. For the suction a 150 cc. graduated cylinder
27.0 cm. high and 3.1 cm. in diameter is used. This
should be attached to a firm ringstand so that its
bottom is about 15 cm. above the table upon which
the stand rests. The cylinder (see illustration) is
securely closed with a rubber stopper through which
pass a thermometer 0.6 cm. in diameter and two
pieces of glass tubing each approximately 0.5 cm. in
diameter. The one glass tubing that enters the
liquid should almost reach the bottom of the cylinder
while the bottom of the thermometer should reach
some point below 45 cc. Ten grams of the sample
are weighed out into a beaker and carefully washed
into the cylinder with a mixture made up by adding
to 90 cc. ethyl ether an amount of absolute alcohol
to bring the total volume up to 100 cc. The solution
of fat in this ether-alcohol mixture is brought to a
total volume of 96 cc. When the thermometer and
glass tubing are immersed in this solution it should
reach a point between the 100 and 102 cc. marks on
the cylinder, the level of the solution being adjusted
by raising or lowering the thermometer. The suc-
tion is so conducted that the air first passes through
some 95 per cent alcohol in another flask. The speed
of suction should be so regulated that it will take about
10 min., not more than 12 and not less than 8 min.,
to reduce the level of the liquid to the 60 cc. mark
on the cylinder. The temperature of the solution
should be controlled, after it has been lowered to 1 50 C.
in the course of the suction, so that it is maintained
as near as possible to 12. 5 ° C. throughout the process.
It should after this never fall below 10° C. or rise above
1 5° C. This temperature control is accomplished
by raising and lowering a beaker containing water at
400 to 50° C. so as to immerse the lower part of the
cylinder.
The designation "turbid" may be defined when ap-
plied to the present method as that point at which
the liquid becomes opaque to the extent of making
it impossible to view through it a pencil or other
object held upon the opposite side of the cylinder.
The liquid usually begins to become slightly turbid
3 to 4 cc. before this point is gradually reached. The
suction is continued until the liquid becomes turbid,
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CBEMISTRY Vol. 10. No. 8
and the point noted. If this is above 60 cc. the suc-
tion is carried on until the level of the liquid is re-
duced to 60 cc. and the liquid then filtered through
a perforated Gooch 2.5 cm. in diameter, using a cir-
cular piece of filter paper. This paper should be
moistened with a little alcohol and fit securely into
the Gooch so that none of the precipitate can pass
through. The filtration should be rapid and the fil-
trate clear. When all the liquid possible has been drawn
off from the residue the paper is removed and the resi-
due carefully detached from it with a keen-edged
spatula, care being taken not to include any fibers
from the paper. The amount of this residue is then
determined after the solvent still adhering to it has
been evaporated off in an oven.
It may be well again to emphasize at this point
the necessity of maintaining with the greatest exact-
ness the conditions outlined above in order to get
concordant results. Another precaution which it is
desired to point out here is the importance of mixing
the sample well before using. On numerous occa-
sions the writer has made the observation that the
higher melting point of glycerides, on solidifying first,
settle to the bottom. On again warming, these gly-
cerides liquefy so that seemingly the sample has be-
come completely homogeneous. Another factor that
may well lead to error are the changes produced in
butter fat due to heating it at too high a temperature.
Butter fats that have been affected in this way, indi-
cated usually by a slight darkening, become turbid
at an abnormally high point, caused probably by the
oxidation of the oleates.
SUMMARY OF RESULTS
In order to determine the limits of variation for a
pure butter fat by this method, constants were se-
cured from 100 samples of butter of known purity.
The results are given in Table I. Xos. 1 to 10.
Table I-
-Con
TANTS 0
f Pure Butter Fat (100 Per Cent)
Tur.
'0. Point
No.
Tur.
Point
Tur. Tur.
No. Point No' Point No.
Tur.
Point
l<a) 62
21
54
41 56 61 57 81
58
(a) Residue = 0.311 g. (6) Residue = 0.248 g.
(c) Residue - 0.449 g. (d) Residue - 0.150 g.
inclusive, were butters secured from a particularly
pure source and which there is every reason to believe
were unadulterated. Their Reichert-Meissl num-
bers were determined and found to be normal in every
case. Xos. n to 16, inclusive, were derived
from creams also secured from a very satisfactory
source and which there was every reason to assume
were unadulterated. Nos. 17 to 100, inclusive,
were derived from cream samples brought to
this laboratory by inspectors of the department for
the ordinary routine determination of fat content.
The constants for turbidity secured from all of these
samples show a very satisfactory concordance, which
may be taken as an additional confirmation of the
purity of the samples. In Table II these results are
Table II — Summary of Results of Table I
Turbidity Number of
Point Samples
48
50
51
52
53
54
summarized. This shows that the great majority
of the turbidity values, namely 94 out of a total of
100, range between 50 and 60 cc. inclusive. The ex-
treme limits observed were 64 cc. and 48 cc. Some
additional allowance may be made at each of these
points to constitute a doubtful zone and the maximum
and minimum turbidity limits for a pure butter placed
at 44 cc. and 68 cc, respectively. In only 4 cases did
a turbidity occur above 60 cc. The maximum resi-
due secured was 0.449 S-
Table III shows the effect of the addition to butter
fat of varying amounts of tallow, lard, oleomargarine,
and hydrogenated fat. While for tallow, oleomar-
garine, and the same hydrogenated fat, and also to a
lesser extent for lard, there is a fair conformity be-
tween the turbidity points and the per cent of added
fat, such is not the case with respect to the residues.
These show very considerable variations even within
the same percentage of any given added fat, particu-
larly, however, for lard. The cause for this does not
seem clear to the writer. However, the same effect
can be noted in Amberger's16 results and indicates
the advantage of using the turbidity points instead
of the amount of residue as a standard. In a number
of cases the melting points of the residues were de-
termined and found to vary between 500 and 55° C.
No distinction could be noted in the melting points
of the residues secured from samples containing differ-
ent foreign fats. However, the quantity of the resi-
due may be determined as a confirmatory test. If it
should amount to above 0.5 g., it would serve in con-
nection with a high turbidity point (above 68 cc.)
to show the addition of a foreign fat such as ether
tallow or highly hydrogenated fat.
From the table it will be seen that 10 per cent or
above of added tallow can be detected in every case
by this method. The results for lard vary considera-
bly. The addition of 25 and 30 per cent of this can
be detected with certainty in every instance investi-
gated; the detection of 10, 15, and 20 per cent additions
is, however, in some cases doubtful. The results for
the oleomargarine given in the table show that the
addition of 20 per cent did not influence the turbidity
point sufficiently to assure its detection. It was,
Aug., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
621
Sample No.
Foreign
Fat. %
Tallow
5
10
Lard No.
30
Oleo. 56
0.454
K025
o!917
Res.
G.
0.485
0^746
o!885
Table III — Showing the Effect
Res. Tur. Res.
79 0.906 85 0 914 82 0
70 0.719 66 0.377
0.360
0^395
70 0.433
74 o!46o
71 0.280 72 0
FECT C
F Addeij Fof
f-:ign
Fats
6
7
8
9
10
Res.
Tur.
Res.
Tm
Res.
Tur
Res.
Tur
Res.
Tur
Res
G.
Cc
G
Cc.
G.
Cc
G.
Cc.
G.
Cc
G.
1.198
62
0.325
64
0
489
62
0
434
64
0
558
73
0
S.S4
1.467
73
0.586
71
0
859
71
0
663
71
i)
780
77
n
568
81
0.846
80
0
774
79
0
696
80
1
065
8?
0
951
1.993
72
0.358
64
0
439
65
0
470
66
0
629
72
0.507
65
0
199
6X
0
»7S
M
0
482
70
1.193
68
0.560
67
0
636
73
0
552
72
0
530
1.190
70
0.280
72
0
497
70
0
493
70
• ■*
76
0
571
).497
70
0.497
70
0
426
AMPLE NO.
18
Foreign
Fat, %
Hyd. Fat
No. 2
Tur
Cc.
Res.
G.
5
10
66
77
0.35C
0.63«
Foreign
Fat. %
Hyd. Fat
No. 1
100 per cent
Oleo
Lard
Tallow
Hyd. Fat No. 1
Hyd. Fat No. 2
*Hyd. Fat No. 3
Coconut Oil Stearin .
Res.
G,
Foreign
Fat, %
Hyd. Fat
No. 3
Tur.
Cc.
Foreign
Fat, %
Coconut Oil
Stearin
Tur.
Cc.
Tur
Cc.
1 .469
2.228
3.530
20
25
30
30
59
50
20
25
30
45
40
40
Res.
G.
0.782
2.060
however, possible to notice the addition of this fat
in quantities of 25 and 30 per cent and above with
certainty. Oleomargarine, as has already been
pointed out, may be of varying constitution dependent
upon the source from which it is derived. The re-
sults are influenced accordingly. It was for this
reason not possible to detect the addition of another
sample of oleomargarine evidently containing larger
proportions of the less soluble glycerides even in
quantities of 25 and 30 per cent. It will be noticed
that the results for the different hydrogenated fats
vary considerably. The iodine numbers of these
fats were determined and found to be as follows:
No. 1, 73.4; No. 2, 34.5; and No. 3, 3.4. In No.
1, having a higher iodine number, the amount of
unsaturated oleates is high, while the amount of the
saturated and less soluble glycerides is comparativ3ly
small, so that these latter do not raise the turbidity
point of butter fat sufficiently to serve for their de-
tection. The effect of the saturated glycerides pro-
duced by the hydrogenation is also seen in a compari-
son of the results between hydrogenated fats No. 2
and 3 given in the table. In the case of No. 3,
having an iodine number of 3.4, the addition of even
5 per cent can be detected with certainty, while No. 2,
which has an iodine number of 34.5, can be detected
in quantities of 10 per cent or above. Where the
iodine number of a hydrogenated fat is high, as in the
case of No. 1, so that its addition cannot be detected
by the suction method, the determination of this
value in a suspected sample of butter fat would in
many cases give evidence of the presence of the added
fat.
The table also shows the effect of the addition of
a sample of coconut oil stearin to butter fat. The
effect of this fat also may vary with the constitution
of different samples. The results for 100 per cent
of the various fats used illustrate to what extent the
effect produced is due to their insoluble glycerides.
REFERENCES
1 — "Oils, Fats, and Waxes," 5th Ed., Vol. II, p. 823.
2 — "Organic Analysis," Rev. Ed., p. 191.
3 — "Oils, Fats and Waxes," 5th Ed., Vol. II, p. 825.
4 — Ibid., p. 816.
5— J.Am. Chem. Soc, 21 (1899), 823.
6—Compl. rend.. 102 (1886), 1022.
7— Z. Nahr. Cenussm., 21 (1912), 457.
8— J.Am. Chem. Soc., 29 (1907), 32.
9— J.Agr. Res., 6 (1916), No. 3, 101.
10^Z. Nahr. Cenussm., 26 (1914), 2, 65.
11 — "The Chemistry of Foods," Vol. II, 14.
12— Ibid.
13— Chem.Abs.. 11 (1917), 1695.
14— This Journal, 9 (1917), 855.
15— Bull. soc. chim. belg., 25 (1911), 210.
16— Ibid.
Chemical Laboratory
Department of Health
City of New York
COMPARISON OF PERCENTAGES OF NITROGEN IN
TOPS AND ROOTS OF HEAD LETTUCE PLANTS
By H. A. NOYBS
Received March 27, 1918
In the investigations of the growth of head lettuce
in the greenhouse being conducted by the horticul-
tural department of the Purdue University Agricul-
tural Experiment Station, it has been found that the
plants grown on different soils and on the same soil
with different fertilizer treatments vary considera-
bly in their. nitrogen content. The reports of analyses
of the same species of plants show that the analyses
of a species are not constant but the variations found
622
THE JOURNAL OF INDUSTRIAL AND ENGINEERING < HEMISTRY Vol. 10, No. 8
Bank Sand
5"
^
*• * 5; * «
8anK Sand & Manure Mix
* s & I *
-4r> ^- 4? ^
Brown Silt loam
a
45%
$*§*■£$**■* €*.$?$«% €ct%^%^
in the preliminary investigation here reported were
so large that we are endeavoring at present to ascer-
tain the optimum analysis for the head lettuce plant.
SOILS USED AND FERTILIZER TREATMENTS GIVEN
i — Bank sand containing very little available plant
food.
2 — A mixture of bank sand and partially rotted
horse manure at the rate of 3 bu. of sand to 2 bu. of
manure.
3 — A brown silt loam which produces good crops
in the field.
The fertilizer materials used were partially rotted
horse manure, nitrate of soda (NaNO»), acid phos-
phate, and muriate of potash (KC1).
The following table gives the specific treatments
given the individual plots:
Table I
Aabreviation Treatment
Check Nothing
P Acid phosphate at rate of 400 lbs. per acre
N/3. P.. Sodium nitrate at rate of 133 lbs and acid phos-
phate at rate of 400 lbs. per acre
N. P/3 Sodium nitrate at rate of 400 lbs. and acid phos-
phate at rate of 133 lbs per acre
N 3, P, K Sodium nitrate at rate of 133 lbs .. acid phosphate
at rate of 400 lbs. and muriate of potash at rate
of 200 lbs per acre
N. K Sodium nitrate at rate of 400 lbs. and muriate of
potash at rate of 200 lbs. per acre
N Sodium nitrate at rate of 400 lbs. per acre
M, N/3, P. .. Manure -il rate ,>/ .'n tons, nitrate of soda at rate of
133 lbs . and acid phosphate at rate of 400 lbs.
per acre
M Manure at rate of 20 tons pel acre
The treatments given in the table were run on all
three soils, the only exception being that no manure
plots were run on the sand and manure mixture.
Head Lettuce Plant
VARIETY OF LETTUCE USED AND PERIOD OF GROWTH
The variety of lettuce grown was May King. The
plants were started in flats and transferred to the
greenhouse plots when about 3 in. in diameter. The
plots were harvested 10 weeks after setting in the
greenhouse when it appeared that they had matured
as much as they would under the treatments given.
SELECTION OF PLANTS FOR ANALYSIS AND THEIR PREP-
ARATION FOR ANALYSIS
Each plant was cut and weighed individually.
Those two plants which weighed nearest the average
weight for all the plants of each plot were selected
for the moisture and nitrogen determinations. The
roots of these two average plants were taken out,
washed, dried, and prepared for analysis.
The plants and roots were dried in bags hung just
over, but not touching, steam radiators. The air-
dry samples were ground to pass a sieve having holes
0.75 mm. in diameter.
The nitrogen determinations were made according
to the regular Kjeldahl method. The ammonia was
collected in N/5 acid and titrated with iV/10 sodium
hydroxide and methyl red as an indicator.
Table II gives the crop and nitrogen results, and
Graph 1 shows the nitrogen content of the roots and
tops by soils and fertilizer treatments.
Table II brings out the following:
(A) IN CONNECTION WITH THE AVERAGE WEIGHT OF
THE PLANTS GROWN ON THE DIFFERENT PLOTS I. The
brown silt loam grew the largest plants.
2 — The different fertilizer treatments gave effects
varying with the soil.
Aug., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
623
(B) IN CONNECTION WITH THE MOISTURE CONTENT
or the plants i. — The greatest variation in mois-
ture obtained was between 93 . 1 per cent on the brown
silt loam, with the manure treatment and 89.4 per
cent on the bank sand with nitrogen and potassium
treatment.
2 — The extreme variation in moisture on the bank
sand series was approximately three times that in
the silt loam series which in turn was one-half that in
the sand and manure series.
Table II — Crop and Nitrogen Results
Average
green wt.
per plant
Tops
56
Water Nitrogen in
in plants air-dry plants Ratio of per cent ]
Tops Tops Roots in roots to per
Percent Per cent Per cent cent N in tops
Check
P 58
N/3. P 64
N, P/3 59
N/3. P, K 59
N, K 63
N 74
M, N/3, P 87
M 84
Average 67
Variation 31
Check 75
P 112
N/3, P Ill
P, N/3 75
N/3, P, K 71
N. K 75
N 58
Average 82
Variation 54
Check 129
P 108
N/3. P 114
N, P/3 112
N/3, P, K 114
N, K 118
N 130
M, N/3, P 153
M 146
Average 125
Variation 45
89.5
89.5
90.6
90.3
90.3
89.4
90.6
92.4
91.8
90.5
3.0
1.02
1.05
1.05
0.84
1.06
1. 12
1.10
0.94
1.18
Bank Sand and Manure Mixtu
3.68
3.59
3.65
3.66
91.9
91.4
91.1
90.8
90.7
90.9
2.2
Brown Silt Loa
92.4
92.0
92.2
92.5
92.6
92.5
92.6
92.8
93.1
92.5
3.05
2.87
2.86
3.00
1.1
4. 12
3.78
3.83
3.46
3.75
3.85
3.75
0.66
100 to 235
100 to 164
100 to 207
100 to 196
100 to 212
100 to 194
100 to 236
100 to 222
100 to 203
100 to 208
100 to 121
100 to 125
100 to 127
100 to 122
100 to 132
100 to 115
100 to 105
100 to 121
100 to 122
100 to 134
100 to 139
100 to 128
100 to 122
100 to 119
100 to 141
100 to 182
100 to 140
100 to 136
63
(C) IN CONNECTION WITH THE NITROGEN CONTENT
of the plant (top) i. — The lowest average nitrogen
content was obtained on the bank sand series, namely,
2.16 per cent, and the highest was obtained on the
brown silt loam series, namely, 3.75 per cent.
2 — The fertilizer treatments varied the nitrogen
content most on the bank sand which was lowest in
plant food content and least on the bank sand and
manure mixture which was highest in plant food con-
tent.
3 — Phosphorus by itself lowered the nitrogen con-
tent of the plants on all three soils.
4 — Nitrogen by itself increased the nitrogen content
of the plants grown in the bank sand but decreased
the nitrogen content when used on the other two
soils.
5 — The effects of the phosphorus and nitrogen
when used jointly were different for each of the three
soils.
6 — The soil had a greater effect on the nitrogen
content of the plants (tops) than the fertilizer treat-
ment did.
(D) IN CONNECTION WITH THE NITROGEN CONTENT
of the roots i. — The lowest average per cent
nitrogen of roots was obtained in the bank sand series.
namely, 1.04 per cent, and the highest was obtained
in the sand and manure mixture series, namely, 2.97
per cent.
2 — The fertilizer treatments varied the per cent
nitrogen of the roots most in the brown silt loam
series and least in the bank sand series.
3 — Phosphorus by itself lowered the nitrogen con-
tent of the roots in the brown silt loam and sand and
manure series but raised it slightly in the bank sand
series.
4 — Nitrogen alone raised the nitrogen content of
the roots on the bank sand and the sand and manure
series but lowered it considerably on the brown silt
loam series.
S — The effects of the nitrogen and phosphorus
when used jointly were different for each of the three
soils.
6 — The soil had a greater effect on the nitrogen
content of the roots than the fertilizer treatments
did.
<*. & ,^
240
230
Graph .?— Thb Nitrockn Composition op thk Tops Comparkd to th
nltrogbn contbnt op thb roots (nltroobn composition op
Roots Taicbn as 100)
624
THE JOURNAL QF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 8
COMPARISON OF NITROGEN IN TOPS AND ROOTS
Graph 2 gives the ratio of the nitrogen in the roots
to that in the tops and shows the wide variation in
the nitrogen content of the tops in relation to that in
the roots.
1 — In the bank sand series the nitrogen in the tops
averages a little over twice that in the roots. On 6
out of the 9 plots there was over twice the per cent
of nitrogen in the tops that there was in the roots.
The 3 plots on which the nitrogen in the tops is far
removed from the average are the check plot, phos-
phorus plot, and the nitrogen plot.
2 — In the sand and manure series the nitrogen in
the tops averages approximately i'/s times that in
the roots. The only fertilizer treatment which is
widely divergent from the average is the nitrogen
(alone) plot.
3 — In the brown silt loam series the nitrogen in
tne tops averages a little over il/i times that in
the roots. Only one plot is widely divergent from
the rest, namely, the manure-nitrogen-phosphorus
plot.
4 — -Leaving out the plots that are widely divergent,
we have the following: 2.06 times the per cent nitro-
gen in the tops of plants grown in bank sand as
there is in the roots; 1.31 times the per cent nitro-
gen in the tops of plants grown in brown silt loam as
there is in the roots; 1.24 times the per cent nitrogen
in the tops of plants grown in brown silt loam as
there is in the roots.
SUMMARY
I — The nitrogen content of head lettuce plants
grown in different soils varies greatly.
II — Different fertilizers affect the nitrogen content
of head lettuce plants on the same soil.
Ill — The same fertilizer treatment affects the nitro-
gen content of plants grown on different soils in differ-
ent ways.
IV — Between the brown silt loam, which was in a
good state of fertility, and the bank sand, enriched
with manure, there was less difference between the
ratio of the nitrogen per cent of the roots to that in
the tops.
V 1 11 the bank sand and manure series where manure
was used at the rate of 2 bu. of manure to 3 bu. of
sand, fertilization varied the ratio of the per cent
nitrogen in the roots to that in the tops from 100 in
roots to 105 in tops, to 100 in roots to 132 in
tops.
VI — The per cent nitrogen in the tops of the head
Lettuce plant does not tend to bear a constant rela-
tion to that in the roots.
VII — With the per cent nitrogen in the roots taken
as ioo, the closest ratio obtained was 100 parts in
roots to 105 in the tops; the widest ratio was 100
parts in roots to 236 in the tops.
Acknowledgments are made to Mr. Lester Yoder and
Mr. Ira Baldwin for assistance in the analytical work.
Agricultural Experiment Station
I'ikdi.'i: University
J.apaybttb. Indiana
AN ANAEROBIC CULTURE VOLUMETER
By Zae Northri-p
Received May 18. 1918
During the past year, in studying qualitatively and
quantitatively the gas production in fruits and vege-
tables canned in tin and glass, several types of bac-
teria were isolated. It was desired not only to de-
termine whether these organisms were gas producers
and anaerobes, but also to determine with as much
accuracy as possible the composition and compara-
tive amounts of the gases evolved in pure culture
for purposes of comparison with the gas in the can
from which they were taken.
An apparatus was needed to fulfil these require-
ments which would furnish sufficient gas for anal-
ysis, simulate can conditions as nearly as possible, and
enable the gas evolved to be conducted directly to
the gas burette for analysis as had been done with the
gas collected from the blown cans.
After several preliminary experiments the appara-
tus illustrated was constructed and found to work
satisfactorily. One of the ideas in its construction
was that such an apparatus, to be of general use to
laboratories studying gas-producing organisms fin
canned goods especially), should consist of stock
laboratory equipment and not require the purchase
of special and costly apparatus, or the use of large
quantities of media. Another idea in its construc-
tion, which is mentioned above, was to imitate can
conditions by fostering anaerobiosis, ». e., the organ-
isms grow in this apparatus under anaerobic condi-
tions and produce gas, which collects under pressure
as in the can, and to imitate conditions in a glass-
covered glass can where pressure is not first evidenced
by a bulging top as is usual with the tin can or Mason
jar.
Dr. Wm. Mansfield Clark brought forth the objec-
tion to this apparatus that it did not give quantita-
tive results since the gases evolved, being under enor-
mous pressures, were partially dissolved in the liquid.
However, this same contention would hold true in
the study of gases direct from swells and as these
gases must be studied under the conditions under
which they are produced it seems as if Dr. Clark's
argument would not hold in this case.
METHODS OF USE
As will be noted in the accompanying illustration,
the materials necessary for the construction of the
anaerobic culture volumeter are a separatory funnel
with glass stopcock (Squibb's pear-shaped funnel
with graduations possesses some advantages over
other shapes), one-hole rubber stopper to fit, glass
stopcock and tubing, tall wide-mouthed bottle of
about 300 cc. capacity fitted with a two-hole rubber
stopper, a short piece of rubber tubing, and a small
Berkefeld filter.
Aug., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
625
The separatory funnel and connecting tubing are
first filled with the desired liquid culture medium.
Enough medium is also poured into the bottle so that
the level of the liquid is slightly over the top of the
filter. When the stopcock on the funnel is closed,
the medium remains in the separatory funnel, due to
atmospheric pressure.
For sterilizing the apparatus and the contained
medium, a piece of cotton is placed in the tube at the
top of the separatory funnel. The cock in the con-
necting tube is then closed and that at the top of the
funnel opened.
After sterilization, the cock in the separatory funnel
is closed and that in the connecting tube opened.
When the apparatus has cooled sufficiently the cock
in the connecting tube
is closed and that at
the top opened. The
inoculation is now
made by pipetting
into the stem of the
separatory funnel any
inoculated liquid med-
ium and if the medium
does not then reach
the stopcock, suffi-
cient sterile medium
is introduced to make
the funnel culture
anaerobic when the
cock is closed. After
this is accomplished
the cotton is replaced,-
the top cock closed,
and the lower cock
opened.
In the experiments
performed, the organ-
isms grew in the med-
ium in the separatory
funnel and produced
gas which forced the
liquid medium down
and out through the
Berkefeld filter into
the bottle; the cotton
plugged vent prevents
the development of
pressure in the bottle.
Contrary to expecta-
tions and much to
the advantage of the
experiment the organ- ■
isms did not grow
Anaerobic Culture Volumeter
through the filter for b— Coupling
several days thus al- c"B-'"ial fil««
D— Separatory funnel
F— Cotton
E— Glass tubing
lowing ample time for analysis of the gas formed.
The separatory funnel was connected up directly with
the gas burette after removing the cotton, and
the upper cock was opened very carefully as the gas
was under considerable pressure. Samples of gas were
drawn from time to time from the apparatus and
showed but little variation in composition quantita-
tively and qualitatively.
After the organisms grew through the filter, any
gas produced escaped through the vent, so this
culture could still be used for obtaining gas for anal-
ysis under practically the same conditions as before. On
the whole this apparatus has proved very satisfactory
for the purpose for which it was designed. I have been
aided in the perfection of this apparatus by Mr. G. I.
Blades, a senior horticultural student.
The suggestion has been made since that the Dore-
mus apparatus for quantitative extraction of gases
employed by Baker1 could be used in the study of
pure cultures by simply inoculating cans, sealing and
incubating them, instead of utilizing the apparatus
described above. Perhaps in many instances this idea
can be put in practice. I employed the Doremus
apparatus used by Baker, in the study of gases direct
from naturally formed "swells," previous to devising
the above apparatus and found it entirely satisfac-
tory in this respect, but for pure cultures it has the
following disadvantages: the large hole punctured by
the Doremus apparatus renders it exceedingly diffi-
cult to reseal without introducing either solder, HC1,
or foreign organisms. It was found necessary to cut
a little square tin, sterilize it, and solder it over the
opening when further cultivation was desired. If
the Doremus apparatus was constructed to punch a
smaller hole, this tube would become easily and quickly
clogged with seeds, skins, pulp, etc., of the food un-
der investigation.
Again, because of the use of pure cultures it would
be very undesirable to force water into the can through
the gas extraction apparatus as is suggested by Baker.
Water has been found to be an undesirable liquid
over which to collect gas from the cans on account of
its absorptive power. Mercury has been employed
in all our tests.
It is not easy to regulate the amount of gas taken
from the can when tin cans and the Doremus appara-
tus are used, in fact, immediately as the can is punc-
tured, all the gas escapes into the retaining bottle
before it is possible to control it. It is not possible
to tell whether all gas has been extracted and shut it
off, until the contents of the can reach the first glass
connection. This results in the contamination of the
connections and perhaps of the gas apparatus itself
with the organisms under study, and if these are spore-
formers this is an especially serious disadvantage.
The transparency of the glass is one of the biggest
arguments in its favor; another argument before men-
tioned is that it stimulates the conditions in the all-
glass can which is one of the most highly advocated
for the cold pack method.
Bacteriological Laboratories
Michigan State Agricultural College and Experiment Station
East Lansing. Michigan
I H. A. linker. "Apparatus for Quantitative Extraction of the Gases
in Canned Food Containers," Eighth International Congress 0/ Applied Chem-
ii.Ti on Hygiene, 18 ( 191 21. 4.1-44. 3 figs.
626
THE JOURNAL OF INDUSTRIAL AND ENGINEERING < HEMISTRY Vol. 10, No. 8
LABORATORY AND PLANT
AN ELECTRICAL CONDUCTIVITY RECORDER FOR
SALINITY MEASUREMENTS'
By E. E. Weibei. and A. L. Thukas
Received May 3, 1918
The electrical conductivity of brines and other salt
solutions varies with the degree of concentration. A
recording instrument might, therefore, be of value
where a continuous record of the density or concen-
tration of a solution is desired. Recently such an
instrument2 has been designed at the Bureau of Stand-
ards for obtaining a continuous record of sea water
salinity to a high degree of accuracy. A brief de-
scription of the method is given with the hope
thai it will be of value in its application to other
solutions.
DESCRIPTION OF METHOD
The method consists in measuring the ratio of the
resistance in two equal or nearly equal electrolytic
cells, A and B, Fig. I. One cell, A, is sealed and con-
tains an average sample of the solution to be meas-
ured, whose salinity or concentration is known. The
other cell, B, is open and has flowing through it the
solution to be measured. This ratio is obtained by
a W'ncatstone bridge using alternating current to
eliminate polarization effects in the cells. A calibra-
tion of the apparatus can be made at any time lo-
using solutions of known salinity in the open cell or
by carefully measuring the solution flowing through
the open cell by some accurate method. A record of
the resistance ratio of the two cells is made by a re-
corder similar to those now in use for measuring tem-
perature, but some changes will have to be made to
his recorder to the use of alternating current.
1 Published by permission of the Director of the liureau of Standards.
This publication is made without obtaining the consent of the senior author,
who recently lost his life ;it the front in Prance. The junior author has
added a paragraph "i new matter relating to solutions varying greatly in
resistance (Para. 4) and has suggested the application of the method to a
widei i in| . ,>i solutions tii. in sea water.
Weibei and Thuras, J. Wash. Acad. Sci.. 8. No. 6.
The new and important feature of the method is
the use of two cells containing liquids of nearly the
same properties which make it possible to compensate
almost entirely for the large temperature coefficient
of the solution. The two cells are placed in a uni-
form temperature bath and the only error introduced
is that due to the small differential temperature coeffi-
cient of the two solutions.
For very dilute solutions which may vary greatly
in resistance, as for instance distilled water contain-
ing traces of salt, the replacing of resistances C and D
by an open and closed cell, respectively, is recom-
mended. Then no matter how much the resistance
of the solution changes in the two open cells B and C,
the current through the two branches of the bridge
will be equal, and consequently if all of the cells are
geometrically equal the bridge will be completely
compensated for polarization. With high resistance
cells and high voltages the use of direct current on
such a bridge is suggested. This modification has also
the advantage of doubling the sensitivity of the
bridge.
MIASUREMEXTS OF SEA WATER
Preliminary experiments using sea water of differ-
ent concentrations showed that :
i — Good balances can be obtained with a simple
.Wheatstone bridge circuit containing the two electro-
lytic cells, using either a telephone at 500 cycles per
second or an alternating current galvanometer at 60
cycles per second.
• 2 — The temperature compensation is sufficient.
For the maximum difference in salinity in the two cells,
which is about o. 5 per cent, the lack of compensation
did not exceed 0.03 in salinity (0.03 g. of solids per
kg. of water) for a change of io° C.
3 Xo appreciable change in balance due to the
flow of the sea water through the open cell was ob-
tained.
4 — To obtain a continuous record of salinity an alter-
nating current galvanometer similar to the usual
direi I current galvanometer is needed to operate the
recorder. This galvanometer was constructed of the
electromagnetic moving coil type1 and has a sensi-
tivity and other operating constants as good as those
of the direct current galvanometers now used.
Aster these preliminary experiments had shown the
Lty of the method, a more careful study was
'i certain sources of error in order to obtain
data upon which to base the design of proper cells.
These effects are:
1 — Heating produced by the current in the cells.
Temperature lag of the sealed cell when the sea
water temperature in the bath suddenly changes.
3 — Time necessary for the resistance ratio to reach
its true value when the sea water passing through the
open cell changes in salinity.
1 E. E. Weibei. Bureau of Standards, Scientific Paper, *97 (1917), :J
Aug., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Consideration of these effects leads to the design
of specially constructed cells.
MULTIPLE TUBE CELLS
Each of the two cells, Fig. II, contains 6 parallel
glass tubes 14 cm. long and 1 cm. in diameter. These
tubes are joined at each end to bulbs containing an-
nular shaped platinum electrodes. Each electrode
has an area of 5.3 sq. cm. and is held rigidly in place
by 4 platinum pins which are welded to the electrode
and sealed into the glass wall of the cell. The cells
are designed so that there are no pockets in which
air can collect and the sea water is admitted in such
a manner as to sweep off any bubbles which might
collect on the electrodes. The inlet and outlet tubes
are sufficiently large to respond to the maximum change
in salinity.
RECORDER
In order to secure a continuous record of salinity or
concentration the Wheatstone bridge and galvanom-
eter must be embodied in a recorder mechanism
such as that developed by the Leeds and Northrup
Company. The electrical connections are as shown
in Fig. I. The most important changes in their pres-
ent recorder are due to the use of alternating current.
This current may be obtained from the usual 60-cycle
supply, but if only direct current is available then the
small direct current motor used for driving the re-
corder mechanism can be equipped with slip rings
and be operated as a converter. The recorder paper
should be ruled so that salinities can be read directly.
627
Side view
Fig. II — Electrolytic Cell
INSTALLATION AND OPERATION
The recorder should be properly mounted in some
convenient place and with insulated wires leading
from it to the cells. The cells. Fig. Ill, should be placed
close together in a bath through which water direct
from the solution continuously flows, or the cells may
be immersed directly in the solution if convenient.
This will insure a uniform temperature throughout
the bath. A flow of water, also taken dircci I
the solution, should be maintained through the open
cell. This flow must be broken as it leaves the open
Plan view
Fig. Ill — Connections of Bath
cell in order to eliminate the resistance error due to
shunting the cell.
S D U MARY
An apparatus is described to give a continuous
record of the salinity or density of a solution by the
measurement of its electrical conductivity. A pair
of electrolytic cells is described which, when used with
a suitable alternating current galvanometer, will give
satisfactory operation in connection with a recorder.
The temperature compensation is obtained by placing
both cells, which are in the two arms of a Wheatstone
bridge, in a uniform temperature bath or directly in
the solution which is to be measured. The applica-
tion of this method, with such modifications in details
of construction and arrangement as are necessary to
meet the needs of a particular case, is suggested for
the measurement of the salinity or concentration of
brines and other salt solutions and also many other
substances whose composition is constant throughout
changes in concentration.
Bureau op Standards
Washington. D. C.
AN ALINEMENT CHART FOR THE EVALUATION OF COAL
By A. F. Blake
Received April 16, 1918
Some time ago the writer published a description
of "A Graphic Chart for the Evaluation of Coal."'
which, to judge from 1 lie inquiries received regarding
it, has proved of value to a number of chemists and
engineers. As a result of a recent study of nomog-
raphy it has become evidenl thai the method of
charting can be very much improved by the substi-
tution ol alini incut principles for those of ordinary
i This Journal, 8 (1916), 1140.
628
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 8
EVALUATION OF COAL
r-(,S0
3
— 710
-6 40
2-7.0
-f50
3
3 . .. .
2-7 00
|-t90
— 610
3
3
r'»
~blO
2-MO
—too
|-6 to
3
3
— tso
— rjo
3
3 -,.
|-640
— XfO
5"'M
|*70
|-H0
3
— JtO
|-t.w
3
f-too
-i-jo
3
|-5"90
—S.10
3
2-f»0
=3
i
|-f70
3
2-fM
3 cS
-stio1-
|-J" 30
2-S40
— s.oo
3
3 .
XJ
d
§-S"30
—310
—4 90
3
3
4l
L.
|-3~I0
—480
3
-a
|-3T00
2-470 g
Q_
j-490
2-4M
~
s
5-4 JO
3
•o
a.
|-470
—4 SO
3
-440
Q.
2-460
|-4f0
2-4.30
-
2-440
3
£
3
2-430
—410
5 Ha
3
— 410
3
2-4.10
3 .
— 4oo
2-400
3 ,**
2-390
— 3 90
3
— 3»0
2-3.S0
2-J70
g-3.70
2-3 W
D
|lM
|-3fo
3
2-340
2-3.5-0
—3 30
2-3.40
3
—310
2-3.30
3
§-J/0
2- j 00
—110
F-3IO
E-30O
Direction* For Use,
By means of a straight line connect the price per
long ton on the left ans with the percent water on.
the inclined mi's. Note, the point of interjection witk
the "Cost per million Btb." mis. Connect this point with,
the ' % dry ajh. mmus standard V. dry ash. and note
the point of intersection on the left a»is Connect
this point with the B.tu per pound dry coal on. the
inclined aiis and read the required result on the
'Cost per million B.tu. ems.
£ i -§
analytical geometry. It may be stated as a general
rule that cross-section charts, though very useful for
the visual presentation of the relationship of different
variables, are not nearly as suitable as alinement
charts for the purposes of numerical calculation. The
latter are more compact and more easily read, are
entirely self-interpolating, and allow less opportunity
for error, since there is no necessity for projecting
points first vertically and then horizontally over con-
siderable distances.
The chart given here, like the one previously de-
scribed, is designed to determine the relative values
of different coals, given the price per ton and the chem-
ical analysis, by calculating the relative costs of a
8 J
million heat units in accordance with the methods
established by the United States Bureau of Mines.
The equations to be solved are as follows:
100 a
100 — b
f =
/ =
e +
(d—e)*
200
c — 0.02 (e-
1,000,000/
2,240 g
d)
T 100 a
l_ioo — I
+
(d—e)
K 1, 000, 000 1
1,240 < J
(1)
(2)
(3)
(4)
(5)
Aug., 1 918 THE JOURNAL OF INDUSTRIAL
[lOOa "I ri,000,00o"| / ..
- — 0.02 e- d)\\ (6)
100 — b J (_ 2,240 g J '
a = Price per long ton (in dollars) of the coal as
received.
b = Per cent water in coal as received.
c = Cost per long ton (in dollars) of the dry coal.
d = Per cent of ash on the dry basis.
e = Per cent ash selected as the standard-
/ = Cost per long ton (in dollars) of the dry coal
corrected for ash.
g = B. t. u. per lb. dry coal.
* = Cost per million B. t. u. (in dollars).
The theoretical considerations upon which these
equations are based are all discussed in the previous
paper. Equations 2 and 5 apply when the ash is
greater than standard and 3 and 6 when the ash is
(d — e)2 .
less than standard. is an algebraic expression
200
which, happens to represent almost exactly the price
deduction to be made for excess ash as given in the
tables of the Bureau of Mines Bulletins, and accounts
for the increased labor charges, diminished efficiency
of combustion, etc., resulting from high ash coal. The
values which the Government deducts from the price
per ton to be paid we add to the cost per ton. When
the ash is below standard a premium of 2 cents per
ton for each whole per cent less is paid. This ex-
plains Equation 3. Equation 5 is a combination of 1,
2 and 4, and Equation 6 of 1, 3 and 4.
The tedious arithmetical calculations which would
be required to solve these equations are all eliminated
by the use of the chart shown herewith. The directions
for use are given in the cut. To illustrate its use sup-
pose it is desired to know which of two coals, A or B,
is the more economical, the prices and analyses being
as follows:
a B
Price per long ton 4 . 54 $5.38
Percentwater 4.30 3.50
Per cent dry ash 10.40 6.00
B. t. u. per lb. dry coal 13,550 14.350
By means of a ruler, a drawing triangle, a fine silk thread, or
best of all a strip of celluloid with a straight line ruled on its
under side, connect 4.54 on the left-hand axis with 4.3 on
the inclined axis. The line intersects the "Price per dry ton"
axis at 4 . 74. If 6 is taken as the standard ash, this point, 4 . 74,
is then connected with 4 .4 on the lower part of the ash axis and
the line cuts the left-hand axis again at 4.84, the cost per dry
ton corrected for ash. This point is connected with 13,550 on
the inclined axis and the desired result, 0.1595, read at the in-
tersection with the "Cost per million B. t. u." axis. Proceeding
similarly with B, we obtain o. 1734 as the cost per million B. t. u.
A is therefore the cheaper coal and the extra price of B is greater
than justified by its better quality. Or, if it were desired to
know what price should be charged for B to have the heat cost
equal to that of A, we would start with 0.1595, the cost of a
million heat units in A, and work backwards on the analysis of
B obtaining $4.95. The intermediate values obtained, if not
interesting, need not be noted at all, the straight line being
merely pivoted over the point of intersection. The first
alinement solves Equation 1, the second either 2 or 3, and
the third 4.
AND ENGINEERING CHEMISTRY
629
This chart shows how even a very complicated
equation, such as 5, involving several multiplica-
tions and divisions, as well as additions, subtractions,
and a square can be readily and easily solved by a
properly constructed alinement chart. It is impossi-
ble in this paper to go into the mathematical details
governing the construction of the chart, but the reader
is referred to "A Manual of Chemical Nomography"
by Dr. Horace G. Deming1 for information which should
make the matter clear. The chart is, in fact, a sort
of adaptation of the calculating device known as the
nomon.2
Atlantic Sugar Refineries, Limited
St. John, N. B., Canada
NOTE ON THE USE OF THE DIPPING REFRACTOMETER
By Wyatt W. Randall
Received June 3, 1918
Experiments recently made in this laboratory seem
to the writer to justify the publication of a note of
warning to chemists who may have occasion to use the
dipping refractometer for exact determination of the
refractive properties of liquids, especially where the
latter are rather volatile.
Two samples of whiskey containing an unusually
low percentage of alcohol were under examination by
Mr. C. O. Miller. The density of each of the alcoholic
distillates having been determined with the aid of the
pycnometer, the refractometer reading at 20 ° C. was
made as a means of estimating the amount of methyl
alcohol, should any be present. In order to prevent
any inaccuracy of reading through evaporation of
alcohol, in each case the distillate was placed by Mr.
Miller in the metal cup secured by a bayonet joint
to the instrument. The readings gave a percentage-
of-alcohol-by-weight which differed notably from that
found by the use of the pycnometer, and which indi-
cated the presence in each distillate of about 1.25
per cent of methyl alcohol to 98.75 per cent of ethyl.
Similar results were obtained by two other chemists,
working independently. As the presence of methyl
alcohol in any noticeable amount in these whiskeys
was a matter of importance, all the distillations and
determinations were carefully repeated by Mr. Miller;
while the general results were the same, the figures
obtained were not as close as was considered necessary
in a case in which much was at stake. Accordingly,
the writer obtained fresh distillates, determined their
respective densities and refractometer readings, using,
however, in the latter work, glass beakers instead of
the motal cup, in the belief that evaporation would
play a very small part in the case of a 25 per cent
alcohol at 20 ° C. The beakers were of course corked
while they hung in the bath, and the corks were with-
drawn only when alcohol and refractometer prism were
both unquestionably at 200 C, that is, about after half
an hour's immersion in the bath. The readings gave
no evidence of the presence of methyl alcohol. The
original distillates were reexamined, this time using
• Unittrsity Press, Champaign. Illinois.
• J. Am. Chem. Soc, 39 (1917), 2137.
630
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 8
glass beakers and, again, no evidence of the presence
of methyl alcohol was obtained.
The only simple explanation of these differences is
that the temperature of the liquid in the metal cup was
distinctly higher than that of the bath. Accordingly,
the following experiments were made: The bath was
brought to, and maintained at, 200 C, according
to bath thermometer A (brass-jacketed, about 10
in. long and graduated in tenths of degrees). Com-
parison of A with thermometer B (not jacketed, about
4 in. long and graduated in fifths of degrees), while the
bulbs of both were in the bath, showed no noteworthy
differences.
I — An alcohol of about 22.75 Per cent by weight was
put in a glass beaker and also in the metal cup. Both
these vessels were then fitted with corks and placed
in the bath. After about 25 min. thermometer B
was inserted in each in turn, after the cork had been
withdrawn and readings obtained as follows:
Temperature of alcohol in glass beaker 20.02° C.
Temperature of alcohol in metal cup 20.03° C.
II — Readings made with the refractometer dipping
in the alcohol in the glass beaker were: 55.78, 55.80,
55-79, 55-79. 55-78, 55.79— Average, 55-788, which
corresponds to 22.75 per cent by weight.
Ill — Readings made with the alcohol in the metal
cup, following Zeiss filling directions, were: 55.40,
55.49, 55.47, 55-49, 55-50, 55.48— Average, 55-487,
which corresponds to 22.60 per cent by weight.
IV — Readings made with the alcohol in the metal
cup, the latter having been filled while off the re-
fractometer and then clamped on, were: 55.55, 55-52,
55-56, 55-54, 55-55 — Average, 55-543, which corre-
sponds to 22.62 per cent by weight.
V — After these readings had been made, the metal
cup was detached and the temperature of the alcohol
contained in it quickly read.
Temperature of bath, thermometer A 20.0° C.
Temperature of bath, thermometer B 20.0° C.
Temperature of alcohol, thermometer B. . . 20.5° C.
VI- Readings made with water in an open beaker
were: 14.65, 14.67, 14-67, 14-66. 14.67, 14.66 — Average,
14.663.
VII — Readings made with water in the metal cup,
filled as directed by Zeiss, were: 14.57. 14.56, 14.57,
14.58, 14-57, 14-58— Average, 14.572-
VIII After these readings had been made, the metal
cup was detached, and the temperature of the water
in it quickly determined.
Temperature of water in bath 20.0° C.
Temperature of water in cup 20.6° C.
The temperature difference in V appeared to be
alioui 0.5°, in YIII about o.6° C. I believe these are
distinctly too great. In the effort to maki
quickly. I do not believe time enough was given for
the liquid andthe thermometer to come to equilibrium.
Besides, the metal cup was probably somewhat warmed
iching from the refractometer, the quantity of
liquid was small, and the whole bulb of B was not im-
mersed; 1 believe, therefore, that about 0.40 or 0.450
would be nearer the true difference. The effect of a
0.50 C. difference in temperature was tried.
IX — Readings of alcohol in an open beaker at
20. 50 C. were: 55.40, 55.41, 55.40, 55.41, 55.41,
55.41 — Average, 55.407, which corresponds to 22.55
per cent by weight.
It thus appears that the low readings obtained when
the closed metal cup is used are due, at least chiefly,
to a difference in temperature between the water
of the bath and the liquid in the cup, and that a
similar difference in temperature does not exist when a
glass beaker is used instead of the metal cup.
It now became a matter of interest to learn under
what conditions the data were secured upon which
Leach and Lythgoe based their method for the detec-
tion and estimation of methyl alcohol in the presence
of ethyl. Inquiry of Dr. Lythgoe brought word that
glass beakers only had been used in their work.
The next question was, What is the cause of this
difference of temperature in the contents of the metal
cup, according as it is attached or not attached to the
refractometer? I was informed by Dr. W. J. A. Bliss
that, at the Johns Hopkins physical laboratory, Dr.
Pfund had found that, in standardizing a dipping
refractometer, complete accord in the readings could be
secured only when the temperature of the room was
close to that of the bath. This suggested that heat
was conducted by the metallic parts of the instrument
and of the cup to the contents of the cup. Accordingly,
Dr. Bliss and I made readings of the two thermometers
when the bath was only 1 ° to 1.5 ° colder than the air.
No effort was made to keep the bath at a fixed tem-
perature; B's readings in the water of the bath
averaged 0.07° higher than A's. In the liquid in the
metal cup, immediately after detaching it from the
refractometer, B's readings averaged 0.100 higher
than A's readings in the bath, which indicates that the
contents of the cup were, under these conditions, only
about 0.03 ° warmer than the surrounding water of the
bath.
Later, I cooled the bath to about 15° while the
room temperature was 27 °. B, hanging alongside the
cup, with the bottom of its bulb about a half inch
above the water of the bath, read 220. When placed
side-by-side in the water of the bath, A read 15.000,
B, 14.92 °. (Probably A's brass jacket was keeping
dings somewhat higher than B's.) The tem-
perature of the bath was slowly rising: when A read
15. 150, B, placed in the alcohol in the cup just after
it was detached, gave a reading of 15.650, quickly
falling to 15-50°.
These rather rough experiments seem to bear out
the conclusion that heat is conducted from the air
to the contents of the metal cup through the metal
parts of the instrument, and that the diffen
temperature between the contents of the metal cup
and the water of the bath is roughly proportional
to the difference between the air temperature and that
of the bath.
Laboratory of the
Statu of Maryland Department of Health
Baltimore. MARYLAND
Aug., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
631
DECANTING
By H. TauscK
Received January 10, 1918
The decanting of liquids from residues is generally
a very tedious operation. The time required for the
separation can be much abbreviated without me-
chanical means, if the tube simply is held in an in-
clined position, e. g., at an angle of 45 °. The liquid
will then form a channel in the upper part of the tube,
while the residue will go along the under part to the
bottom. In this way the two currents, upwards
anddownwards, will be separated from each other.
. Clear
nun / n 1 1 n j 1 n n 1 n 1 / n 1 / iiu/i) ) mi
The decanting operation can thus be finished in one-
third of the time required by the usual method of
using vertical tubes. It is common practice to use
narrow inclined tubes, etc., for obtaining a rapid de-
canting in liquids or for separating dust from air. The
same principle can, as shown, be of use in the laboratory.
The common tube holders ought to be slightly
modified for easy decanting in inclined tubes. The
modification is suggested in the diagram.
Aariius, Denmark
A DEVICE TO INSURE TIGHT CONNECTIONS BETWEEN
GLASS AND RUBBER TUBING
By C. C. Kipunger
Received April 17, 1918
In gas analysis trouble is experienced frequently
in the attempt to make tight connections between
glass and rubber tubing. Experience has shown that
this is accomplished best by wrapping a single turn
of wire about the joint and twisting tightly. However,
there are two objections to this method. The wire
tends, if twisted tightly, to cut the rubber, and if the
rubber tubing is appreciably over -size, the tubing is
■ compressed or pinched near the twisted portion of
the wire, frequently making a small channel through
which leakage occurs.
The device herewith described overcomes these diffi-
culties, permits the use of over-size rubber tubing, and
insures gas- and water-tight joints. It has been used
throughout the year with Liebig condensers and gas
apparatus and has given complete satisfaction. A is a
piece of stout wire bent in
U form of such size that the
limbs of the U will just
slip over both tubes. A loop
of stout cord is tied about
the connection, the wire
U is slipped through this .n---.
loop as shown in dotted lines,
the cord now twisted, using <-Xv^-- ■
the wire as a lever, and as
soon as the joint is tight, the
U is turned as shown at A.
Cord is better than the
usual copper wire for this
purpose in that the former distributes the force more
uniformly throughout its length.
A further advantage of this mode of attachment
lies in the ease with which it may be dismantled, re-
quiring as it does no pliers or other tools for this pur-
pose.
344 Harrison Avenue
Lexington, Kentucky
A SIMPLE AND ENTIRELY ADJUSTABLE RACK FOR
KJELDAHL DIGESTION FLASKS
By Frank E. Rice
Received March 11, 1918
The apparatus here described can be made by any
pipe fitter from standard pipe, and unions, and with-
out any specially prepared parts. It will be found
to cost much less than similar equipment on the
market. It takes up but little space when in use,
and its great flexibility in adjustment makes easily
possible still further contraction when it is not being
used.
A A' is an iron pipe in which are mounted burn-
ers, a, each with a stopcock. At the ends of this pipe
an- found stopcocks, h, for gas intake. This line is
adjustable up and down on standard B 1?', which is
in turn adjustable forward and back orj support C C.
An iron rod, D D', is adjustable up and down on
standard ER', which is also in turn adjustable Eoi
632
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 8
ward and back on C C Set-screws are used in up
and down adjustments, but are not necessary in for-
ward and back adjustments, provided the sliding
members fit the supports reasonably snug. Rings,
c, for supporting flasks are of iron and of the straight
stem type. They are attached to the rod D D'
with. fasteners, d.
IWELCiAHL RACK
F F' is a pipe with outlet in the rear to hood suc-
tion. Holes, e, are of sufficient diameter to admit
the mouths of digestion flasks and act as supports
for the same. This pipe should have a slight fall with
an opening at the lower end and drain, /, for carrying
off condensation acid.
Department of Chemistry
N. Y. State College of Agriculture, Cornell University
Ithaca. New York
RELATIVE VISCOSITY OF OILS AT ROOM TEMPER-
ATURE
By C. Frank Sammet
Received April 13, 1918
Oftentimes it is desirable to arrive at a relative ex-
pression for the viscosity of oils without having re-
course to the elaborate apparatus and means for de-
termining the absolute viscosity.
A rapid procedure which has proven satisfactory
for a relative determination is based on the time
of absorption of an oil when dropped upon blotting
paper under uniform conditions.
A piece of heavy weight blotting paper, about three
inches square and having a rapid absorption,1 is sup-
ported by a beaker so that the absorbing area is not
in contact with the support, as such contact would
interfere with the absorption. The oils to be com-
pared are brought to room temperature, then 0.5 cc.
of oil is withdrawn by a 1 cc. pipette, and allowed to
flow onto the blotter with the end of the pipette held
in the surface of the oil. The pipette is then with-
drawn after a few seconds draining, with a certain
amount of oil still remaining in the end by capillarity.
> Reed. Tins Journal. 10 (1918), 44.
This method of draining has given the most uniform
results.
The time of absorption in seconds is noted on the
stop watch from the first contact of the oil with the
blotter until the complete absorption has taken place,
It is plainly visible in reflected light,
which is essential that the comparison be made under
like conditions.
Blotters from the same package run very uniformly
if of high quality, but since the test is so easily made,
several results should be averaged.
If different pipettes are used for each oil, they should
have approximately the same time of delivery for
a given liquid.
When oils are too viscid at the temperature of com-
parison, they may be reduced in viscosity with a small
but definite volume of solvent, such as kerosene, or
with some other low viscosity oil.
Cranb & Company
Dalton, Mass.
AN ASPIRATOR
By J. M. JOHLIN
Received April 17, 1918
An aspirator which has been found convenient can
be easily made from a large bottle, a few rubber
stoppers, and a few pieces of glass tubing, as illus-
trated in the accompanying figure. Methods of
operating the aspirator suggest themselves.
Through the tube b the bottle B can be either filled
with water or emptied again. When the water can-
not be forced out by pressure but must be siphoned,
a rubber tube may be used as an
extension. Tube a serves as an in-
take or outlet for the gas. The
gas is displaced from B by allowing
a capillary stream of water to flow
into c from e. This arrangement
operates on the principle of a
constant-level water bath, the side
neck d carrying off any overflow.
The outlet of e should be small
or the stream of water will carry
air bubbles into the aspirator. The
outlet of a should be sufficiently
above c to prevent water from
flowing through it when all gas
has been displaced. The force of
the stream of water flowing into c
generates a pressure slightly greater
than that of the water column in c.
This type of apparatus is far less clumsy and less
top heavy than is the average form of aspirator; a
considerably increased pressure can be developed
without adding materially to the weight of the ap-
paratus or without decreasing its stability; operating
on the principle of the constant level bath, the aspira-
tor needs no attention during operation until all the
gas within the apparatus has been displaced.
Syracuse University
Syracuse, New York
Aug., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
633
PIPETTE USED IN TITRATION OF OILS FOR ACIDITY
By J. Jacobsen
Received April II, 1918
The use is as follows:
The rubber bulb is squeezed and the oil to be ex-
amined is sucked into the lower tube, which has a
capacity of 5. 5 cc, *. e., 5 g. of oil. The cock is turned
and the upper tube is filled with a suitable quantity,
for instance, 10 cc, of a mixture of ether and methyla-
ted spirit, conveniently taken from a tubulated bot-
tle, which is fixed just above the pipette. Then the
cock is turned again and the oil, followed by the ether-
alcohol mixture, is run into a flask and titrated with
alkali. In that way the lower tube is cleaned out
automatically and is at once ready for a new sample.
Aarbus Olibpabrix, Ltd.
Aarhus, Denmark
A SAFETY VALVE
By E. RlTTENHOCSB
Received December 17, 1917
The safety valve shown in the sketch has been
found very useful and may
be of interest to other
chemists. It is very easy
to make and quite reliable.
The valve is intended for
use in a distilling flask
when determining ammonia
by absorption in standard
acid solution. It will pre-
vent the acid from going
up into the flask by letting
air in and breaking the
vacuum. The valve is made
, .entirely of glass with a
UU/ler drop of mercury in the
bulb. It is very effective,
never sticking, always set.
The principle, namely, the
pressure due to a column
of mercury, can be adapted to all low-pressure work
■both above and below that of the atmosphere.
1822 So. Broad Street, Philadelphia
Mercery
A TEST FOR WOOL
By Harry LeB. Gray
Received May 4, 1918
The detection of wool in the presence of cellulose
fibers, in cases where the treatment has been such as
to destroy the characteristic appearance of wool and
Fig. I — Characteristic Appeai
Magn
Wool Fiber
= 100
after Treatment
where the fibers have bejn dyed in dark colors, is ex-
ceedingly difficult. In such cases the following
method of procedure has been found satisfactory.
iff fe;;- ^
r **€» v
% ^^P^*"i"^\^\3«* '
^9f~*
Ob
Ifl&rfPJfv
0^*
w:\K
^5? tiW'fiSVNM
V i
ftWr ^ri
J^"**!
^%
l
l^H/
Y&jsr I
*HK \> '
M
IK"**
^7] wy£v- i
. mm ^L
w
;•
ft
*<2
'vl^L
Fir.. II — Wool and Cellulose Fibers after Treatment
Magnification — 100
The fibers to be examined are placed on a micro-
scope slid;; and covered with two drops of a 30 per
634
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 8
cent sodium hydroxide solution. The slide is then
gently heated over a flame until vigorous boiling just
takes place, whereupon it is immediately removed
and examined under the microscope.
Wool fibers become greatly swollen, in some cases
partially dissolved, and present the appearance,
which is characteristic, of being full of cells or bubbles.
Undyed wool gives a dirty yellowish brown color.
Cotton and wood pulp fibers are unchanged except that
they become somewhat clearer and slightly shrunk.
Research Laboratory, Eastman Kodak Company
Rochester, N*. Y.
ADDRL55L5
GILMAN HALL: THE RESEARCH UNIT OF THE CHEM-
ISTRY GROUP AT THE UNIVERSITY OF CALIFORNIA
By Merle Randall
Received May 29, 1918
The department of chemistry at the University of California
is now housed in three separate buildings — Chemistry Hall, the
Freshman Laboratory, and Oilman Hall. The first is a ramb-
ling, vine-covered, red-brick structure, with a fine record of past
achievement; the second, a temporary wooden structure; and
the third, a massive, reenforced concrete monolith, built as a
part of the permanent University along the lines of the Hearst
plan.
The original building, Chemistry Hall, was built in 1890,
and various additions have been made to it from time to time.
The lecture rooms, museum, and the storeroom for all depart-
ments are located in this structure. The laboratories are now
used by the departments of organic and analytical chemistry
for both instruction and research.
In 191 2 a temporary, three-story, wooden building, known
as the Annex, was erected and, until the occupancy of Oilman
Hall, was used exclusively for graduate research in physical
chemistry. It is to be hoped that the research spirit, so well
nurtured in the little annex, will continue to grow in the new
quarters.
Another three-story wooden building, known as the Freshman
Laboratory, was built in 1914 for the purpose of accommodating
the general introductory course in inorganic chemistry and
qualitative analysis. This building is unique in that it is used
for the one course only. It contains storerooms, two dis-
tributing rooms, and eleven small laboratories, each of which
accommodates twenty-five students working simultaneously,
thus making room for a total of eleven hundred working in four
different sections. The capacity of each laboratory was limited
to twenty-five students in order that each instructor should
become intimately acquainted with his students.
In 1916-1917 Gilman Hall, the first wing of the new chemistry
F 1 R.5T F LOOR. PLAN
rm
"JU6 BAiLMLNT PLAN
dAJEMLNT PLAN
Fig.' I — First and Basement^ Floors. Oilman Hall
Aug., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
635
building, was erected. It was named in honor of Daniel Coit
Gilman, president of the University, 1872-1875, later president
of Johns Hopkins University, under whose administration the
College of Chemistry was organized. Gilman Hall is devoted
exclusively to research and instruction in physical and technical
chemistry.
GENERAL DESCRIPTION
Gilman Hall, with a ground area of 189 by 57 ft., is nominally
a two-story building (Figs. 1 and 2). There is an attic entirely
finished which is lighted by large dormer windows. The base-
ment is entirely above ground and under a portion of it is the sub-
basement, also above ground level. And beneath the sub-
basement is a small sub-sub-basement.
The walls, floors, and roof are heavy monolithic reenforced
concrete. The exterior is a cement plaster, the roof covered
with red tile. Much credit is due to the architect, Mr. John
Galen Howard, for the manner in which he has succeeded in
combining artistic composition, permanency, and chemical
usefulness.
The interior presents many features unusual in a permanent
building. Every square foot of floor space is utilized. Each
room was planned for a specific purpose, but at the same time
every effort was made to obtain a general uniformity of equip-
ment, thus admitting of change when necessary.
The interior wood trim of Oregon pine (Fig. 14) and the
cement base are arranged so as not to project beyond the plaster
line. Apparatus or tables can therefore be placed directly
against the wall without interference.
All piping and conduits are carried exposed on the ceilings.
In order to facilitate the future installation of additional or
temporary piping or equipment, metal inserts were placed in the
ceilings, and pipes l/s m- m diameter in the neutral plane of each
floor beam and girder. The concrete ceilings were left un-
plastered and then painted. A smooth finish was obtained by
oiling the forms before the concrete was poured. Several metal
sleeves with covers (Fig. 14) connect each room with those
above and below. Modified picture moulds (Fig. 14) permit
of fastening upon the walls without marring the plaster. Re-
movable wooden panels over the transoms and between the rooms
(Fig. 10) near the ceiling provide ready communication between
rooms on the same floor. A complete piping system can be in-
stalled to each room without cutting floors or walls.
Redwood panels (Fig. 11) are located in every room beneath
the electric power switches. Two styles of lockers (Fig. 14)
are used. The desk tops are, for the most part, sugar pine
finished in aniline black stain. Members of the laboratory are
permitted to fasten apparatus on any exposed woodwork, or
to the bench tops.
Alberene stone tops have been used in the technical rooms
and in the hoods (Fig. 16). Ventilation is by individual tile
flues directly to the roof. Over some spaces hanging glass
ventilating hoods (Figs. 6, 8, 10, ti) have been provided.
PIPING SYSTEM
In general, the piping systems are arranged to furnish five
different supplies, namely, gas, low-pressure air, suction, oxygen,
and water, available in each laboratory. The mains are in the
basement and second floor corridors (Fig. 3). The following
systems are installed:
JtCONO F LOOR. PLAN
ATTIC PLAN
Pio. ' \ tin ind Second Ploors. Gilman Hall
636
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. 8
GAS — 4 in. main from Pacific Gas and Electric Company.
water — 4 in. main from People's Water Company; 4 in. main
from University system, for fire protection, condensing water,
etc.
distilled water — Block tin line from special stills and 100
cu. ft. storage tank in Room 308 on upper floor.
high-pressure air at 85 lbs. pressure is supplied by a 7 in.
by 6 in., 50 cu. ft. per nun., Ingersoll Rolger, short belt, drive
compressor (Fig. 7), with 3 ft. by 8 ft. storage tank. This unit
is supplied with General Electric automatic control for starting
and stopping the motor.
low-pressure air is supplied through four reducing valves.
second-floor rooms by three-stage, oil-sealed Trimount pumps.
Glass vacuum cocks are used on these hihg vacuum lines.
Oxygen is stored in tanks at high pressure and supplied to
the line through reducing valves.
exhaust steam at 5 lbs. pressure is supplied for heating from
the University power house. A separate vacuum return line is
provided.
steam AT 30 lbs. pressure is also provided by the University
power house for experimental purposes, and for the stills, hot
closets, hot plates, etc.
steam at 250 lbs. pressure is supplied to a special line from
a small vertical oil-burning boiler located in the basement.
! s^.
jp >
gHaL'jS ^
1
'
m"
j*m j
i
I
w
K^32cf£*«L'— i.
Fig. 3 — Basement Corridor. Showing Val
Piping Systems
Fio. 4 — Cai
Rook
rER. Sheet Metal, and Plumbing Shop.
(Pattern Lathe and Scroll Saw
Not Shown)
Fio. 5 — Instrument Shop. Room 7. (Metal Saw, Drill Press,
and Rivett Lathe Not Shown)
Later a separate low pressure blower will be installed for use
when larger volumes of air arc required.
suction at from 20 to 25 in. vacuum is supplied from an
automatically controlled, 2 cylinder Packard vacuum pump
(Fig. 7).
HIGH vacuum is supplied to Rooms i, ioi, and 103 through a
lead line, by a Langmuir condensation pump, backed by a
General Electric, two stage, oil-sealed pump.
high vacuum ;it 0.001 mm mercury is supplied through a lead
line to the optical rooms on the attic floor, and to some of the
II
T-«
III
ri
n
■ —
1
1
r
5m«2ir *
OPil
i fan*;:
/m II "1
m& m
V
k#i
Fig. 6 — Glassblower's Shop. Room 210. (Mbrcury Still and
Vacuum Bench Not Shown)
condensing and cooling water, etc., is sent to the power
house through the 30 lb. steam return line.
circulating brine is furnished by a 2 h. p. brine circulating
pump from a 72 cu. ft. cooling tank.
liquid ammonia for cooling is supplied by a 4 in. by 4 in York
ammonia compressor (Fig. 7) equipped with automatic control.
A special section of the high vacuum room is reserved for use
of liquid ammonia from cylinders.
crude iti:i. on, and stove distillate lines are supplied by
Fess gear pumps from 150 gal. storage tanks outside the building.
Aug., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
63 7
ELECTRIC SYSTEM
The electric system is centralized in the feeder board (Fig. 9).
This board forms the partition between the electric furnace
laboratory and the motor generator room. Not all the electric
equipment is as yet installed.
4OOO VOLT, 60 CYCLE, 3 PHASE, STAR CONNECTED A. C is
brought to two oil switches from the University power house.
110—220 volt, three-wire d. c. is also supplied to a 300
ampere breaker by the power house.
44O VOLT, 60 CYCLE, 3 PHASE, DELTA CONNECTED A. C is
supplied through an oil switch from three 40 kv. amp., 2300 volt
of 220-440 volt primary transformers will be used for supply-
ing the furnaces.
no VOLT D. c. is generated by a 17.5 kw. motor generator
set with a Thrill regulator. This will be used for special work.
no volt D. c. is also generated by a 12.5 kw. motor
generator.
440 volt D. c. can be obtained by putting the above machines
in series with the 220 volt service from the university power
house.
6-12 VOLT D. C. is supplied by a 5 kw. double commutator
machine with no volt field excitation.
' — Cryogenic Laboratory. Sub-Basembnt. Air Compressor,
Liquid Air Plant. Suction Pump, and Ice Machine
(Note Floating Foundation)
Fig. 8 — Cryogenic Laboratory, Upper Portion. Rooms 1 1
Control Panels and Burdett Electrolytic Oxygen
Hydrogen Generators
Fig. 9 — Electric Furnace Laboratory. Room 19. Feeder Panel
(Unfinished) behind Which Are the Motor Generators
and Oil Switches
transformers located in the transformer room. This is used
for general power purposes.
220 volt, 3 phase, delta connected a. c. is obtained from
the above transformers.
IIO-22O VOLT, 60 CYCLE, THREE-WIRE, SINGLE PHASE A. C
for lighting and experimental power is supplied by a 30 kv. amp.,
2300 volt transformer.
220-440 VOLT, 60 CYCLE, 3 PHASE, DELTA CONNECTED OR
srNGLE phase for furnace work will be supplied from a bank of
three 100 kv. amp., 2300 volt transformers. The primaries of the
transformers are connected to a double throw switch so that the
bank can be thrown 3 phase, star, or in parallel on a single phase.
The secondary sections are brought to the board. Another set
Fig. 10 — Technical Electrochemical Laboratory, Room 119.
Main Distribution Board
12-24 volt d. c. will be supplied for furnace work by a 50
kw. double commutator machine.
A 100 CELL Edison storage BATTERY will be installed behind
the left end of the feeder panel.
By means of the distributing system any voltage on the feeder
board or in any part of the building is available on any other
board. The fields of the generators can be controlled from any
room. Only heavy currents are taken directly from the feeder
panel.
The main distribution board (Fig. 10) is in Room no directly
above the feeder board. From the fuses on this board 17 No.
6 wins run to each of the <> distribution boards. (RikI'I hand
portion of board, Fig. 10.) From the fuses on the distributing
638
TEE JOVRN l/- Of INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 8
C 1
pu'.jaii, ai
<> -fill
1 jW,
■^g?
board 7 No. 8 wires run to each of the room panels (Fig. 10), from
which two 2 -wire, 60 ampere and one 3-wire circuit can be used
at the same time. Ordinary no volt A. c. and D. c. may be
brought to the switches on the room panels by means of fuses
alone, but by moving these fuses to other positions and using
flexible leads, any other circuit may be connected to these
switches. By paralleling the circuits 180 amperes of a single
kind of current may be brought to the room panel. Means of
locking the fuses and plugs on the distribution board are provided.
AU machinery is individual motor-driven by 440 volt, 3
phase, A. c. motors, except the machines in the instrument and
glass-blowing shops which are driven by 220 volt D. c. motors.
SHOPS
Probably the most important feature of the laboratory is
the shops. Each of these is in charge of a full-time mechanic
with occasional assistance. These shops exist for the primary
purpose of constructing research apparatus and for aiding the
research men of this department.
The CARPENTER, SHEET METAL, AND PLUMBING SHOP (Fig. 4)
is equipped with a Wells pattern lathe, a Greenlee tilting saw-
table with boring and mortising attachments, a Porter 6 in.
jointer, a Beach tilting table scroll saw, a 32 in band saw,
sheet metal working tools, and a complete line of fittings and
tools for pipe as large as ; in. in diameter.
Fig. 12 — Main Technical Laboratory, Room 121. Piping Systems
and Suspended Balcony
The instrument shop (Fig. 5) has an 8 in. Rivett lathe com-
plete, an 8 in. Stark lathe, a 12 in. Seneca Falls lathe, a Robbins
and Myers buffer and grinder, a Cincinnati universal tort
grinder, a Browne and Sharpe 2A milling machine, a 20 in.
Barnes drill, a Sigourney sensitive drill, a Canedy-Otto drill,
a Grabo metal saw table, an oxyhydrogen welding equipment, a
2 ton travelling Peerless hoist, and a large number of small
tools and stock. A 14 in. Hendey lathe and a 20 in. Lodge and
Shipley lathe are contemplated.
The glass-blower's shop (Fig. 6) has various blow torches
for glass and quartz and machines for grinding and polishing.
In an adjoining room is a very complete stock of stopcocks, and
about 3000 lbs. stock of soda, lead, pyrex and quartz glass
tubing of all sizes.
the students' shop — Members of the laboratory do not,
except in special cases with the permission of the mechanics
in charge, use the above shops. They may, however, make free
use of the students' shop. Room 20, which is equipped with a
limited amount of machinery and hand tools.
LIBRARY, STUDIES, ETC.
The University fortunately possesses a very complete library,
and a large number of the books relating to chemistry are shelved
in the chemistry department library, Room 109. Books
may be taken, without formality, to the library annex. Room 105,
Fig. H — Office anc
F10. 1J — Skmii
Aug., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
639
where there are tables and blackboards, and where violent and
heated scientific discussions may take place without disturbing
the readers. A study for the men, Room 320, and one for the
women, Room 302, are also provided.
The seminar room (Fig. 13) is arranged for small discussions
or faculty meetings around the central table, but its capacity
may be increased to about 60 people without losing much of
the congenial atmosphere of the small seminar. Discussion is
encouraged by easy access to blackboards which line the walls
of the room.
Fig. 15 — Potentiometer
Calorimeter Laboratory. Room 2
A small lecture room, Room 219, with seats for 60 people,
is used for the courses in advanced physical and technical
chemistry.
The drafting room, Room 304, is equipped with cross-sec-
tion paper, drawing tables, and instruments. A glass top
table illuminated from below is a special feature.
THE laboratories
CONSTANT TEMPERATURE ROOM — A pit 1 4 ft. by 1 4 ft. and 10
ft. in depth is located under a portion of the sub-basement.
A trap door in the ceiling and traps in the various floors above
provide for a clear height of about 70 ft. for experimental pur-
poses. The walls are heavily reenforced so that dangerous
apparatus may be operated in this room. Since the room is
underground and there is no access to it except through the
trap in the ceiling very uniform temperatures can be maintained.
The cryogenic or low-temperature laboratory (Figs. 7
and 8) occupies the sub-basement and Rooms 1 and 3 of the
basement. The compressors and heavy moving machinery rest
upon a floating foundation. This foundation consists of a 10-
in. slab of reenforced concrete floating on 6 in. of dry sand and
isolated from the rest of the building by a 2 in. sand joint (see
foreground Fig. 7). With all the machinery in motion the
laboratories are so completely free from vibration that the most
sensitive galvanometers may be mounted directly on the walls
(Fig. 15). The motor generator sets, Room 15, are mounted on a
similar floating foundation.
The liquid air plant at present consists of a new 20 h. p., 4
stage, Norwalk compressor and Brin liqueficr. A modern,
high-efficiency, liquid air plant is planned for this laboratory and
the present compressor will be used for the production of liquid
hydrogen. A liquid helium plant is also planned. Two standard
commercial units of Burdett electrolytic oxygen-hydrogen
generators for the production of pure gases are installed. The
liquefiers are on the floor above the compressors, which are
visible through a 10 ft. by 10 ft. opening in the floor. Ample
space and facilities for research at low temperatures are pro-
vided.
The potentiometer and calorimeter laboratory (Fig. 15)
adjoins the cryogenic laboratory and contains large oil thermo-
stats and suitable high-resistance potentiometers permanently
installed for the measurement of electrode potentials. A
potentiometer sensitive to 0.000,000,01 volt and free from
parasitic e. m. f.'s., and several 50-junction thermo-elements and
twin calorimeters are in use. A second potentiometer of like
characteristics is being installed.
cold room — Certain experiments cannot be carried out in
the open air since the temperature in Berkeley is never below
freezing. One-half of one of the small research rooms in the
basement (Room 4) is therefore used as an ice box and provided
with direct ammonia expansion coils. A standard laboratory
desk and the usual laboratory piping and electrical service,
with the exception of water, are available.
The high vacuum laboratory, Room 101, is provided with a
series of 8 low benches, 6 ft. long, 18 in. wide and 18 in. high,
at the back of which is a framework of '/: in. steel rods upon
which complicated glass apparatus may be conveniently mounted
(Fig. 14). These benches are arranged end-on on each side
of a central bench upon which is the usual laboratory piping and,
in addition, 0.001 mm. of mercury vacuum.
The physical chemical laboratory (Fig. 16) has space for
42 students. Five thermostats will be installed in this room.
A special research laboratory (Room 205) is provided for
seniors doing advanced physical chemistry and researches which
do not require large complicated apparatus.
A large number of small rooms are devoted to special purposes.
Of these the polariscope room, No. 303, the spectrophotometer
room, No. 305, the conductivity room, No. 311, and the high
frequency conductivity room, No. 313, deserve special mention.
A separate, well ventilated room, No. 316, is provided for work
involving dangerous or unpleasant gases. Metallographic and
photochemical laboratories. Rooms 322 and 301, are being
equipped. There are two large dark rooms. A 60 ft. optical
path is available in Rooms 303-313.
Thermostats
For the most part offices and private research laboratories
have been combined. There are a large number of these, Room
103 (Fig. 14) being a typical example.
Tin- analysis room, No. 209, is equipped as a general anal) deal
laboratory with electrolytic bench and other analytical con-
veniences. It is not intended for instruction, and it is probable
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THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 8
that a full-time analyst will be put in charge, who will do routine
analysis connected with the various researches, prepare solutions,
etc.
Small balance rooms which can be kept free from moisture,
carbon dioxide, etc., open off the analysis room.
The combustion laboratory, Room 213, adjoins the analysis
room. It is equipped with organic and carbon combustion
trains, multiple unit electric tube, crucible, and muffle furnaces.
The organic laboratory. Room 222, is fitted with a Kjel-
dahl rack, thermostats, and the general equipment of an organic
laboratory. This laboratory is not connected with the organic
department but is for the convenience of those who need to do
organic synthesis, etc., incidental to theoretical and technical
researches.
TECHNICAL LABORATORIES
The TECHNICAL LABORATORIES, Rooms 21, 22, 121, and 221,
form in effect a four-story factory. The upper room is equipped
for the analytical control of technical operations, the factory
laboratory, and a part of the room is reserved for large apparatus.
The main room (Fig. 12) contains a steam table, a drying closet,
a large shelf dryer, 8 in. and 15 in. International basket centri-
fuges, a large International centrifuge, two 250-lb., 50-gal.
jacketed autoclaves, two 2-gal. autoclaves, combination column
still, extractor, condensers, etc., Kestner type evaporator, a
500-gal. tank, 5-gal. and 25-gal. jacketed cast iron kettles with
extension pieces and covers. The kettles fhay be combined to
make such pieces as vacuum pans, vacuum agitators, vacuum
crystallizing evaporators with or without agitation, nitrators,
sulfonators, etc. This equipment is being added to very rapidly.
The heavy technical rooms, Nos. 21 and 22, contain a steam
boiler, a cement kiln, a suction filter, a filter press and grind-
ing machinery.
The electrochemical laboratory has been already partly
described. Operations are worked out on a small scale in Room
119 (Fig. 10), and on a larger scale in Room 19 (Fig. 9). This
room is provided with a traveling 2-ton Peerless hoist. A large
stock of electrodes, refractories, and materials for furnace con-
struction are carried in Room 1 1 . The steel has been omitted
from the floor in order to diminish eddy current losses. The
furnace laboratory houses several gas and oil furnaces and a
Herreshoff mechanical pyrites burner with six 24-in. hearths.
STORES
Stores are distributed from Rooms 214 and 216. Only a
small number of instruments of general use are here. Most
of the apparatus is stored in apparatus closets built in the labora-
tory in which it is most often used. A large room, No. 32i,ispro-
vided for large set-ups temporarily out of use. AU apparatus
and stores are catalogued by the number of the room, a section
letter, and shelf number. This number appears on the ap-
paratus, and a tag giving the temporary location is left in the
permanent location when the instruments, etc., are in use. It
is the policy of the laboratory to keep all apparatus in use, and
easily available day or night.
In this brief outline only those features which are unique in
laboratory construction and equipment have been described.
The accompanying photographs are designed to show certain
of the rooms as they appear under actual working conditions.
University op California
Bbrkslby
DYEING OF KHAKI IN THE UNITED STATES'
HISTORICAL AND THEORETICAL
By John >.'. HSBDBN
The khaki-dyed fabrics are used almost wholly for military
purposes. The use of this color for uniforms had its origin
in the Boer War. The peculiar shade of the terrain of South
1 Address delivered before the New York Section, Society of Chemical
Industry, May 24. 1918.
Africa made it possible to conceal the presence of troops from the
enemy by adopting a shade for uniforms which blended with the
color of the landscape. Military observers, noting the effect
of the use of this kind of uniform, gave their attention to its de-
velopment in other countries.
The history of the dyeing of khaki is spread through the
literature, and really originates in the first patents taken out by
Gatty in Great Britain in 1884. It was not, however, until
1897 that the development of this color was taken up seriously.
The British dye houses then began to give particular attention
to the production of this color, both on cotton and wool.
At about the year 1900 the American Government took up
the use of khaki-colored fabrics for the manufacture of tents,
kits, and uniforms. From that time there has been a steady
development in the improvement of both the shade and quality
of the fabrics. The early shades of khaki used by the American
Government were comparatively light and of a greenish yellow
tone. This shade was changed to a darker and more yellow
brownish khaki. As the German field gray came into use, our
Government adopted what is now known as the olive-drab.
At the present time the three shades of khaki seem to be in use.
When the use of khaki was taken up by the American Army,
our soldiers were clothed in uniforms made from woolen fabrics.
Although the quality of the wool used was the best, such fabrics,
in order to have strength, were of necessity heavy. Mr. T. B.
Owen, between the years 1900 and 1902, while he was acting as
superintendent of the Atlantic Mills in Providence, R. I., called
to the attention of the Quartermaster's Department the supe-
riority of worsted fabrics or worsted serges, particularly for the
manufacture of blouses and shirts. These fabrics were tried
by the Army and found to be superior to the woolen fabrics.
To-day there is scarcely any woolen fabric used, except for
blankets and overcoats.
Khaki is usually dyed on cotton or wool. The production
of a khaki shade on silk is required so infrequently that methods
for producing this color on this fiber need not be discussed.
The dyeing of khaki both on cotton and wool may be classed
under the following methods:
1 — Chemical or oxidation methods for both cotton and wool.
2 — Mordant dyeing methods, particularly for dyeing wool.
3 — -After-chroming methods, or one-bath chrome methods,
for wool.
4 — Direct or substantive dye methods, with or without after-
treatment, particularly for cotton, but also applicable to wool.
5 — Sulfur color dyeing methods for cotton.
6 — Vat color dyeing methods for cotton.
The chemical or oxidation method generally used for dyeing
cotton cloths or yarns for khaki-colored fabrics, for use in uni-
forms, tents, and kits, is based upon the production in and on the
fiber of a mixture of the oxides of iron and chromium. Before
the shades thus produced were used for military purposes
particularly, these dyes were usually designated as iron buffs.
The browns produced by the use of salts of manganese, usually
called manganese bister, are too deep and too red to be used as
khaki shades or as the basis for khaki colors.
In the production of khaki by this method, the cloth is padded
or saturated with a mixture of iron and chromium salts, and then,
either with or without ageing, is passed into a solution of an
alkali in order to precipitate the mixture of iron and chromium
oxides in and on the fiber. An alternative method is to pad
or saturate the cloth, dry at a low temperature, age in an ageing
machine, and then pass into a solution of alkali in order to
precipitate the oxides and produce the khaki color on the fiber.
In tin- padding or precipitating method, when the padded or
saturated goods are not dried, it is necessary to make several
passages of the fabric through the solutions of the salts of iron
and chromium, and through the alkaline solution. When the
method in which the cloth is padded, dried, and aged before
Aug., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
64 1
treatment with alkali is used, it is rarely necessary to make
more than one passage through the different solutions. Thus
it will be seen that while it is necessary to have special ma-
chinery and equipment in order to dye khaki by the short
method, it is more economical and the shade of color can be
more easily controlled. The first method described may rightly
be termed the wet method, and the second the drying
method.
The following recipe may be given as an illustration of the
wet method :
75 lba chrome alum are dissolved in
25 gal. water. To this solution are added
5 qts. commercial nitrate of iron, 90° Tw.
5 qts. commercial pyrolignite of iron, 25° Tw.
The goods are first thoroughly boiled out, or half or full
bleached, as may be required for the particular fabric. They
are then padded in the above solution, so that the fabric is
thoroughly saturated. After padding, the goods are passed
through a boiling solution containing 6 ozs. of calcined carbonate
of soda per gal. The passage through the iron and chrome
salt solution, followed by the passage through the alkaline solu-
tion, may be repeated 4 or 6 times before a full shade of khaki
is produced. After the depth of shade required is obtained, the
goods are thoroughly washed to remove excess of alkali and to
prepare them for any after-treatment required.
To produce a khaki color by the drying method, the following
recipe will serve as an illustration:
10 gal. acetate of chrome, 32° Tw.
5 gals, pyrolignite of iron, 20° Tw.
10 gals, water are mixed together
The goods are padded in this solution, and dried at a low
temperature. The goods may then either be passed through a
boiling solution of carbonated soda or passed through an ageing
machine after drying, and then through a boiling solution of
carbonate of soda. One passage through the solution of chrome
and iron acetates will produce a full or medium shade of khaki.
It is rarely necessary to make two passages through the acetate
solution.
Many modifications of the typical recipes given above have
been used. These modifications have been attempted principally
to modify the shade, *. e., to make a color more olive in tone,
and also to increase the fastness of the color produced to the
chemical tests to which the fabric is subjected after dyeing.
Thus, attempts have been made to add other salts than the salts
of chromium and iron to the bath, with the idea of increasing
the fastness to acids. None of these attempts, however, have been
particularly successful, so that it is safe to say that the chemical
or oxidation khaki on cotton cloth or cotton yarn is produced
by the use of a mixture of iron and chromium salts. It is to be
noted, however, that goods dyed with acetate of iron, or with
iron salts other than the pyrolignite, are liable to become tender
in storing. This is due to the gradual oxidizing and deoxidizing
of the iron oxides formed in the dyeing process, this oxidizing
process being accelerated apparently by the cotton fiber. When
pyrolignite of iron is used, the impurities contained in this
product seem to have a modifying action upon the oxidation
process and less tendering is observed.
Khaki colors when dyed by either of the above methods or
modifications of these methods are not particularly fast to acids,
and do not meet the tests in this respect required by the military
authorities. The colors, however, are very fast to light, scour-
ing, washing, and the ordinary treatments to which the fabrics
are subjected.
Many attempts to render the khaki-dyed fabrics, when dyed
by the iron and chromium method, fast to acid, have been
proposed. These methods consist in after-treating the dyed
fabrics- with various salts or acids, as, for instance, copper salts,
boracic acid, tungstates, etc. None of these methods have
produced a fabric which would meet the tests. The only method
thus far published which will produce an iron and chromium
khaki fast to acid is the one patented by Gatty, which con-
sists in treating the steamed goods with a solution of silicate
of soda.
Very fast bronze colors are produced on cotton by oxidizing
on the fiber meta-phenylene or meta-tolylene diamine. A
typical recipe for producing these so-called fast bisters or browns
is the following:
1 lb. phenylene diamine hydrochlorate or acetate
'A lb. chlorate of soda
t/i lb. yellow prussiate of soda
are dissolved in one gallon of water
Pad the well-boiled or bleached goods through this solution,
dry at a low temperature, pass through the ager, wash and
soap. The color may be modified by making various additions
of oxidizing agents to the solution, or by adding various bases,
as, for instance, alpha-naphthylamine, aniline salt, diamido-
diphenylamine, sulfocyanate of ammonia, or even salts of iron
and other compounds, which will produce dyes on the cotton
fiber by the above oxidation method.
These colors, although remarkable for their fastness to light,
scouring, and acids, have not been produced successfully in a
large way, owing to the fact that the padding solution is con-
stantly oxidizing and changing in composition. The color is
thus produced in the solution before the fabric is wetted, and
dried. In the case of phenylene diamine, the oxidation is so
rapid that in order to obtain results it is necessary to make up
the various solutions of ingredients separately, and mix these
solutions together in the proper proportion as they are fed into
the padding machine. This involves so much care and attention
that the process does not seem to be suited to our manufacturing
conditions. The author has made many attempts to overcome
the oxidizing action in the solution, but thus far there seems to
have been no method devised which will make it possible to
make a comparatively permanent solution, as is the case in the
solution used in dyeing aniline black by this same method.
We may safely say that the iron-chromium method for dyeing
khaki on cotton is the only chemical or oxidation method in
practical use. For the dyeing of khaki, however, on wool, both
the iron-chrome method and the diamine method have been
used very successfully.
The dyeing of khaki colors on wool or worsted yarn or tops,
with a combination of iron, chromium, and manganese salts was
worked out at the Atlantic Mills in Providence, R. I., in the
years 1900 and 1902, by Mr. Herbert Fulsom, who was then
chemist for the company. The details of the process were not
made public. Mr. Fulsom succeeded in producing a color
which was free from the harsh feel usually produced in mordant-
ing wool with iron. This permitted the wool dyed after his
method to be drawn and spun in the usual manner, and to
produce yarns of excellent quality. The color was extremely
fast to light, washing, and scouring, but was not remarkably
fast to acid treatment. Its fastness in this respect, however,
was sufficient to meet the Government test. The shade of
khaki in vogue at that time was much lighter than the dark
shade used at the present time. It would hardly have been
possible to have produced as deep a color as is required by this
method. Furthermore, it is not possible to produce the olive-
drab by this method.
In 1903 and 1904, the author produced at the Peacedale
Manufacturing Co., Peacedale, R. I., an oxidation khaki
based on the diamine method. This color is remarkable for its
fastness to light, scouring, fulling, acids, reducing agents, and
rubbing. The maximum shade produced by this method is too
light to match the shade of khaki now in vogue. When darker
shades of color than the shade used at that time were attempted,
this method failed. The process, however, can be used on tops,
642
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. 8
yarns, or piece goods; the shades produced are remarkable in
that they are level and uniform The fiber is particularly
soft, and spins practically as well as white wool. The method
used is as follows:
For 450 lbs. worsted tops: Add to the dye bath the following
products in the following order:
5 lbs. meta-tolylene diamine dissolved in
6 gals, acetic acid. No. 8
After the addition, enter the goods into this bath, keeping the
temperature at about 1200 F., and work the goods for 15 to 20
min. to allow the liber to take up the diamine. Lift the goods,
and then add the following solution:
7 '/i lbs. ferric chloride
18 lbs. chromium chloride or fluoride
Bring the bath to the boil, and work in the boiling bath until
the shade is produced. The goods are then thoroughly washed,
and need no subsequent treatment to prepare them for the
spinning operations. The khaki thus produced is the fastest for
the depth of shade of any of the dyes known to date.
Before discussing the mordant dyeing after chroming, one
bath chrome, and the direct dye methods for the production of
khaki shades, let us consider the relation of fastness to scouring
and alkali to the chemical constitution of dyestulTs in general.
From a careful study it will be seen that the fastness to scour-
ing and alkali depends upon the chemical constitution of the dye
molecule, and upon the nature or chemical reactivity of the
elements or molecules substituted in the nucleus or nuclei of
this molecule. The substitution of halogen, nitro groups,
amido groups, sulfo groups, hydroxyl, carboxyl, and other
groups, not only react as chromophobe radicals, but modify the
chemical reactivity of the dye molecule. These substituted
groups thus determine the dyeing properties of the compounds,
the fastness of the colors produced to scouring and alkali, and
also modify the shade due to their chromophoric character.
From a study of these substitutions in the molecule, the dyeing
properties and fastness to scouring and alkali can be predicted.
Generally speaking, a dyestuff, in order to be applied to the
fiber, must be soluble in water. This solubility is generally
dependent upon the substitution in the molecule of a sulfo,
hydroxyl, or carboxyl group. If these groups be present and
ari ""< in the ortho position, the solubility of the dyestuff, even
,,lt,i being dyed upon a mordant or fixed by after-treatment,
ufficicnt to render the color not fast to scouring. There
is a class of colors containing an amido group in the molecule
which, after the dye is fixed upon the fiber, can be diazoti/ed
and developed, as it is termed. If there are too many sulfo,
carboxyl, or hydroxyl groups in the molecule, the color pro-
duced, even after developing, is not fast to scouring. The fast-
ness to scouring and alkali is decreased in proportion to the
increase in the number of these groups substituted in the dye
molecule.
Colors fast to scouring and alkali cannot be produced unless
those groups which arc- capable of dyeing upon a mordant, or
being after treated after the dye is fixed upon the fiber, are
present in the molecule and are in such a position one to the
other, that definite compounds can be produced by combining
with the mordant or by the aftei treatment The sulfo groups
of a dye molecule cannot be treated by any reagent now known.
which will under them fast to scouring or alkali. Neither can
Hi hydroxy! or the carboxyl groups be treated and made in-
soluble unless they be in the ortho position one to the other.
Thus, two hydroxy! groups, one hydroxyl and one carboxyl
group, and certain hydroxy azo groups, when in the ortho
. determine the property of fastness to water and scour-
ing when the dyestufi i-; either deed upon a mordant "i aftei
treated with a compound "inch will render the color insoluble.
Kostauecki showed that the propertj ol dyt in : on ,1 mordant,
possessed by certain color acids, was due to the fact that those
color acids which dye on a mordant, have either two hydroxyl
groups in the ortho position in the molecule, or a hydroxyl
and a carboxyl group in the ortbo position, or that the com-
pound was an orthonitroso, or orthoquinone oxime. When the
dyemg method now known as the after-chroming method was
studied and analyzed with reference to the chemical constitution
of the dye-stuffs, it was found that the ortho position was the
determining factor. Thus, orthodihydroxy, peridihydroxy,
orthohydroxycarboxy, and certain orthohydroxyazo dyes were
all not only modified in color, or developed in shade by after-
treating the dyed fiber with bichromate or by dyeing with
chromate or chrome salts, but they all had distinct mordant
dyeing properties following the Kostanecki rule.
Not all fives, however, which meet the requirements of the
Kostanecki rule, or those which may be after-treated, are fast
to scouring. This lack of fastness is due to the modifying in-
fluence on the solubility of the dye, of the groups substituted
in the molecule other than those which give the dye the mordant
dyeing or after-chroming property. These substituted groups
have sufficient influence upon the solubility of the after-treated
or mordant-dyed color, to render the dye produced not fast to
scouring and alkali.
To illustrate these facts, a few concrete examples may be cited
in order to show the relation of dye constitution to the production
of fast khaki shades.
Alizarine is an orthodihydroxy anthraquinone, the hydroxy
groups being in the 1,2 positions. The Turkey red produced
by the use of true alizarine is the fastest red to boiling and
bleaching. The scarlet reds made from anthrapurpurine and
flavopurpurine, as well as the red made from purpurine, are
not as fast as true alizarine red made from alizarine. This lack
of fastness is due to the presence in the molecule of a third
hydroxy group. This group readily unites with any alkali,
rendering the lakes formed with the mordant soluble. True
alizarine, not having this third hydroxy group, is practically
insoluble. Those alizarine blues which are penta- and hexa-
hydroxyanthraquinones are not as fast to scouring as alizarine,
because all of these dyes have a hydroxy group whicti can react
as does the hydroxy group in anthraflavine or flavopurpurine.
Sulfo, nitro, and carboxyl groups can react in the
same way as does the hydroxy group when not in the
ortho position. Colors containing these groups are invariably
not fast to scouring or alkali unless the sulfonic acid nitro com-
pound, or other compound, in which the group is substituted,
is of itself difficultly soluble. An increase in the number of
these groups in the dyestuff molecule generally produces very
soluble compounds, and therefore the colors produced therefrom
are not fast to scouring and alkali.
The mordant dyeing methods require two operations: First,
the mordanting proper ; second, the dyeing. For the production
of khaki shades there are really only two mordants which may
be considered, viz., the chrome and titanium mordants. Iron,
nickel, cobalt, and aluminum mordants produce, when com-
bined with the proper dyestuff s, khaki shades; but the colors
produced fail either in fastness to light, scouring, alkali, or acid.
The colors produced in a titanium mordant are remarkably
fast 111 every respect, but the colors which dye on this mordant
and produce khaki shades are very limited. The chrome
mordant, however, permits of the use of a wide range of dye-
stulTs. and has this advantage, that khaki shades can be pro-
duced by the chrome mordanting method by the use either of
the regular mordanting method, the after-treating method, or
by the one-bath chrome method. The chrome after treating
method, and the one bath chrome methods are the methods
usual!} used. Neither of these methods are applicable to the
production of khaki on cotton.
The true mordant dyeing yellows, as, for instance, the oxy-
ketone colors represented by alizarine yellow or gallo.ie-eto-
Aug., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
643
phenone and the yellow dyestuffs derived from dye woods,
tannins, and from natural sources, while they can be combined
with red and blue mordant dyeing dyestuffs and produce khaki
shades, are not fast to scouring and alkali because of the pre ence
of a hydroxy group in the molecule, which does not unite with
the mordant. These dyes follow the rule laid down for anthra-
purpurine and similar dyestuffs. The strictly mordant-dyeing
dyestuffs are not, therefore, used in producing khaki colors.
Many, however, of the acid dyes which produce khaki shades can
be dyed on a mordant; but the method is long and does not yield
the fastest colors, nor is the method as practical as the after-
treating or one-bath chrome method. The mordant-dyeing
method has, therefore, found very little use for this purpose for
the dyeing of wool. Except as a printing method it has found no
use on cotton.
The dyestuffs used for the production of the yellow-orange
or yellow-brown used as a basis for khaki, to be shaded to the
true khaki shade with blue, black, or green, and with red or a
reddish browrL are nearly all azo dyes derived from salicylic
acid. The hydroxyl and the carboxyl groups in the ortho posi-
tion in the salicylic acid molecules give these dyes the property
of dyeing on a mordant. They follow the Kostanecki rule in
this respect. At the same time, the chromogen in the color,
being the azo group, and the substitutions in the molecule being
acid in character, the dyes are true acid dyestuffs. They there-
fore can be dyed either as acid dyes or as mordant dyes, or can
be after- treated. Many of these dyes, also, can be dyed by the
chrome in the bath method. The fastness of the dyes to scour-
ing and alkali varies in proportion to the numbers of those
groups substituted in the molecule, which tend to render the
compound soluble. The colors are uniformly fairly fast to light
and acid; certain members of the series are exceptionally fast to
all the tests required. The major part of the coloring entering
into a khaki shade is yellow, so that the amount of blue and red
required to produce a true khaki color, or an olive-drab in con-
junction with the yellow or orange or yellow-brown, is very
small. For this reason only those dyes, which in very light
shades are fast to scouring and light, can be used for shading
purposes.
As types of the dyestuffs that may be used, the following
are cited :
Alizarine Yellow — Salicylic acid plus nitro anilines
Milling Yellow — Salicylic acid plus amidoazobenzol and its mono-
sulfonic acid
Chrome Fast Yellow — Salicylic acid plus amidocresolether
Chrome Fast Green H acid plus orthoamidoparanitrophenol
Acid Alizarine Garnet — Resorcine plus orthoamidophenolparasulfonic
acid
Changes may be run on these combinations by using dyes
which produce the same relative amounts of yellow, red, and blue
when dyed. Thus, the acid alizarine garnet may be in part or
wholly replaced by a red-brown; the green by a black or a blue,
which yields, when dyed, a fast gray. Again, the yellow derived
from the salicylic azo compound may be replaced by the fast
yellows derived from primuline, which are usually termed
chloramine yellows. The khaki colors produced to-day on wool
are made from combinations of dyestuffs similar to the colors
enumerated above.
The khaki colors produced by the direct or substantive dye
methods are in no case, even when after-treated or developed,
on cotton or wool, sufficiently fast to pass the Government test.
This method of dyeing is used, however, at times. The com-
binations of dyestuffs that may be used are almost without
limit but the colors obtained are uniformly not sufficiently
fast. The dyeing method is simple, involving a dyeing in a
salt or soap bath for cotton, or a weak acid bath for wool. The
color produced by the direct dyeing may be used as such, or
may be after treated with a mixture of bichromate, sulfate of
copper, and acetic acid, or diazotized and developed on the
fiber, as the case may be.
The sulfur colors form an important group of dyestuffs for the
production of khaki shades and olive-drab on cotton. The
dyeing method is simple and direct, and the fiber is, when
properly dyed, uniformly soft and strong. The dyeing method
consists in boiling the cotton in a solution of the dye made by
reducing the color with sodium sulfide, and adding alkali and
salt to this solution in order to fix the dye on the fiber. Dye-
ings made from sulfur colors should always be thoroughly
washed with water, and then soaped and wrung or extracted
in the centrifuge, so that some of the soap solution may be left
in the fiber, and the fiber or cloth thus be rendered alkaline.
, This after-treatment or finishing operation is necessary in order
to render the fiber soft, and to prevent the oxidation of any
sulfide compound which may be left in the fiber. This subse-
quent oxidation of the dye on the fiber may result in tendering
of the cotton. The oxidation and tendering, however, is pre-
vented by the alkaline condition of the fiber.
Direct dyeings of sulfur colors are usually not sufficiently
fast to scouring and acid to meet the Government requirements.
However, if a proper selection of dyes be made, and the direct
dyeings made from these be after-treated with a solution of
bichrome, sulfate of copper, and acetic acid, colors which meet
the ordinary Government test are obtained. The use of mineral
acid in this after-treatment may produce a subsequent tendering
of the fiber, even though the dyeings be after-treated or finished
from soap solution. For this reason, acetic acid only should be
used in this after-treatment.
The sulfur dyes are all manufactured by empirical methods.
The constitution of the colors and the chemical reactions in-
volved in their manufacture are not known. It is, therefore,
necessary to select the dyes to be used, only after careful dyeing
tests have been made, and these dyeing tests subjected to the
required tests for determining the fastness to scouring, alkali,
acid, etc. By making combinations of dyes selected from the
evidence obtained from such dyeing tests, satisfactory khaki
shades can be produced. The sulfur colors are not applicable
to wool.
The vat dyes, so-called, because they are dyed in reduced
condition in a vat, as is indigo, produce, next to the oxidation
or chemical method, the fastest khaki colors. These dyestuffs,
when reduced to leuco compounds by the use of hydrosulfite
of soda or other reducing agents, and dissolved in alkali, have
an affinity for the cotton fiber. If the cotton, either as raw
stock, yarn, or in the piece, be immersed in the dye, the fiber
will take up the leuco compound from the solution. This
dissolving of the leuco compound in the fiber continues until the
solubility of the compound in the alkaline solution and in the
fiber reaches an equilibrium. The equilibrium varies for each
dye. If the cotton which has taken up the reduced dye be
wrung out to remove the excess solution, and subjected to the
action of the air, the leuco body is oxidized, and the color is
produced on the fiber.
Not all dyestuffs belonging to this class are fast. But there
are several which produce the fastest shade known on cotton.
From these exceedingly fast dyes, a great variety of very useful
shades can be produced. The dyeing method is applicable to
raw stock or yarn, and by special methods cotton piece goods
may be dyed with these dyestuffs. The colors produced by the
fast dyes of this class are fast to the severest scouring and boil-
ing, fast to acids and bleaching, and exceedingly fast to light.
The dyeing being performed in an alkaline bath, the cotton fiber
or cloth is therefore uniformly soft and strong.
In dyeing khaki by this method, the yellow entering into the
shade is again the major part of the dyestuffs used. The yellows
that may be employed are those known under the trade name of
ALGOL YELLOWS AND ORANGES, CIBANONE YELLOWS AND ORANGES,
644
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 8
HELINDONE YELLOWS AND ORANGES, and INDANTHRENE YELLOWS
and oranges . By the use of the proper dye methods these
yellows can be shaded to product khaki colors and olive-drab,
meeting the severest tests as to fastness. For shading these
yellows to produce a khaki or an olive-drab, it is necessary to
use colors of the same class, giving the red or blue-gray tones
necessary to produce the shad conjunction with the
yellow used. The colors available for this purpose are those
known commercially as algol Corinth, algol red, algol olive,
algol brown, cibanone brown, indanthrene corintb, indanthrene
brown, algol brilliant violet, and indanthrene blue.
By using combinations of these dyes, the fastest khaki shades
for cotton are produced. It would be interesting to study the
chemical constitution of these dyestuffs, and note the effects of
constitution, first, upon the dyeing method, and, second, upon
the fastness of the colors produced. This discussion involves
so many factors that it is not possible at this time. The vat
colors cannot be used for the dyeing of wool (at least, according
to the present dyeing method) because the amount of caustic
soda required to dissolve the leuco compounds is sufficient to
dissolve or permanently weaken or destroy the wool fiber.
The khaki-dyed fabrics, being primarily for military purposes,
should be manufactured having in view the production of a
fabric of the highest quality, the production of the greatest
yardage in a given time, and the manufacture of the cloth at
the lowest possible cost per yard. The specifications have
uniformly called for a fabric to be made from wool or cotton
dyed in the stock. The production of fabrics following these
specifications is thus of necessity confined to the mills having
facilities for dyeing raw stock. The cost of yarns manufactured
from stock-dyed cotton or wool is greater than the cost of yarns
spun from white or gray cotton or wool. The quality of the
fabrics made from stock-dyed yarns is no better, and frequently
is inferior to the quality of piece-dyed goods. The production
per unit of machinery of stock-dyed fabrics is lower than the
production of gray or white goods. It is the opinion of the
author that to procure the highest quality of fabrics, the greatest
quantity in the shortest time, and at the same time the lowest
cost, the piece-dye method should be adapted both for cotton
and wool and worsted fabrics. A large percentage of the cotton
fabrics now used for military purposes is manufactured by the
piece-dyeing method. If these goods are satisfactory there is
no argument against extending this method of manufacture to
include all fabrics. Serge blues or worsted piece goods, as they
are termed, are recognized as standard for quality. There is no
valid argument against making khaki-colored serges, dyed in the
piece, standard also.
When we consider the work done, and the progress made in
the dyeing of khaki in the United States, we need not feel
ashamed. Our manufacturers have produced fabrics equal to
the best foreign goods. Our dyers have developed methods not
used abroad, and have accommodated dyeing methods to manu-
facturing procedure, so that the foreign manufacturer has been
compelled to imitate some of the methods developed in this
country.
We arc dyeing cotton piece goods by the iron-chrome chemical
or oxidation method, equal in quality to the foreign goods.
Our dyers have developed machinery for this process, so that
the process may be said to be truly American, as it is practiced
in this country to-day.
It is true, we have not developed the diamine oxidation
process foi cotton; but, should economic conditions recom-
mend oi warrant the development of this process, it can be safely
predicted that the method will soon be developed into a practical
dyeing process for khaki-colored piece goods.
We have developed both the iron-chrome and the diamine
oxidation methods foi wool These methods have been used very
successfully, and have demonstrated that tl I lined are
the fastest for the depth of shades produced. It does not appear
that either of these methods has been used abroad.
The after-treating or chrome-in-the-bath methods are practiced
by our dyers, producing goods by the raw stock, yarn and piece-
dyeing methods equal to the best foreign fabrics.
Large quantities of sulfur dyestuffs are used for dyeing raw
cotton for khaki-colored goods, and for dyeing piece-goods
producing both the true khaki shades and the olive-drab colored
cloth. The dyeing methods generally used are the same as
those used abroad, and the quality of the color produced is
equal in every respect to the color on the foreign fabrics. We
have an American method, however, for dyeing piece goods with
the sulfur colors, which permits the dyer to produce a full shade
of either khaki or olive-drab by making one passage through the
dyeing apparatus. The color produced by the use of this method
is equal to the best produced by other methods. This con-
tinuous method of dyeing piece goods is not generally in use
here, however, and had apparently not been used abroad.
We have produced from raw stock and yarn dyed with the
vat colors the fastest known shades for cotton fabrics used for
military purposes. The fabrics have been manufactured in
large quantities, and have proved the value of both the dyeing
and manufacturing method used. The continuous process for
dyeing piece goods for sulfur colors may be, with slight modifica-
tion, used for the dyeing of piece goods with the vat dyestuffs.
By this special method cotton fabrics dyed with the vat colors may
be manufactured at the lowest cost, and in the greatest volume.
When we cast up the account as rendered by the American
dyer, we must be convinced that he has made a particularly good
showing in this particular branch of his industry. With intelli-
gent cooperation between the Government, the dyer, and the
manufacturer, we can have an army clothed with the strongest,
best-wearing, and warmest uniforms in the world. May this
result be attained!
New York City
THE STATUS OF CHEMICAL ENGINEERING IN OUR
UNIVERSITIES AND COLLEGES IMMEDIATELY
PRIOR TO THE DECLARATION OF WAR
By Harper F. Zollsk'
Received May 3, 1918
It was while I was engaged in gathering data on a certain
problem connected with curriculum work that I forwarded the
following questionnaire to the departments of chemistry in the
various universities and colleges. The questionnaire was mailed
on February 5, 1917, and by March 21, 191 7, all replies that were
forthcoming had been received. In respect to the nature of the
questionnaire and the replies, several have suggested to me
that they should be tabulated and published, since they reflect
the probable status of the chemical engineering courses in our
schools at the time the United States declared war. The re-
plies have, therefore, been arranged in a table as far as their
nature would permit. I take this opportunity to express my
appreciation of the readiness on the part of those in charge of the
departments of chemistry to cooperate by answering the ques-
tionnaire. Of the total number sent out, only one failed to
answer and I attribute that instance to the inexactness of the
third question. A few colleges have been included in the table
to which the questionnaire were not sent. These are indicated.
The data concerning these was secured from Volume II of the
Report of the Commissioner of Education. A bulletin or
catalogue of the courses in chemistry was also requested of
each of the schools and received.
QUESTIONNAIRE
1 — Do you offer a course in chemical engineering?
is the course first offered?
3 — Do you lay special emphasis on the course5
■ Formerly of the department of chemistry of the Kansas State Agri-
cultural College, Manhattan, Kansas.
Aug., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
645
Course in Year Course
Chemical En- Was First
Name of Institution gineering Offered
Alabama, University of1 Yes
Amherst College No
Arizona, University of1 Yes
Arkansas, University of Yes
Armour Inst, of Tech Yes
Brown University No
Bucknell University1 Yes
California, University of Yes
Carnegie Inst, of Tech Yes
Chicago University No
Cincinnati, University of Yes
Clark University No
Clemson Agr. College No
Colgate University No
Colorado, University of Yes 1903 '
Colorado School of Mines1 Yes
Columbia University Yes
Connecticut Agr. College No
Cornell University Yes 1910
Dartmouth College No
Drake University1 No
Florida, University of No
Georgia Inst, of Tech Yes 1 90 1
George Washington Univ. > No
Harvard University No
Idaho, University of Yes 1910
Illinois, University of Yes 1894
Indiana, University of Yes
Iowa, University of Yes 1904
Iowa State Agr. College Yes 1908
James Milliken University1 No
Johns Hopkins University No
J. B. Stetson University1 Yes
Kansas, University of Yes 1900
Kansas State Agr. College No
Kentucky, University of No
Lehigh University Yes 1902 '
Leland Stanford Jr. Univ Yes 1892 *
Louisiana, University of Yes
Maine, University of Yes
Maryland Agr. College. No
Massachusetts Inst, of Tech Yes 1900 '
Massachusetts Agr. College No
Michigan, University of Yes 1898
Michigan Agr. College Yes 1916 '
Minnesota, University of Yes
Mississippi, University of1 No
Missouri, University of Yes
Montana, University of No
Nevada, University of No
Nebraska, University of No
New Hampshire Agr, College1 Yes
New York University Yes 1898 *
New York, Coll. of the City of No
New Mexico, University of1 Yes
North Carolina, University of Yes
North Carolina Agr. College1 No
North Dakota Agr. College Yes 1911
North Dakota, University of No
Northwestern University Yes
Notre Dame, University of Yes 1908
Ohio State University Yes 1906 '
Oklahoma, University of Yes
Oklahoma Agr. College No
Oregon, University of Yes
Oregon Agr. College No
Pennsylvania, University of Yes 1893 '
Pennsylvania State College Yes 1902 *
Pittsburgh. University of - Yes 1913 *
Polytechnic. Inst, of Brooklyn1 Yes
Princeton University No
Purdue University Yes 1907
Rensselaer Polytechnic. Inst No
Rochester, University of No
Rose Polytechnic. Inst Yes 1909
Southern California, Univ. of Yes
South Carolina, University of No
South Dakota, University of No
South Dakota Agr. College No
Swarthmore College Yes 1904
Syracuse University Yes
Tennessee, University of Yes 1912
Texas, University of No
Texas Agr. College Yes 1908
Throop Polytechnic. Inst Yes 1916
Tufts College Yes
Tulane University Yes 1913
Utah, University of Yes 1905
Vermont, University of No
Virginia, University of Yes 1909
Virginia Polytechnic Inst Yes 1913
Washington, University of Yes 1904
Washington State College Yes 1915
West Virginia, Univ. of1 No
Wisconsin, University of Yes 1904
Wyoming, University of No
Yale University No
1 Questionnaire not sent.
'Same as other courses in engineer-
ing."
Hope to institute course soon."
'Four years' work in chemistry."
'Same as other engineering courses."
Designed to train young men in the
profession of chemistry."
Cooperative course ii
neering.
Course in chemistry.
chemical engi-
Special emphasis since 1914."
Receiving special impetus through the
introduction of five-year courses.
Four-year A.B. degree. Five-year
engineering degree.
important place at Five-year courses offered.
Receiving special announcement
through department bulletins.
Coordinated with school of engi-
neering."
Equal prominence with civil
mechanical engineering."
Yes.*
Yes '
Yes."
Yes."
No."
Five-year course anticipated.
"Course in chemistry" (1908); elect
from engineering courses.
Pushing as rapidly as possible."
Receiving special stress."
No, because of lack of proper
equipment."
Four-year cc
course in cl
Courdtniilely
neering.
rse A.B. Five-year
nncal engineering,
ith college of engi-
646
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 8
DISCUSSION
One might engage in endless differentiations of the courses as
"Hi i. '1 in the above schools, but this would be neither apropos
n< ii beneficial. My purpose is merely to call attention to some
erroneous impressions which might be received on a too hasty
glance at the foregoing tabulation
In glancing through the bulletins one Ends that several of
ili< i called courses in chemical engineering are nothing other
than courses in industrial chemistry and often weak ones at
that, and would not fit a young man for plant control; that is,
he would not be an engineer in the true sense of the term. Other
schools give an abridged engineering course; abridged in the
sense that the course is given through the department of engi-
neering and not through the department of chemistry. This
would tend towards the production of chemical engineers defi-
cient in chemistry, whereas the former would produce chemists
without the fundamental knowledge of engineering. It is to be
hoped that the present situation into which this country has
been plunged as regards hasty, efficient, and voluminous pro-
duction, will influence educational institutions to recognize the
danger in these two extremes, and will lead them to correct it.
Those universities which instituted chemical engineering in the
early oo's have emerged with a well-rounded engineering course
for the chemist. They have also found that the engineer can
not acquire very special knowledge along chemical lines within
the 4-year limit, and have therefore offered 5 and 6 year courses
in chemical engineering with appropriate degrees.
One or two universities, notably the University of Iowa,
have instituted courses in business training along with the
engineering work. Whether or not this will be a success remains
to l>e seen, though one must admit that the plan is a good one.
The time element has been considered by making the combined
course require 5 years for completion.
The University of Michigan and the University of Washing-
ton, following the early example of the University of Kansas
as planned by the late Professor Duncan and the later example
of the Mellon Institute, are offering industrial fellowships to
chemists of ability. Michigan, 1 believe, has been doing this
for several years. While this is not strictly a chemical engi-
neer's problem, it serves to stimulate interest among the student
engineers and furnishes to them an opportunity to witness some
of the manipulations and also to consider some of the problems
which they may be called upon to solve.
One will judge from the table that the Middle West and
West were foremost in developing courses in chemical engineer-
ing, tin pioneers being Leland Stanford Jr. University, Uni-
versity of Pennsylvania, University of Illinois mentioned
in the order of priority. However, these early courses were
much like the courses in industrial chemistry as now offered
and contained few engineering subjects. It would be entirely
wrong to allow the impression to remain concerning the similarity
"I 1 1. in 1 s among those institutions which base signified that a
course 111 chemical engineering is offered. Some of the in-
stitutions offering it are not in proximity to manufacturing
mdii tin of am size, neither do they plan inspection trips for
their engineering students. The courses are. therefore, at their
I " it, onlj weak courses in industrial chemistry as before inti-
111, 1 1. .
I might be criticized for not including the number of graduate
students in chemical engineering for the various schools in the
abovi table, but 1 purposely refrained from so doing The
figures would have been entirely misleading, since I found that
in some institutions where tin courses wen well ordered only
.1 sin. ill number of graduates appeared, whereas the converse
was aisn pronounced.
In closing it should be mentioned that the AMERICAN CHEMICAL
SOCIETY as a unit has done vers little towards the influencing of
young men to take up chemical engineering as a life-work.
Neither has it offered to act in an advisory capacity for the1
young men by suggesting to them the type of training that they
should seek, or for that matter what should be embodied in a
chemical engineering course. Very often the administrative,
officers of the institutions interested would welcome destructive
and constructive criticism while they were shaping their hemical
engineering curricula. It has frequently entered my mind that!
This Journal could well afford to give over one page to uni-|
versity and school activities in the field of chemistry'. While
the Personal page now run deals primarily with the personnel of I
various enterprises, the one I have in mind should treat ex-,
clusively of chemical department curricula, improvements andl
changes in school laboratories, school problems, open criticism Ii
on the nature of various chemical courses now given with uni-
fication and improvement as an objective. This Journal,
since it is to be found on the periodical shelves of nearly every]
city library in the country, would then become an object of|
value to the high-school student, as well as to the young man ■
who has become infected with the chemical engineering bacillus.
A young man should, when planning to enter a university or
college to study chemical engineering, carefully consider the
following questions, and not immediately pick up his grip andl
hie himself to a college of his father's or teacher's connection I
or for some other similar unsound reason: (1) Has the school I
a well-balanced department of chemistry with an efficient corps
of teachers? (2) Is the engineering department among the I
best in the country3 (3) Is the equipment of laboratories I
sufficiently modern to train the chemist in the modern methods I
and processes? (4,1 Is the course in chemical engineering of I
standard type, or is it of hyphenated nature, or possibly I
camouflaged? (5) Is the school contiguous to large manufactur-
ing enterprises involving chemical control and chemical pro- |
cesses, or does it offer opportunity to its students in chemical
engineering to visit such plants at a distance?
It would be well if the bacillus mentioned above would produce
a wholesale epidemic during the coming decade, or better still
if This Journal could sow the seed of infection broadcast.
However we should control the nutritive character of its medium
by the employment of standardized constituents.
Washington, D. C.
COLLEGE COURSES FOR INDUSTRIAL CHEMISTS
By Chaju.es W. Hill
Received December 4, 1917
In secondary education, we have recognized the fact that a
large proportion of students are compelled by force of circum-
stances to become self-supporting at the end of their high school
course. We have successfully supplemented the old college
preparatory course by business and trade courses, and have
established technical high schools, with the object of giving these
students the best preparation possible for their entrance into the
commercial or industrial world. Similarly in university educa-
tion, we have supplemented the classical course by courses in
engineering, agriculture, forestry, etc., and have established
technical institutions for the benefit of students who are limited
to four years of college training.
Among our students in chemistry we have those who are limited
to four years of college and those who may pursue special or ,
graduate work. For the first class, we have courses in chemical
engineering and the B.S. course in chemistry. The latter course
usually sen es as the undergraduate work for those who will
continue above the four years.
Judging by the volume of published discussion on the subject,
there is a serious question whether we are giving our four-year
students in chemistry the best preparation possible for their
future work in the chemical industries. It is the writer's opinion,
after some years of contact with a large number of graduates
from various colleges, that our chemical engineers are quite
Aug., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
647
likely to be hyphenates with the accent on the last word of their
title. They seem to be engineers primarily and secondarily,
and chemists — at best — only thirdly. They are well grounded
in engineering but not in chemistry, either pure or applied. They
are frequently weak in the application of their engineering knowl-
edge to industrial chemical processes or machines.
The B.S. course in chemistry seems to leave the graduate de-
cidedly "up in the air" as far as the industrial applications of
his training are concerned. If he is trained for anything, it
may be for the duties of an analytical chemist. However, I
have been told by some who are experienced in this line, that he
is not well trained for this work. Be that as it may, it does not
seem to the writer that this is a field for which we should train
more than a small proportion of our students. It is his ex-
perience that the position of analytical chemist in the industries
is one in which "the maximum of labor means the minimum of
pay" to paraphrase a recent war poem. The opportunities for
increasing compensation usually depend upon the transfer of
the chemist into the factory. Possibly if we could keep more of
our graduates from becoming analytical chemists, the diminished
supply would result in higher pay for the analytical chemist
who usually deserves much more than he is receiving.
The sins of our teaching are those of commission and omission.
It strikes the writer that our greatest sin of commission is the
time and energy required by courses in analytical chemistry,
which could be used on other matters of more importance and
usefulness. We have qualitative analysis, general quantitative
analysis, and a host of small courses such as gas and fuel, water,
mineral, food, electro, etc. The laboratory work of nearly all
these courses consumes a large portion of the student's time.
Like the classics, many teachers cherish these courses for their
"disciplinary" value. We administer them to all comers.
Engineers and others who will never be called upon to make an
analysis (and could not make it were they called upon) are sent
through the routine. An engineer or an industrial chemist
should of course appreciate the general methods and operations
of analytical chemistry. He should appreciate the accuracy
or lack of it in an analysis. How many colleges teach the theory
of errors in connection with analytical chemistry? He should
know when to call upon an analyst for his services and he should
be able to interpret the analysis. Do the tedious hours spent in
following a laboratory outline for the analysis of a limestone or
a clay teach him this? It is very doubtful if the usual experi-
ments in analysis give the student a broad view of the accuracy
or the application of the subject.
It has often occurred to the writer that a course might well be
arranged of the nature of the following outline, which could be
given in a shorter time than the present courses to engineers and
industrial chemists. The engineers could then be given the
elementary principles of physical chemistry, while the industrial
chemists would have more time for the same subject and a course
in advanced inorganic chemistry and increased work in industrial
chemistry along the lines outlined in the latter part of this article.
Sampling (Fineness and Size of Sample)
Influence on value of analysis
Preparation of Sample
Weighing
Error
Weight of sample for analysis
Solution
Precipitation
Effect of
Concentration
Acidity
Temperature
Time
Precipitate
Occlusion
Washing
Drying
Igniting
Weighing
Titration
Indicators and test plates
Oxidation and Reduction
Absorption Methods
Gas analysis
Combustion Methods (Including Calorimetric Determinations)
Electrochemical Methods
Interpretation of Analysis
Short Tests
Specific gravity
Ash, etc.
Study of errors and variables in all operations and determina-
tion of accuracy in each step
The cardinal sin of omission in our instruction of industrial
chemists is that we give them little training in industrial chemistry
that is of real benefit. The usual course in industrial chemistry,
so-called, consists in a brief study of the chemical reactions in-
volved in a wide variety of chemical industries. The information
given regarding any one industry is naturally general and limited
in amount. Doubtless the student can learn more regarding
any one industry during a week or two in a factory than he can
get in college from the best of texts or teachers. The chances
of his ever becoming directly interested in any one of the industries
usually described are not great, and if he does, he can soon learn
the business first-hand. The remainder of the time spent on
other subjects is largely wasted except as a matter of general
information. This information he can get after graduation by
reading a standard text on the subject.
However, there are matters which apply to almost any in-
dustry and which might well be substituted for the usual course
in industrial chemistry, using some of the time gained by shorten-
ing the work in analytical chemistry. The writer had the oppor-
tunity of giving a course along the lines indicated by the following
outline to a class of senior chemists and chemical engineers.
Since these students have gone out into industrial work, un-
solicited letters have been received from several of them to the
effect that this course was the most beneficial of all their college
work. Admittedly this is an exaggeration, since the course de-
pended for its success on the training which the student had
received in previous courses; but it is a good check on the applica-
tion of the material to several industries. Naturally, the writer
in presenting the course was limited by his experience to those
phases of the subject in which he had had industrial experience.
Since this is not full, as shown by the outline, it would be interest-
ing to publish the outline in order that others may suggest addi-
tions which will then present to our educators a rather complete
outline of subjects which those in industrial work regard as im-
portant and which it would be desirable to have covered in the
college training of our young industrial chemists. There is
pressing need for a good book on this line, which could be used
not only in college but in actual practice. Special chapters
should be written by those in authority on the various lines and
the book should be edited by one of broad industrial ex-
perience.
The criticism has been made of the course that it is really
chemical engineering and not industrial chemistry. The name
is not important. While some of the subjects are touched upon
in the course in chemical engineering, the topics are usually
developed from the purely engineering standpoint. It is not
necessary for one to be able to design an electric motor to be able
to use it properly, and no great amount of electrical training is
needed to enable the student to recognize the various types of
motors, their characteristics and their applications.
In presenting the following course, the students were required
t. > work up a bibliography from the scientific and patent literature,
and to prepare a paper on one of the general subjects, using in-
dexes, abstracts and catalogs with which so many of our graduates
are unfamiliar. They were asked to order books for a library
and to make a list of manufacturers of certain important raw
materials, equipment, and apparatus.
648
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. 8
LITERATURE
Indexes and Abstract Journals
Scientific and Trade Journals
Books
Patent Records
Private Files of Data and Reference
F0WU
Production
Steam
Boilers — Boiler Water
Combustion — Flue Gases
Stokers — Draft
Producer Plants
Gas Engine
Electric
Distribution
Shafts — Belting — Gears
Electrical
A. C. and D. C. Systems
Transf or men — R esistances
Circuit Breakers — Switches
Motors
Fuel
Liquid
Coal — Kinds and Properties
Powdered
Gas — Kinds — Production
MEASUREMENTS
Weight
Scales
Automatic Weighers and Propor-
tioning Apparatus
Meters
Use9 — Accuracy — Calibration
Electric
Types and Application
Wiring
Pressure
Volume — Gas and Liquid
Recording
Heat
Thermometers
Cones
Thermocouples
Optical Pyrometers
Time
Speed
OR
POINTS COVBRSD IN STUDY OF BACH
PROCESS
Machines
Manufacturer
Principle
Design
Capacity
■ Power
Starting — Operating
Running Idle
Outline op Course
Machines {Continued)
Cost
Purchase
Operating
Power
Supervision and At-
tendance
Repair
Depreciation (and
Interest)
Cost of Product
Variables
Controlled
Uncontrolled
Effect of Variables on Product
Sources of Trouble
Processes
Principle
Variables
Controlled and Uncontrolled
Effect on Product
Efficiency
Costs
PROCESSES AND MACHINES
Handling — Conveying — Storing
Solids
Conveyers
Bins
Liquids
Pu naps — Lifts — Val ves —
Sprays
Flow of Liquids
Tanks
Gases
Pumps and Blowers
Tanks
Purifying and Absorption
Apparatus
Sampling and Testing
Crushing and Grinding
Classifying
Screens — Filters - Centrifuges
Mixing
Solution and Absorption
Gas in Liquids
Solids in Liquids
Washing and Purification
Air Conditioning
Autoclaves
Evaporation — Distillation — Drying
Crystallization
Heating or Baking
Furnaces
Gas
Melting Types
Baking and Heat
Treatment
Continuous
Furnaces {Continued)
Electric
Resistance — Indue -
tance
Vacuum
Arc
Shaft Type
Destructive Distillation
Retorts
Refractories
Properties
Tests
Heat Flow — Radiation
Bonds
Finishing
Fumes
Mechanical Retention
Electrical Precipitation
INDUSTRIAL APPLICATIONS OP PHYSICAL
CHEMISTRY
Change of State — Vapor Pressure
Law of Mass Action
Phase Rule
Catalysis
Adsorption — Surface Action
Colloids
Electrochemistry
INDUSTRIAL MATERIALS
Construction
Building and Apparatus
Cements
THEORY OP ERRORS
Industrial Applications
INDUSTRIAL ORGANIZATION
SCIENTIFIC MANAGEMENT
Motion Study — Bonus Systems, etc.
LIGHTING AND VENTILATION
SPBCtPICATIONS AND PURCHASES
COST ACCOUNTING
M a t e rial s — Processes — Labor
Overhead — Depreciation
PATENTS
GRAPHIC REPRESENTATIONS
Scientific Data — Production — Follow-up
Systems
Process Records
INDUSTRIAL RESEARCH
Factory Control
Processes
Machines
Outline and Attack
Establishment of Variables
Reduction to Factory Practice
Laboratory work may be made extremely interesting and in-
structive. Frequently local manufacturing plants have machines
or processes which the student may study directly as a laboratory
exercise, while the manager is often interested in securing the
power or production data which result from the tests.
East Pittsburgh, Pa.
CURRENT INDUSTRIAL NLW5
By A. McMillan. 24 Westend Park SL, Glasgow, Scotland
OIL OF CLOVES
According to the Times, London, there is a considerable prob-
ability that distilleries of a fairly large scale will be set up in
Natal for the purpose of treating the cloves brought in from
Zanzibar and other East African producing centers The
enormous demand for clove oil for a particular war purpose has
caused the supply available for vanillin manufacture to run very
short, and British distillers have all they can do to fill their
orders. Vanillin has, in the meantime, risen to very nearly
$14 per lb.
SHELLAC SUBSTITUTE
Naphthol pitch, according to a recent German patent, can be
converted into a shellac by the following treatment: Two parts
of 0-naphthol are dissolved in 16 parts alcohoj and the filtered
extract evaporated to drive off the solvent. The residual resin
is dissolved in 24 parts of benzol, toluol, xylol, or solvent naphtha
and mixed with 4.S parts of ligroin. This precipitates the
mahogany-colored resin and leaves in solution a colorless resin
which is recovered by evaporating the solvent. Both resins act
as substitutes for shellac.
Aug., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
649
SOUTH AFRICAN REQUIREMENTS
One of the most urgent problems, says the Mining World,
04 (1918), 325, which have arisen in South Africa since the out-
break of war has been the discovery of a suitable disinfecting
and oxidizing agent to take the place of permanganate of potash
which, owing to the cutting off of supplies of potash from Ger-
many, is now only obtainable in very small quantities at pro-
hibitive prices. It is noted with satisfaction that a South
African firm of chemical manufacturers recently erected a plant
for the production of chloride of lime, the demand for which is
proving so insistent that the firm in question in order to meet
the situation has taken steps temporarily to utilize their gold
chlorination plant for the purpose. By this means the company
has succeeded in supplying the most pressing needs of clients
pending the erection of the special plant necessary for the pro-
duction of the article on a larger scale. The new plant has been
designed to supply the whole of the estimated requirements of
South Africa, and the successful production of this important
commodity, from materials wholly within the Union, marks a
further step in the industrial development of the country.
ACID-PROOF ALLOYS
Some experiments by Dr. R. Irmann described in Metall
und Erz, have an interesting bearing on acid-proof alloys. It
has been assumed that electrolytic corrosion tests of voltaic
couples of two metals afford an indication as to the corrosion of
the alloys of these metals. The investigation by Dr. Irmann
of alloys of copper and nickel to which tungsten and iron were
further added apparently disproves this assumption. Much
depends upon the proportion and the formation of compounds.
Irmann was in search of an alloy not to be attacked by hot con-
centrated sulfuric acid. An alloy of nickel with 20 per cent
tungsten was more resistant in this respect than nickel alone,
but was difficult to machine, and expensive. To introduce
tungsten into the nickel, he started from copper-nickel. A
voltaic couple of nickel and copper gave an e. m. f. of 0.55 volt
which soon went down to 0.25 volt. Nickel was dissolved, the
copper becoming polarized with hydrogen. He then introduced
other elements, especially tungsten, into the nickel-copper
alloys, studying also the alloys of copper and tungsten. An
alloy of 47 per cent copper and 4.98 per cent tungsten proved
highly resistant and mechanically strong. The electric re-
sistance was greater than that of constantan. Very good re-
sults were also obtained with ternary nickel-tungsten-copper
alloys, but quaternary alloys containing also iron proved far
superior to the ternary alloys.
FACTORY LIGHTING
A list sent by the British Thomson-Houston Company, Upper
Thames St., London, gives details of the Mazdalux metal re-
flectors for use in connection with the lighting of factories, work-
shops, and other industrial buildings. About a dozen different
types, suitable for lamps of both the half-watt and the vacuum
types, are described, including dispersive, extensive, focusing,
concentrating, intensive, and the various angle types of distri-
bution. The focusing-concentrating type for half-watt lamps
is a new design which is characterized as being most generally
suitable for average industrial lighting conditions; it is supplied
for all sizes of half-watt lamps, including the largest, of 1,500
watts and 3,000 c. p. All the reflectors are made of sheet
steel with a reflecting surface of vitreous enamel, though for
vacuum lamps there are alternate designs in steel with alum-
inum matte reflecting surfaces. The list also describes weather-
proof and other housings with adequate ventilation for half-
watt lamps and contains four pages of tables, illumination charts
and instructions to facilitate the calculation of illumination and
the preparation of plans for direct lighting equipment.
CHEMICAL INDUSTRY IN CHINA
Japanese activity in establishing works in Kwantung has
prompted the suggestion that great possibilities exist for the
establishment of similar enterprises in other parts of China.
The factories already set up cover the manufacture of sulfuric
acid, compounds of barium, caustic soda, creosote, bean oil for
soap, manufacture of stearin and glycerin. There is little doubt
that these products emanate from materials available in Man-
churia itself and that a further investigation of China's natural
products would result in the discovery of numerous further
sources of supply which could be advantageously exploited.
Oil suitable for making ointments and medicated soaps, etc.,
should be readily obtainable from China. Wool is available
for the preparation of lanolin, kelp for the manufacture of iodine,
and Shantung cotton for the manufacture of sterilized and
medicated cotton. Raw material is within reach for the produc-
tion of calomel, and caffeine could be produced from the tea
sweepings in Hankow, while a wide range of valuable products
could be extracted from coal deposits and coal oil. A writer in
the Far Eastern Review asserts that alcohol and ammonia could
be made in any quantity; the most important acids could be
cheaply made together with such products as nitrate of silver.
It is suggested that a conference of Chinese and foreign physicians,
chemists, and pharmacists should take up the question of in-
teresting capitalists in the matter and should place themselves
at their disposal with a view to supervising manufacture.
COPPER AND ALUMINUM IN GERMANY
Discussing the statements recently made by the chairman of
the British Aluminum Company, a leading German newspaper
observes that it is no secret that Germany has embarked upon
the production of aluminum on a large scale during the war,
although opinions differ as to whether Germany, in this matter,
will be able to meet international competition after the war.
It is considered to be certain that the reported increase in British
production of aluminum proceeding simultaneously with a very
large augmentation in the output of copper in the period suc-
ceeding the war will render not improbable some over-production
of the latter metal. If the copper needs of Britain and her allies
are estimated at 50,000 tons per month for war purposes, the
requirements will be considerably reduced the moment peace is
declared. This circumstance is regarded as of importance to
Germany as the same newspaper states that it awakens the hope
that the present exceptionally high prices for copper will fall
through this disproportion between supply and demand, and es-
pecially that there will be no question that it will be rendered
possible for Germany to obtain supplies of the indispensable
copper despite the competition of aluminum and other metals.
COLOR PHOTOGRAPHY SCREENS
A new process for making screens for color photography was
recently described in La Nature. It is the versicolor process
of Dufay. A thin sheet of celluloid is passed between two cylin-
drical rolls; the lower roll is plane, the upper is provided with
very fine parallel ring grooves, flat on top; fine hollows are thus
rolled into the upper surface of the celluloid. This surface is
inked with a red transparent matter and the ink wiped off again
so that the hollows are left red. The ridges are then inked with
blue and in this way a two-coloi screen is obtained. The process
may be repeated with the lower surface of the celluloid or the
two systems of rulings may simultaneously be produced. The
first two colors, for example, may be yellow and blue, and the
third and fourth, red and green; or the four colors may be yellow,
red, blue and orange. In these cases, the third color is the one
missing in the first pair and the fourth color is complementary
to the latter.
650
THE Jul i:\ l/. OF INDl ST RIAL AND ENGINEERING CHEMISTRY Vol. 10. Xo. 8
THE ALCOHOLS AND BASES IN VACUUM TAR
Messrs. Ame Pictct, O. Kaiser, and A. Laboucherc have sent
a note to the French Academy of Science on the alcohols and
bases found in vacuum tar. The alcohols amount 1
2 per cent and the bases to about 0.2 pel cent of the whole.
Tin bases may be extracted from the oils by hydrochloric acid
and the remainder treated with sodium when hydrogen is given
off and the alcoholates are deposited in solid form. The simplest
of the alcohols is />-methylcyclohexanul, the others are more
1 omplicated ami readily oxidizable to phenols, but each of them
forms several distinct phenolic products. The simplest of the
bases belong to tin toluidine group, the others are secondary and
unsaturated. The authors believe the alcohols to exist in the
coal, tin liases they consider to be products of decomposition,
in spite of the low pressures under which the vacuum tar was
found. The bases that can be extracted from coal are not the
same as those found in tar.
GREASE RECOVERY
The recovery of grease from waste materials by the solvent
extraction process was explained by Mr. J. H. Garner at a recemt
meeting of the Society of Dyers and Colorists held at Bradford,
England. There is no doubt, he said, that a very large propor-
tion of the oils and fats used in the form of soap and wasted as
suds ought to be recovered, not only from mills engaged in the
woolen industry, but from the sewage of those towns in which
the industry is established and where considerable volumes of
trade waste are discharged into the sewers. The main considera-
tion, he observed, is to make the process of extraction an econom-
ical one.
MODERN EXPLOSIVES
Thermite, according to a paper by Mr J Young, of Woolwich
Military Academy, is the explosive used by Zeppelins in their
attacks on England and may be taken as the modern substitute
for the ancient burning oil. It causes molten blazing iron to
fall through the air at a temperature of 5000° C. The famous
fiery furnace, according to him, was a cooling place compared
with it. It is used in incendiary bombs and shrapnel, and it
sets even wet grass on lire Mr. Young expresses surprise that
some chemists should imagine that if we kept cotton from Ger-
main it would stop the war He did not believe this to be true
as Germany was doubtless getting what it required from wood.
PRIMUS STOVES
The Primus stove is ordinarily started by a flame of methylated
spirit which heats the burner until it gasifies the paraffin forced
into it by the air pressure in the container. Methylated spirit
is practically unobtainable now and many of these stows have
.miis, quently gone out of use. To enable them to be again em-
ployed Messrs. Condrup, 78 Fore St . London, have brought
..lit .1 paraffin starter to replace the spirit starter. This com-
mi annular dish which replaces the former spirit dish
below tin burnei ami contains an asbestos wick A small quan-
tity of paraffin is placed in the dish and burns from the «i>k
heating the main burner to the required temperature.
NEW ALUMINUM ALLOY
According to the Queensland Mining Journal, aluminum
alloyed with [O pel cent of calcium makes a metal of superior
qualities, lightei than aluminum These castings machine well.
trom briulciicss. ami take the minutest impressions
of the mould. Alloys of copper, tin. or zinc with aluminum are
less resistant to corrosion The calcium also neutralizes the
n mini. \ ..i the aluminum t.> oxidize. It does not decompose
in watei and can in- remelted 1 readil} as pure aluminum.
DEMANDS FOR GLASS
In nearly all the South American capitals, says the Times
Trade Supplement, there is a great shortage of plain plate glass.
The largest quantities of this ordinarily came from Great Britain,
but French manufacturers are reported to be making a strong
bid for the Latin-American market and they are impressing
upon the Argentine importers among others that delivery is
There is also a demand for wire mesh glass which,
to be saleable, should be 6 mm. to 7 mm. (0.236 in to o J75 in.j
thick Since Austria-Hungary ceased to supply the market
with opaque and fancy glass, there are opportunities here for
manufacturers of these goods.
ALCOHOL PRODUCTION IN GERMANY
To crown the restrictions placed upon the technical pro-
duction of alcohol in Germany, says the Chemical Trade Journal,
62 (1918), 415, all such production from cellulose and calcium
carbide is now, under the Imperial Monopoly Bill to be laid
before the Reichstag, to be reserved for the Empire. Another
clause of the Bill embodies an even severer attack upon the
chemical industry subjecting acetic acid produced chemically
by the calcium carbide factories, the aldehyde vinegar industry,
and the wood vinegar industry to a special tax of $40 per cwt.
in comparison with the acetic acid produced by fermentation
from potato alcohol. The quantity of acetic acid produced
in the 680 vinegar factories amounted in 19 13 to about 12,000
tons, while the quantity produced from calcium acetate and wood
vinegar amounted to 23,000 tons of anhydrous acid. During
the war, several large factories for the production of acetic acid
from carbide have been completed, while others are in course of
construction with a view to the manufacture of artificial rubber.
The factories, if fully utilized, are capable of producing 25,000
tons of acetic acid annually. Before the war, 3,400,000 cwt.
of potatoes were worked up annually for fermentation vinegar;
this quantity could be saved for human food without difficulty
if the chemical synthetic process for spirit production were
employed and not stifled by an immense burden of taxation.
Apart from all such considerations, an important step in chemical
progress, viz., the production of acetic acid from purely inorganic
substances, is being obstructed in its incalculable further de-
velopments for the sake of protecting agrarian interests.
URUGUAYAN MARKETS
The Republic of Uruguay has had, says the Times Trade
Supplement, a very good market for the best quality of textile
goods. There are a few small factories in existence but the
people are refined enough and wealthy enough to demand the
best that can be produced in the way of cotton fabrics, dress
materials, laces, ribbons, gloves, and all feminine requirements.
The large and handsome emporiums in Montevideo vie with
some of the leading Paris and London houses in the diversity
and attractiveness of their drapery displays. The value of the
textile market in Uruguay largely exceeds S6,ooo,ooo, including
cotton, silk, and woolen goods.
BRITISH BOARD OF TRADE
During the month of May, the British Board of Trade re-
ceived inquiries from firms at home and abroad regarding sources
of supply for the following .11 tales. Firms which may be able
to supply information regarding these things are requested to
communicate with the I (irector of Commercial Intelligence
Branch, Board of Trade. - .; Basinghall St., London, I
nine mottled soap, Jnoo cases Wax coating cardboard
Macbinbkv mi Plant for.
Making cardboard food holders
Moulding paper pulp
Making papiec D
Making small glass beads per
forated for threading
Slicing cabbages
Aug., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
651
SCIENTIFIC SOCIETIES
FOURTH NATIONAL EXPOSITION OF CHEMICAL
INDUSTRIES
The Fourth National Exposition of Chemical Industries will
be held in the Grand Central Palace, New York City, during the
week of September 23 this year. The managers are Charles F.
Roth and F. W. Payne. The advisory committee consists of
Charles H. Herty, Chairman, Raymond F. Bacon, L. H. Baeke-
land, Henry B. Faber, EUwood Hendrick, Bernhard C. Hesse,
A. D. Little, Wm. H. Nichols, H. C. Parmelee, R. P. Perry, G. W.
Thompson, F. J. Tone, T. B. Wagner, and M. C. Whitaker.
• The Exposition is a war-time necessity and, regarding it as
such, each exhibitor is planning his exhibit to be of the greatest
benefit to the country through the men who visit it, all of whom
are bent upon a serious purpose — that of producing war materials
in large quantities and constantly increasing this production
until the war has been won by the United States and its Allies.
The managers report that the amount of floor space already
engaged is greater than last year, that the exhibits will be much
more attractive, and that a movement is under way to show all
exhibits of machinery in operation under actual working condi-
tions as they would be found in the plants.
Some sections of the South are again sending exhibits, and
Canada is taking the opportunity of presenting the materials it
has available for development by the chemist and financier.
A section for the Glass and Ceramic Industry has been added
with which the American Ceramic Society is cooperating.
The program for the Exposition is in active preparation.
Opening addresses will be made by Dr. Charles H. Herty,
chairman of the Advisory Committee, and Dr. G. W. Thompson,
president of the American Institute of Chemical Engineers.
There will be a series of symposiums on "The Development of
Chemical Industries in the United States, Notably since July
191 4." This will embrace the period since the beginning of the
European War, which, by removing the source of supply for our
domestic industries, inspired the development of our own
chemical industries which, now that we ourselves have entered
the war, are proving so effective. The subjects to be discussed
are Potash Development, Chemical Engineering, Acids, In-
dustrial Organic Chemistry, the Ceramic Industries, and the
Metal Industries. Among the speakers will be:
C. A. Higgins. Recovery of Potash from Kelp.
Linn Bradley. Recovery of Potash from
Sources by Electrical Precipitation.
A. Hough. Chemical Engineering in Explo
Picric Acid, and Nitrobenzot.
E. J. Pranke. Development of Nitric Acid Manufacture.
S. P. Sadtler. Development of Industrial Organic Chemistry.
George H. Tomlinson. Wood as a Source of Ethyl Alcohol.
C. A. Higgins. Kelp as a Source of Organic Solvents.
Alcan Hirsch. Pyrophoric Alloys.
Joseph W Richards. The Ferro-Alloys of Silicon, Tungsten, Uranium,
Vanadium, Molybdenum, Titanium.
Theodore Swank. Ferromanganese.
Leonard Waldo. The Development of the Magnesium Industry.
The American Ceramic Society, which will hold its meeting
at the Exposition on Thursday afternoon, September 26, has
already upon its program :
A, V. BLBININGBR. Recent Developments in the Ceramic Industries.
I.. E. Barrinobr. Manufacture of Electrical Porcelain (illustrated)
H. Ribs. American Clays.
Iv A Whitakbr. Manufacture of Stoneware (illustrated)
Following this meeting a series of motion pictures of the
ceramic industries will be shown.
The motion picture program, in the arrangement of which
the Bureau of Commercial Economics is again cooperating,
carries forward the idea of the symposiums, the pictures ap-
ent Dust and Othe
T. N. A
propriate to a subject being shown on the same day as the
symposium on that subject is held.
In addition there will be shown a series of motion pictures
depicting studies of lakes, waterfalls, and hydroelectric power
possibilities. The development of some of these sources of
power will be shown through the several stages of construction,
generation, and transmission of the power and its use in industrial
operations. Films of several electrochemical operations will be
shown, together with pictures of many chemical, mining, and
related industries, and the application of electricity and electrical
equipment to industrial work. Pictures of the oil industries,
petroleum, asphalt, fatty oils, soaps, paints, linoleum, and oil
cloth will be shown. In fact, every field of chemical endeavor
will be represented. There will be a series of films depicting
the results of carelessness in the destruction of life, wealth,
and resources, and showing hazards and risks in industrial plants
and how they may be overcome. The dangers of fire and ex-
plosives will be demonstrated, and the prevention of disease by
vaccines.
The list of exhibitors is a very complete one of the best firms
among or supplying the chemical industries, men who have faith
in the future of America and are building to successfully conclude
this war and to meet world trade competition after its close.
More complete details of the program, motion pictures,
and exhibits will be given in our next issue.
AMERICAN INSTITUTE OF CHEMICAL ENGINEERS
The 10th Semi-Annual Meeting of the American Institute of
Chemical Engineers was held at Gorham and Berlin, New
Hampshire, June 19 to 22, 1918. The meeting was a pronounced
success from the opening to the closing session. The meeting
was called to order in the Berlin City Hall by Secretary J. C.
Olsen in the absence of the President, G. W. Thompson, on
urgent business. Mr. Hugh K. Moore introduced Hon. George
F. Rich, Mayor of Berlin, who welcomed the Institute to Berlin,
emphasizing not only the interesting technical developments
of the region but also the great natural beauty of the locality.
The Institute was also welcomed by Mr. John Hulan, represent-
ing the Chamber of Commerce of Berlin.
Vice President Henry Howard then took the chair. At the
business session which followed, reports from the various officers
were presented. The Secretary reported a membership of nearly
300, showing a substantial increase since the last meeting.
The Treasurer, Dr. F. W. Frerichs, reported a balance on hand
of $4,148, in addition to Liberty Bonds amounting to $1250.
The Membership Committee reported that no applicants for
membership were recommended for election who were not known
to be loyal to the U. S. Government or its Allies in the present
war.
Mr. Hugh K. Moore then read a paper on "The Human
Element in the Mill" which led to a very interesting discussion
on mill management, those who took part in the discussion
being Dr. T. B. Wagner, Dr. A. C. Langmuir, Mr. Henry Howard,
Mr. Colby Dill, and Mr. L. D. Vorce.
Mr Walter H. Taft read a paper on "Maintenance, Con-
struction, and Organization of a Sulfite Mill " In this paper
Mr. Taft presented the technical methods employed in the
operation of the mill, supplementing Mr. Moore's paper on the
management of the personnel of the organization.
The meeting adjourned to The Grotto where luncheon was
served, after which Vice President Howard introduced Mr.
O. B. Brown, of the Brown Company, who gave a brief but very
interesting account of how the business of the Company had
grown from that of an old-time sawmill in the heart of the
65-z
THE JOURNAL OP INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 8
White Mountains in 1850-54 to an aggregation of chemical
plants including two pulp and paper mills, an electrolytic caustic
and chlorine plant, a hydrogenated oil plant, carbon tetrachloride,
chloroform, sulfur chloride, and carbon disulfide plants. All
of these processes had been developed for the purpose of utiliz-
ing some by-product which was going to waste. Mr. Brown on
behalf of the Company invited the members of the Institute to
visit the various plants of the Company during the succeeding
days of the convention.
The first plant visited was the Brown Company Sulfite Mill
which is the largest sulfite mill in the world. The supply of
raw material consisted of a small mountain consisting of 100,000
cords of wood. The daily wood supply if piled up 4 feet wide and
4 feet high would extend over 2 miles in length. Members were
very much interested in the enormous wood-debarking drums
in which the bark is mechanically removed from the logs.
On Wednesday evening the Institute met in joint session with
the local section of the American Chemical Society at the
Mt. Madison House, Vice President Howard presiding. Prof.
Ralph H. McKee read a paper on "The Manufacture of Alcohol
from Sulfite Waste Liquor." Prof. McKee showed that if air
is blown through the liquor the sugars can readily be fermented
with ordinary brewer's yeast. The paper was discussed by
Messrs. H. O. Chute, Hugh K. Moore, Wm. Garrigue, and T. B.
Wagner.
The Secretary then read a paper by Wm. M. Booth on "The
Manufacturer and the Fuel Situation." An interesting dis-
cussion followed on fuel production and fuel economy partici-
pated in by Mr. Hugh K. Moore, Dr. Chas. Hollander, Dr.
A. C. Langmuir, Mr. Henry Howard, Dr. J. C. Olsen, Prof.
Wm. P. Mason, Dr. J. Bebie, and Mr. John Weiss.
Mr. Graham read a paper by H. E. Zitkowski on "The Seeding
Method of Graining Sugar." Other methods of inducing
crystallization were given by Dr. A. C. Langmuir and Dr. T. B.
Wagner.
Mr. G. A. Richter read a paper on "War Pyrotechnics,"
giving various methods by which light and cloud effects were
being produced in the present war. The Secretary read the
paper by Dr. Alcan Hirsch on "Some Phases of Chemical Manu-
facture in Japan." Dr. Hirsch gave an interesting account
of the recent chemical developments in Japan which though of
great variety are not of great capacity.
Thursday morning the Brown Company saw mill was visited
where lumber is being produced from the larger logs while the
waste and smaller logs are sent to the pulp mill. At the photo-
graphic department members were shown by Mr. John H. Graff
how color photography had been developed for the analysis of
pulp and fiber.
Luncheon was again served at The Grotto, after which the
Y. M. C. A. building was visited, and a paper by Dr. Edward
Gudeman on "Food Conservation" was read and discussed.
During the afternoon the Cascade Paper Mill was visited.
This mill produces 200 tons of news print paper daily The four
immense paper machines producing 48 tons of paper daily were
examined w|th interest. The paper passes through the machine
at the rate of 600 ft. per minute.
On Thursday evening the Institute was delightfully enter-
tained by the Burgess Minstrel Show of the Brown Company.
"A Joyous Jumble of Junk" was presented in three acts en-
titled "Somewhere in America." Mr. Herbert Spear, the
chemist of the Burgess Mill, lead the company of ninety which
presented a series of very clever and excellently acted numbers
The endmen had a variety of excellent jokes, some of which were
clever take-offs on members of the Institute.
On Friday morning the Institute met at the Mt Madison
House for a short business session and the reading of a numltcr
of papers. Dr. A. C. Langmuir presided. A report by Dr.
Chas. F. McKenna as chairman of the Committee on Chemical
Catalogue was read showing the success attained by the com-
mittee in charge of this important publication.
The paper on "Chemical Stoneware and Its Properties" by
A. Malinovs cy was read by Mr. P. C. Kingsbury. Mr. Whitaker
in discussing the paper showed that resistance to the action of
acid was not so important in chemical stoneware as ability to
stand temperature changes. The paper was also discussed by
Dr. Zimmerli, Mr. Kingsbury, Mr. H. O. Chute, and Dr. J.
Bebie.
The Symposium on the Coal-Tar Industry was opened by a
paper by Mr. F. E. Dodge on "Expansion of the Coal-Tar
Chemical Industry." The paper by Mr. W. M. Russell on
"The Expansion of the By-Product Industry of Coal and
Water-Gas Plants in the United States" was read by the Sec-
retary. The paper by Mr. A. G. Peterkin on "The Manu-
facture of Phenol" was read by Mr. John Weiss.
These papers were discussed by Mr. H. O. Chute, Dr. A. C.
Langmuir, Dr. J. Bebie, and Mr. L. H. Grove.
A paper by Mr. L. A. Thiele on "The Multiple Tangent System
for the Manufacture of Sulfuric Acid" was read by the Secretary.
On Friday the members of the Institute visited the chemical
plants of the Brown Company. They were first shown the
electrolytic cells of a design by Moore and Allen, only one of the
electrodes (the anode) being immersed in the brine, the cathode
being in a hydrogen chamber. A small brick furnace with a
condenser consisting of a silica tube was shown and the mem-
bers were surprised when told that this was a hydrochloric acid
plant in which the acid was produced by burning hydrogen in
chlorine gas. The caustic soda plant was also shown in which
40 tons of very pure caustic soda are produced daily, the multiple
effect evaporators having been designed by Mr. Moore.
The sulfur chloride, carbon disulfide and chloroform plants
were also shown. Medicinal chloroform is produced in car-
load lots. The carbon tetrachloride plant was not in operation.
The hydrogenated oil plant in which "Kream Krisp" is pro-
duced from peanut oil was greatly admired, as well as the fiber
tube mill.
The banquet of the meeting was held at the Mt. Madison
House on Friday evening. One hundred and four covers were
laid at the tables. This marked a record in the history of the
Institute as being the largest attendance at any meeting. Dr.
Wm. P. Mason acted as toastmaster and kept the company
in the best of humor with his seemingly inexhaustible fund of
stories and jokes. Mr. W. R. Brown spoke for the Brown
Company, expressing their pleasure at having the Institute
meet in Berlin and Gorham. Ex-Mayor Daily of Berlin spoke
for the municipality. After a selection by the Glee Club of the
Burgess Mill, Vice President Langmuir was called upon and
spoke of the pleasure and profit which members of the In-
stitute had derived from their visit to Berlin and its various
industries. Mr. Hugh K. Moore was called upon and related
how some of the ladies had asked as to what part of the log
gave out the "Kream Knsp ." Mr. David Wesson showed one
of the ladies a knot in one of the logs and explained that "Kream
Krisp" is knot-lard. The ladies were toasted by the Secretary.
Mr. Herbert Spear spoke for the local chemists. Mrs. A. C.
Langmuir responded for the ladies.
During the entire three days the ladies were entertained by a
ladies' committee headed by Mrs. O. B. Brown and Mrs. Hugh
re. The magnificent scenery of the White Mountains
was shown to the visiting ladies on several automobile rides.
In spite of rain on Saturday a party of 28 started by automobile
for a 33-mile drive through Thirteen-Mile Wood to Erol Dam
where the party was taken by motor boat up the Androscoggin
rner .m.l across Ombagog Lake to Sunday Cove. Here auto-
mobiles had been provided by the Brown Company for the 5-
mile carry to Middle Dam This trip proved very delightful
in spite of the weather and the party arrived at Middle Dam ready
Aug., 1018
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
653
for the camp dinner and the cosy fireplaces in the cottages.
Seven of the party started fishing immediately. Mr. Colby
Dill proved the champion fisherman and landed seven fine trout.
After supper Mr. Stephen F. Tyler read his paper on "Fused
Silica: Its Properties and Uses," which was discussed by the
members sitting around the huge office fireplace.
Sunday was spent in walks through the Maine Woods or story-
telling around the firesides. Mr. Hugh K. Moore was voted the
champion story-teller. Some of the party returned to New
York while the remainder took the trip by motor boat to Upper
Dam, spending the night there and returning to New York
Monday morning by motor boat to Bemis and then by the
Rumford Falls Railroad to Boston.
The meeting had proved to be the best attended in the ten
years' history of the Institute; also the most profitable from a
technical standpoint and the most delightful on account of the
beautiful mountain and lake scenery afforded by this popular
vacation region
CLEVELAND MEETING, AMERICAN CHEMICAL SOCIETY
The 56th General Meeting of the American Chemical Society
will be held at Cleveland, Ohio, September 10 to 13, 1918. A
Council meeting will be held on the afternoon of September 9,
and the Council will be entertained at dinner at the University
Club by the Cleveland Section. On Tuesday there will be a
general meeting at the Hotel Statler, which is to be headquarters.
A dinner will be given in the evening at the Statler Hotel, fol-
lowed, after a convenient interval, by a smoker at the same
place. Divisional meetings will be held on Wednesday morning
and all day Thursday. On Wednesday afternoon trips wid be
taken, probably as follows:
A — Sanitary trip. Sewage disposal experiments. Water filtration.
Garbage disposal.
B — Steel industries. Blast furnaces, by-product coke, steel, Bessemer,
and open hearth.
C — Industrial tour of Cleveland, including all the manufacturing
centers, but only a few stops.
D — Trip by special cars to Oberlin.
In the evening the President's address will be given and this
will be followed by a reception at the Hotel Statler.
After the divisional meetings on Thursday, automobile trips
will be taken to one of the country clubs for dinner and to the
Cleveland Museum of Arts. On Friday a special excursion is
planned for Akron, Ohio, where there are interesting rubber,
pottery, soda, match, and other factories. Luncheon will be
served in Akron and the party can leave for home from that city.
The Cleveland chemists are arranging special entertainment,
not only for the men but for the ladies who may be present,
and every effort is being put forth to make the meeting a success.
Special symposiums are being arranged by the chairman and
secretaries of Divisions and it is believed that an unusual oppor-
tunity will be given in these active chemical times for chemists
to get together and exchange views and ideas, many of which can-
not at present be published.
A preliminary notice of the meeting, containing some addi-
tional data, will reach the members about the time that this
issue of This Journal goes to press. A final program will be
sent shortly before the meeting to those who request it.
Chas. L. Parsons, Secretary
NORTHERN OHIO SECTION, AMERICAN CERAMIC
SOCIETY
The Northern Ohio Section of the American Ceramic Society
met in Cleveland on Monday, June 10, 1918.
An inspection trip occupied the greater part of the afternoon.
The first plant visited was that of the Cleveland Metal Products
Company, manufacturers of enameled oil stove parts, light
reflectors, cooking ware, etc. From here the members went
to the Euclid Glass Division of the National Lamp Works
where they saw the making of all the glass parts for electric
light bulbs. They next visited Nela Park, the laboratories
of the General Electric Company. In the auditorium of the
Engineering Building they were entertained with motion pictures
of the obtaining of the raw materials and subsequent treatment
of the same in the process of manufacture of Mazda lights.
A short business meeting completed the afternoon session.
After dinner together, the members met with the Cleveland Sec-
tion of the American Chemical Society in the Assembly Room
of the Olmstead Hotel. Here Mr. A. A. Klein, of the Norton
Company, Worcester, Mass., gave a highly interesting and in-
structive talk on "Petrographic Studies in Ceramics." This
dealt with the practical application of petrography to the manu-
facture of cement, porcelain, brick, abrasives, and other ceramic
products.
CALENDAR OF MEETINGS
American Pharmaceutical Association — Annual Convention,
Chicago, 111., August 12 to 17, 1918.
American Chemical Society — Fifty-sixth (Annual) Meeting,
Cleveland, Ohio, September 10 to 13, 1918.
National Exposition of Chemical Industries (Fourth) — Grand
Central Palace, New York City, September 23 to 28, 1918.
NOTLS AND CORRESPONDENCE
AN AMERICAN EMBLEM FOR AMERICAN CHEMISTS
Editor of the Journal of Industrial and Engineering Chemistry:
In yesterday's parade a feature was a float demonstrating the
use of the oxy-hydrogen torch. Not long ago a movie in color
showed the use of this same torch in the Navy Department
cutting ingots and cleaning castings. It is of invaluable use to-
day in very many of the manufactures through which we intend
to win the war.
Revisions are the order of the day. Paris honors President
Wilson in naming an avenue for him. Other recognitions of
American achievement are being made.
The official insignia of the American Chemical Society and
of the Chemical Service Section of the United States Army are
perpetuating German devices. That of the Society has a Liebig
bulb, that of the Army a "benzol ring." Now, Robert Hare
announced to the world the source of the greatest convenient arti-
ficial heat and light in 1801 (two years before Liebig was born),
founded the platinum industry in this country, and made
possible the untold advances of recent years in metallurgy, in-
cluding the building of our fleet of naval and merchant vessels.
He also produced calcium carbide in an electric furnace about
1840, long before the hexagon was thought of. Besides, in 1831
he devised the present method of exploding charges at a distance,
plunge battery, and incandescent wire. Then, too, he was a
member of the first Chemical Society in the world, the Chemical
Society of Philadelphia.
We have just commemorated the lighting of the Torch of
Liberty at Philadelphia; why not also perpetuate this Scientific
Torch, with its glowl Let it be the emblem for American
chemists whether in military or civil life.
Yours for patriotism,
Charles A. Doremtjs
229 East 68th St., Nsw York City
July 5, 1918
654
THE JOURNAL Of INDUSTRIAL AND ENGINEERING I HEMISTRY Vol. 10, No. 8
TRANSFER OF THE EXPERIMENT STATION AT AMER-
ICAN UNIVERSITY TO THE WAR DEPARTMENT
The White House
Washington, June 26, 1918
])r Van. H. Manning,
Chief, Bureau of Mines,
Department of tin Int. rioi
My Dead Dr. Manning:
I have had before me for some days the question presented
by the Secretary of War involving the transfer of the chemical
section established by you at the American University from the
Bureau of Mines to the newly organized Division of Gas War-
fare in which the War Department is now concentrating all the
various facilities for offensive and defensive gas operations. I
am satisfied that a more efficient organization can be effected
by having these various activities under one direction and con-
trol and my hesitation about acting in the matter has grown
only out of a reluctance to take away from the Bureau of Mines
a piece of work which thus far it has so effectively performed.
The Secretary of War has assured me of his own recognition of
the splendid work you have been able to do and I am taking
the liberty of enclosing a letter which I have received from him
in order that you may see how fully the War Department rec-
ognizes the value of the services.
I am to-day signing the order directing tin- transfer. I want,
howrever, to express to you my own appreciation of the fine
and helpful piece of work which you have done and to say that
this sort of team work by the bureaus outside of the direct war-
making agency is one of the cheering and gratifying evidences
of the way our official forces are inspired by the presence of a
great national task.
Cordially yours,
(Signed) Woodrow Wilson
War Department
Washington, June 25, 1918
My Dsar Mr. President:
In connection with the proposed transfei of the chemical
section at American University from the Bureau of Mines to the
newly constituted and consolidated ('.as Service of the War
i.iit, which you arc considering, I am specially con-
cerned to have you know how much tin Wai Department ap-
preciates the splendid services which have been rendered to the
country and to 'he Army by ill' Department of the Interior
and especially by tin- Hunan of Minis under the direction of
■Dr. Manning. In tin- early days of preparation and organiza-
tion 1 >r Manning's contact with scientific men throughout
the country was indispensably valuable, He was able to sum
moil from the universities and the technical laboratories of the
country, men of the highest quality and to inspire them with
enthusiastic zeal in attacking new and difficult problems which
had to be solved with the utmost speed. 1 do not see how the
Id havi been bettei dom than he did- it and the present
suggestion that the section now pass under the direction and
control of the War Department grows out of the fact that the
whole subject of eas .■ b pressure and
and thi directoi of it must have the widest control so
as to be able to use the h sources at his command in the most
effective way possible The proposal does not involve the dis-
ruption ol roup of scientific men Dr. Manning has
brought together, but mere]] their transfei to General Sibert's
direction
Rt spi ctfullj yours,
Si| 'i. .1 Newton d. Raker
EXECUTIVE ORDER
It is hereby ordered that the Experiment Station at American
University, Washington, I). C, which station has been estab-
lished under the supervision of the Bureau of Mines. Interior
Department, for the purpose of making gas investigations for
the Army, under authority of appropriations made for the
Ordnance and Medical Departments of the Army, together
with the personnel thereof, be, and the same is hereby, placed
under the control of the War Department for operation under
the Director of Gas Service of the Army.
(Signed) Woodrow Wilson
The White HOUSE
June 25, 1918
CHEMICALS AND EXPLOSIVES DIVISIONS
WAR INDUSTRIES BOARD
The War Industries Board has created two new divisions
to be known as the Chemicals Division and the Explosives
Division. Charles H. MacDowell, formerly chief of the Chemi-
cals Section, has been made Director of the Chemicals Division,
and M. F. Chase, Director of the Explosives Division.
The Chemicals Division will be sub-divided into sections
to handle the various commodities with which it is concerned,
the chiefs of which will be as follows:
Acids and Heavy Chemicals — Albert R. Brunker, Russell S. Hubbard,
and A E. Wells.
Artificial and Vegetable Dye — J. F. Schoellkopf. Jr.
Alkali and Chlorine— H. G. Carrell.
Asbestos, Chemical Class, and Stonr^are — Robert M, Torrence.
Coal Gas Products (benzol, toluol, etc.. including commandeering and
allocation of toluol) — J. M. Morehead. Ira C. Darling, associate.
Rare Cases, Xitrogen and Oxygen — Chief not named.
Creosote — Ira C. Darling.
Electrodes and Abrasives — Henry C. DuBois.
Ethyl Alcohol (molasses and grain) — William G. Woolfolk.
Ferro-alloys (chrome, manganese, and tungsten ores) — Hugh W .
Sanford, C D. Tripp. J. II McKenzie.
Fine Chemicals — A. G. Rosengarten.
Nitrates — Charles H. MacDowell. J. A. Bocker.
Paint and Pigment— Russell S. Hubbard.
Platinum— C. H. Conner. R. H. Carleton, G. I. DeNike.
Refractories — Charles Catlett.
Sulfur and Pyrites— William G. Woolfolk. A. E. Wells.
Tanning Material (including inedible oils, fats, and waxes)— E. J.
Haley, E. A. Prosser, Frank Whitney. Harold G. Wood.
Technical and Consulting — E. R. Weidiein. Herbert E. Moody, Thomas
P. McCutcheon.
Wood Chemicals— C. H. Conner. A. II Smith, R. D. Walker, Frank
Whitney.
Statistics. Chemical (joint officel — Captain Willis B. Rice, Army;
Lieutenant M. R. Gordon. Army: Assistant Paymaster Raymond P. Dun-
ning. Navy: Arthur Minnick. Chemicals Division.
A representative of the Army, the Navy, the Marine Corps,
and other departments have been assigned to each section, and
with the Commodity Chief constitute the sections' member-
ship.
In the Explosives Division. Mr. Chase coordinates with rep-
resentatives of the Army, the Navy, and other departments
concerned, and consults with the various section chiefs of the
Chemicals I livision
THE OFFICIAL U. S. BULLETIN
( Iwing to the enormous increase of Government war work,
rnmental departments at Washington are being flooded
with letters of inquiry on every conceivable subject concerning
the war. and it has been round a physical impossibility for the
cleiks. though they number an army in themselves now. to give
manv of these letters propel attention andreply There is published
daily at Washington, under authority of and by direction of the
> eminent newspaper, The Official I'. S. Bulletin.
This newspapei punts every day all the more important rulings.
Aug., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
655
decisions, regulations, proclamations, orders, etc., etc., as they
are promulgated by the several departments and the many
special committees and agencies now in operation at the National
Capital. This official journal is posted daily in every postoffice
in the United States, more than 56,000 in number, and may also
be found on file at all libraries, boards of trade and chambers
of commerce, the offices of mayors, governors, and other federal
officials. By consulting these files most questions will be
found readily answered; there will be little necessity for letter
writing; the unnecessary congestion of the mails will be ap-
preciably relieved; the railroads will be called upon to move
fewer correspondence sacks; and the mass of business that is
piling up in the Government departments will be eased con-
siderably. Hundreds of clerks, now answering correspondence,
will be enabled to give their time to essentially important work,
and a fundamentally patriotic service will have been performed
by the public.
COLLAR INSIGNIA FOR CHEMICAL WARFARE SERVICE
Editor of the Journal of Industrial and Engineering Chemistry:
The present collar insignia of the Chemical Service Section
of the National Army is shown in the accompanying figure.
For the newly organized Chemical Warfare Service, with which
the Chemical Service Section has been merged, it has been
proposed to adopt the insignia of the latter. The only criticism
which has been raised is that this emblem is not sufficiently
warlike in appearance and suggests too much the peace and
seclusion of the laboratory. Our artistic fellow-chemists are
requested, therefore, to sharpen
their pencils and send us de-
signs which they regard as pref-
erable. The device must be, of
course, compact and simple, and
not likely to be confused with
the insignia of any other branch of the service.
The sketches can be sent to the undersigned and, in the event
of one being adopted in place of the present insignia, the fact
will be published in This Journal together with a copy of the
design and the name of the chemist. The designer will have the
satisfaction of knowing that his emblem will be brought forcibly
to the attention of the Hun by the boys "over there."
Marston T. Bogert
Col., Chem. Warfare Service, N. A.
L'nit F, Corridor 3, Floor 3.
7th and B Streets, N. W.
Washington. D. C.
July 12, 1918
GERMAN POTASH AND THE WAR1
Germany has a world monopoly on potash. Even before the
war foreign countries were making efforts to find potash outside
of Germany, and rumors have often been afloat as to potash
finds in France, Spain, Russia, Austria, and California; but
nowhere has potash been found to any extent which in any way
could compare with the German supply. During the war the
enemies have suffered greatly from lack of potash. Grain and
cotton harvests in the countries where these are the most im-
portant crops show the results of potash shortage. More
energetic efforts than ever arc now being made to find potash.
After the war the enemies, now intent on an economic war,
will again have to ask for German potash. Only the dreamers
are still hoping that it will be possible to force the turning over
of the Alsatian potash mines to France. In reality, not only
France, but the whole Entente will be dependent upon Germany
for potash. Before the war the Alsatian works delivered about
1 Translated from Deutsche Wirtschafts-Zeilung of Jan. 15, 1918.
one-tenth of the whole German potash output. It has, how-
ever, been possible to increase their yield considerably, so that
it is a fact that many countries could be supplied with potash
from Alsace alone. As it is out of the question that Alsace will
be separated from Germany, all dreams of breaking the German
potash monopoly are vain.
It is extraordinary that while the Entente countries are
dreaming of supplying themselves from Alsatian potash works,
they are at the same time trying to discredit the German potash
industry at large. This has even gone so far that the Reuter
Bureau one day brought the information that the German potash
fields were exhausted, and that when peace came, Germany
would not again be able to export potash. Before the war the
complaint was constantly made that Germany had too much
potash and too many potash works. The German potash
industry did not suffer from exhaustion, but rather from over-
production. Although the whole world was being exclusively
supplied from Germany, the demand did not keep up with the
increasing capacity of the potash works. The potash mines had
to reduce their output from year to year. The combination
of German Potash Works (Kali Syndicate) finally had to close
some of the new mines until the potash already on hand could
be disposed of; it had to develop a great propaganda at home
and abroad for potash fertilizer.
To what great extent the war has changed these conditions!
The enrolling of laborers in the Army hit the potash industry
as well as others. When the export was stopped, the decrease
in demands for potash was only natural. Soon, however, a
greater demand for potash developed among German agri-
culturists, so that the potash works again had to put out all
energy to satisfy the demands. Partly in consequence of the
lack of other fertilizer, the German agricultural demands for
potash are, after three years of war, as great as that of the whole
world before the war. And if the deliveries are not still larger,
it is due to various causes which have prevented the mining of
the potash, mainly the lack of skilled laborers (in the potash
works it is hardly possible to use unskilled workmen or war
invalids), and the transportation difficulties. The demands
upon the German potash works are now, after three years of
war, only a little less than the highest yields ever reached, in
1913. When peace comes, the difficulties which are now pre-
venting the full utilization of the works will disappear. The
demands for potash will be much greater than before the war.
German agriculture uses much more than before, and according
to their own reports the agriculture of the United States and other
countries is simply starving for potash.
Will the German potash works be able to satisfy these greater
demands? The reply to this in competent circles is that only a
lack of sufficient labor, transportation, and coal can prevent the
German potash works from doubling their present production;
that is to say, they will be able to yield a value of 500 million
marks, or twice the production of former peace times. After
a few years the yield might reach 1000 million marks. It is not
possible to think of exhausting all the potash fields which actually
are found all over Germany. It is hardly exaggerating to say
that the potash mines of Germany will be able to supply tin-
whole world for 500 years and more. The potash fields are
practically inexhaustible. There are now in Germany 209
potash works with a complete outfit, and their mines will last
for several hundred years. The value of these mine products
show the great importance which potash wilt have in bringing
German currency again to a normal footing.
The potash monopoly is an important weapon in the economic
war which the Entente intends to carry on with Germany
Even during the war, potash has been an important article in the
exchange trade between Germany and its neutral neighbors,
whose agriculture has derived great benefit from this important
fertilizing clement.
656
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 8
CHECK MEAL CONTEST
The Society of Cotton Products Analysts announces the
conditions of their check meal work for the coming season.
There are to be forty weekly samples of carefully prepared
cottonseed, or other feed meal, sent to, not only any of its mem-
bers, but also to any other chemist in the country who so desires.
These samples are to be analyzed for moisture, oil, and ammonia
content and prizes of silver cups given to those who turn in the
most accurate results for oil and ammonia.
The conditions of the contest are stated in the July number of
The Cotton Oil Press and any chemist interested should obtain
a copy of this or apply to F. N. Smallcy, Chairman, Southern
Cotton Oil Co., Savannah, Ga., for details.
This work, now in its third year, has done a great deal of good
as a means of bringing closer agreement between all chemists
engaged in cottonseed work, and the committee in charge of the
contest believe that chemists engaged in other lines of food work
where similar analyses are made would gain much by entering
the contest.
PLATINUM RESOLUTION BY THE STATE COUNCIL OF
DEFENSE FOR CALIFORNIA
838 Phelan Building
San Francisco, California
June 6, 1918
Mrs. Ell wood B. Spear
27 Walker Street
Cambridge, Mass.
My Dear Mrs. Spear:
At a recent meeting of the Executive Committee of the Cali-
fornia Women's Committee of Councils of National and State
Defense, the following resolution was adopted :
"That, in view of the shortage of platinum, due to the fact
that 95 per cent of the world's supply comes from Russia, and
the need for platinum to make the assets which are necessary
for explosives and the making of guns, and in the laboratories
which are at the service of the Government; and because one-
third of the whole world's entire supply of platinum has been
put into the production of jewelry, the California Women's
Committee of the Councils of National and State Defense
resolves to discourage the use of platinum for jewelry, or other
articles not necessary for the winning of the war."
I have sent the leaflets throughout the State and will be glad
to distribute anything further.
With cordial regards, I am
Yours sincerely,
(Signed) Julia George
ORGANIC REAGENTS FOR RESEARCH AND INDUSTRY
Editor of the Journal of Industrial and Engineering Chemistry:
In order to provide for the supply of organic reagents for re-
search and industrial purposes the Eastman Kodak Company
has determined to commence their preparation in its Research
Laboratory.
This decision was arrived at as a result of the articles published
by Dr. Roger Adams and of a recent letter by Professor Gortner
in Science (June 14, 1918. p. 59°). which drew our attention
to the need for an adequate supply of these materials produced
by a firm of standing.
In order to carry on the work a separate section of the Labora-
tory has been established under the title of the "Department
of Synthetic Chemistry" which will be under the immediate
direction of Dr. H. T. Clarke, well known for his publications
on organic chemistry.
In order to make available to research laboratories in this
country the organic chemicals which they require, it is proposed
that chemicals for research work shall be supplied at the lowest
possible price. At first, no doubt, this price will necessarily
be higher than that charged by the German firms before the
war, but it is hoped that eventually the profit made on chemicals
supplied for commercial purposes may enable the rarer materials
made in small quantities for research work to be sold at a price
which will be within the reach of all who require them.
At first, of course, the Laboratory will be able to supply only
a limited number of substances, and these in small amounts,
but the department will be expanded to meet the demand, and
with the assistance of other laboratories interested in organic
chemistry, and of the firms who are producing dyes and inter-
mediates, it is hoped that after a time an adequate supply of
synthetic organic reagents can be made available.
It is possible that laboratories may have in stock unusual
reagents which they are unlikely to require. If any laboratories
possessing such reagents will write to us, we shall be glad to make
an offer for the materials, thus making them available on the
market.
Our thanks are due to many of the chief chemists of the
country who have encouraged us to commence this work and
especially to Dr. Roger Adams for the way in which he has
received our proposals and has assisted us by placing at our
disposal the information as to this work which he has accumulated.
Communications regarding reagents should be addressed to
the Research Laboratory, Eastman Kodak Company, Rochester,
N. Y.
C. E. K. MEES
Eastman Kodak Company
Rochester, V V.
July 12, 1918
WASHINGTON LETTER
By Paul Wooton. Union Trust Building, Washington, D. C.
Since plenty of advance notice had been given, no flurry fol-
lowed the announcement by the War Industries Board that it
would take full control of all sulfur materials. William G.
Woolfolk, who is to represent the War Industries Board in con-
trolling the production and distribution of sulfur materials,
already i- known to the trade interested in those commodities
a* the chief of the Hoard's sulfur -pyrites-alcohol section
It is known that the War Industries Board lias entire con-
fidence in the Chemical Alliance and there is every 1,
believe thai this body will fcx tically .1 free hand in
m looking to equitable distribution of brim-
stone, pyrites, and coal brasses. It also is known that the
War Industries Hoard Ikis been unusuallv impressed with the
abilit] "i \ \> Ledoux, who is the chairman of the Production-
Distribution-Control Committee of the Chemical Alliance
With everything favoring harmonious cooperation between the
War Industries Hoard and ii Uliance, n is believed
that the intricate problems involved can Ik- solved without
serious disturbance of the industries concerned. With Mr.
Ledoux on the committee are W. D. Huntington and C. G.
Wilson. At this writing, the committee has not gone deep
enough into its plans to make any announcement. A ques-
tionnaire, which is to go to all users of sulfur materials, is now in
progress of compilation. The office of the committee will he
in Room 135 of the Interior Building. The offices of the Chemical
Alliance will continue to be maintained in the Woodward Bldg.
The full text of the announcement of the War Industries Board
in taking over the control of chlorine is as follows:
to the shortage of chlorine in the United States, the War In-
dustries Board, with the approval of the President, has passed a resolution
taking over control of its production and distribution. For the present,
however, the Board is doing no more than allocate the product, and this is
being done under the direction of H. G. Carrell. Chief of the Alkali and
Chlorine Section of the War Industries Board.
Aug., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
°57
Chlorine has a wide range of uses, the most important from the present
Government point of view being in the manufacture of gas shells and in
carbon tetrachloride, which is the basis of one of the most effective smoke
screens and also of the best fire extinguishers.
One of the most important commercial uses of chlorine is in the bleach-
ing of paper and various cloth fabrics.
Judging from the communications being received by members
of Congress, much interest was aroused by the appearance be-
fore the Ways and Means Committee of representatives of the
chemical industry and of the jewelry trade. Meyer D. Roths-
child, of New York, represented, as he said, every jewelry
organization with the exception of the National Jewelers'
Association. Robert B. Steele also contributed voluminously
to the record. Dr. Charles H. Herty, of New York, presented
to the committee the view of the platinum situation as taken by
chemists.
While an effort was made to discredit the entire proceedings
by alleging that the committee was taking up two days of its
time to enable the chemists and the jewelers to stage a row, this
version of the matter was not accepted. Representative Long-
worth, of Ohio, one of the members of the committee, expressed
the opinion that the threshing out of the platinum situation in
such a thorough manner was one of the most important things
that the committee had done.
The jewelers took particular exception to the fact that the
Bureau of Mines is cooperating with the American Chemical
Society in a campaign to discourage the use of platinum in
jewelry. There was extended discussion of the various pro-
prieties involved which finally led Mr. Longworth to ask, "Which
is more essential now to this country in the prosecution of the
war, jewelry or chemistry? If there is one thing more useless
in time of war than is jewelry, I do not know what it is, unless
it be artificial flowers. The jewelers made the same fight against
the abolition of aigrettes that they are making now against the
sale of platinum. Congress took the 'bull by the horns' and
provided that they should not sell aigrettes, although they said
that they would be ruined."
The high point of Dr. Herty's testimony was that there should
be no platinum available for taxation. He recommended that
all the platinum in the hands of jewelers be taken over by the
Government, after equitable compensation had been allowed
and placed in the vaults of the subtreasuries, where it would be
accessible when the need comes. He suggested that it would not
be necessary to call for the platinum in the hands of private
individuals, as he believes they will hold on to the platinum
until it is needed, thus relieving the Government of the expense
of carrying it.
After asking special permission to insert it in the record, Dr.
Herty made this significant addition to his testimony: "My
conviction in this matter is that any chemist who sells his
platinum to any one other than the Government would be just
as unpatriotic as would be any jeweler."
After a hearing on the national trade mark bill before the
Senate Committee on Commerce, it was agreed that the measure
should be made more concise but should retain the salient
features of the measure which was recommended by department
officials. It contains the essential features of the International
Convention of August 20. In the opinion of J. T. Newton, the
commissioner of patents, of Dr. L. S. Rowe, assistant secretary
of the treasury, and of C. P. Carter, of the Bureau of Foreign
and Domestic Commerce, the measure "if enacted into law will
be of great advantage to American trade mark owners who are
doing business in the Central and South American republics."
The principal objection to the bill which was before the
Senate was to the first section of that bill. Concerning this
section, Mr. Newton said, "My idea about this bill is that there
is no use in passing any bill at all, if we cannot benefit our own
people. The first section provides for an examination of some-
thing that the Patent Office already has granted as a trade
mark; because probably four-fifths of these registrations will go
from this country, and I think it is the sense of the convention
that nothing will be done in Havana until the mark has been
registered in the country of origin." The bill which will be
substituted, however, will take care of that point.
In their zeal to keep from the Germans such few facts con-
cerning American-made war gases as would have been valuable
to Hum, those charged with such work seem to have been most
successful in keeping from the chemical industries, and the
public in general, the information to which many believe they are
entitled. The principal criticism heard in this connection is
that the chemists of the country are not being allowed to con-
centrate such time as they have available on gas problems.
As it is, so little is known of the situation that a great force of
brain power, which might be directed against these problems,
is not being utilized. Even in the War Department itself there
were examples of appalling misinformation regarding the gas
situation. One high official of that department made the state-
ment that no gas mask developed by the Allies was able to with-
stand effectively the gas used in the March drive. To counter-
act very general misinformation in this regard, the Chemical
Warfare Section on July 12 issued the following statement:
Protection against any of the gases now in use by the Germans is
given to American soldiers by the masks now being worn. Statements
that American masks do not protect soldiers from the effects of mustard
gas are not warranted.
The masks now worn will protect soldiers as long as they are required
to remain in areas drenched by gas. The clothing worn by the soldiers will
resist the effects of the gas for a normal period. As an added precaution,
the soldiers are now provided with a neutralizing ointment to be rubbed
on those parts of the body where mustard gas is likely to penetrate through
the clothes.
This ointment is being prepared in quantities greater than the demand
for it. The first month's shipment consisted of 800,000 tubes. It is a
new preparation made after a formula prepared by chemists connected with
the Chemical Warfare Section. Rubbed on the body before a gas attack,
it has the power to neutralize the poisonous effects of mustard gas.
For the protection of the special men whose duty it is to clear trenches
of all traces of the gases, special underwear is now being provided. These
suits are chemically treated and neutralize poisonous gases.
Men are being thoroughly trained in gas defense so that every soldier
who enters the zone of fire thoroughly understands the measures of gas
defense. Every man is drilled in the adjustment of his gas mask before
he is subjected to a gas test, either here or overseas.
An announcement by the Secretary of War issued July 2 with
regard to the Chemical Warfare Service reads as follows:
The organization of the Chemical Warfare Service has been com-
pleted. Henceforth all phases of gas warfare will be under the control
of the Chemical Warfare Service commanded by Major General William
L. Sibert.
Heretofore, chemical warfare has been carried on by divisions in the
Medical Department, the Ordnance Department, and the Bureau of Mines.
All officers and men who have been connected with offensive or defensive
gas warfare here will be responsible to the Chemical Warfare Service. The
field training section at present is under the Corps of Engineers.
Defensive warfare has been under the control of the Medical Depart-
ment. This work has consisted of the designing and manufacture of masks
both for men and animals and the procurement of appliances for clearing
trenches and dugouts of gas.
Offensive gas warfare consists principally of manufacturing gases and
filling gas shells. The work has been under the direction of the Ordnance
Department.
The new department will take over the work of chemical research for
new gases and protection against known gases, which work has been carried
on by the Bureau of Mines. All testing and experiment stations will be
under the direction of the Chemical Warfare Service.
The responsibility of providing chemists for all branches of the Govern-
ment and assisting in the procurement of chemists for industries essential
to the success of the war and Government has been entrusted to the Chemi-
cal Warfare Service.
All chemists now in the army will be removed from their units and
placed under the authority of the Chemical Warfare Service. Newly
drafted chemists will be assigned to the Chemical Warfare Service.
Authority to assign enlisted or commissioned chemists to establish-
ments manufacturing for the Government has been granted to the new
section.
A number of amendments to the Trading with the Enemy
Act have been drafted. One of these amendments will enable
the Alien Property Custodian to grant licenses for the full term
of life of a foreign patent. The amendments have been sub-
mitted to the Committee on Commerce of the Senate, but as
yet have not come up for consideration.
As a means of cooperating in the efforts being made by the
Government to stimulate production of the war minerals,
Fuller Calloway, who has been referred to as "one of the most
progressive thinkers among business men in the South,' has
perfected an organization among southern producers of pyrites.
An effort is being made, without actually pooling all the product,
for the pyrite miners to secure the benefits of the pooling method
in so far as there is need,
THE JOl RNAL OF INDUSTRIAL AND ENGINEERING I HEMISTRY Vol. 10, Xo. 8
PERSONAL NOTL5
Mr. R. Norris Slircvc has been made assi 1 ml ;i qi ral manager
of Hi' ix organic plants of the Maiden, Orth and Hastings
ion, i ontrol "I whii '1 at the plant
of^the Calco Chemical Co., Bound Brook, N. J., recently acquired
by the ( orporatii m
Mi R. II. McK< ■(• v. 1 : in chemical engineer-
ing at -Columbia Univei i professor of chemical
engineering. Professor McK' ctor of the Tennessee
t oppei Company and consulting chi mical engineer for the
U.JS. Industrial Alcohol Company.
i D. D. Jackson, Columbia University,
las'Ju'ii made professoj ol chemical engineering.
Mr. Ellwood Hendrick, President of the Chemists' Club,
tlj addressed the New Jersey Science Teachers' Associa-
president of which writes, "It was the consensus of
opinion that his talk was not only delightful but masterful."
Dr. James F. Norris, who has been with the Bureau of Mines
Experiment Station, has been commissioned a Lieutenant
Colonel in the Chemical Service Section of the National
Army and is to be stationed in London as the representative of
iln Army, in chi mical warfare, in England. The following men,
all iii the Chemical Service Section, are to be with him to help
intheworl Capl A. B. Kay, Capt. G M Rollason, Lieut.
H. A. F. Eaton, and First Sergeants E. (l Hobbs, L. C. Bene-
dict, C. Iv. Wood, and J. A. Bowers.
Mr. R. E. Parks, assistant general manager of the Aluminum
Company ol Vmerica, Maryville, Term., has been promoted to
the position of general manager of the company's plant at
Badin, N. C.
Colonel John Joseph Cam, Signal Corps, U. S. Army, was
the recipient of the Edison medal awarded by the American
Institute of Electrical Engineers on May 17, iyi8.
Mr. George B. Hogaboon has been granted a leave of absence
by the Scovill Manufacturing Company in order to accept the
Lppointment as electroplating advisor for the Bureau of Stand-
ards.
Mr. John A. Traylor has resigned from the position of Western
. of the Traylor Engineering and Manufacturing Com-
pany, and will devote his time to his mining interests, with
headquarters in Salt Lake City.
Mr. Joseph V. Meigs, formerly research chemist for the
Barbel Asphalt Company, is now serving in the Ordnance De-
partment ni tin' National Army. He is detailed for chemical
duty at South Charleston, Charleston, W. Va.
Mr. Harold K. Woodward, for six years connected with the
Food Rest. mil Laboratory of the Bureau of Chemistry in Phila-
delphia, is now doing research work in the Jackson Laboratory
of E. I du Pont de Nemours and Company at Deepwater, N.J.
Mr. 11. B. C. Allison, Schenectady, N. V., died on May 7, 1918.
Mr. Allison graduated From the Massachusetts Institute of
Technology in 1911. in the fall of that year he became asso-
ciated with the resi arch laboratory of the General Electric Com-
pany, Schenectady, N. Y , where his capabilities and diligent
work rapidly advanced him to .1 position of importance and
responsibility.
Mi Irving S. Ellison, who has been studying at the I'm
versityol Michi in has been called to serve with the Medical
Supply Depot at Camp Wheeler, Macon, Ga.
Mi. \\ \\ Battle, cit) chemist of Dallas, Tex., ha
una of the Central Texas Section of the
Van 1 11 hi Chemical Socif t y.
I >r. F. E. Cai 1 nth, who was formerly with the chemical division
ol tin North Carolina Experiment Station, has become asso
elated with the Sehaefer Alkaloid Works. Maywood, X. J.
1 'i 11 L, Abramson, foi the past five years assistant health
Office] in New Yoik, has been appomled chief of the public
health laboratories foi New Brunswick, Canada, with head-
quai tej 1 at St fohn
I 'i R F. Ruttan, direct 1 the department of chemistrj
"i M' 1 oil 1 nivei lity, and chairman of the chemical committee
of the Honorarj Vdvisorj Council foi Scientific and Industrial
n, was recentlj elected vice president of the Royal Society
oi Canada Di Rutl lident this year of the
Society of Chemical industry of Great Britain.
Provost I'd. n F Smith received the honorarj di
Doctoi ol Letters from Swarthmore College at its commence
incut on Mai
Dr. Eugene R. Kelley, formerly commissioner of health at
tor for the past three years of the de-
partment of communicable diseases in the Massachusetts
organization, has filled the vacancy in the health commissioner-
ship of Massachusetts left vacant by the recalling of Dr. Allan J.
McLaughlin to the United States Public Health Service to be-
come assistant surgeon-genera! in charge of the Division of
Interstate Quarantine.
m-rlv professor of chemistry at the Uni-
versity of Wyoming, I his position to become chief
or the Midwest Refining Company. His office will be
located at Casper, Wyoming.
Mr. W. J. McGee, formerly of the Bureau of Chemistry, U. S
ulture, stationed at Savannah, Ga., has
been transferred to San Juan, Porto Rico, where he is engaged
in the inspection of food and drugs.
Dr. Lauder W. Jones, head of the department of chemistry
in the University of Cincinnati, has resigned to become head
of the department of chemistry in the University of Minnesota.
He has been granted a leave of absence for a year in order to
take charge of the Research Division of the Gas Offensive at the
American University in Washington.
Dr. Harry S. Pry. associate professor of chemistry at the
University of Cincinnati, has been appointed acting head of the
department of chemistry in the University of Cincinnati.
Mr. Walter M. Russell, who for several months has been chem-
ical engineer for the Providence Gas Company, is now superin-
tendent of manufacturing.
Mr. James II. Readio, Jr., who recently came from the Paw-
tucket Gas Company to the Providence Gas Company, R. I., as
assistant chemical engineer, will take over most of the work of
the chemical department, also assisting in plant operation.
Mr. M. L. Hartmann, formerly professor of chemistry at the
South Dakota State School of Mines, has resigned his position
to accept a position as research chemist-in-charge for the Car-
borundum Company, at Niagara Falls.
"Mr. Walter M Scott, formerly in charge of the department
of chemistry at the Osceola Township High School, Dollar Bay,
Michigan, is now connected with the Aluminum Company of
America, at Masscna, N. Y.
Mr John Putnam Marble has resigned his position as assistant
in chemistry at Williams College and is now awaiting his call
to the Chemical Service Section of the National Army.
Mr. H. C. Holden has resigned his position as research chemist
with the Washburn Crosby Co . of Minneapolis, and has accepted
the position of research chemist for the N. K. Fairbank Co.,
Chicago, 111.
Prof. T. Brailsford Robertson, formerly professor of
trj and pharmacology at the University of California,
has been appointed professor of biochemistry at the University
of Toronto
Dr. E. B. Forbes has been commissioned a Major in the Food
Division, Sanitary Corps. Dr. Forbes was head of the depart-
ment of nutrition of the ( Hiio Experiment Station.
Dr. Abraham Eienwood, of the Philadelphia Section of the
A. C S . has relinquished his connection with the faculty of 1 'revel
Institute and entered the service of the Hercules Powder Com-
pany u irch work.
Prol Charles H LaWall, of the Philadelphia Section of the
\ , C S., has been elected chairman of the U S. Pharmacopoeia
Revision Committee.
Dr. I' L. Randall has resigned his position with Baker Uni-
versity. Baldwin City, Kansas, to accept an associate professor-
ship at Wesleyan University, Middletown, Conn. During the
summer months he is working in the research laboratory of the
Merrimac Chemical Company at North Woburn, Mass.
I>i Henry Drysdale I 'akin received the degree of doctor of
science at the commencement exercises of Vale University.
The following named officers of the Food Division, Surgeon-
on duty in France Majors Philip A.
Shaffei and A. J. Carlson. Captains Waltei II Eddy, Arthur W.
Thomas, F B King-tuny, and M. C. Mastin, all S C, N. A.
Dr. Raymond lirector of Mellon Institute, Uni-
il Pittsburgh, and Lieutenant Colonel in charge of the
chemical work of the American forces in France, has received
from the I Diversity of Pittsburgh the degree of Doctor of Science.
Aug., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
659
Dr. N. Edward Loomis, for the past four years in charge of
physical chemistry at Purdue University, has resigned to become
chief chemist of the Wood River, 111., plant of the Standard
Oil Company.
Mr. A. Strickler, assistant professor of chemistry at the
Michigan State Normal College, Ypsilanti, is on leave of absence
for the summer. In the Fall he will resign his position to take
up his new work as research chemist for the National Biscuit
Company in their new laboratories, 14th Street, New York City.
Mr. R. B. Stringfield, formerly chemical engineer with the
Western Precipitation Company, has accepted the position of
chief chemist with Poindexter and Company, Manufacturing
Chemists, of Los Angeles and Vernon, Cal.
Dr. William Battle Phillips, formerly of Chapel Hill, N. C,
died recently at Houston, Texas. At the time of his death Dr.
Phillips was a private geologist at Houston. Dr. Phillips had a
varied career. He had been president of' the Colorado School of
Mines, chemist at the North Carolina Experiment Station,
professor of agricultural chemistry and mineralogy at the Uni-
versity of North Carolina, professor of chemistry and metal-
lurgy at the University of Alabama, chemist for the Tennessee
Coal, Iron and Railway Company, and director of the Texas
Mining Survey.
Mr. Ralph T. Govilivin, formerly employed at the Hercules
Powder Company, San Diego, California, has accepted the ap-
pointment as organic chemist with the Bureau of Aircraft
Production, Pittsburgh, Pa.
It was inadvertently stated in the July issue of This Jocrnal
that Prof. Herman I. Schlesinger had been promoted to an
assistant professorship at the University of Chicago. This should
have read "an associate professorship."
Dr. Chas. W. Burrows, associate physicist and chief of the
Magnetic Section of the Bureau of Standards, Washington,
D. C., has resigned to take up the work of commercial research
and consultation, with laboratories equipped for research on
problems involving magnetic materials and apparatus and
located at Grasmere, Borough of Richmond, New York City.
He opened his laboratory July 15, 1918.
Mr. Walter T. Schrenk has joined the Chemical Service
Section and is stationed temporarily at the Edgewood Arsenal,
Edgewood, Md., until assigned to active duty.
Mr. William T. Pearce, formerly associate professor of general
chemistry at the North Dakota Agricultural College, has been
promoted to a full professorship.
Mr. Julius Alsberg has recently opened metallurgical and
chemical engineering consulting offices in the Tribune Building,
Chicago.
Mr. P. B. Chillas, Jr., formerly in trie research laboratory
of the National Carbon Company, Inc., is now at the Frankford
plant of the Barrett Co., Philadelphia, Pa.
Mr. A. Lincoln Konwiser, formerly superintendent of the
Hygiene Chemical Co., Elizabethport, N. J., and until recently
connected with the chrome plant of the Metals and Thermit
Corporation, has been appointed factory superintendent and
chemical engineer for J. S. & W. R. Eakins, Inc., Brooklyn,
N. Y.
Mr. Frank Marvin, formerly chief chemist of the Howard
Smokeless Powder Company plant and Aetna Research Labora-
tory at Emporium, Pa., has been appointed explosives chemist
in the Bureau of Mines, and is stationed at Pittsburgh, Pa.
Mr. E. P. Mathewson, who has been with the Anaconda
Copper Company, then with the British-American Nickel
Corporation, recently returned to the American Smelting &
Refining Company as consulting metallurgist. He will be
stationed in the New York office.
Mr. Roger Taylor, formerly with the engineering firm of
Frederick deP. Hone & Co., New York, has been assigned to the
Ordnance Reserve Corps.
Mr. W. F. Geddes, of the Ontario Agricultural College,
Guelph, Ont., has accepted a position with the British Chemical
Company, Ltd., of Trenton, Ont.
Dr. Ernest Anderson is now professor of agricultural chemistry
at Transvaal University College, Pretoria, Transvaal.
Dr. H. H. Helmick has entered the Sanitary Corps and is now
attending the training school at the Rockefeller Institute.
INDUSTRIAL NOTES
List op Applications Made to the Federal Trade Coms
for Licenses under Enemy-Controlled Patents Pvs
"Trading with
the Enemy Act"
I'EAR
Pat. No.
Patentee
Assignee
Patent
1912
1,014,824
Gottlob Honold, Stuttgart,
Robert
Bosch, Stuttgart,
Electric ignition system for
Germany, Max Rail, Paris,
Germai
y
internal-combustion en-
France. Paul Mumprecht,
gines
Brussels, Belgium
1912
1,030.817
Gottlob Honold, Stuttgart,
Robert
Bosch, Stuttgart,
Binding-post for connecting
Germany
Germai
y
electric cables
1908
982,897
Karl Sehirmacher and Her-
Farbwerk
e vorm. Meister
Red vat dye
mann Landers. Hochsl-on-
Lucius
& Briining. Hoehst-
the-Main, Germany
on-the-
Main. Germany
1908
906,367
Oscar Bally, Mannheim, and
Badische
Anilin & Soda
Anthracene dye and process
and Hugo Wolff, Ludwigs-
Fabrik
Ludwigshafen-on-
of making same
taafen-on-the-Rhine, Ger-
the-Rh
ne. Germany
1909
916,029
Albrecht Schmidt and Ernst
Farbwerk
e vorm. Meister
Red-violet dye and process of
Bryk, Hochst-on-the-Main.
Lucius
& Briining, Hochst-
making same
Germany
on. the- Main, Germany
1909
925,917
Filip Kacer, Mannheim, Ger-
Badisehe
Anilin & Soda
Compound of the anthracene
Fabrik.
Ludwigshafen-on-
series and process of mak-
the-Rh
ne, Germany
ing same
1909
929,442
Max Henry Isler, Mannheim,
Badisehe
Anilin & Soda
Anthracene dye and process
Germany
Fabrik.
the-Rhi
Ludwigshafen-on-
ne, Germany
of making same
1909
931,598
Louis Haas, Heidelberg, Ger-
Badisehe
Anilin & Soda
Sulfur dye and process of
many
Fabrik.
the-Rhi
Ludwigshafen-on-
u Germany
making same
1906
818,336
1 Iscar Bally, Mannheim, and
Badisehe
Anilin & Soda
Blue dye and process of mak-
Hugo Wolff, Lugwigshafen-
Fabrik,
Ludwlgshafen-on-
ing same
on-tbe-Rhine, Germany
the-Rh
„, . Germany
1906
809,892
' 'scar Bally and Max Henry
Badisehe
Anilin & Soda
Violet dye and process of
Islc-r, Mannheim, Germany
Pabrik
the-Rhi
hafen-on-
le, Germany
making same
1905
807,422
Karl Elhel. Biebrich. Ger-
Kallc and Company. Aktienge-
Zinc azonaphthol dye and
man y
91 11 1, 1, ,
1. Biebrich, Ger-
process of making same
1905
787,859
Roland Heinrich Scholl.
1; .1 1 hi
Anilin & Soda
Anthracene compound and
Karlsruhe, and Oscar Bally.
Fabrik.
Ludwigshafen on-
process of making same
Mannheim, Germany
the-Rh
11 Gei many
1905
796,393
Oscar Bally. Maiinhcn
Barlisrllc
Anilin & Soil.,
Anthracene coloi ll
many
Fabrik.
Ludwigshafen-on-
and process of making
the-Rh
ne, Germany
same
1904
770,177
Paul l.ilins. Hans Reindel,
Badischc
Anilin .- -ii
A/.o dye and process of mak-
and Fritz Carl Gunthcr,
Pabril
1 u.lw 1;
ing same
Ludwigshafen - on - thc-
the-Rh
11c, Bavai '
Rhine. Germany
many
Applicant
Splitdorf Electrical Company,
98 Warren St., Newark,
N.J.
Splitdorf Electrical Company,
98 Warren St., Newark.
N.J.
National Aniline & Chemical
Company, Inc., 21 Burling
Slip, New York City-
National Aniline & Chemical
Company, Inc., 21 Burling
Slip. New York City
National Aniline & Chemical
Company, Inc., 21 Burling
Slip, New York City
National Aniline & Chemical
Company, Inc., 21 Burling
Slip, New York City
National Aniline & Chemical
Company, Inc., 21 Burling
Slip, New York City
National Aniline & Chemical
Companv. Inc., 21 Burling
a York City
National Aniline & Chemical
Company, Inc., 21 Burljng
Slip, Neu York CitJ
National Aniline & Chemical
Company, Inc.. 21 Burling
Slip, Neu York I'm
National Aniline ,\ Chemical
Company. Inc. 21 Burling
Slip, New Yoil
National Aniline & Chemi, .1
Companv. Inc.. 21 Burling
Slip, New York City
National Aniline & Chemical
i pan] Inc.. 21 Hurling
Slip, New York City
National Anllini 8 • I al
i pany, Inc., 21 Burling
Slip, New York City
66o
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 8
V'BAR
190 J
1903
1903
1902
1902
1907
1908
1907
1907
1907
1907
1906
1906
1913
Pat. No.
741,029
734,866
734,325
715,662
714,882
863,397
948,204
955,105
938,566
876,810
875,390
858,065
856,811
853,041
828.778
818,992
1,063,173
1913 1,063,172
1911
1911
1911
1911
1910
1910
1910
1910
1910
1910
1910
1910
1,003.268
999,439
999,06 '
998,596
970,878
968,697
961,612
961,048
958,325
937,042
I
957.040
Patentee
Richard Gtcy and Otto Sic-
bert, Berlin. Gel
Edward Hcpp, Frankfort -on-
thcMain. and Brut Wol-
Gerraany
Ldward Hcpp, Frankfort-on-
Ilartmann. I !'»chst-on-the-
M:um, ( '.tTiiiiiny
Otto Hess, Hochst-on-the-
Main, Germany
Max II. Isler. Mannheim
Germany
Otto Ernst. Hocbst-on-the-
Main, Germany
Max Isler and Filip Kacer,
Mannheim, Germany
Rene1 Bohn, Mannheim, Ger-
Roland Scholl. Gratz, Austria-
Hungary, and Max Henry
Isler, Mannheim, Ger-
many
Paul Fischer, Elberfeld, Ger-
many
List op Applications, Etc. (.Concluded)
.see Patent
Acticn-Gesellschaft fur Anilin Red azo lake
Fabrikation, Berlin, Ger-
Farbwerke vorm. Meister
Lucius & Bruning, lluchst-
on-the-Main, Germany
Farbwerke
Ma
Mann-
Otto Ernst and Gillis Gull-
bransson, Hocbst-on-the-
Main, Germany
Roland Heinrich Scholl,
Karlsruhe, Germany
Christian Rampini, deceased,
by William E. Warland,
administrator, Brooklyn,
N. Y.
Christian Rampini, deceased,
by William E. Warland,
administrator, Brooklyn,
N. Y.
Richard Just and Hugo Wolff,
Ludwigshafen - on - the -
Rhine. Germany
Wilhelm Bauer, Vohwinkel.
and Alfred Herre and
Rudolph Mayer, Elberfeld,
Germany
Ren* Bohn, Mannheim, Ger-
many
Albrccht Schmidt, Ernst
Brvk, and Robert Voss,
HOcbst-onthc Main, Ger-
965,170 Karl Elbel. Bicbrich, Ger-
Max Henry Isler. Mann-
heim, and Hugo Wolff.
■ ;
Rhine, GermanyJ ,_ j
Fritz llllmann. Berlin, Ger-
many
Albrccht Schmidt and Georg
Kr.iulcin. Hochst-on-the-
Main, Germany
Joseph Deinet, Elberfeld,
Germ
Joseph Deinet, Elberfeld.
rocess for making
quinone dyea
bwerke vorm. Meister Blue anthraquinone dye and
,ucius & Bruning, Hochst- process of making same
n-the-Main, Germany
Farbwerke vorm. Meister
Lucius & Bruning, Ilochst-
on-the-Main. Germany
Badische Anilin 8c Soda
Fabrik, Ludwigshafen-on-
the-Rhine, Germany
Farbwerke vorm. Meister
Lucius & Bruning, Hochst-
on-the-Main. Germany
Badische Anilin & Soda
Fabrik, Ludwigshafen-on-
the-Rhine, Germany
Badische Anilin & Soda
Fabrik, Ludwigshafen-on-
the-Rhine. Germany
Badische Anilin & Soda
Fabrik, Ludwigshafen-on-
the-Rhine, Germany
Farbenfabriken vorm. Friedr.
Bayer & Co., Elberfeld,
Germany
Badische Anilin 8r Soda
Fabrik, Ludwigshafen-on-
the-Rhine, Germany
Farbenfabriken vorm. Friedr.
Bayer & Co., Elberfeld.
Germany
Farbwerke vorm. Meister
Lucius & Bruning, Hochst-
on-the-Main, Germany
Badische Anilin & Soda
Fabrik, Ludwigshafen-on-
the-Rhine, Germany
Farbenfabriken vorm. Friedr
Bayer & Co., Elberfeld,
Germany
Badische Anilin & Soda
Fabrik, Ludwigshafen on-
the-Rhine, Germany
Badische Anilin & Soda
Fabrik. Ludwigshafen-on-
the-Rhine, Germany
Badische Anilin & Soda
Fabrik, Ludwigshafen-on-
thc-Rhine, Germany
Badische Anilin 8c Soda
Fabrik, Ludwigshafen-on-
the-Rhine, Germany
Badische Anilin & Soda
Fabrik, Ludwigshafen-on-
the-Rhine, Germany
Katie & Company, Aktienge-
sellschaft, Biebrich, Ger-
many
Chemische Fabrik Griesheim
Elektron, Frankfort -on-the-
Main, Germany
Farbenfabriken vorm. Friedr.
Bayer & Co.. Elberfeld,
Germany
Badische Anilin & Soda
Fabrik, Ludwigshafen-on-
the-Rhine, Germany
Farbwerke vorm. Meister
Lucius *: Bruning, Hochst-
on-the-Main, Germany
Kallc & Company Aktienge-
scllschaft, Biebrich, Ger-
many
Badische Anilin & Soda
Fabrik, Ludwigshafen-on-
tlic-Rhine. Germany
Acticii Geselbchaft far Anilin
Fabrikation, Berlin. Ger-
many
Farbwerke vorm. Meister
Lucius & Bruning, HV:hst-
on-the-Main, Germany
Farbenfabriken vorm. Friedr.
Bajrtl & Co, Elberfeld,
Germany
Farbenfabriken vorm. Friedr.
at B Co.. Elberfeld,
Germany
Producing a
quinones
thereof
Producing
quinones
thereof
Applicant
National Aniline & Chemical
Company. Inc., 21 Burling
Slip, New York City
National Aniline & Chemical
Company, Inc., 21 Burling
Slip, New York City
National Aniline & Chemical
Company, Inc., 21 Burling
Slip, New York City
National Aniline & Chemical
Company, Inc.. 21 Burling
Slip, New York City
National Aniline & Chemical
Company, Inc., 21 Burling
Slip. New York City
National Aniline 8c Chemical
Company, Inc., 21 Burling
Slip. New York City
National Aniline & Chemical
Company, Inc., 21 Burling
SUp, New York City
National Aniline & Chemical
Company, Inc., 21 Burling
Slip, New York City
National Aniline & Chemical
Company, Inc., 21 Burling
Slip, New York City
National Aniline & Chemical
Company, Inc., 21 Burling
Slip, New York City
National Aniline & Chemical
Company, Inc., 21 Burling
Slip, New York City
National Aniline 8c Chemical
Company, Inc., 21 Burling
Slip, New York City
National Aniline & Chemical
Company, Inc., 21 Burling
Slip, New York City-
National Aniline & Chemical
Company, Inc., 21 Burling
Slip, New York City
National Aniline & Chemical
Company, Inc., 21 Burling
SUp, New York City
National Aniline & Chemical
Company, Inc., 21 Burling
Slip, New York City
National Aniline 8; Chemical
Company. Inc., 21 Burling
Slip. New York City
National Aniline & Chemical
Company, Inc., 21 Burling
Slip, New York Citv
ainoanthra- National Aniline & Chemical
nd derivatives Company, Inc., 21 Burling
Slip, New York City
Green anthraquinone dye and
process of making same
Anthracene dye and process
of making same
Monoazo dye and process of
making same
Anthraquinone compound
and process of making
same
Indanthrene monosulfonic
acid and process of making
same
Anthracene dye and process
of making same
Anthracene dye and process
of making same
Anthraquinone derivative
Dye of the anthraquinone
series and process of mak-
ing same
Anthraquinone derivative
Compound of the anthra-
quinone series and process
of making same
Anthracene dye and process
of making same
Vat-dyeing coloring-matte
Vat dye and process of mak-
Vat dye and process of
ing same
Process of condensing reduc-
tion products ot acenaph-
thenequinone, etc.
Anthracene compound and
process of making same
Anthraquinooe-diacridones
Urea of the anthraquinone
scries and process of mak-
ing same
Vat dye
National Aniline & Chemical
Company. Inc.. 21 Burling
Slip, New York City
National Aniline & Chemical
Company, Inc., 21 Burling
SUp, New York City
National Aniline 8c Chemical
Company, Inc., 21 BurUng
Slip, New York City
National AniUne & Chemical
Company, Inc., 21 BurUng
SUp, New York City
National AniUne & Chemical
Company, Inc., 21 BurUng
SUp. New York City
National AniUne & Chemical
Company, Inc., 21 BurUng
Slip, New York City
National AniUne & Chemical
Company, Inc , 21 Burling
Slip. New York City
National Aniline & Chemical
Company. Inc., 21 Burling
Slip, New York City
National AniUne & Chemical
Company, Inc.. 21 Burling
Slip. New York City
National AniUne & Chemical
Company. Inc.. 21 Burling
SUp. New York City
National Aniline 8: Chemical
Company, Inc., 21 Burling
SUp. New York Cits-
National Aniline & Chemical
Company. Inc., 21 BurUng
Slip. New York City
Aug., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
661
An item in the May issue of This Journal, taken from Drug
& Chemical Markets, April 3, 1918, announcing the establish-
ment of a school for poison-gas workers at the Case School of
Applied Science, Cleveland, Ohio, was incorrect. We have re-
ceived, a note from Prof. W. R. Veasey stating that no such
schooljrhas been contemplated.
On' the afternoon of June 18, 191 8, the National Aniline and
Chemical Company held open house in their recently equipped
Main Office Building, 21 Burling Slip, New York City, the whole
building being open for the inspection of the visitors.
The third trial of the suit of the Baugh Chemical Company
against the Davison Chemical Company for $500,000 damages,
breach of contract by failure to deliver the quantity of sulfuric
acid stipulated in a contract entered into between the two cor-
porations being alleged, ended in the Supreme Court, June 2,
when the jury returned a verdict for $139,433.65. The award
was not only for damages held to have been sustained by the
Baugh Company, but also for interest added from the date of
the breaking of the contract.
Under the direction of Dr. E. R. Pickrell, chief chemist of the
United States Appraiser's Laboratory in New York City, the census
of chemical imports being taken for the Government is pro-
gressing rapidly, and definite ideas of value, which the completed
work will have, are now apparent. Data concerning the tonnage
brought into the country, valuation concerning some 2,500
chemical descriptions, and allied products not heretofore avail-
able anywhere, have been unearthed, so to speak, and are now in
process of tabulation by Dr. Pickrell and his small staff of as-
sistants. While a great amount of work has been ac-
complished in the two months that have elapsed since the work
was started, there still remains a vast amount of detail to be
completed, and it will be probably a number of months more
before the results can be published. This work was undertaken
primarily to show those engaged in the chemical and allied
industries in the United States just what foreign competition
they will encounter after the war.
The Bragdon, Lord and Nagle Company, Textile World
Journal, has issued a directory of textile brands and trade
marks which is a most valuable reference book, and is the first
of its kind issued in this country. A list of over 13,000 trade
marks and brands is in the first issue, and a brief description is
given to identify the product.
The War Trade Board has adopted the following additional
rule and regulation with respect to the issuance of licenses to
export any commodity to the United Kingdom, France, Italy,
and Belgium (excluding their respective colonies, possessions,
and protectorates) : Written approval of the mission in the
United States of the country to which the exportation is to be
made must be obtained in order to file applications for licenses
to export any commodity to the Allied Nations.
Due to the increasing need of petroleum oil which is steadily
outdistancing the visible supply, oil shales are already being
considered not only to make up a developing shortage, but as
the future oil reserve.
Several western coast concerns are now engaged in the manu-
facture of potash from kelp. The Bureau of Soils of the United
States Department of Agriculture began the construction of an
experimental plant for the extraction of potash from kelp last
April at Summerland, California. The purpose of this plant
is to determine the cost of producing potash from kelp, and also
to determine what by-products can be produced commercially.
The kelp char, containing about 30 per cent K20, has been the
most important product up to date.
Due to the excessive prices charged in some instances for
toluol when sold under release for other than military purposes,
the War Industries Board has extended the Government price
to cover all toluol sold.
The Kaiser has approved the foundation of a Trust to be known
as the Kaiser Wilhelm Trust for Promotion of the Science of War.
The aim of the Trust is to further the development of scientific
and technical aids to warfare, by uniting the scientific and the
military forces of the country for work together. The scientific
work is to be carried on by the following technical committees:
1 — Committee for the chemical raw materials for the pro-
duction of munitions-manufacturing materials.
2 — Committee for chemical war materials (powder, explosives,
gas, and the like).
3 — Committee for physics, including ballistics, telephony,
telegraphy, determination of targets and distances, measure-
ments, and the like.
4 — Committee for engineering and communication.
5 — Committee for aeronautics.
6 — Committee for obtaining and preparation of metals.
The Cleveland Salt Company has bought land near Lorain,
Ohio, for a plant which will produce salt and by-products used
in the manufacture of pharmaceutical chemicals. The invest-
ment will be close to $6,000,000.
The Grand Jury of Richmond County, S. I., handed up a
statement to Supreme Court Justice Kelby on June 21 con-
demning the Staten Island garbage plant as a nuisance. At
the same time the Grand Jury agreed to give the Metropolitan
By-Products Company, the operators of the plant, an extension
of sixty days in order that they might install machinery to abate
the nuisance complained of.
44.347,78o barrels of petroleum taken from the oil fields east
of the Mississippi River were marketed in 191 7, compared with
44,628,693 barrels in 1916 and 51,083,331 barrels in 1914. The
value of the oil at the wells in 191 7 was $15,887,864, which was
26 per cent more than the value of the output from these fields
in 1916, though the 191 7 production was a fraction smaller than
the output of 1916.
The Gulf Sulfur Company, Big Hill, Texas, is developing a
sulfur mine at Big Hill, Texas. The company has already bored
several wells and has penetrated a large deposit of sulfur of great
thickness.
The Applied Chemical Corporation, Manhattan, N. Y.,
manufacturing chemicals, has been incorporated with a capital
of $100,000. The incorporators are J. S. Robinson and others.
The Palatine Aniline and Chemical Corporation, Pough-
keepsie, N. Y., has been incorporated with a capital of $150,000.
The incorporators are A. R. Mullaly, C. O. Terwilliger, and D.
DeForest.
Spalding, Inc., of Manhattan, N. Y., manufacturing drugs,
chemicals, etc., has been incorporated with a capital of $100,000,
by D. H. Dutton, L. Lens, G. C. Spalding.
The United States Chemical Laboratory in Madison, Wis-
consin, reports that turpentine may be produced from resin and
pitch of the larch trees of the Montana forests, especially in
District No. 1.
The output of all potash materials produced and marketed
in the United States in 1917, as reported by the manufacturers
to the United States Geological Survey, Department of the
Interior, was 126,577 short tons, which contained 33,366 short
tons, or an average of 26.4 per cent of pure potash. This is
more than three times the quantity produced in 19 16 and corre-
sponds very closely with the output predicted for 1917 by H. S.
Gale, of the Survey, from a review of the mid-year statistics.
The total value of the potash produced in the United States in
1917 was $13,791,922.
The Commercial Cylinder Co., Hackensack, N. J., has been
incorporated with a capital of $800,000. The incorporators are
A. R. Oakley, Pearl River, N. Y., and Paul E. Britsch, Brooklyn,
N. Y.
With a capital of $150,000 the Croton Color and Chemical
Company has been incorporated at Croton, Westchester County,
N. Y., to manufacture aniline dyes. The incorporators are
Paul P. Ihrig, Edward R. Vollmer, and Frank C. Schmitz:
The United States Government has bought five acres of land
east of the Niagara Smelting Company's plant as a site for the
.new million-dollar electrolytic alkali plant. The contract for
the erection of the plant has been given to J. G. White Engi-
neering Co., New York City.
The Hercules Oil Company, Delaware, has been incorporated
with a capital of $2,000,000. The incorporators are W. F.
O'Keefe, G. G. Steigler, and J. H. Dowdell of Wilmington.
The War Industries Board announced on June 27 that, as a
result of a meeting of the manufacturers of sulfuric and nitric
acid with the Price-fixing Committee of the War Industries
Board, maximum prices have been agreed upon and approved
by the President, taking effect immediately, and expiring
September 30, 1918. The prices agreed upon are as follows:
Sulfuric acid, 60 ° Be., $18 per ton of 2,000 lbs.
Sulfuric acid, 66° Be., $28 per ton of 2,000 lbs.
Sulfuric acid, 20 per cent oleum, $32 per ton of 2,000 lbs.;
f. o. b. at manufacturers' works in sellers' tank cars.
In carboys in carload lots, l/2 cent per lb. extra. In carboys
in less than carloads, */« cent per lb. extra. In drums, any
quantity, l/« cent per lb. extra.
Nitric acid, 42 ° Be., 8l/a cents per lb., f. o. b., manufacturers
works in carboys.
A schedule of maximum prices on mixed acids is being prepared,
and will be announced later. It is understood and agreed that
any deliveries made after Sept. 30 will be subject to any revision
in price which the Government may make.
662
THE JOl RNAL "I INDl si HI AL AM) ENGINEERING ( BEMISTRY Vol. 10, No. 8
GOVLRNMLNT PUBLICATIONS
By R. S. McBridk, Burea
NOTICE — Publications for which price is indicated can be
purchased from the Superintendent of Documents, Government
Printing Office, Washington, D.1 C. Other publications can
usually be supplied from the Bureau or Department from which
they originate. Commerce Reports are received by all large
libraries and may be consulted there, or single numbers can be
secured by application to the Bureau of Foreign and Domestic
Commerce, Department of Commerce, Washington. The regu-
lar subscription rate for these Commerce Reports mailed daily is
$2.50 per year, payable in advance, to the Superintendent of
Documents.
GEOLOGICAL SURVEY
Lime in 1016. ('. I* LouGHUN. From Mineral Resources
of the United St ill 30pp. Published March 11.
The total quantity of lime sold in 19 16 was 4.°73-433 short
tons, valued at $18,509,305, an increase over the revised figures
for [915 of 450,623 tons, or mure than 12 per cent, in quantity,
and of J4.085.269, or 28 per cent, in value. This was the first
year in which the lime marketed in the United States equaled
or exceeded 4,000,000 tons.
The increase in output was accompanied by the greatest
111 average price per ton ever recorded by the United
Geological Survey, an increase due both to greater de-
mand and to greater cost of fuel and labor. These same causes
account largely for the decrease of 128 in the number of active
plants, which in 1916 was 778, the lowest ever recorded by the
Survey. The decrease was principally among the small pro-
ducers in Pennsylvania, where there were 116 fewer operators
active in 1916 than in 1915. The number of kilns in operation
increased from 2,340 in 1915 to 2,341 in 1916.
A quantity of marl burned or dried for agricultural use. some
of which has been formerly included in the lime figures for Ar-
California, New York, Pennsylvania, South Carolina,
and Virginia, is here stated separately for the first time. The
total quantity of marl sold for this use in 1916 was 35,588 short
tons, valued at 5.107,768, or S3.03 a ton. Individual reports
gave prices ranging from Si to S3 a ton in the Southern States
and from S4 to $6 a ton in the Xorthern States and California.
I.imi: Soli, in tut; I'mthi' states in 1916 i .
Building lime 1 ,509,968
... ,,r;.' 621,120
Paper mills 353.187
Suxrir factories 21,923
59.919
Agriculture
KluxinK 180,018
uses not specified 373.01 1
.140,701)
Value
7,859,614
2,298.246
1,461.412
118.572
278.003
712.101
;s siw.nis
3.626,998
Average
Price
Per Ton
5.21
3.70
4.14
5.41
4 64
3.63
3.96
5.02
4.54
5.06
4.073.433
Percentage of increase in 1916
Hydrated lime (included in total) 717,382
Percentage of increase in hydrated lime
,„ 1916 23.4
Fuel Briquetting in 1917. 1 E LSSHBR From Mineral
Resources ol the i nited States, 1917, Part II. 3 pp. Pub-
lished May 6 The production of fuel briquets in 11117 was
net tons, valued .it $2,233,888, an increase compared
with mi'' of 111.701 ton-, or 38 per cent, in quantity, and
$788,226, or So per cent, in value. The production in 1017
was the greatest recorded The progress of the industry' for
the 11 \c.us from 1907 to 1017. inclusive, is shown graphically
in a diagram the article,
of the 13 plant', in operation in 1017. 4 used anthracite as
.1 i.iu material; 1, Arkansas semi anthracite ; .'. a mixture of
anthracite and bituminous slack; 2, bituminous slack and sub-
bituminous coal, i. semi-bituminous coal; i, brown lignite;
i of Standards, Washington
and 2, oil gas residue. At 2 plants coal tar pitch was used as
a binder, al t. mixed coal-tar pitch and asphaltic pitch; at 5,
asphaltic pitch; at 1, a patent binder; and at 4, no binder what-
Petroleum in 1916. J. I) Northrop. Separate from Mineral
Resources of the United States, 1916, Part II. 207 pp. Issued
April 26 The quantity of petroleum marketed from the oil fields
of the 1 nited States in 1916, which amounted to 300,767,158 bar-
rels of 42 gallons each, establishes a new record of petroleum out-
put in this country that is nearly 7 per cent greater than the former
maximum yield of 281,104,104 barrels, established in 1915.
The average price received at the wells for this oil was $1.10 per
bbl., and the total market value of the output was S330.899.868,
a gain of 40 cents in average unit price, and of $151,436,978,
or 84 per cent, in gross market value, compared with 1915.
DISTRIBUTION OF PETROLEUM MARKETED IN THE UNITED STATES D» 1916
The accompanying figure shows graphically the relative
importance of the several States as contributors to the marketed
production of petroleum in the United States in 1916.
Natural Gas in 1916. J. D. Northrop. Separate from
Mineral Resources of the United States, 1916, Part II. 93 pp.
Issued May 4, 1918.
The volume of natural gas commercially utilized in the United
States in 1916 was greater than that so utilized in any other
year in the histtiry of the natural-gas industry. The volume used,
which amounted to 753,170.253.000 cu. ft., constituted a new
record of production, exceeding by nearly 125,000,000,000 cu. ft.,
1 cent, the former record, established in 1915.
The market value of this gas likewise attained record pro-
portions It amounted to $120,227,468, a gain of $18,915,087,
or 18.6 per cent, over the market value of the output in 1915-
The average price per [OOO cu. ft was 15.96 cents, a loss of 0.16
cent compared with 1915.
Credit for the increased production in 1916 belongs, in the
order given, to West Virginia. Oklahoma, Pennsylvania. Cali-
fornia. Louisiana. Kansas, Texas, and Arkansas, which together
produced 132,000,000,000 cu. ft. more gas in 1916 than in 1915.
Of the total volume of natural gas produced and consumed
111 1916, it is estimated that 255.380,764,000 cu. ft., or 31 per
cent, were distribute.'. | domestic consumers at an
Aug., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
663
Distribution by States of Production of Natural Gas in the
United States in 1916
average price of 28.63 cents per 1000 cu. ft., and that the re-
maining 69 per cent, or 517,789,489,000 cu. ft., was distributed
to 18,278 industrial consumers at an average price of 10.21
cents per 1000. Compared with 19 15, these data show gain of
8 per cent in volume, of S per cent in number of consumers,
and of 1 per cent in average unit price of gas supplied for domestic
use, and a gain of 26 per cent in volume and of 5.5 per cent in
average unit price, but a decrease of 0.4 per cent in the number
of consumers of gas supplied for industrial use.
The proportion of natural gas supplied to industrial consumers
in 1916 was 4 per cent larger than in 1915.
The history of the natural-gas gasoline industry in the United
States is the history of one of the most effective movements in
the direction of true conservation of natural gas that has ever
been undertaken in this country. Although the foundations
of this industry were laid in 1903 and 1904, the period of its
greatest expansion is included in the seven years since 1909.
In 191 1, the first year for which statistics on the subject are
available, 176 plants in 9 states produced 7,425,839 gal. of raw
gasoline from natural gas. In 1916, only 5 years later, 596
plants in 12 states produced 103,492,689 gal., a gain in this re-
markably brief period of nearly 239 per cent in the number of
plants and of nearly 1,294 Per cent in the annual output of raw
gasoline. The volume of natural gas treated in the production
of the output of gasoline in 191 1 was only 0.5 per cent of the
volume of gas produced and utilized in the entire country in
that year. The volume treated in 1916 represents 27.7 per
cent of the volume produced and utilized in that year and is
greater by 8,330 per cent than the volume treated in 191 1 . The
fact that the output of gasoline from natural gas has increased
in the last 5 yrs. more rapidly than the number of plants is
evidence that the trend of the industry has been toward the
erection of plants of larger individual capacity than were at
first considered feasible. The fact that the volume of gas treated
annually has increased in the same period at a rate far greater
than that of the raw gasoline produced, emphasizes the trend
of the industry toward the successful utilization of gas leaner
in its content of gasoline vapors than was believed possible in
the early days of the industry. The trend in the latter direc-
tion has been most pronounced in the last 2 yrs., as a conse-
quence of the development of the absorption process, which
renders feasible the treatment of gas containing as low as 1 pint
of gasoline to 1,000 cu. ft.
Distribution by States of Consumption of Natural Gas in the
United States in 1916
Prior to 1916 the greater proportion of the gasoline produced
from natural gas was obtained from casing-head gas, oil-well
gas, or "wet" natural gas by the compression and condensation
method which, however, is restricted in its profitable applica-
tion to gas that contains not less than 1 gal. of gasoline to
1,000 cu. ft. The development of the absorption process has
extended the field of the natural-gas gasoline industry to in-
clude practically all the natural gas produced in the United States,
for there is but little gas produced in this country that does not
contain appreciable percentages of pentane and hexane, the
hydrocarbons of the paraffin series that are the principal con-
stituents of gasoline. Much of the so-called "dry" gas obtained
from oil wells when they are first opened and from gas wells
that produce no petroleum has been found sufficiently rich in
gasoline vapors to warrant treatment by the absorption process,
though excluded from successful treatment by compression and
condensation.
Mineral Waters in 1916. A. J. Ellis. With a Comparison
of American and European Mineral Waters by A. A. Chambers.
Separate from Mineral Resources of the United States, 1916,
Part II. 47 pp. Issued March 13.
The number of active mineral springs was slightly smaller,
but the production and value were greater in 19 16 than in 19 15.
The increase in production was 3,814,958 gal., or 7 per cent.
The increase in value of medicinal waters was $61,522 and in
value of table waters was $534,719; thus the total increase in
value of sales was $596,241, or 12 per cent.
Practically four-fifths of the mineral waters was sold at prices
ranging from one-half cent to 10 cents per gal. during 1913,
1914, 1915 and 1916. The percentage sold for more than 30
cents per gal. was nearly double what it was in 1915 and consti-
tuted a little more than 8 per cent of the quantity sold in 1916.
The water from 487 springs was sold for 10 cents or less per gal.
and the water from 9 springs was sold for more than $1 per gal.
Thi- average price per gallon in 1916 was 10 cents.
Tin total imports of mineral waters have decreased more
than 50 per cent in four years, from 3,562,863 gal. in 1913 to
1,723,440 gal. in 1916. It is worthy of note that, large as these
figures for imports are, they represent only a relatively small
percentage of the total consumption of mineral waters in the
United States. Rarely do they amount to more than 6 per
cent of the total consumption, anil lor the years 1913 to 1916,
inclusive, they are somewhat less than 4.5 per cent.
664
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 8
Those who have Found it difficult or impossible to obtain
waters that were previously imported will doubtless be interested
in the possibility of substituting domestic waters for certain
famous mineral waters of Europe as indicated by the following
comparisons of analyses of mineral waters from this country
and from abroad. In the analyses only the more common con-
stituents are given, and for the convenience of those desiring
more detailed information regarding these and other analyses
a bibliography has been appended. To discover two or more
natural waters, each of whose dozen or more constituents is ex-
actly the same in kind and concentration, would be difficult if
not impossible, but an attempt is made here to show that the
waters compared are similar in chemical character, degree of
mineralization, and relative proportion of various constituents.
As medical practice varies sometimes as much as ioo per cent
in the dosage of many of the inorganic substances present in
natural solutions, it seems reasonable to assume that waters
differing not too widely in composition might be used for the
same purpose with similar if not identical physiologic effects.
Five common types of mineral waters are discussed here —
ate (or iron), carbonate, sulfide or "sulfur," chloride,
and sulfate waters.
BUREAU OF FOREIGN AND DOMESTIC COMMERCE
Railway Materials, Equipment, and Supplies in Australia
and New Zealand. F. Riika. Special Agents Series No. 156.
164 pp. Paper, 25 cents.
Textile Markets of Bolivia, Ecuador, and Peru. W. A.
Tucker. Special Agents Scries Xo. 158. 106 pp. Paper,
15 cents.
Construction Materials and Machinery in Colombia. \V. W.
EwiNG, Special Agents Series No. 160. 75 pp. Paper, 15 cents.
COMMERCE REPORTS APRIL IO18
By the terms of the "Nonferrous Metal Industry Act,"
recently passed by Great Britain, no persons or firms having any
enemy connections are permitted for a period of 5 yrs. after the
end of the war to engage in extracting, smelting, refining, or
dealing in nonferrous metals or ores, including zinc, copper,
tin, lead, nickel, and aluminum. (P. 4)
A new Danish by-product of fish offal, known as "cornimite,"
is proposed for electrical insulators and as a substitute for
"galalith." the plastic made from casein. Other products of the
herring industry are fish oil, "fibrin," fish bones, and guano.
(P. 20)
In a report of a special British committee appointed to con-
sider the status of the sulfuric acid and fertilizer industries
after the war, it is suggested that extended measures be taken to
increase the use of fertilizers, by education, cooperation, and
i Uunsportatioii of sulfuric acid and fertilizers. In
order to avoid a future surplus of sulfuric acid from the present
munitions plants, provision is suggested for (a) an increased
rati of deprei iation on acid plants in figuring taxes, (6) scrapping
of plants not required, or (e) tempoi ltj hut downs, with in-
terest paid by the government. Of special interest to chemists
is the following recommendation "in view of the importance
of scientific control of chemical operation, we desire to draw
i t < > the need ior improving the status of the technical
chemist We consider thai it is essentia] to the success of the
chemical industries of the country thai the value of men of liberal
education who have specialized in chemistry and Us cognate
sciences and have experience of manufacturing operations
should lie more adequately tecognized." (P. 29)
The cultivation and preparation of "alia grass" or "esparto"
in Tunisia. Africa, is described in detail [Pp. 40-44)
Among new sources of alcohol suggested in Australia, is the
nut of the /ami. 1 palm, or burrawong palm. The nuts contain
1 Qt of starch, which can l>e malted, fermented, and dis-
tilled, yielding 45 gal. of alcohol per ton, at a very low cost.
(P. 45)
In a report on the dyestuff industry in Great Britain, evidence
of satisfactory progress is shown in the list of important dyes
being made by several companies. P. 52;
In a British conference on careers for girls with secondary
education, emphasis was laid upon the need and opportunity
for women chemists in the chemical industries. (P. 60)
Increased production of pig iron and steel in Canada is due
chiefly to the increased output of electric furnaces. (P. 70)
The use of the metric system has been made obligatory in
Uruguay. (P. 107)
The use of seaweed, previously freed from saline material, as
fodder for horses, is receiving serious consideration in France.
(P. 108)
Production and shipments of nitrate from Chile has increased,
and is now considerably above that of 1914, when it commenced
to decline. (P. 132)
Experiments are in progress in Norway to operate automobiles
with acetylene, which can be readily produced from the calcium
carbide now made by water power. (P. 144)
Production of mica in Brazil has greatly increased on account
of greater demands for mica for electrical insulation, and as an
absorbent of nitroglycerine in dynamite. (P. 148)
Detailed consideration of the natural indigo industry of India
shows that its future prospects depend upon the possibility of
controlling the Eastern (Chinese and Japanese) markets.
(P. 168)
It is estimated that the Tofo iron ore mines in Chile (con-
trolled by the Bethlehem Steel Company) contain 100,000,000
tons of ore with 68 per cent iron. A large loading basin and
breakwater, and large bins, etc., have been constructed at Cruz
Grande, a port 14 miles from the mines. Electric locomotives
will be used, with regenerative braking system on the loaded,
downward-bound trains. (Pp. 170-3)
Bolivian tin ores are now being smelted in Chile, using Cali-
fornia petroleum residuum as fuel. (P. 187)
Wood alcohol, obtained from sulfite pulp mills, is being used
as a substitute for gasoline for motor fuel in Sweden. (P. 218)
Extensive deposits of molybdenum ores have been found near
Christiania, Norway. (P. 311)
A new insulating material known as "molersten" and used
for covering hot air and steam pipes has been developed in Den-
mark. It is made by mixing loam from heath clay beds with
cork dust and molding into bricks which are then burnt, pro-
ducing a porous structure. (P. 312)
Cardboard containers for jams, biscuits, etc., have largely
replaced tin containers in England. (P. 323)
Analyses are given of 25 varieties of coal mined in Japan.
(P- 330
All supplies of fertilizers in Sweden have been requisitioned
by the government. (P. 334)
The Brazilian government has offered to finance factories for
making caustic soda. (P. 353)
Special Supplements Issued ln Apkil
l nitlp Kinodoh — 19a and b French Indo China — 54a
■J 2* Australia — 60a
British India — 506 Algeria — 63a
Statistics of Exports to the United States
Barcelona (P. 87)
Argots
Glycerin
Licorice
Calcium tartrate
Potassium carbonate
cork
Olive oil
Paper stock
Christiania. Norwav Denmark (P. 267)
Oxalic acid
Sodium nitrate
Hides
Matches
Paper
Wood pulp
Cbalk
Diamonds
Flint pebbles
Hides
Ink
r..pcr
Porcelain
Rags
Rennet
Aug., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
665
Calcutta (P. 126)
Drugs
Hides
Manganese ore
Mica
Shellac
London — Sup. 19a
Bismuth
Coaltar products
Senna leaves
Gum copal
Gum lac
Gum shellac
Gum tragacanth
Rosin
Indigo
Mineral wax
Diamonds
Fertilizers
Hides
Rubber
Iridium
Leather
Coconut oil
Palm oil
Palm kernel oil
Paper
Platinum
Graphite
Tin
Chalk
Alkalies
Ergot
Buchu
Gum arabic
Opium
Celluloid
Glue
Grease
Rapeseed oil
Castor beans
Statistics op Exports to the U.
Malaga, Spain
(P. 403)
Thymol
Olive oil
Essential oils
Iron ore
Barite
Ochre
Iron oxide pigment
England (Misc.) —
Sup. 196
Aeroplane parts
Chalk
Ammonium carbonate
Ammonium chloride
Sulfur
Sodium bicarbonate
Glass
Iridium
Indian red
Varnish
Artificial silk
Fullers' earth
Australia — Sup. 60a
Casein
Hides
Manganese ore
Osmiridium
Eucalyptus oil
Tin
Zinc ore
Algiers — Sup. 63a
Argols
Bones
Dyewood
Glue stock
Hides
Zinc ore
Infusorial earth
(Concluded)
Vera Cruz (P. 390)
Chicle
Hides
Lead
Mercury
Silver
Mexico — Sup. 32a
Antimony
Guano
Beeswax
Bones
Calamine
Copper
Cottonseed oil
Cottonseed cake
Glycerin
Gold
Hides
Lead
Lead ore
Mercury
Zinc ore
British
506
Hides
Indigo
Paraffin
Manganese o:
Mica
Myrabolans
Vegetable oil:
Saltpeter
Castor seed
Linseed
COMMERCE REPORTS— MAY 1018
Production of tin and tungsten ores in the Siamese Malay
States is increasing. (P. 418)
Efforts are being made to increase the production of oil from
seeds and nuts in West Africa, including n'gore nuts and
n'kamba nuts. (P. 420)
It is estimated that by proper methods of extraction, over
300,000 tons of potash could be secured annually as a by-product
of the nitrate deposits of Chili. The average potash content of
the crude nitrate is estimated at 1.73 per cent. (P. 437)
Exports of logwood and fustic from Jamaica to the United
States show a marked increase. (P. 454)
The world's demand for bismuth is not great (about 600 tons
annually). The present output could be greatly increased
and the price reduced if there were sufficient demand. The
principal sources are Bolivia and Australia. The chief use is in
alloys, including those used for stereotype metal (very occa-
sionally); for silvering mirrors; for fusible boiler plugs, automatic
sprinklers, electric fuses, low melting solders, and dental alloys;
and for tempering baths for steel. Salts of bismuth are used
medicinally and for porcelain painting and enameling, and in
staining glass. (P. 474)
Brazil is now manufacturing sufficient calcium carbide not
only for domestic consumption, but for export. (P. 475)
Statistics of the War Industries Board show that the annual
consumption of tin in the United States is about 76,000 tons;
and imports only about 70,000 tons. Part of the deficit is made
up by tin recovered by detinning, etc. (P. 506)
More than half of the gypsum mined in England is obtained
from the Nottingham district, where it is especially white. It
is used for making mineral white or terra alba, plaster of Paris
and Keene's cement. (P. 521)
Owing to lack of transportation cottonseed cake is being
used in large amounts as a fuel in Egypt. The ash is a valuable
fertilizer. (P. 531)
The Brazilian government has offered to lend to the first
three parties engaging in the manufacture of caustic soda,
75 per cent of the cost of the plant (but not more than $500,000).
It is expected that electrolytic plants will be erected. (P. 534)
Among measures proposed in Brazil to provide supplies of
fuel for iron smelting is that of planting eucalyptus trees to be
used for making charcoal, and the subsidizing of coal and steel
producers. (P. 568)
Exports of manganese ore from Brazil have increased from
122,000 tons in 1913 to 533,000 tons in 1917. (P. 637)
Efforts to develop the pressing of linseed oil in Argentine
for export, thus conserving cargo space, have failed because of
(a) limited capacity of existing factories, (6) use of pressing
facilities for edible oils, (c) lack of machinery, (d) lack of local
market for linseed cake, and (e) necessity of importing cans or
drums for shipping the oil. (P. 666)
Production of quebracho extract in Argentine could be greatly
increased under favorable conditions. At present a considerable
amount of quebracho wood is exported to the United States,
requiring increased tonnage. (P. 682)
Exports of antimony from China show a decrease, owing
to the return to normal prices. The most successful process in
use is the "oxide process" devised by a Frenchman, Herren-
schmidt. In the process the low-grade ores are mixed with
charcoal, and burned in a furnace, producing antimony oxide,
which partly condenses and is partly recovered by washing the
gases. The oxide is reduced to metal by heating with soda
and charcoal. The processes are described in some detail. (Pp.
699-703)
Mineral products of Tunisia include ores of lead, zinc, iron,
and manganese, and phosphates and lignite. (P. 704)
Production of divi-divi in the Dominican Republic is de-
creasing. (P. 708)
Iron ore containing 66 per cent of iron has been discovered in
Queensland, Australia. (P. 777)
•Other mineral products of Queensland are tin, tungsten,
copper, gold, diamonds, and petroleum. (P. 778)
Imports of chemicals and drugs into Great Britain in March
1918 show an increase of 30 per cent over March 1917. while
exports show a decrease of 8 per cent. (P. 783)
The use in Germany of "cellulon," a fiber produced from
wood pulp, is increasing greatly, especially as a substitute for
jute for army needs. The details of the manufacture are not
available, but it is claimed that some cotton or wool waste is
mixed with the wood pulp cellulose. (P. 788)
Large supplies of dyewoods, including fustic, brazilwood,
and mora, are available in Mazatlan, Mexico. (P. 804)
The following mineral products of Canada show increased
output in quantity: Cobalt, molybdenite, nickel, zinc, mag-
nesite, natural gas, petroleum, pyrites, quartz, salt, lime, sand,
and gravel. These show a decrease; Copper, gold, pig iron,
lead, silver, asbestos, coal, graphite, gypsum, and cement.
(Supplement 23a, P. 7)
Special Supplements Issued
in May
Greece— 7a
Scotland-
-19a"
Netherlands — 9a
Canada—
23a and b
Leeds — 19c
British East Africa — 65a
Statistics of Exports to the United States
Hull. England (P.
Scotland — Sup. l°d
.Glasgow (P. 469)
483)
Linoleum
Acids
Gum copal
Paper
Ammonium sulfate
Cresol
Acids
Rubber
Ammonium sulfate
Corundum
Castor seeds
Bone charcoal
Creosote
Netherlands — Sup.
Brass wire cloth
Corundum
Sodium cyanide
9a
Creosote oil
Fertilizers
Beeswax
Sodium cyanide
Hides
Chemicals
Fertilizers
Grease
Magnesite
Dyes
Hides
Manganese ore
Diamonds
Leather
Sumac extract
Earthenware
Magnesite
Fertilizers
Glassware
Glue
Manganese ore
Paper stock
Sumac extract
Leeds, England-
Sup. 19c
Hides
Vancouver — Sup. 236
Brass
Ink
Coal
Naphthol
Matches
Copra
Phenol
Paper stock
Paraffin
Fertilizer
Cresol
Gold
Orchid liquor
Rubber
Magnesite
Wool grease
Stearin, pitch
Rubber
Leather
666
THE JOl RNAL OF TNDl STRIAL AND ENGINEERING i HEMISTRY Vol. 10, No. 8
BOOK REVIEWS
Methods for the Commercial Sampling and Analysis of Coal,
Coke, and By-Products. Compiled by the Chemical Sub-
Committee of the United States Steel Corporation under the
direction of J. M. Camp, Carnegie Build irgh, Pa.,
1917. 91 pp., 7 figs., 1 plati 1
The main purpose of the work has I
chemical methods used in the various plants of thi
tee] <■ orporation, having special reference to methods
for the sampling and analysis of coal, coke, and by products,
with the addition of a special feature m the form of well-illus-
trated directions for determining the yield of by-products for
the evaluation of coal preliminary to its use in actual coking
processes. This work is of special intere t at the present time
for the reason that the methods cover material which is of \ital
importance now. setting forth, moreover, the methods in actual
use by the chemists whos( daily work is largely taken up with
the proce i h cribed. While the methods for the analysis
i mailable there is not so much litera-
ture it band covering the determination of by-products such as
the ammonia liquors and still wastes, crude tar and tar distil-
lates, light oil and benzol products, etc.
S. W. Parr
Chemistry of Materials. By Robert B. Leighou, Sc.B.,
Associate Professor of Chemistry in the Carnegie Institute of
Technology. 8vo. xv + 440 pp. Illustrated. McGraw-
Hill Book Co., New York, 1017 Price, 83.00.
The full title of this text, "Chemistry of Materials of the
Machine and Building Industries," adequately expresses the
author's object "to supply information concerning the chemical
properties of the materials employed in the various courses in
building construction and equipment and in machinery con-
struction and operation." To this scope the author has rather
rigid!) adhered and no attempt has been made to satisfy the
needs of the enginei 1 md artisan in general.
The text contains chapters on Water for Steam Generation,
Fuels, Refractory Materials, Iron and Steel, Corrosion of Iron
and Steel, Nonferrous Metals, Nonferrous Alloys, Foundry
Sands, Building Stones, Lime and Gypsum Products. Portland
Cement, Clay and Clay Products, Paints, Lubricants, Glue,
Rubber, Electrical Insulating Materials, Primary Electric Cells,
Secondary Cells, and Hydrometry, Thes< topics covet abroad
field in themselves and the discussions throughout are d
to satisfy the requirements of the user rather than the manu-
ds ol manufacturi although
often discussed "have not been emphasized or presented in
detail "
The text as a whole is well written and the material well
Other texts and the original I i1 om which
rial has been drawn, are cited in footnotes and at the
end of each chaptei is both a book and periodical bibliography,
which greatl] enhance its value as a textbook for the class-
room
J] books ni 1 er, the authoi has failed to
the individual requirements of each instructor in applied
chemi trj foi techi ical students, inasmuch i th lection of
ttly a mattei ol judgment No mention
is madi , for examp >a] manu-
facture, powdered coal firing, acetylene gas, natural and tufa
cement, heat insulation, etc The usei might also infer that
tin unit! wcldini is the only process in use, suae no mention
is madi lene and electric welding. On the other
hand, considerable space is given to the theories of iron corrosion
as developed bv Cushniaii, Friend, and Others, to which the user
might well be directed foi a full discussion. Some eighteen
pages are given oxer to a discussion of the metallography of
iron and steel though it is doubtful if the user might not find it
advantageous to consult Sauveur's larger text.
The authoi li in classifying the properties of the
various materials in an excellent manner. Especially is this
true of the paint and rubber industries, where the diversity of
material is very large. The chapters on electric cells are also
timely and a very desirable addition to a textbook of this kind.
The text has been well edited and is a useful contribution to the
subject matter of applied chemistry.
H. K. Benson
The Examination of Milk for Public Health Purposes. By
JOSEPH RACE, vi + 224 pp. John Wiley & Sons, Inc.,
New York. Price, Si. 75-
This compact and well arranged book gives in convenient
compass all the essential information for the public health
official concerning the composition of milk, together with its
chemical and bacteriological examination. The material is
about equally divided between the chemical and biological sides,
although the latter is taken up with possibly a somewhat greater
wealth of detail. Especially worthy of commendation are the
statements regarding the chemical composition and natural
variations in normal milk, and the discussion of methods for the
enumeration of total bacteria and of excremental organisms.
The standard bacterial methods of the American Public Health
Association are discussed in a spirit of friendly criticism.
A pleasing feature is the rather unusually full treatment
given to the effect of breed and of period of lactation on the
protein : fat and lactose : protein ratios. The interesting rela-
tion between the calculated protein derived from the Olsen
and Van Slyke formulae as affected by the addition of water or
the removal of fat is well stated, but the calculation of the
proportion of added water is hardly so mathematically exact
as might be inferred by the unwary reader from the statements
on page 58. The relative importance of preservatives in milk
and of methods for their detection is perhaps somewhat exag-
gerated. The only feeling that remains, however, on laying
the book down, is one of pleasure at finding essential facts so
clearly stated by one who knows his subject through working
with it.
A. G. Woodman
Aids in the Commercial Analysis of Oils, Fats and Their Com-
mercial Products. A Laboratory Handbook. By George
Fenwick PICKERING, Head Chemist and Works Manager,
formerly Research Assistant to the late Dr. J. Lewkowitsch.
133 pp. Charles Griffin & Company, Ltd., London, 1917.
Price, -
A- the title states, this is a book for the laboratory, and the
nnes th.u the user is an experienced analyst and accus-
tomed to oil work As such, it will be found very valuable on
account of its brevity and of the large number of tables. It
will be particularly helpful in the analysis of commercial and
ork of this kind it is not surprising
to noie the absence of references to the literature and of cuts.
Some points ih.it attracted the attention of the reviewer are:
the Statement in the preface that "the following methods are
given as w.nks methods, and it must be clearly understood that
the chemical methods used in the analysis of oils and fats can**
have no preien. , uy Slu.n .,^ js USually found
iii inorganicwork " Thisbeii . th< fact.it is interesting to note
that in very many analyses ri -nit - are given to O.Ol per cent.
The French spi Uing ad centimetre is used through-
out the book. .1. well 1 1 ither than CC I. The refractive
indices are given at 17° C. rather than 25° C. as is usual: also
Aug., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
667
viscosities at 700 F. which has been abandoned. The table,
however, gives as well 140° F., 180° F., and 212° F., and will
be found very useful. It would help, however, to know exactly
what oil is meant by the term "animal oil" used here, and also
in other places in the book. The description of the flash point
(p. 14) is crude. In the extraction of unsaponifiable matter,
no caution is given regarding the "petrol" used — that it should
leave no residue on evaporation at 100° C. The statement
"the original method of Hubl is still the standard" is not true;
it is still somewhat used, but is not the standard. Similarly the
statement (p. 27) regarding the Maumene test, that the addition
of "mineral oil is a hindrance," is not in accord with the fact.
In the directions for the determination of the specific gravity of
pitches (p. 107), the procedures for the light and heavy pitches
have been confused.
The volume is unique, and should be in the library of every
one having to do with the analysis of oils and fats.
A. H. Gill
Reagents and Reactions. By E. Tognoli. Translated from
the Italian by C. AiftswoRTH Mitchell. P. Blakiston's Son
& Co., Philadelphia, 1918. Price, $2.00.
The tests for purity of chemical reagents are useful but being
limited to more important reagents only it is not as useful a
book as many others which are in use. Listing the reactions
under the name of the chemist is unusual and impracticable
unless one is already familiar with the work of the analysts
whose names are given in alphabetical order instead of the
names of the reagents.
J. T. Baker
Coal Gas Residuals. By Frederick H. Wagner, M.E.
2nd Ed. xii + 244 pp., with diagrams. McGraw-Hill Book
Co., New York, 1918. Price, $2.50.
The first edition was reviewed in This Journal, 7 (1915), 362.
The war has greatly increased interest in coal by-products which
are used in making explosives, dyestuffs, fertilizers, etc., and
hence this new edition. The layout of the book is the same as
in the first edition, with very few changes, but with the addition
of some 65 pages.
It is to be regretted that this book, like many other "scien-
tific" books, is so uneven in value. The author as a gas engineer
may give an interesting discussion with dependable conclusions
in some lines, but the ambitious demands of the book lead him
into coal tar and chemical lines with which he cannot be so
familiar and this results in his apparently accepting and setting
forth data without discrimination and containing many mis-
leading statements. The reviewer appreciates it is easier to
sit on the side lines and criticize than to take the active part,
but it does seem that continued publication of books, which pur-
port to be equally authoritative in all directions and are mis-
leading in some parts, will bring so-called "scientific" books into
ever-increasing disrepute. The burden seems to be fairly on
those who wish to be authors to know fully about their subject
or else to differentiate clearly in their books between what they
can personally vouch for and what is condensed or compiled
from other sources, and to give their authorities so that the
reader may have some check on the statements made. It would
also be a most important improvement if scientific authors giving
description of various processes would indicate, when possible,
those which represent good current practice as distinguished
from those which are mere theories or patents.
Speaking more specifically, the main additions in the present
edition are pages 35 to 51, entirely new matter on tar products;
°9 to 73 and 85 to 88, some additions on cyanogen; 154 to 163,
additions on ammonia; 185 to 190, additions on benzol; 191 to
199, a new chapter on sulfuric acid; and 214 to 222, new matter
on determination of benzene, toluene, etc., in light oils.
There is a certain glamor at present surrounding tar and tar
products, and other publications besides this, including some
from Washington, have given a misleading idea as to the scource
of most of the so-called coal-tar products used in explosives and
dyestuffs. Two of the materials most prominent are toluene,
as the source of T. N. T., and benzene, as the source of various
products, particularly synthetic phenol. It is proper to point
out that, strictly speaking, only negligible amounts of these are
derived from coal tar and that the large source is from the so-
called light oil which is separately washed from the gas and is
not condensed with the tar. Some phenol is obtained from oils
distilled from tar as well as considerable naphthalene, some
cresylic and some anthracene, but in practice the portion of coal
tar entering into the coal-tar chemical products prominent to-day
is less than 10 per cent of the total tar and some 90 per cent
remains to be disposed of in less poetic lines. Some little emphasis
is laid on this because the present book, like others, does not
give a fair perspective of this portion of the subject and touches
lightly, and often incorrectly, some of the high spots.
Without commenting in much detail, it may be pointed out
that some of the errors in the first edition continue. For example,
on page 5, alizarin obtained from anthracene is still mentioned
as the base of indigo. On page 30, Table VI, the temperature
of saturation of Oil I presumably should read 89 ° to 76.8°,
instead of 98 ° to 76.8 ° C; and that of Oil III should probably
read 35 ° to 20 °, instead of 78° to 20°. On page 31 the same
doubtful figures are still quoted as to the results obtained with
the Feld process of fractional distillation (should be condensa-
tion) of tar products. Table VIII, page 32, still incorrectly
gives "anyline" instead of aniline. There are many inaccuracies
of statement in the pages on tar products. In several cases
crude products are given as finished products and vice versa.
In others several crudes are mentioned one after another and they
are said to yield several finished products, but no clear idea is
given as to which crude yields a given finished product. The
figures of yield often are far from United States practice.
In the chapter on benzol, the well-known Koppers system is
given first place, as it deserves, in view of its wide use in the
United States, but it is followed by a discussion of the Feld
system in such way that the reader might also think it was a
prominent system here, whereas it is not. The author also
refers to the fact that if the benzol were extracted from the gas
from the coke ovens existing at the time the statement was made
by Puening, certain amounts of benzol would be recovered, and
appears to overlook stating the important fact that all of these
installations have since been made and that more than the
amount of benzol mentioned is being recovered. In general,
the author uses Fahrenheit scale, which is not in conformity
with the practice of this country in such installations.
The chapter on cyanogen contains considerable additions,
comprising the discussion of the processes followed by the British
Cyanide Company and the Commercial Gas Company of London.
pp. 69-93, also the treatment of spent oxides, pp. 84-88. A few
additions have also been made to the detailed description of the
Feld and Bueb processes.
The chapter on ammonia covers a number of recovery systems
in considerable detail. It is not always clear to the reader
whether the description is that of an operating plant or whether
it is based on patent specifications, a distinction frequently
based on important differences. There is an interesting table
from an enemy source on the influence of foreign matter on the
color of sulfate of ammonia. The Feld process both by itself
and in combination with the- Bueb cyanogen plant is covered
very thoroughly, leading to somewhat extensive and argumenta-
tive "conclusions" to the effect that the economy of the Feld
is superior.
There is also brief timely discussion of the methods of con-
verting ammonia to nitric acid and the production o! nitrate
668
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING ( HEMISTRY Vol. 10, No. 8
of ammonia, together with a diagram of a conversion plant, pp.
154-163. This comprises most of the text that has been added
to the ammonia chapter.
It is earnestly to be hoped that when a third edition of the
book is forthcoming it will be thoroughly revised. There is
certainly a demand for a good up-to-date book treating with the
subject in band
R. P. Perry
A Manual of Chemical Nomography. By Horace G. Deming,
Associate in Chemistry, University of Illinois. 71 pp. The
University Press, Champaign, 111., 1918. Price, $1.25.
The subject of nomography or calculation by graphical
methods was developed a generation ago. Outside of a few
elementary books and treatises for engineers, almost nothing is
published on the subject in English. Dr. 1 killing's manual is
panied by a book of charts, 18 in number, for the calcula-
tion of products, quotients, reciprocals, square roots, cube
roots, and the like, all of which can also be found with the aid
of the slide rule. The great advantage in the nomographical
method is that it can be extended to the solution of algebraic
equations, which are frequently encountered in chemical calcula-
tions. Thus, the calculations following the analysis of mixtures
or the analysis of organic compounds are very simple. In the
latter case, after the percentages of C and H are known from
analysis (in a compound containing C, II and O), the formula
is Found by simply joining the percentages on two scales by a
straight edge and reading numbers from other scales traversed
by the straight edge.
The method OOt only gives as accurate results as an ordinary
slide rule but also suggests the construction of special scales for
special problems where algebraic equations must be solved.
Chemists and engineers having many numerical calculations
to make, owe a debt of gratitude to Dr. Deming for bringing to
light another powerful method of simplifying computations.
James M. Bell
Edible Fats and Oils. By C. Ainsworth Mitchell, B.A.,
I'M C. 159 pp. Longmans, Green and Co., New York and
London, 1918. Price, $2 .00.
This little volume is a very valuable addition to the literature
of the subject. It is remarkable how much useful material the
author has condensed into a small space. The treatment of the
manufacturing processes for production of various oils and fats
must lit considered as simply a sketch tending to give general
outlines rather than specific methods. The greater part of
the work consists of a description of up-to-date analytical pro-
11 1 is in Such form as to give anyone unfamiliar with the
subject of fat inalysi ry clear idea of what the various
indicate, while at the same time it is a very useful
reference bonk to the specialist.
The bibliography of the subject, covering 27 pages, is particu-
larly useful
The chapters dealing with margarine manufacture and hydro-
genation, considering the very short space occupied, give very-
clear general ideas of these two processes.
ill In ir in his preface states he has "endeavored to give a
concise outline of the chemical composition and properties of
the more important oils and fats, together with a description of
the methods Of extracting them from the crude materials, and of
purifying ami preparing them fur food purposes. A chapter
dealing with the physical and chemical methods of examining
edible oils is also included, and tallies of so called "constants"
i with tin descriptions of the individual fats, with the
enabling anyone who has no specialized knowledge of
understand the technicalities of an analysis
With this end in view, the principles rather than the working
details ol well known analytical methods have been described."
The book is fully up to the above description.
David Wesson
Annual Report of the Chemical Laboratory of the American
Medical Association. Volume to, January-December 191 7.
Pamphlet, 140 pp. American Medical Association, 535
Dearborn St., Chicago.
This, the tenth volume of what is familiarly termed by its
friends "The A. M. A. Lab. Reports," is as valuable to every
pharmaceutical chemist as has been its predecessors. In fact,
the 191 7 issue is of even more value, since it includes a general
index to the entire ten volumes, so that now the chemist de-
siring information concerning preparations examined by the
A. M. A. laboratory staff need only refer to one index instead of
to ten.
The purpose of the pamphlet is two-fold: (a) to acquaint
physicians, pharmacists, and others interested in the subject,
with the composition of proprietary preparations found in the
American market; (b) to inform pharmaceutical chemists of the
methods found most satisfactory in examining preparations
of complex character. It is in this second function that the
book is of great value to the chemist interested in the pharma-
ceutical side of our calling. t
H. V. Arn-y
The Storage of Bituminous CoaL By H. H. Stoek. 192 pp..
63 figs. Circular No. 6, Engineering Experiment Station,
University of Illinois, Urbana, Illinois, March 4, 1918. Price.
40 cents.
Professor Stoek has prepared a valuable and timely publica-
tion on the storage of bituminous coal, the purpose being "to
present a review of modern practice governing the storage of
coal and a statement of the facts which have developed in the
experience of those who have successfully or otherwise under-
taken to store coal. The discussion is confined largely to
bituminous coal, which has given so much trouble owing to its
tendency toward spontaneous combustion while stored, and to
storage systems and mechanical devices."
The subject matter of the bulletin is given in the following
seven chapters and three appendices:
I — Introduction .
II — Reasons for Storing Coal.
Ill — Places of Storage for Different Purposes.
IV Coal Stoiage Practice.
V Storage Systems.
VI Effects of StoraRe upon the Properties of Coal.
> \pense of Storing Coal.
Appendix I — Questionnaire on Coal Storage Data.
Appendix II — Summary of Conclusions and Suggestions Regard-
ing Coal Storage.
Appendix III — Experiences of Firms and Individuals Storing Coal.
The author is to be commended for not only covering the
published literature on coal storage, but also in collecting much
valuable infi ending out comprehensive question-
es to Coal operators, dealers, and consumers.
meous combustion and the effect of storage on coal
has been treated clearly and concisely, conclusions being drawn
from the excellent experimental work of the Illinois Engineering
Experiment Station, U. S. Bureau of Mines, and the Canadian
1 lepai uncut of Mines.
The chapters on coal storage practice and systems, and on
the expense of storing coal include numerous descriptions with
cuts and photographs of modern storage plants. Actual itemized
cost data au given for many of these plants.
This information is of the utmost value to those charged with
the design of storage plants and should do much to minimize
losses from spontaneous combustion and undue breakage of
coal.
The author is to be congratulated in preparing this publica-
tion at a time when the increase of coal storage facilities becomes
necessary" as a war measure. His publication should be a ready
reference volume on coal storage for anyone interested in the
subject.
A. C. Fleldner.
Aug., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
669
NLW PUBLICATIONS
By Irene DeMatty, Librarian, Mellon Institute of Industrial Research, Pittsburgh
Alkali Industry. J. R. Partington. 8vo. 320 pp. Price, 7s. 6d. Bail-
liere, Tindall & Cox, London.
Analysis: A Manual of Qualitative Chemical Analysis. J. R. Morton.
8vo. Price, 6s. G. P. Putnam's Sons, London and New York.
Bacteriology: A Text Book of Bacteriology. P. H. Hiss and H. Zinsser.
8vo. 852 pp. Price, $3.75. Daniel Appleton & Co., New York.
Cellulose. C. F. Cross and E. J. Bevan. 8vo. New Impression with
Supplement. Price, $4.00. Longmans, Green & Co., New York.
Chemical Pathology. H. G. Wells. 8vo. 707 pp. Price, $4.25. W. B.
Saunders Co., Philadelphia.
Chemists Pocket Manual: A Practical Handbook Containing Tables,
Formulas, Etc., for Chemists. R. K. Meade. 3rd Ed. 16mo. 530
pp. Price, $3.50. Chemical Publishing Co., Easton, Pa.
Coal Tar: The Treasures of Coal Tar. Alex. Findlay. 8vo. 137 pp.
Price, $2.00. D. Van Nostrand Co., New York.
Crystallography: A Manual of Geometrical Crystallography Treating
Solely of Those Portions of the Subject Useful in the Identification of
Minerals. G. M. Butler. 16mo. 155 pp. Price, $1.50. John
Wiley & Sons, Inc., New York.
Cyanide Process. A. W. Fahrenwald. 16mo. 256 pp. Price, $2.00.
John Wiley & Sons, Inc., New York.
Dyeing: A Manual of Dyeing. Edmund Knecht and Others. 4th Ed.
2 Vol. 8vo. 914 pp. Price, 42s. Charles Griffin & Co., London.
Engineering Physics: A Textbook of Physics for the Students of Science
and Engineering. J. Duncan and S. G. Starling. 5 Parts. 8vo.
Price, 16s. The Macmillan Co., London and New York.
Gravity and Temperature Tables for Mineral Oils. E. N. Hurlburt.
16mo. 204 pp. Price, $1.00. Taylor Instrument Co , Rochester.
N. Y.
Laboratory Glassware Economy. H. B. Duncliff. 8vo. Price, 4s
The Macmillan Co.. London and New York.
Mining Engineers' Pocket Book. Robert Peele. 12mo. 2385 pp
Price, $5.00. John Wiley & Sons, Inc., New York.
Oils and Fats: Edible Oils and Fats. C. A. Mitchell. 8vo. 159 pp
Price, $2.00. Longmans, Green & Co., New York.
Organic Chemistry: A Class Book of Organic Chemistry. J. B. Cohen
12mo. 344 pp. Price, $1.40. The Macmillan Co., New York.
Organic Compounds of Arsenic and Antimony. G. T. Morgan. 8vo
375 pp. Price, $4.80. Longmans, Green & Co., New York.
Steam Engines: A Thorough and Practical Presentation of Modern Steam
Engine Practice. L. V. Ludy. 2nd Ed. 8vo. 192 pp. Price, $1.00.
American Technical Society, Chicago.
Wood: The Preservation of Wood. A. J. Wallts-Taylor. 8vo. 344
pp. Price, $4.00. D. Van Nostrand Co., New York.
Wood: Seasoning of Wood. J. B. Wagner. 8vo. Price, 15s. Crosby,
Lockwood & Son, London.
RECENT JOURNAL ARTICLES
Belt Concentrators and Wet Concentration. Alex. McLaren. Engineer-
ing and Mining Journal, Vol. 106 (1918), No. 1, pp. 11-12.
Bisulfite Liquor and Its Constituents. James Beveridge. Paper, Vol.
22 (1918), No. 16, pp. 11-14.
Blast Furnace: Principal Changes in Blast Furnace Lines. J. G. West,
Jr. The Blast Furnace and Steel Plant, Vol. 6 (1918), No. 7, pp. 289-
296.
Boron: Its Effect on Crops. F. C. Cook and J. 3. Wllson. Journal of
Agricultural Research, Vol. 13 (1918), No. 9, pp. 451-470.
By-Product Coke Oven Industry. W. H. Blauvelt. The Blast Furnace
and Steel Plant, Vol. 6 (1918), No. 6, 260-261.
Cementation in Illinois Coal Field. M. L. Nebel. Engineering and Min-
ing Journal, Vol. 105 (1918), No. 24, pp. 1080-1082.
Charcoal Precipitation of Aurocyanide. A. W. Allen. Metallurgical and
Chemical Engineering, Vol. 18 (1918), No. 12, pp. 642-644.
Chemistry and Histology of the Glands of the Cotton Plant. E. E. Stan-
ford and A. Viehoever. Journal of Agricultural Research, Vol. 13
(1918), No. 8, pp. 419-435.
Chemistry in the Pulp and Paper Industry. J. N. Stephenson. Pulp and
Paper Magazine, Vol. 16 (1918), No. 24, p. 537.
Color Classification: A System of Color Classification. E. W. Pierce.
Textile World Journal, Vol. S3 (1918), No. 52, pp. 63-65.
Electrification of Textile Fibers. S. A. Shorter. Textile World Journal,
Vol. S3 (1918), No. 49, p. 35.
Export Situation. I. B. Scheibbr. Color Trade Journal, Vol. 3 (1918),
No. 1, pp. 258-259.
Fuel: Substituting Powdered Coal for Other Fuels. C. P. Herington
The Blast Furnace and Steel Plant, Vol. 6 (1918), No. 7, pp. 285-288.
Glass: Some Notes on American Methods and Practice in Glass Makui"
H. H. Pitt. Journal of the Society of Class Technology, Vol. 2 (1918).
No. 5, pp. 19-31.
Glass Making at Bolsterstone. Jos. Kenwortby. Journal of the Society
of Class Technology, Vol. 2 (1918), No. 5, pp. 5-12.
Iodide Copper Method with Sodium Fluoride. A. L. Reese. Engineering
and Mining Journal, Vol. 105 (1918), No. 26, pp. 1170-1171.
Mining Industry: The Keystone of Modern Civilization. R. H. Stretch.
Mining and Scientific Press, Vol. 116 (1918), No. 23, pp. 791-797.
Nitrate Recovery from Water Gas. J. Stephenson. The Canadian
Chemical Journal, Vol. 2 (1918), No. 6, p. 160."
Okell's Method for Size-Fastness. S. A. Okell. Paper, Vol. 22 (1918),
No. 17, p. 19.
Ores: To Utilize Domestic Ores. J. B. Waterhouse. The Iron Trade
Review, Vol. 62 (1918), No. 24, pp. 1493-1494.
Paper Can Manufacture. S. M. Langston. Pulp and Paper Magazine
Vol. 16 (1918), No. 26, pp. 586-588.
Peat: Inorganic Composition of a Peat and of the Plant from Which It Was
Formed. C. F. MlllEr. Journal of Agricultural Research, Vol 13
(1918), No. 12, pp. 605-609.
Phosphorus Effect in Steel. J. S. Linger. The Iron Trade Review, Vol. 62
(1918), No. 24, pp. 1495-1498.
Potash-Feldspar: British Supplies of Potash-Feldspar. P. G. H. Bos-
well. Journal of the Society of Class Technology, Vol. 2 (1918), No. 5,
pp. 35-71.
Powdered Coal: The Use of Powdered Coal. W. G Wilcox. Mining
and Scientific Press, Vol. 116 (1918), No. 25, pp. 849-853.
Refractory Material: Selecting Suitable Refractory Material. J. W.
Haulman. The Blast Furnace and Steel Plant, Vol. 6 (1918), No. 6, pp.
243-244.
Research Laboratory: Problems for the Consideration of the American
Research Laboratory. F. H. Small. Journal of the American Leather
Chemists Association, Vol. 13 (1918), No. 6, pp. 239-248.
Rubber Embargo. A. H. King. Chemical and Metallurgical Engineering,
Vol. 19 (1918), No. 1, pp. 23-26.
Rubber Substitutes. A. H. King. Metallurgical and Chemical Engi-
neering, Vol. 18 (1918), No, 12, pp. 630-636.
Scleroscopes: The Use and Abuse of Scleroscopes. A. J. Smith. The
American Drop Forger, Vol. 4 (1918), No. 6, pp. 212-213.
Sulfur: The Effect of Boiling Sulfur on Copper. C. R. Hayward.
Metallurgical and Chemical Engineering, Vol. 18 (1918), No. 12, pp.
650-651.
Sulfuric Acid: How to Conserve Sulfuric Acid and Why. H. J Brough-
ton. The Metal Industry, Vol. 16 (1918), No. 6, pp. 263-264.
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The Iron Trade Review, Vol. 62 (1918), No. 21, pp. 1299-1304.
Synthetic Indigo. R. W. Smith. Color Trade Journal. Vol. 3 (1918), No.
1, pp. 246-251.
Technical Education: Its Importance and Defects. C V. CorlEss.
Pulp and Paper Magazine, Vol. 16 (1918), No. 27, pp. 605-606.
Thermochemistry of Acid Making. C. K. Textor. Paper, Vol. 21 (1918),
No. 23, pp. 60-64.
Thermocouples: Standardization of Rare-Metal Thermocouples. P. D.
Foote and Others. Metallurgical and Chemical Engineering, Vol. 18
(1918), No. 7, pp. 343-348.
Thermostats. W. N. Ray. The Chemical News, Vol. 117 (1918), No.
3047, pp. 181-184.
Tinning: Mechanical Tinning of Metals. L. J. Krom. The Metal
Industry, Vol. 16 (1918), No. 6, pp. 261-262.
Trade Paper and Its Industry. B. S. Stephenson. The Blast Furnace
and Steel Plant, Vol. 6 (1918), No. 6, pp. 268-270.
Triplex Electric Steel Process. T. W. Robinson. The Blast Furnace and
Steel Plant, Vol. 6 (1918), No. 6, pp. 245-251.
Turpentine: Recovery System for Sulfite Turpentine. H. F. Ober-
manns. Paper, Vol. 22 (1918), No. 4, pp. 11-13.
Ultraviolet Energy and Its Use. M. Luckiesh. MeXallurgical and Chem-
ical Engineering. Vol. 18 (1918), No. 5, pp. 232-236.
Ultraviolet Light: Its Application in Chemical Arts. C. Ellis and A. A.
Wells. The Chemical Engineer, Vol. 26 (1918), No. 5, pp. 181-188.
Valuing Oil Lands. M L Rbqua. Engineering and Mining Journal,
Vol 105 (1918). No. 12. pp. 544-548.
Vanadium Ores, Occurrence and Uses. H. Ribs. Mineral Foote- Notes,
Vol. 2 (1918), No. 5, pp. 3-11.
Vulcanization of Rubber. A. H King. Metallurgical and Chemical Engi-
neering, Vol 18 (1918), No. 5, pp. 243-248.
Waste Prevention in Power Plants. V. J. Azbb. The Iron Trade Review,
Vol. 62 (1918), No. 7, pp. 421-428.
Vater for Bleaching Purposes. J. M. Matthews. Color Trade Journal,
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waterproofed Canvas Manufacture. B » Clark. Textile World Journal,
\,.' S3 I19IHI. No 46. DO -"-45.
6yo
MARKET REPORT-.! ILY, 1918
WHOLESALE PRICES PREVAILING IN THE NEW YORK MARKET ON JULY 17, 1918
INORGANIC CHEMICALS
Acetate of Lime 100
Alum, ammonia, lump 100
Aluminum Sulfate, (iron free)
Ammonium Carbonate, domestic
Ammonium Chloride, white
Aqua Ammonia, 26°, druma
Arsenic, white
Barium Chloride
Barium Nitrate
Barytcs, prime white, foreign
Bleaching Powder, 35 per cent
Blue Vitriol
Borax, crystals, in bags
Boric Acid, powdered crystals
Brimstone, crude, domestic Long
Bromine, technical, bulk
Calcium Chloride, lump, 70 to 75% fused. . . .
Caustic Soda, 76 per cent 100
Chalk, light precipitated
China Clay, imported
Feldspar
Fuller's Earth, foreign, powdered
Fuller's Earth, domestic
Glauber's Salt, in bbls 100
Green Vitriol, bulk 100
Hydrochloric Acid, commercial
Iodine, resublimed
Lead Acetate, white crystals
Lead Nitrate
Litharge, American
Lithium Carbonate
Magnesium Carbonate, U. S. P
Magncsite, "Calcined"
Nitric Acid, 40"
Nitric Acid. 42°
Phosphoric Acid, 48/50%
Phosphorus, yellow
Plaster of Paris
Potassium Bichromate
Potassium Bromide, granular
Carbonate, calcined, 80 @ 85%.. .
Chlorate, crystals, spot
Cyanide, bulk, 98-99 per cent
Hydroxide, 88 ©92%
Iodide, bulk
Nitrate
Permanganate, bulk
:, Bask 75
Red Lead, American, dry 100
Salt Cake, glass makers'
Silver Nitrate
Soapstonc, in bags
Soda Ash, 58%, in bags 100
Sodium Acetate
Bicarbonate, domestic 100
Bichromate
Chlorate
Cyanide
Fluoride, commercial
Hyposulfitc 100
Nitrate, 95 per cent, spot 100
Silicate, liquid, 40° IS6
Sulfide, 60%, fused in bbls
Bisulfite, powdered
m Nitrate
Sowers, sublimed 100
Sulfur, roll 100
Sulfuric Acid, chamber 66° B6
Sulfuric Acid, oleum (fuming)
Talc, American white
Terra Alba, American, No. 1 100
•in. Bichloride, 50°
Tin dxi.le
White Lead, American, dry
Zinc Carbonate
Zinc Chloride, commercial
Zinc Oxide. American process XX
Potassiu
Potassiu
Potassiu
Potassiu
Potassiu
Potassiu
Potassiu
Quicksib
Sodium
Sodium
Sodium
Sodium
Sodium
Sodium
Sodium
Sodium
Sodium
Sodium
Strontii
Sulfu
J'/l @
nominal
nominal
9'/i @
Lb.
9'/.
&
9'/i
Lb.
7'/.
®
10«/i
Lb.
13'/.
®
15
Ton
ninol
Lb.
75
<3
85
Ton
22.00
®
25.00
Lbs.
4
@
Lb.
4'/.
@
5
Ton
20.00
®
30.00
Ton
8.00
@
15.00
Ton
nominal
Ton
20.00
@
30.00
Lbs
1.50
@
3.00
Lbs.
1.15
@
1.25
Lb.
C. P.
nominal
Lb.
4.25
®
4.30
Lb.
17
@
18
Lb.
C
P. 85
Lb.
7"/«
@
8
Lb.
.50
60.00 @ 65.00
1.35
2.00
1.35
38
Lb.
1.75
Lbs.
125.00
Lbs.
10.79
Ton
20.00
Oz.
62'/
Ton
10.00
Lbs.
2
Lbs.
3
Lb.
Lbs.
2.60
@
Lbs.
4.12'
,@
2'
4 @
Lb.
nominal
6
0
Lb.
25
e
Lbs.
4.05
@
Lbs
3.70
e
Ton
18.00
Ton
60.00
9
Ton
15.00
Lbs.
1.17'/,
Lb.
28
•
Lb.
1.00
0
Lb.
9'/
i ®
ORQANIC CHEMICALS
Acetonjlld, C. P., in bbls Lb.
Acetic Acid, 56 per cent. In bbls Lb.
Acetic Acid, glacial, 99'/i%, in carboys Lb.
Acetone, drums II,
Alcohol, denatured. 180 proof Gal.
ominal
Alcohol, sugar cane, 188 proof Gal.
Alcohol, wood, 95 per cent, refined Gal.
Amyl Acetate Gal.
Aniline Oil, drums extra Lb.
Benzoic Acid, ex-toluol Lb.
Benzol, pure Gal.
Camphor, refined in bulk, bbls Lb.
Carbolic Acid, U. S. P., crystals, drums Lb.
Carbon Bisulfide Lb.
Carbon Tetrachloride, drums, 100 gals Lb.
Chloroform Lb.
Citric Acid, domestic, crystals Lb.
Creosote, beechwood Lb.
Cresol, U. S. P Lb.
Dextrine, corn (carloads, bags) Lb.
Dextrine, imported potato Lb.
Ether, U. S. P. 1900 Lb.
Formaldehyde, 40 per cent Lb.
Glycerine, dynamite, drums extra Lb.
Oxalic Acid, in casks Lb.
Pyrogallic Acid, resublimed, bulk Lb.
Salicylic Acid. U. S. P Lb.
Starch, cassava Lb.
Starch, corn (carloads, bags) pearl 100 Lbs.
Starch, potato, Japanese Lb.
Starch , rice Lb.
Starch, sago flour Lb.
Starch, wheat Lb.
Tannic Acid, commercial Lb.
Tartaric Acid, crystals Lb.
OILS, WAXES, ETC.
Beeswax, pure, white Lb.
Black Mineral Oil, 29 gravity Gal.
Castor Oil. No. 3 Lb.
Ceresin. yellow Lb.
Corn Oil, crude 100 Lbs.
Cottonseed Oil, crude, f . o. b. mill Lb.
Cottonseed Oil, p. s. y 100 Lbs.
Menhaden Oil, crude (southern) Gal.
Neat's-foot Oil, 20° Gal.
Paraffin, crude, 118 to 120 m. p Lb.
Paraffin Oil, high viscosity Gal.
Rosin. "F" Grade. 280 lbs Bbl.
Rosin Oil, first run Gal.
Shellac, T. N Lb.
Spermaceti, cake Lb.
Sperm Oil, bleached winter, 38° Gal.
Spindle Oil, No. 200 Gal.
Stearic Acid, double-pressed Lb.
Tallow, acidless Gal.
Tar Oil. distilled Gal.
Turpentine, spirits of Gal.
METALS
Aluminum, No. 1, ingots Lb.
Antimony, ordinary Lb.
Bismuth, NY Lb.
Copper, electrolytic Lb.
Copper, lake Lb.
Lead, N. Y Lb.
Nickel, electrolytic Lb.
Platinum, refined, soft Oz.
Silver Qz.
Tin, Straits Lb.
Tungsten (WOi) Per Unit
FERTILIZER MATERIALS
Ammonium Sulfate ioo Lbs.
Blood, dried, f. o b. Chicago Unit
Bone 3 and 50. ground, raw Ton
Calcium Cyanamide Unit of Ammonia
Calcium Nitrate, Norwegian 100 Lbs.
Unit
Fish Scrap, domestic, dried, f. o b. works.. . .Unit
Phosphate, acid, 16 per cent Ton
Phosphate rock. f. o. b. mine: Ton
Florida land pebble, 68 per cent Ton
Tennessee, 78-80 per cent Ton
Potassium "muriate" basis 80 per cent Ton
Pyrites, furnace size, imported Unit
Tankage. high-grade, f. o. b. Chicago Unit
4.95
92'/,
8'/i @
15'/, @
3.25
90 @
1.00
6.50 8
7.00
13'/. @
13'/,
12'/, @
13
9'/, @
10'/,
nominal
63 @
^3
17
17.50
17'/,
20.50
1.00
3.45
9»/i
40
13-/4
3. 65
nominal
95'/.
nominal
24.00
8.90
7.75 @
8.00
6.70 @
6.75
37.00 @
40.00
nominal
7.30 and
10c
16.00 @
17.00
nominal
3.50 @
3.75
5.50 &
6.00
nominal
nominal
6.65 @
6.70
Tfte Journal of Industrial
and Engineering Chemistry
Published by THE AMERICAN CHEMICAL SOCIETY
AT 8ASTON. PA.
Volume X
SEPTEMBER 1, 1918
No. 9
Editor: CHARLES H. HERTY
Assistant Editor: Grace MacLeod
Advertising Manager: G. W. Nott
ADVISORY BOARD
H. E. Barnard H. K. Benson F. K. Cameron B. C. Hesse A. D. Little A. V. H. Mory
Published monthly. Subscription price to non-members of the American Chemical Society, $6.00 yearly; single copy, 60 cents
Price per single copy to American Chemical Society members, 50 cents. Foreign postage, seventy-five cents, Canada, Cuba and Mexico excepted
Entered as Second-class Matter December 19, 1908, at the Post-Office at Easton, Pa., under the Act of March 3, 1879
Acceptance for mailing at special rate of postage provided for in Section 1103, Act of October 3. 1917, authorized July 13, 1918.
All communications should be sent to The Journal o! Industrial and Engineering Chemistry.
Telephone: Vanderbilt 1930 35 East 41st Street, New York City
Subscriptions and claims lor lost copies should be reierred to Charles L. Parsons, Box 505, Washington, D. C.
ESCHBNBACB PRINTING COMPANY, EASTON, Pa.
TABLE OF
Editorials :
Secretary Crowell at Cleveland 672
No Change in Exposition Plans 672
Turn About is Fair Play 672
An" International Courtesy 673
The Custodian in Action 673
War Chemistry in the Alleviation of Suffering 673
A Dyestuff Section of the American Chemical Society . . 674
The Bull's Eye 674
Chemical Warfare Service ■' 675
Ax Army without Reserves 685
Effect of the War on American Chemical Trade. O. P.
Hopkins, Washington, D. C 692
The Chemical Markets of South America:
The Chemical Markets of Argentina, Brazil and
Uruguay. O. P. Hopkins, Washington, D. C 701
Original Papers:
"Jelly Value" of Gelatin and Glue. A. Wayne Clark
and Louis DuBois 707
A New Method for the Quantitative Estimation of
Vapors in Gases. Harold S. Davis and Mary
Davidson Davis 7°9
The Application of the Differential Pressure Method to
the Estimation of the Benzene and the Total Light
Oil Content of Gases. Harold S. Davis, Marv
Davidson Davis and Donald G. MacGregor 712
Studies 011 the Absorption of Light Oils from Gases.
Harold S. Davis and Mary Davidson Davis 718
The Effect of Frost and Decay upon the Starch in
Potatoes. H. A. Edson 725
The Reticulation of Gelatine. S. E. Sheppard anil
F. A. Elliott 727
Laboratory and Plant:
Methods of Analysis Used in the Coal-Tar Industry.
I — Crude Tars. J. M. Weiss 732
Synthetic Phenol Albert (',. 1'eterkin, Jr 738
CONTENTS
Current Industrial News:
Fan Dynamometer Brake; Soap and Glycerin Manu-
facture in India; New Voltaic Cell; Oilseed Industry
of Rhodesia; Cane By-Products in Natal; The
Synthetic Market; Sulfate of Ammonia; Explosive
Chemicals; Determination of Oxygen in Iron; Italian
Dye and Chemical Industry; Skoda Works Peace
Preparations; Machinery in South America; Cement
Mortars and Magnesium Chloride; Blast Furnace
Practice; Chrome Tanning; Electrical Machinery;
Electrolytic Process; Recovery of Tin; Analysis of
Aluminum Alloys; Catalyst from Metallic Salts; New
Mining Explosive; New Sources of Oil Supply in Ger-
many; Ultra-Filter; Lubricating Material; Indian
Resin; British Board of Trade 744
Scientific Societies:
Cleveland Meeting, American Chemical Society; The
Chemical Societies in New York City; Calendar of
Meetings; Fourth National Exposition of Chemical
Industries, Grand Central Palace, New York, Week
of September 23 to 28, 1918; American Electro-
chemical Society Fall Meeting at Princeton; American
Electrochemical Society; General Symposium on the
Chemistry of Dyestuffs 748
NOTES and Correspondence:
Association of British Chemical Manufacturers; The Sul-
furic Acid Industry; Chemistry for the Public; Civil
Service Rules Waived for War ('.as Investigators;
Research Fellowship, State College of Washington;
Chemical Engineering in Our Universities 75'
Washington Letter 753
Personal Notes 755
Industrial Notes 757
Government Publications 758
New Publications 765
Market REPORT 766
THE JOURNAL Of INDl SI RIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 9
EDITORIALS
SECRETARY CROWELL AT CLEVELAND
Assistant Secretary of War Benedict Crowell will de-
liver the opening address at the opening session of the
Annual Meeting of the American Chemical Society
at Cleveland on September 10, 191 8. Secretary
Crowell has been a member of the Society since 1909.
It will be both a pleasure and a privilege for those
attending the meeting to hear the words of one who
has played so important and so intimate a part in the
organization of the great military machine which is
destined to deliver the deciding blow for the cause of
democracy.
The titles of all the addresses at the opening session
indicate clearly that the keynote of the meeting
will be how American chemists can contribute further
to a quick and complete military victory.
The days of defensive warfare are behind us. From
now on greater and still greater must grow the power-
ful offensive program which will crush every obstacle
of resistance. The opportunity for personal conferences
at the Cleveland meeting should prove an efficient
means for discussion of many important problems
which must be quickly solved. This feature alone
should draw together for common counsel a host of
chemists.
NO CHANGE IN EXPOSITION PLANS
The Fourth National Exposition of Chemical Indus-
tries will be held at the Grand Central Palace, New
York City, during the week September 23-28, 1918, as
originally planned. This definite announcement has
been made public by the exposition management fol-
lowing conferences with representatives of the War
Department.
The building will be taken over by the Government
on September 15, 191 8, for conversion into a great
base hospital. No one connected with the exposition
management or with the chemical industries would be
willing even to suggest that any previously made plans
should interfere with the promptest possible provision
of relief and comfort for our returning wounded
soldiers. The size of the building, however, is so great
that the work of conversion into a hospital cannot
hi three floors to be utilized for the Exposition
before October 1, 1918. Government officials have
therefore given full sanction to the holding of the
Exposition.
TURN ABOUT IS FAIR PLAY
For the past four years American chemists, particu-
larly those in the organic field, have been working to
supply serious economic needs, notably in dyestuffs
and medicinals. Worthily have they met the situa-
tion! Yet in doing this these chemists have been
under .1 serious handicap, the shortage, pro-
duced likewise by war conditions, of available sets of
the greatest of all n i.sin organic chemistry,
Beilstein's Handbuch dcr Organischen (hemic. That
want should be met, and met quickly. Turn about is
fair play!
Some day when the strenuous demands for war
supplies happily no longer exist, American chemists
must seriously face the necessity of compiling in an
authoritative manner great reference works for all
fields of chemistry, books written in our own language
and adapted to our own methods of work. This,
however, is no time for that undertaking. Every
chemist is now, or soon will be, engaged upon problems
directly bearing upon war supplies.
A translation of Beilstein has been suggested, but
this again calls for chemists not at present available,
as the work of translation should be carried out
by those to whom not only German, but also the
language of chemistry, is known. Furthermore, a
translation is not needed, for those who are quali-
fied to use Beilstein are able to read German.
We would suggest and urge a reprinting of Beilstein
under conditions which would make it available
quickly to all organic chemists. To do this through
the ordinary processes of linotyping and proof-reading
would be impracticable because of the present shortage
of labor and the lack of knowledge of German on the
part of linotypists and proof-readers accustomed to
chemical literature. Fortunately, photographic
methods are available, requiring a minimum of labor
and insuring speed and absolute accuracy of reproduc-
tion.
To make the proposition definite we have obtained
prices for zinc etchings from one of the largest en-
graving houses of New York City. For the 11,126
pages of Beilstein the cost of zinc etchings at standard
prices would be 830,040.20. For the paper and press
work (calculating on the quality of paper and charges
for press work in publishing This Journal), $6,119.30
would be required for one thousand sets, making a
total of 836,159.50. Allowing for constantly ad-
vancing prices, and for royalty charges, $40,000 should
safely cover the entire costs, not including binding, of
course.
The legal right could undoubtedly be obtained
from the Federal Trade Commission, under the Trading
with the Enemy Act, for matters of copyright are in-
cluded within the Act.
Do we feel any qualms of patriotic conscience about
such a reproduction? Well, we should worry! Ger-
mans are daily profiting in the conduct of the war
through the utilization of American inventions, the
submarine, the telegraph, the telephone, the machine
gun and what not. Let some one donate $30,000 and
let the sets be sold at $10 each (the ordinary cost is
$100) so that every organic chemist could have one
right at his hand, then— let the Germans worry.
We commend this subject to the Council of the
American Chemical Society at its Cleveland meeting.
Where is the $30,000 that will promptly set the zinc
to etching?
Sept., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
673
AN INTERNATIONAL COURTESY
It is a pleasure to reproduce here the invitation
from the Secretary of the Chemical Society (London)
to all chemists who visit England, and the reply of
Secretary Parsons of the American Chemical Society.
Chemical Society
Burlington House, London, W. 1
July 25, 1918
Mr. Charles L. Parsons
Secretary, American Chemical Society
Dear Sir:
No doubt there are many members of your Society ordinarily
residing in America who are now in this country, and I am
writing to ask you to be good enough to use such means as may
occur to you to inform your members that they are most cordially
invited by the Council of this Society to avail themselves of the
use of our Library and Rooms, and to attend our meetings.
Perhaps, also, you would be good enough to place on your
notice board a notice to this effect so that any of your members
who are about to leave your shores for this country may be in-
formed of this.
I may say that I have been in communication with Sir Harry
Britain, who has very kindly promised to place on the notice
board of the American Club for Officers a notice inviting them
to make what use they can of this Society.
Believe me,
Yours very truly,
(Signed) Samuel Smiles
Honorary Secretary
Washington, D. C.
August 15, 1918
Samuel Smiles, Esq.
Honorary Secretary, Chemical Society
Burlington House, London, W. 1, England
' Dear Sir:
Your letter of July 25 is fully appreciated.
Lieutenant Colonel James F. Norris at the American Embassy
is one of the members of our Council and a prominent member
of the American Chemical Society. He is the scientific attache
on chemical problems to the American Embassy, and I would
suggest that you write him a letter calling the same facts to his
attention that you have sent me. I would communicate with
him, but I think he would appreciate a letter of this kind from
you direct. He will be in touch with most of the American
chemists that come to England, and through him I believe more
of them can be reached than through me, as I do not always
know when they are ordered to your country.
I am sending your letter to the Editor of our Journal of In-
dustrial and Engineering Chemistry, who, I am sure, will be
glad to publish your kind invitation so that it may reach all of
our members who may be going abroad.
With full appreciation of the courtesy of yourself and your
Society, I am
Sincerely yours, •
(Signed) Charles L. Parsons, Secretary
THE CUSTODIAN IN ACTION
The appointment of Mr. James A. Branegan, of Phil-
adelphia, as Vice President of the Heyden Chemical
Works, an enemy-owned corporation recently taken
over by the Government, will prove gratifying to all
chemists, not only because of the high esteem in which
Mr. Branegan is held by his many personal friends,
but because the appointment evidences the sound
policy of the Alien Property Custodian of appointing on
the directing boards of seized organizations technical
experts fully qualified to assure that the purposes of
the Government will be carried out.
Custodian Palmer and his corps of able associates
have evidently taken .no vacation this summer. The
thorough anti-financial-camouflage campaign which is
being quietly and patiently conducted is bearing fruit,
and we have a hunch that the results disclosed so far
are but the forerunner of a great mass of important
contributions to truth still to be made.
The interesting researches now being conducted by
Custodian Palmer should be aided by every loyal
chemist in possession of facts which would contribute
to proof of enemy ownership masquerading in Ameri-
can garments.
WAR CHEMISTRY IN THE ALLEVIATION OF SUFFERING
A few days ago we asked a well-known organic
chemist, one who has been particularly successful
in working out methods for the manufacture of cer-
tain much-needed coal-tar medicinals, "Suppose
during your researches you made some new compound
which you believed would prove more efficacious against
certain diseases than any of the known compounds
whose details of manufacture you have solved, where
would you turn to have it tested thoroughly?" He
replied, "I don't know."
We were returning from a baseball game at the Polo
Grounds, had walked over to Broadway and were about
to enter the subway when the conversation took place.
The subject proved so mutually interesting, that,
perched upon an iron railing amidst the upper
Broadway crowds, we carried on the discussion for
an hour. He had been engrossed in the problem of
reproducing compounds already known and used for
the relief of the physical sufferings of humanity; we
were thinking of the still greater service American
scientists should be enabled to perform.
The negative answer was not surprising, rather it
was confirmatory. It is a peculiar situation that
exists in this country to-day. The three great com-
mercial applications of the so-called "coal-tar chemi-
cals" are, first, explosives, for which means are never
lacking for the thorough testing of new products;
second, dyestuffs, for which fortunately the equipment
for testing as to standard, fastness, durability and
aesthetic suitability is simple, inexpensive and accessible
to every worker; third, medicinals, and here the prob-
lems of investigation become much more complex
and the responsibility even greater. Rarely does the
chemist possess the technique for their testing; he must
rely upon the pharmacologist and the physiologist to
determine the therapeutic value of his product.
In university circles there is often lacking that spirit
of cooperation between the several classes of research
workers which would insure a thorough examination of
these new products of the organic chemical laboratory,
or, if the spirit be willing, the means for conducting
the tests are too limited, especially now when uni-
versity finances are so severely contracted. In a few
manufacturing establishments' provision is made for
animal experimentation, but these facilities are entirely
inadequate and not available to all organic chemists.
In government laboratories some provision is made
for this work, but restrictions are enforced by in-
adequate appropriations. And still people suffer,
674
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. o
though much suffering has been alleviated by dis-
coveries made in o1 her
nately, through the generous provision of
ij individuals, certain institutions ha-.
establi d where the chemist and the
n work in the closest cooperation. The
importance of the intimate cooperation of these workers
is evidenced by the work on the synthesis of a new
philitic drug which was recently accomplished
ute for
■arch. This remedy is now tested from
the clinical viewpoint in the hospital of the same
institution. Similar institutions, however, an
number and the capacity for work of this kind is
necessarily restri'
The laboratory technique, from the chemist's stand-
point, is fortunately quite similar whether in prepar-
ing explosives, dyestuffs or medicinals; and the war
has developed many brilliant organic chemists
'dent could be applied to the relief of suffering.
How ran this application 1- A suggestion
over the situation
admirably, namely, that an institution somewhat
o the Mellon Institute be found"
which adequate provision for laboratory tests of all
kinds would be tn to which, through the
establishment of fellowships, manufacturing organiza-
ould send well-trained young men for working
problems. Cooperation shoul
lished between this institution and the organic labora-
ol our universities, as well as witli the hospitals
e country.
t i i u t ion of this character would prove a great
stimulus to the creation of more adequate research
facilities within the manufacturing establishments.
for the great glory of the Mellon Institute lies, it
■ us, not so much in the actual results ol
under its roof as in tin- indirect creation of research
ii industries which first caught the full
irch through the fellowships estab-
I in that institution.
Perhaj omplish this
object. The columns of Tins Journai stand at the
my who will contributi nssion.
in behalf of
humanity to till tl im the abui
of his riches, he can COUnl with certainty upon the
counsel of the ablesl scientists of this country iii work
ing out the and many details of so im-
I an undertaking.
A DYESTUFF SECTION OF THE AMERICAN CHEMICAL
SOCIETY
The Ann : icturers' Associa-
Of the Chemical Alliance
v t.. care for questions of
general poHi and external, affecting the
newly developed industry in this country. The
ever, are strictly trade organizations. Without de-
siring to inflict any further burden of organization
upon the industry, which has its hands full in supplying
pressing commercial needs, we would like to second
the suggestion of Mr. R. Norris Shreve (page 750) as
to the formation of a dyestuff section of the American
' in mh w. Society.
The days of experimental and large scale production
of known dyestuffs have been accomplished. To rest
content with the present status of the industry would
not be characteristic or worthy of this nation, which is
justifiably proud of its initiative, resourcefulness, and
inventive spirit. New lines must be developed and
new advances made in technical methods, if we are
to be more than mere copyists. Xo surer provision
could be made for these efforts than the semi-
annual gathering of the research men from the various
dyestuff laboratories, in the atmosphere of a great
assembly of chemists. The presentation of papers
and their discussion would establish facts of value
to all, broader viewpoints would be obtained and
hetic personal relationships formed which would
stand in good stead.
It is natural, perhaps, that each commercial organi-
zation should desire to retain for itself the benefits of
research, yet, carried too far, it is a short-sighted
policy, in view of the varied workings of different
minds. Too much secrecy as to certain fancied ad-
vantages has already proved in some cases the cause
of industrial "dry rot." Community of knowledge as
to scientific achievement, safeguarded by critical dis- .
cussion of results, will prove so valuable a means of
industrial advance that it must not be neglected.
Success to those who are taking the preliminary
steps for the formation of a dyestuff section of the
Ami rican Chemical Society!
THE BULL'S EYE
Look out for the bull's eye on the
chemical products (not machinery 1
to be exhibited at the Fourth
Xational Exposition of Chemical
Industries.
Since its inception this annual
display of the results of chemists'
activities has sought to accomplish
one thing above others, namely, an exhibition of prog-
ress made in products manufactured for the first
time in this country during the war period. Un-
fortunately in the past no distinguishing mark has-
been given to such products, consequently only a
confused idea could be obtained by the layman, and
even by many chemists, as to actual progress made.
An effort will be made to correct this during the coming
ion by placing a "bull's eye" upon all new
products whose manufacture has been developed since
break of the war.
This new feature will prove of interest to all, and
we are equally sure that the large number of exhibits
bearing no such distinguishing mark will be a revela-
the public of the manifold achievements of
American chemists prior to the war.
Sept., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
675
CHEMICAL WARFARE SERVICE.
The unexpected waves of chlorine gas at Ypres, with
the resultant casualties, called at once for intense
activities by chemists, at first of a purely defensive
character. Gradually, reluctantly, and finally with
characteristic aggressiveness, especially after the
disasters of Cambrai and Armentieres, this defensive
functioning was enlarged by offensive preparations
which will give to our men every advantage of this
most modern development of warfare.
Into such work more and more of our chemists have
been called. Some have been sent overseas for work
at the front. At home,
research has been con-
ducted on an intensive
and extensive scale, mate-
rial has been tested, small
scale operations have been
proved, and finally plants
have been built for manu-
facturing in enormous
quantities products which
before the war were merely
laboratory curiosities, but
whose deadly mission may
now, in strange antithesis,
bring lasting peace to the
world.
Through the gradual pro-
cesses of organization there
has been created within
the War Department the
Chemical Warfare Service.
For preservation in the
chemical literature of this
country there is printed be-
low a complete personnel of
the commissioned officers
of this service. We are
indebted to Major F. E.
Breithut, of the Organiza-
tion Division, in charge of
personnel, for this material.
There is also printed,
through the courtesy of the
heads of the several di-
visions, the commissioned
personnel of each division. — Editor.
MAJOR GENERAL WILLI
Director. Chehicai
GENERAL ORDERS, NO. 62
CREATING CHEMICAL WARFARE SERVICE
War Department
Washington, June 28, 19 1-8
I — (1) Under authority conferred by Sections 1, 2,
8 and 9 of the Act of Congress, "Authorizing the Presi-
dent to increase temporarily the military establish-
ment of the United States," approved May 18, 191 7,
and the Act "Authorizing the President to coordinate
or consolidate executive bureaus, agencies, and offices,
and for other purposes, in the interest of economy and
the more efficient concentration of the Government,"
approved May 28, 1918, in pursuance of which Act
the President has issued an Executive Order dated
June 25, 1918, placing the experiment station at
American University under control of the War De-
partment, the President directs that the gas service of
the Army be organized into a Chemical Warfare Ser-
vice, National Army, to include:
(a) The Chemical Service Section, National Army.
1 /> ) All officers and enlisted men of the Ordnance De-
partment and Sanitary Corps of the Medical Depart-
ment as hereinafter more
specifically specified (regu-
lar officers affected being
detailed and not trans-
ferred).
(2) The officers for this
service will be obtained as
provided by the third para-
graph of Section 1 and by
Section 9 of the Act of
May iS, 19 1 7, the en-
listed strength being raised
and maintained by vol-
untary enlistment or draft.
(3) The rank, pay, and
allowances of the enlisted
men of the Chemical War-
fare Service, National
Army, shall be the same as
now authorized for the
corresponding grades in the
Corps of Engineers.
(4) The head of the
Chemical Warfare Ser-
vice, National Army, shall
be known as the Director
of the Chemical Warfare
Service, and, under the
direction of the Secretary
of War, as such, he
shall be, and hereby is,
charged with the duty
of operating and main-
taining or supervising the
operation and maintenance
of all plants engaged in the investigation, manu-
facture, or production of toxic gases, gas-defense ap-
.. the filling of gas shells, and proving grounds
utilized in connection therewith and the necessary
research connected with gas warfare, and he shall exer-
cise, full, complete, and exclusive jurisdiction and con-
trol over the manufacture and production of toxic
gases, gas-defense appliances, including gas-shell fill-
ing plants and proving grounds utilized in connec-
tion therewith, and all investigation and research
work in connection with gas warfare, and to thai end
he shall forthwith assume control and jurisdiction over
.,11 pending Governmenl projects having to do or con-
Harris & E
AM I. SIISERT. U.
Warfarb Service
676
THE JOVRNAl OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. 9
nected with such manufacture, production, and opera-
tion of plants and proving grounds for the Army
and heretofore conducted by the Medical De-
partment and Ordnance Department under the
Col. H. C. Newcomer, C. E.
jurisdiction of the Surgeon General and the Chief of
Ordnance, respectively, and all material on hand
for such investigation or research, manufacture or
production operation of plants and proving grounds
and all lands, buildings, factories, warehouses, ma-
chinery, tools and appliances, and all other property,
1 sonal, or mixed, heretofore used in, or in con-
nection with, the operation and maintenance of such
plants and proving grounds for the purpose of in-
vestigation or research, manufacture or production, al-
ready procured and now held for such use by, or under
C01 w I 1. Lystb«, Mia. Corps
the jurisdiction and control of the Medical Depart-
ment of the Ordnance Department, all books, records,
5ce equipment used by the Medical De-
nt or the Ordnance Department in connec-
tion with such investigation or research, manufac-
ture or production, or operation of plants and proving
grounds, all rights under contract made by the Med-
ical Department or Ordnance Department in, or in
connection with, the operation of such plants and insti-
tutions as specified herein, all rights under contract made
by the Medical Department or Ordnance Department
in, or in connection with such work, and the entire
personnel (commissioned, enlisted, and civilian) of
the Ordnance Department and Sanitary Corps of the
Medical Department as at present assigned to or en-
gaged upon work in, or in connection with, such in-
vestigation or research, manufacture or production, or
operation of plants and proving grounds, are hereby
transferred from the jurisdiction of the Ordnance De-
partment and the Medical Department and placed un-
der the jurisdiction of the Director of the Chemical
Warfare Service, it being the intention hereof to trans-
fer from the jurisdiction of the Medical Department
and the Ordnance Department to the jurisdiction of
the Director of the Chemical Warfare Service every
Major J. H. Brightman
function, power, and duty connected with the investi-
gation, manufacture, or production of toxic gases, gas-
defense appliances, including the necessary research con-
nected with gas warfare, gas-shell filling plants, and
proving grounds utilized in connection therewith, all
property of every sort or nature used or procured for
use in, or in connection with, said operation of such
plants and proving grounds and the entire personnel
of the Ordnance Department and Sanitary Corps of
the Medical Department as at present assigned to, or
engaged upon work in, or in connection with, the
operation and maintenance of such plants engaged in
the investigation, manufacture, or production of toxic
gases, gas-defense appliances, ' including gas-filling
plants and proving grounds utilized in connection
therewith.
(5) All unexpended funds of appropriations hereto-
fore made for the Medical Department or Ordnance
Department and already allotted for use in connec-
tion with the operation and maintenance of plants now
engaged in, or under construction for the purpose of
Sept., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
677
engaging in, the investigation, manufacture, or pro-
duction of toxic gases or gas-defense appliances, in-
cluding gas-shell filling plants, are hereby transferred to,
and placed under the jurisdiction of, the Director of the
Chemical Warfare Service for the purpose of meeting
the obligations and expenditures authorized herein;
and, in so far as such funds have not been already
specifically allotted by the Medical Department and
the Ordnance Department for the purposes specified
herein, they shall now be allotted by the Secretary
of War, in such proportions as shall to him seem best
intended to meet the requirements of the situation
and the intentions of Congress when making said ap-
propriations, and the funds so _ allotted by the Secre-
tary of War to meet the activities of the Chemical War-
fare Service, as heretofore defined herein, are hereby
transferred to, and placed under the jurisdiction of,
the Director of the Chemical Warfare Service for the
purpose of meeting the authorized obligations and ex-
penditures of the Chemical Warfare Service.
(6) This order shall be and remain in full force and
effect during the continuation of the present war and
for six months after the termination thereof, by proc-
lamation of the treaty of peace, or until theretofore
amended, modified, or rescinded.
II — By direction of the President, Maj. Gen. Wil-
liam L. Sibert, United States Army, is relieved from
duty as Director of the Gas Service, and is detailed as
Director of the Chemical Warfare Service, National
Army.
[322.06 A. G. 0.] By Order of the Secretary of War.
Peyton C. March,
General, Chief of Staff
[Official] H. P. McCain,
The Adjutant General
ORGANIZATION PLAN OF CHEMICAL WARFARE SERVICE
DIRECTOR
Maj. Gen. Wm. L. Sibert
Staff
Medical Officer, Col. W. J. L. Lyster, S. C.
Assistant. Capt. H. C. Bradley
Ordnance Officer, Lt. Col. C. B. Thummel, O. D.
Assistant, Maj. C. S. Stevenson, C. W. S.
Representative of British Military Mission, Maj. J. H. Brightman.
HEADQUARTERS ORGANIZATION
Assistant Director
Col. H. C. Newcomer, C. E.
To act for the Director in his absence, in charge of all military matters
and new projects. Chairman, Board of Review.
Military Assistants
Maj. J. H. Walton, C. W. S. Capt. J. S. Baker, C. W. S.
Capt V. L. Bohnson, C. W. S. Capt. A. Bolenbaugh, C. W. S.
Capt. S. J. Delancy, C. W. S. 1st Lt. R. C. Henderson, C. W. S.
2nd Lt. F. C. Perkins.
Technical Assistants
Maj. S. A. Tucker, C. W. S. Capt. R. Franchot
Capt. G. M. S. Tait, C. W. S.
1st Lt. L. Van Doren, C. W. S.
Office Administration
Major W. W. Parker, C. W. S.
In charge of files and clerical personnel, receipt and distribution of
mails, collection and transmission of papers between various sections of the
office, office disbursements.
Assistants
1st Lt. F. W. Dasher, C. W. S. 2nd Lt. B. W. Tipton, C. W. S.
2nd Lt. W. F. Kunkle, C. W. S. 2nd Lt. W. D. Towler, C. W. S.
Relations Section
Col. M. T. Bogert, C W. S.
In charge of relations with Universities, with industries, with the office
of the Director of Purchases, Storage and Traffic, and with the War In-
dustries Board, including its committees.
Maj. Victor Lenher, C. W. S.
Maj. W. J. Noonan, C. W. S.
Maj. Allen Rogers, C. W. S.
Maj. Samuel Avery, C. W. S.
Assistants
Capt. C. V. Shechan, C. W. S.
Capt. W. H. Hickin, C. W. S.
1st Lt. H. F. Scharer, C. W. S.
Mr. Geo. S. Case. C. W. S.
Personnel Section
Major F. E. Breithut, C. W. S.
In charge of all matters pertaining to procurement and assignments of
commissioned and enlisted personnel of the Chemical Warfare Service.
Assistants
lit Lt. G. W. Phillips, C. W. S. 1st Lt. H. B. Bramlet, C. W. S.
2nd Lt. A. E. Case. C. W. S.
Contracts and Patents Section
Captain W. K. Jackson, C W. S.
In charge of Section, Member of Board of Review
Assistant
Capt. R. B. Meckley, C W. S.
Finance Section
Major C. C. Coombs
In charge of estimates, appropriations and allotments, of administrative
audit of all disbursing accounts and of property. Member of Board of
Review, C. W. S.
Assistant
Capt. Ben Jenkins, C. W. S.
Requirements and Progress Section
Capt. S. M. Cadwell, C. W. S.. In charge of Section.
Assistants
2nd Lt. J. A. Sohen, C. W. S.
Confidential Information Section
Major S. P. Mulliken, C. W. S.. In charge of Section.
Assistant
2nd Lt. H. E. Moore, C. W. S.
Transportation Section
Officer in charge not yet selected.
Assistant
Capt. H. R. Sharkey, C. W. S.
FIELD ORGANIZATION
Gas Offense Division
Officer in Charge, Col. W. H. Walker
The production of gas, containers and other material for use in offensive
gas warfare.
Gas Defense Division
Officer in Charge, Col. Bradley Dewey
The production of material such as gas masks for use in the defensive.
Proving Division
Officer in Charge, Maj. W. S. Bacon
Charged with the duty of proving the efficiency of n
condition.
Development Division
Chief, Col. Frank M. Dorsey
For the development of material received from
to the point where it may be turned over for proving
aterial under field
the Research Division
Charged
Research Division
Chief, Col. G. A. Burrell
.ith research into all matters pertaining to gas warfare.
European Division
This division includes personnel assigned to all divisions and corps and
my headquarters in addition to those required for the supply of material
the field in France.
Medical Division
Officer in charge. Col. ~W.*J. L. Lyster
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. g
Major i
Capt. s. m. Cadweh
Sept., iqiS THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
670
Major Wilmam .S. Bacon
I I' M D01
THE JOURNAL OF I V DVSTRIAL AND ENGINEERING ( II1.M1STRY Vol. 10, No. 9
COMMISSIONED PERSONNEL. CHEMICAL WARFARE SERVICE
MAJOR GENERAL
Sibert, William L.
COLONELS
Ardery, Edward A.
Bacon, Raymond F.
Bogcrt, Marston T.
Burrell. George A.
Dewey. Bradley
Fries. Amos A.
Johnston. Edward N.
■ ■■ J. L
Newcomer, H. C.
Schulz. John W. N.
Walker, Win. II.
LIEUTENANT COLONELS
Ucsse, Arthur I..
Chance, Edwin M.
McPherson, Win.
Norris, Jas. F.
Thummel, C. B.
Vaughn, Chas. F
HAJOBS
Almy, Chas., Jr.
ttmel A.
Bacon, Win S
Barth, Theo H.
Breithut, Frederick E.
Brightman. J H.
Chance, '1' Mitchell
Clark, Edward B
Conant, J. 11
Connel. K.irl
Coombs, C. C
Demorest, Dana J.
Dewey, Frederick A.
Dunn, Hi!
Evans. Wm. L.
Frary, Prai
Free, Edw. E.
Gallowhur, Wm G.
\\u
. Hugo H.
Haughton, Percy D,
Heritage, Arthur M.
Hildebraud. Joel II.
Johnson, Cleon R.
Jones, W Catesby
Lcniier, Victor
Lewis, Gilbert N.
Lockwood. Wm. G.
Mart, Frank W.
Morey, Stephen E-
Mulliken, Samuel P.
Nagelvoort, Adrian
Noonan, Wm. J.
Parker, Walter W.
Reed. Philip L.
Richardson. Chas. B.
Rogers. Allen
Rose. Reed P.
Schuit, Henry P.
Sibert, Wm. O.
Sill. Theo W
Stevens. Oscar E.
Stevenson
Sweeney. Orland R.
Temple, Sterlim: M
Tucker. Samuel A.
Van ICeuren, Edgar P.
Wagner, Frank 1
Walton, .1 11
Wilson, Irving W.
Wilson, Robert B
Woodruff, John C.
Wraith, Chas R.
Wyckoff. Arcalons W.
Zinsser, Frederick G.
CAPTAINS
Akers, James G.
Armory, John A.
Armstrong. James
Att.rburv, Kirbv
Babbitt, J Stanley
Hailev. R. O.
Maker, Ross A.
Balfe, T. W.
Lawrence L.
:to S.
nisiiop. r B
Itl.ibe. Kenneth It.
ltlam-hnrd. Ross C.
BUn, p. w
blossom, Geo W
I II
llohnson. V I,
Holenbaugh, A.
lloolhmaii. Pale M
..I (',
11 C
llriiit.in, Paul II M.
Hrodhcacl. Nathl It.
llrophv. Wm B
Bruce. I
Burns. Arthur R.
Byen, Horace G.
captains (Continued)
muel A.
Cadwell, Sidney M.
Campau
Carleton Paul M
Chalfant, Charles C.
Chandler. Henry P.
Clucas. Richard M.
Cohurn. Wm II
Coll. v. I b
Coleman. W. H.
Corrill, Chas, H.
Corry. Edwin i:
Cover, Lester C.
Crocker. Ralph H.
Cutler. Thov H.
Dana. Lowell E.
Dee. Thos J.
Delancy. S. J.
Dickinson, Arnold C
Monk. Marion G.
Douglas. Stephen A
Duff, Levi B.
Eldredge, Orrin S.
Flood, Frank R.
Foster, Harold B.
Fulford, lister E.
Garner, II L.
Gartner. II A
Giesv. Paul M
Gill, Benj.
Godfrey, William S.
Gordon. Robt. D.
Goss. Byron G.
Gowdy, Robt C.
Graham, Robert McC.
Graves. Caswell
Grove, Winfield S.
Guiteras, Harold G.
Hall, Ralph R.
Hardesty, Geo. R.
Harmd. H. S.
Harshberger, Clarkson E.
Haydcn. Fred I.
Heath. Michael Y.
Herbert, Wilyn
Herkncss, Wayne
Herman
Hickin, William H.
Hoffman, Wm. B.
Hunt, Geo. A
Jackson, W. K
Jenkins, Ben
Joly. Chas. L.
Kay, Wm. DeY.
Kenney. A. W.
Keyes, Frederick G
Kops. Waldemar
Kramer. Richard L.
Larson! A. T.
Latimer. Lewis L.
Lawrence, James
Lawton, Stanley H.
Levering. Arthur C.
Little, John S
Livermore, Harris
Llewellyn, Paul R.
Lockwood, Wm. G.
Long, Chas. F.
Lovell, Frederick A.
I. von. F. J.
una, Wm, H.
McChesney, A. G.
McGovern, Thos. T.
McGrath, David J.
McKcnna. Wm J.
McKinnev, Wm. S.
Mack ill. "Colin
Macomber, Leonard
Martin. Wm. C.
Meckley, Robt B.
Melendy, R. P.
Merrill, Hamilton
Millar, Hudson C.
Millar. R W
Nieolct, Ben H.
Northrup. John H.
Oberfell. Geo. G.
Parks. G. A.
Parsons. I. W.
Patterson. Earl
Peabody. Stuyvesant
Pearce. Chas. H.
Perry. Gl<
Pope. Frederick
iond V.
Ray. Arthur B.
Renihaw, R. R.
Richardson, Jos. C,
Rile. Win M.
Roberts. O. E.
Wm. O.
Rollason, Geoffrey M.
Rowan, Hugh W.
Rue, John I>
• H . Jr.
K
Schlcsingcr, Bcrthold E.
captains (Concluded)
Schmidt, Victor B.
.Selfridgc. John S.
Sharkey II R
Sharpe, Harold C.
Shattuck. Edmund J.
Shaw. George Edward
Sheehan. Charles V.
Silver. Jos. E.
Smith, Earl C.
Smith. Raymond T.
Smyth, Frederick H.
Stapleton, Edward L,
St. John, Adrian
Sutherland Leslie T.
Tail. Godfrey W. S.
Taylor. Alfred L.
Taylor, David P.
Tavlor, R E.
Teague. M. C
Thompson, Thos. E.
Throop, Benj H.
Torry, Harry W.
Trumbell. Harland L.
Uhlinger. Roy H.
Urbain, Leon F.
Ward, Ralph 1 1.
Warner. Stuart D.
Wells. Harry E.
Wesson, L. G.
Wheeler, Thorne L.
Whitehousc, H. D.
Whilloek, Chas. M.
Wilkinson, J. A
Winkclmann. Herbert
Wolf, James S.
Wood. Alfred W.
Wright, Burnett
Zanetti, J. Enrique
FIRST LIEUTENANTS
Abrahams, Clinton D.
Abrams, Allen
Adams. James F.
Alden, J. L.
Allen, Roger E.
Anderson. Harry P.
Andnis, Leonard A.
Armstrong, Charles D.
Arnold, II. C.
Ashe, Lauron H.
Ashman. L. A.
Ashman, L. H.
Ayer, Paul P.
Bach. Ronald P.
Bailey. Albert E.
Baroett. Joseph J.
Barry. John G.
Beal. William D.
Bear, H. K.
Becker. Hason K.
Bedford. Edward T.
Bell, Thomas R.
Bennett, H. S.
Best, Arthur F.
Blakney. Geo. P.
Bogue, Joseph C.
Boon, C. J.
Bowman, Reginald C.
Bramlet, Hubert B.
Bristow. James J.
Brock. Earlc A.
Brodesser, R. E.
Brown, Carl II.
Brown. Lester B.
Burt. R. A.
Cahill. Michael
Callemon. Clarence*B.
Clancy. Richard W.
Clapp, Dudley
.Clark S. C.
Clarke. Theodore
Clarkson. John L.
Clifford. C. W.
Cochran. Marshall G.
Coghlan. S. R.
Cole. Howard I.
Colebrook. M. W.
Collette. W R.
Conohav. John R.
Cool, Claude A.
Cox, Samuel F.
Cretcher. Leonard H.
Cronshaw, James L.
Cross6eld. Albert S.
Cuff. James B.
Dale. Stewart T.
Darling. Harry C.
Dasher. Frances W.
Davidson. A W
Davidson, Joseph G.
Davis. George W.
Dunbar. Noel S.
Dwyer, C I.
Eason, Harrv Mc.
Eaton. Harrv A. F.
Elden. John A.
Eldridge. Arthur C.
first lieutenants (.Continued)
Elliott, Lowell A.
Elsbey, Alden G.
Emory, Si
Esser. A
Fairbanks Herbert S.
Fairchild, Tappen
Felsing. W. A.
Fisher, Abram M.
Fitzgerald, Heber D.
Fleming, Walter F.
Francke, Hugo
Frederick, E. L.
Fuller. E. W.
Gage, Roscoe M.
Gaines, O. I.
Gauger, Alfred W.
Gibson, Richard
Goldschmidt, Samuel
Gordon. Marcus A.
Gruse, William A.
Gurae} , Harold P.
Hartshoi
Hartshorn. Fred M.
Hayden, E. M.
Henderson. L. M.
Henderson. R. C.
Heneage. Thomas H.
Hentz, William A.
Hetherington, George F.
Hillerv, Harrv M.
Hobson, H. T.
Hoguot, Rene
Holland, Martin A.
Holm, George E.
Holmes, Raymond M.
Hooper, Noel J.
Horton, W'inthrop S.
Howe. Robert A.
Howlett. Arthur E
Hudson, H. H.
Hudson, W. E.
Hull. Edwin J.
Hunter. Robt. C.
Iddles. Alfred
Jackson, William M.
Johnson, Robert L.
Jones. Spencer L.
Katz, Sidney H.
Keitt, Geo. W.
Keller, Alexander W.
KeJogg. Edward A.
Kempton. Robert E.
Kerns. J. T.
Kerr, George M.
Kienle. R. H.
King, Arthur C.
King, John L.
King. T. S.
Kipka. Ross E.
Kirkpatrick, Walter
Klauber, Murray
Knox, W. L.
Koldon, Dudley F.
Lamb, Lloyd B.
Lambert, Marion L. J.
Latson. Frank W.
Le.ivitt. George F.
Lee. Elwood B.
Lewis. Walter H.
Leyden, James, Jr.
Lloyd, Edward C.
Long, David R.
Long, Howard A.
McBride. George H.
McCoy, John G.
McCune, J. S.
McCurdy. Phillip R.
McGowan, Henry G.
McNeil. Winfield I.
McWilliams. John C.
MacNeill. X M.
MacConneU, John G.
MacDonald. Alexander D.
Mack. Edward
Mahlman, Osburn L.
Manning, Edwin C.
Mansur. Charles I.
Marshall. William D.
Martin. H. A.
Mayer. Gustave
Mayham, Ray E.
Mavnard. Leonard A.
Merrill Leslie M.
Merrvman, James R.
Meserve. Philip W.
■Mitchell. John H.
Mollitt. H. R.
Morawski. Frederick
Morgan.
Morgan. John D.
Molt. John
Moulton. Paul B.
Mueller, William A.
Mulford, William J.
Murphy. Alfred L.
Murphy. Ray D.
Murtfeidi. W Scott
Sept., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
681
COMMISSIONED PERSONNEL, CHEMICAL WARFARE SERVICE {Concluded)
FIRST LIEUTENANTS (Contil
Nasseit, Harry B.
Noble, Edson J.
Noer, Oyvind J.
Norlin, F. C.
Northrup, William C.
Norton, A. R.
Norton, F. A.
Nowry, Irvin W.
O'Brein, Bernard
Olson, A. R.
Ott, J. E.
Parks, James G.
Parmelee, Paul R.
Patterson, G. P.
Perkins, Granville A.
Perrott, G. St. J.
Phillips, George W.
Pierce, Edward T.
Popp, Earl C.
Pratt, Francis S.
Prentice, Phillip B.
Proctor, William R.
Pyle, David H.
Racicot, P. A.
Rahn, Reinhard
Rambo, Joseph D.
Ranson, William J.
iRapee, Frank J.
Recter, Thomas N.
Regan, Edward F.
Reiling, Howard A.
Rhode, Leon M.
Riddell, John F.
Rixey, Eppa
Robinson, Chas. R.
Rogers, Rollins W.
Romilly, Edgar P.
Rowe, David H.
Royce, Harrison S.
Russell, G. P.
Rutledge, George F
Salisbury, Donald W.
Sampson, Ernest
Sawders, J. C.
Scory, J. W.
Scharer, H. F.
Schaufele, H. J.
Scheirz. E. R.
Schmidt, Mott B.
Schultz, Addie D.
Schwarz, M. W.
Senior, James K.
Shaw, Guthrie
Shaw, Joseph T.
Shaw, Leon E.
Sibert, Eugene
Sidelinger, Roy L.
Silsbee, James A.
Smith, Lawrence W.
Smith, Lee I.
Smith, Leslie D.
Smyth, C. P.
eS)
{Concluded)
FIRST LIEUTE
Spaulding, E. G.
Spriggs, C. I.
Staples, Scott D.
Stearns, Albert M.
Steenken, F. L.
Steinbach, E. S.
Stephens, Charles W.
Stump, Horace E.
Stupp, John G.
Suydam, John R , Jr.
Swanson, F. J.
Talbot, John C.
Talcott, Harrison W.
Thomas, Ralph M.
Thomas. Richard W.
Thompson, Louis E.
Todd, William T.
Towler, Thomas W.
Trenkman, Frederick
Truax, Harold W
Truhee. William E.
Tuttle. Neal
Urquhart, George R.
Van Doren, Lloyd
Vanvoorsees, Harold E.
Vile, Norman B.
Vincent, Max G.
Visscher, Raymond
Walker, Lester V.
Wallace, E. S.
Walsh, James F.
Wangler, Albert F.
Wardon, Edward W. •
Watson, Warren M.
Weeks, Robert W.
Weinert, R. B.
Wells, Arthur G.
Welsh, Thomas W. B.
Wemple, Holland R.
Whetzel, Joshua C.
Whiton, Louis G.
Wightman, Eugene P.
Williamson, Robert B.
Willis. Oliver E.
Wilson, David W.
Wilson, John E.
Wilson, Otto
Winter, Edwin M.
Wiswall, Paul M.
Withington, Lathrop
Woodbury, Horace G.
Woodruff, William W.
Woodward, Paul G.
Wylde, Wildred A.
Yablick, Max
Yoe, John H.
Zimmerman, Joseph
SECOND LIEUTENANTS
Acker, Ernest R.
Austin, Robert W.
Bangs, B. C.
SECOND LIEUTENANTS (Conti:
Barren, Edmund D.
Barrho, W. H.
Battley, J. F.
Benton, Arthur F.
Biance. Fred
Birckhead, Peter H.
Blank, J. F.
Blicke, Frederick F.
Bliss, Roland R.
Bly, Robert S.
Boardman, Roland S.
Borbeck, Archibald F.
Bowers, Paul C.
Bowes, Almond N.
Bowman, Ira J.
Bowman, Lee
Brown, Raymond G.
Brumhalt. John W.
Carry, John R.
Case. Arthur E.
Chaplin, John H.
Charron, Roy C.
Clark, Ernest M.
Conrad, Frederick U.
Crowell, Geo. W.
Davidson, Benj. B.
Dennis, Richard C.
Diven, John M.
Donoho, J. B.
Duckworth. John S.
Dunn, Chas. K.
Dunn, J. S.
Eiselot, Lewis G.
Ellison, A. D.
Embree, Spencer D.
Emmons. W. H.
Fannan, H. B.
Funsten, S. R.
Giles, Jeremiah D.
Greninger, R. R.
Gross, Paul M.
Hall, Robert B.
Hammond, William A.
Harper, Walter J.
Hast, Julian A.
Heath. John R.
Heffner, Oden C.
Heidingsfeld. Ralph
Heins, Ralph W.
Higbee, Clarence W.
Holt, Herbert B.
Hood, Harrison P.
Hooker, Albert H.
Huff, W. J.
Jennings, M. E.
Kearns. J. J.
Killam, Luther L.
Kinney, Selwyne P.
Knapp, Ralph
Kunkle, Walter F.
Law, James D.
Levy, Gaston J.
ued)
1 lieutenants (Concluded)
Lindsay, Walter S.
Loeb, Edward H.
McKenzie, Clyde
McLane, Howard B.
McNaugher, Joseph W.
Miller. Russell W.
Milligan, Lowell H.
Moore. Herbert E.
Neff, Chester M.
Nichols, H. Janney, Jr.
Osmer, John W.
Overstreet, John B.
Page, C. W. C.
Pauly, Robert C.
Pease, Robert N.
Peck, Edward B.
Pelton, Harold A.
Penfield, F. Joel
Penfield, Richard
Perkins, F. C.
Pettengill, Francis W.
Probeck, E. J.
Rees, John G.
Reichert, S. Joseph
Reyerson, Lloyd H.
Ribble, Keith P.
Richardson, George C.
Riker, Carlton B.
Robinson, Otto L.
Ross, William B.
Rothchild, Henry A.
Rundlett. Arnold D.
Schoetz, Francis H.
Schweizer, James A.
Scott, Warren P.
Sebastian, Reuben L.
Serson, Fred J.
Shakn
Sha
Sha
Shu
, J. G.
nhouse, J. G.
r, Ralph K.
Ellis M.
in S.
Smith, Charles V.
Sohon, Julian A.
Spofford, Charles B. Jr.,
Stone, Sam P.
Stuarn, James V.
Taylor, David B.
Thayer. Bruce W.
Thompson, Frank D.
Thorp, Gerald
Tipton, Ben. W.
Towler, Eugene D.
Towler, W. D.
Vealey, W. D.
Walther, Owen N.
Wannamaker. Geo.
Weber, Harold C.
White, James M.
Woodbury, V. P.
Woods, Basil G.
Wright. Douglas B.
PERSONNEL OF DIVISIONS
EUROPEAN DIVISION
COLONELS
Ardery, Edward A.
Bacon, Raymond F.
No
LIEUTENANT COLONELS
s, James F.
MAJORS
Connel, Karl
Hamor William R.
Hildebrand, Joel H.
Lewis, Gilbert N.
Lockwood, William G.
Richardson. Charles B.
Sibert, William O.
CAPTAINS
Akers, James Greaff
Corrill, Charles H.
Corry. Kdwin B
Cutler, Thomas H.
Douglas, Stephen A.
Eldredge. Orrin S.
Goss, Byron G.
Hardesty, George R.
Hunt, George A.
Joly, Charles L
Keyes, Frederick G.
Mackall, Colin
Nicolet, Ben H.
Patterson, Earl
Perry, Glenn L.
Pope, Frederick
Ray, Arthur B.
captains (Concluded)
Rollason. Geoffrey M.
Rowan, Hugh W.
Smith Earl C.
St. John, Adrian
Taylor, Alfred L.
Torry, Harry W.
Urbain, Leon F.
Ward, Ralph D.
Zanetti, J. Enrique
FIRST LIEUTENANTS
Alden, J. L.
Allen, Roger E.
Anderson, Harry P.
Ashe, Lauren H.
Bach, Ronald P.
Barnett, Joseph J.
Barry, John G.
Blakney, George P.
Bowman. Reginald C.
Clancy, Richard W.
Clapp, Dudley
Clarkson. John L.
Cole, Howard I.
Cool. Claude A.
Cronshaw, James L.
Cretcher, Leonard H.
Dale, Stewart T.
Darling, Harry C.
Eaton, Harry A. F.
Fisher, Abram M.
Francke, Hugo
Gauger, Alfred W.
Goldschrnidt, Samuel
Gordon, Marcus A.
Hartshorn, Fred N.
Hunter, Robert C.
Keitt, George W
first lieutenants (Concluded)
Knox, W. L.
McGowan, Henry G.
Mack, Edward
Maynard, Leonard A.
Meserve, Philip W.
Morgan, John D.
Murphy. Ray V.
Noer, Oyving J.
Norton, Ario R.
Nowry, Irvin W.
O'Brein. Bernard
Olson, A. R.
Parks, James G.
Parmelee, Paul R.
Popp. Earl C.
Rambo, Joseph D.
Rhode, Leon M.
Robinson, Charles R.
Rowe, David H.
Salisbury. Donald W.
Senior, James K.
Shaw, Leon E.
Sidelinger. Roy L.
Stearns. Albert M.
Stump, Horace E.
Thomas, Ralph M.
Thompson, Louis E.
Vanvoorsees, Harold E.
Walker, Lester V.
Whiton, I.ouis G.
Wightman, Eugene P.
Williamson, Robert B.
Wilson, David W.
Wylde, Wildred A.
SECOND LIEUTENANTS
Acker, Ernest R.
Austin, Robert W.
second lieutenants (Concluded)
Birckhead, Peter H.
Bowers, Paul C.
Bowman, Ira J.
Brumhalt, John W.
Conrad, Frederick U.
Crowell, George W.
Davidson, Benjamin B.
Dennis, Richard C.
Dunn, Charles K.
Eiselot, Lewis G.
Hall, Robert E.
Hast, Julian A.
Higbee, Clarence W.
Holt, Herbert B.
Hooker, Albert H.
Knapp, Ralph
Law. James D.
McNaugher, Joseph W.
Miller, Russell W.
Neff, Chester M.
Nichols, H. Janney, Jr.
Pauly, Robert C.
Peck. Edward B.
Ribble, Keith P.
Riker, Carlton B.
Robinson, Otto L.
Schotz. Francis H.
Scott, Warren P.
Sebastian. Reuben L.
Shaw, Ellis M
Skinner, Glenn S.
Stuam. James V.
Taylor, David B,
Thayer, Bruce W.
Thompson, Frank D.
Wannamaker, George
White, James M.
Wright, Douglas B.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 9
OAS OJFENSE DIVISION
1 .-.ANT CO
Chance, Edwin M
McPherson, William
Vaughn, Charl. I
MAJORS
I ■ 1"
Dcmorest, Dana J.
Prei Edward 1
Qallowhur, \\ m 1
1 mi . 1 1 11 0 H
'w thut M,
Mack, Prank W.
Nagelvoort, Adrian
Parln.l. Clai
, ' >r l.i ikJ ]<
Sterling N.
Van Keureh, I .1 B
Wagner, Frank J.
Wraith !.
Zinsser, F.-G.
Bcebc, Lawrence I..
Hishop, Richard E.
1:1.. ... hard Ross C
Uoothman. Male M.
Brouwer, Harold
Hums, Arthur 1< .
• II,, S
Campau, M W
Chai tr, Henry P
Clucas, Richard M.
Donk, Marion C.
Pranl forter, Clarenc
Gartner, Henry i >.
1 -ill Benjamin M
COLONEL
1 i.wey, Bradley
LIEUTENANT COLONEL
Hesse, Arthur I..
MAJORS
Alniv, Charles
Bacon, William S.
Harth, Theodore II.
I lewey, Frederick A.
Johnson. Cleos R
Moonan, William J.
Reed. Philip I.
Schuil, Iletirv I'
Sill. Theod,,i, \\
Itevens, Osi ai I
\\ biting, Tasper
Wilson. Irving w
Woodruff, John l
\ I 1 ' 1 I 1 1 1 1 ) k 1 1 I . J
n J. Stanley
nnetfa B
Bopp. Carl 1 ',
Bradley, 11 irold I
Hrodhead. Nathaniel B
llrophy. Win E
iinuel A.
1 oburn, Win II.
iter E.
I 'in 1 I "well B,
I 'ee. 'I In
on, Arnold C.
Duff, Levi I!
Foster. Harold B
Full.ird. Lester E.
Gilbert, Rollin P
Green, Raymond w
1 (rove, \\ii
Herbert, Wilwyi
1.1, .
LIBUTBNANT
I M,
William, 1 I
CAPTAI
Borncbev " I I
Folgcr. R C
Hering. 1-
captains (Concluded)
1 Gordon, Robert D.
Hall, Ralph E.
Heath, Michael Y.
William !•:.
Hope, Robert D.
atingsbui
Lawton, Stanley H.
Levering, Walter H
Long, Charles I'*.
Lovell, Fred A.
McGovern, Thomas F.
McKenna. Win J
Martin, Wm C.
Olin, Hubert L.
■ rles II .
Richardson, los. G.
Robinson. Win ' I
Ross. Wm H.
hn D.
Schmidt, Victor R
I'llm S
Seybold, Eugene
Shark, v, Howard R.
harp 11 u-old 1
Taylor, David P
Thompson, Thomas P.
Trumbull, Harlan L.
Wesson, Lawrence G.
WbitlOCk, Charles M.
Wilkinson. John A.
FIRST LIEUTENANTS
Armstrong, Charles D.
Ashmun, I. .wis II
Becker, Hasen K.
Brock. Earle A
Brown, Lester B.
Carley, Joseph T.
Carter, Donald 1'.
Conohay, John R.
Cud. Jam.
first i.iei thnan'TS {Continued)
Cummiskey, James E.
Davidson, Albert W.
Davis George W.
i nir. ,nt. Thomas G.
Dwyer. Chail
Eldridge, Arthur C.
Uden G
Pairbank, Hi i
Felsing. Win A
Haist, Theodore V.
ii,,-.. 1. 1, i-: m.
1. 1.11. s. Alfred
Johnson. Robert L.
Jones, Thomas W.
Kerr. George M.
Killam Luther M.
Kipka. Ross E.
Kearney. David R.
Lamb, Lloyd
' Leach. Win H
Loving, Henry W.
M. Bride, George H.
McCoy, John G.
McGhee. Burt G.
McWilliams, John O.
Manning. Edwin C.
Marshall, William D.
Martin, llarrv A.
Mueller. William E.
N'assoit . llarrv 11
Pierce. David H.
Rahn. Reinhardt
Royce, Harrison S
Rutledge. George F.
Sawders 1
Schermerhorn, George D.
Schmidt. Mott B.
Schultz. Addle I>.
Silsbee, James A
Sprague, Charles
is. Charles W.
Stupp, John G.
GAS DEFENSE DIVISION
captains (Concluded)
Kay. Wm. D.
Kops, Waldcmar
Little, form S.
Llewellyn, Paul R.
Macolnber. Leonard
McGrath, David J.
MeKinnev, William S.
Merrill Hamilton
Puff, Raymond V.
Rile. Wm \l
Russell Jos. B.
Schlesinger, Barthold E.
Shattuck, Edmund J.
\
Silver, roseph R.
Smith. Raymond T.
Stapleton, Ldward L.
I i I.,, :
Throop. Benjamin A.
Warner, Stuart 11.
West. Clarence J.
Uliil. I lalctice W.
Winklemann, Herbert A.
Wolf. Jas S,
Wood. Alfred W.
FIRST LIEUTENANTS
Andrtis, Leonard A.
P ml P.
Bailej Albert E.
Heal Win D
i Edward T.
Bell. Thomas R.
lei \tihurF.
Bogue, Joseph C.
is s.
I .raes J.
Cahill. Michael
. ,11,, man Clarence B.
Marshall G.
Colebrook, M. W
1.1. Albert S.
I lunbar, Noel s
I ' "" H iiry Mc,
Lasl.ti, Lester H,
FIRST lieutenants (.Continued)
Elden. John A.
Elliott, Lowell A.
Ksser. Alvah E.
Fairchild, Tappen
Fitzgerald, Heber I).
Fleming, Walter F
Gage. Roscoe M
Gibson, Richard
Gurney, Harold P.
Haggard, Howard W. (S. C.)
Heneage. Thos. H.
Henlz, Wm. A
Hetherington, George F.
Hillery. Harry M.
1 In. n, i , Rene
Holden. Dudley F.
Holm, George E.
Holmes, Raymond M.
Hooper, Xoel J
Howe. Robert A
Howlett, Arthur E.
Hughes. Dale C,
Hull. Edwin I
Jackson Wm. M.
Jones. Spen
Keller. Alexander W.
Kcinplon. Robert B.
i.'lm L
dauber, Murray
« ,r,l \
Latson. Frank W
Leavitt, Geo. P.
Lee. i:iwood B
Jr.
Lloyd, Edward (
Long, I 'avid R.
mil, lohn G.
Mahltuan. I tsborne
Mansur, Charl
M.iv.i i
Mayham, Ray 1
McNeill. Winlield L.
Meeker. Lawrence
Merrill. Leslie M
Merryman, James R.
Mitchell, b.ii'i H
DEVELOPMENT DIVISION
captains (Concluded)
W H.
Ma, I ..
SI lohn, 11 M.
I-
Wright, B. B.
FIRST L1EUTBN
Baton I
SIS
Calaghan, J o
Cheever. I P
Chenej . M B
Dabncy. R P.
Dol.e, P
Fulks, B. F.
C.raeev W
Randall. P.
first lieutenants (Concluded)
Suydam. J R., Jr.
Thomas, Richard
Truax, Harold W.
Trubee, William E.
Wadsworth. Chas.
Wallace, Edwin S.
Weeks, Robert W.
Welch, Thomas B.
Wells Arthur C.
Wells, Burling D.
aver E.
Wilson. John E.
Woodward, Paul G.
second lieutenants
Bakken. Herman E.
Bliss. Roland R.
Howes, Almon N.
Brown. Raymond G.
Chaplin. John H.
Divcn, John M.
Pannoi Harry E.
Ford, Arthur O.
Frederick. John H.
Heidingsfeld. Ralph W.
Ileitis. Ralph W.
Joyce, Floyd E.
Lindsay, W. S
Loeb, Edward H.
McLanc, Howard B.
Milligan, Lowell H.
Osmer. John W.
Penfield, Richard
Probeck, Edwin
Reese, John G.
Sersen, Fred J.
Sharer, Ralph W.
Thornburg, George W
Tolmach, Louis
Wadd, James
Watts, Anderson H.
Woods, Basil G.
first lieutenants (Concluded)
Morawski. Frederick H.
Morgan. Arthur M.
Moukon. Paul B.
Mulford, Wm. J. (S. C.)
Murphy. Alfred
Murtfeldt. W. Scott
Nimick, Francis B.
Noble. Edson J.
Xorthrup. William C.
Pierce, Edward P.
Prentice, Philip B.
Proctor, William R.
Rammel, Chas. L.
Ransom. Wm. J.
Rapee, Frank J.
Rector, Thos. M.
Regan, Edward F.
Reiting. Howard A.
Riddell. John F.
Rodgers. Rollins W.
Romilly. Edgar P.
Sampson. Ernest (S. C.)
Scott. Henrv P
Shaw. Guthrie
Smith. Lawrence W.
Staples. Scott D.
Stephenson. Morris L.
Talbot, John C.
Talcott. Harrison W.
Todd Wm. T.
Towler. Thos. W.
Trenkman. Frederick
Urquhart, Geo
Vile, No
Max G.
Visscher, Raymond
Walsh, James
Wangler, Albert W.
Wardin. Edward
Watson, Warren
Wemple. Holland R_
Whitfield.
Wilson. Otto
Winter. Edwin M
U isw.,11 Paul M.
Woodbury. Horace G.
Zimmerman. Joseph
i ieutena
Rice W W
Royce. C.
Hi.m, W P
Sotven. H.
"ii. W.
Weber, L.
Westbrook, L.
Wilkins. W P.
Sept., 1918
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
683
1 i * 5 *
11*
j
|
-
h
_
■
MAJOR
Bacon, Win. S.
CAPTAINS
Blossom. Geo. W., Jr.
Graze, Boswell
Hampton, Frank
Marsh, Robert McC.
Throop, Benjamin H.
Winkelmann, Herbert A
FIRST LIEUTENANTS
Crossfield. Albert S.
Derch, William S.
Emery, Stuart R.
Holland, Martin A.
King, Arthur G.
PROVING DIVISION
first lieutenants (Concluded)
Kirner, Walter R.
Proctor, William R., Jr.
Pyle, Joseph F.
Riddell, John F.
Wood, Charles S.
SECOND LIEUTENANTS
Badden, William
Boring, Bonnell H.
Brooks, Reese G.
Brown, Edward P., Jr.
Fink, Harvey Hoyl
Knisely, Alton S.
Matthews, Alfred G.
Wenrich, Martin B.
Wood, Robert E.
CENSUS OF CHEMISTS
The following announcement, questionnaire, and
letter are being sent to all chemists:
At the beginning of the present war the foresight and
energy of Dr. Charles L. Parsons were responsible for
the taking of a census of the chemists of the United
States by the Bureau of Mines of the Department of
the Interior, and the American Chemical Society.
This census has been of incalculable value to the
Government in the prosecution of the war during
the past year, and without it the present state of
progress of the United States in the branch of chemi-
cal warfare would have been impossible of attainment.
During the same period, however, conditions have
undergone rapid and radical changes. The old census,
excellent as it is. is no longer completely adequate.
Much information is now necessary which a year ago
was apparently of little importance. It is obvious,
too, that the War Department cannot remain in the
position of relying on another branch of the Govern-
ment for its information on so vital a matter; it must
have its own system of records, made largely from the
viewpoint of the military status of the chemists.
This is especially true now that all the various agencies
engaged in poison-gas warfare have been transferred
to the Chemical Warfare Service. These are the
reasons for the present census.
The envelope in which this announcement is sent con-
tains also a letter from Major General Sibert . Director of
theChemical Warfare Service, a four-page questionnaire,
and a franked return envelope. The questionnaire
is designed to cover all possible cases, and to supply the
Government with all the information which may be
of use in assigning chemists to duty. Please fill out
the questionnaire, in so far as it applies to you, and
return it in the enclosed franked return envelope at
once. You will not thereby become bound in any way
to enter the service of the Government, but you will
aid in putting the War Department in possession of
knowledge which will enable it in turn to advise you
as to your course of action. At present your greatest
opportunity to serve is to answer the Government's
questionnaire with all possible speed.
(Last)
Present address.. . .
Permanent address.
I — General
1. Horn (!l) Date (6) Place 2. Age..
I Place Of birth (0) of father (») of mother
I \,, you U A„„ ,1, :m"citizcn>. . ..5. If naturalized, give dale
684
THE JOURNAL Of INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 9
6. Are you married? 7. Is your wife living?
8. How many people are dependent upon you (a) wholly?
(6) partially ?
II — Training
9. Give the names of the schools, colleges, universities, graduate schools,
or technical schools, which you have attended, with dates of at-
tendance, courses pursued, and degrees granted.
Institution Dates Course Pursued Deorbb
10. State any other training you have had
1 1 . State fully the courses of study in which you have specialized .
12. What foreign languages do you (a) speak?. . . .
((>) read? (0 write? . .
I J. Of what technical societies are you a member?
Ill — Practical Experience
14. In what foreign countries have you had experience, and how much?
15. How many years of continuous experience have you had?
(o) Industrial (d) Teaching . (c) Otncr
16. What experience have you had along executive and administrative
lines'
17. State in detail your duties in your various positions:
Nature Salary
From — To Employer Title of Work (Statement
optional and
confidential)
chemical materials and chemical man power. Of these two
essential elements chemical man power has so far received less
attention. The census of American chemists made by the
American Chemical Society in 1917 has been of great assistance
to the War Department. Without it the present state of prog-
ress of the United States in chemical warfare would have been
impossible of attainment.
However, during the same period conditions have undergone
rapid and radical changes. The old census, excellent as it was,
is no longer completely adequate. With the organization of the
Chemical Warfare Service as an independent branch of the War
Department, unifying all the elements of chemical warfare, it is
obvious that the War Department must have its own set of
records on a matter so vital to its own success. Moreover, these
records must contain information which a short time ago was
apparently of little importance. The new census must be made
primarily from the viewpoint of the military status of
chemists.
The importance of a prompt return of the census blank,
properly filled out, by every chemist of the country, cannot be
overstated. American chemists are presented at this moment
with one of the greatest opportunities to serve their country by
the simple process of answering this questionnaire with all
possible speed.
(Signed) William L. Sibert,
Major General, U. S. A.
Director, Chemical Warfare Service
18. Publications:
Title
19. State specifically the kind of work you do best.
20. In the present emergency how and where, in your opinion, could you
be of most service to your country ?
IV — Service
21. Do you desire to enter the service of the United States at once (a) in a
civilian capacity? (6) in a military capacity?
Note — // you answer this question in the affirmative, answer the rest of
the questions in this section insofar as they apply to your case: Other-
wise, skip to Section V .
22. What rank (or salary, if you desire a civilian appointment) would you
accept?
23. What has been your total military experience?
24. Arc you registered in the draft?
25. What is your Order Number?. .. .26. What is your Serial Number?
27. Have you received the draft questionnaire?
28. How have you been classified?
29. Give names and addresses of three or four responsible persons (not
relatives) or send letters of recommendation herewith:
No
A.Mr, aa
Y Miscellaneous
anything else, which will aid us. or which you want us to know,
which is not covered by the questions on this folder. (Answer this
question last.)
Rh Read rats Whole Qusstionnaikb and Sign Below
WAR DEPARTMENT
micai. WARFARE service, WASHINGTON, D. C.
September i, iqiS
to tub chemists of tin: initei> mates:
Tins is :i chemical wai therefore the War Department must
mediately available all possible information regarding
CHEMISTS IN CAMP
As the result of the letter from the Adjutant
General of the Army, dated May 28, 1918, 1749 chem-
ists have been reported on. Of these the report of
action to August 1, 1918, shows that 281 were ordered
to remain with their military organization because
they were already performing chemical duties, 34
were requested to remain with their military organiza-
tion because they were more useful in the military
work which they were doing, 12 were furloughed back
to industry. 165 were not chemists in the true sense
of the word and were, therefore, ordered back to the
line, and 1294 now placed in actual chemical work.
There were being held for further investigation of their
qualifications on August 1, 1918, 432 men. The re-
maining 23 men were unavailable for transfer, because
they had already received their overseas orders.
The 1294 men, who would otherwise be serving
in a purely military capacity and whose chemical train-
ing is now being utilized in chemical work, have,
therefore, been saved from waste.
Each case has been considered individually, the
man's qualifications and experience have been studied
with care, the needs of the Government plants and
bureaus have been considered with equal care, and
each man has been assigned to the position for which
his training and qualifications seem to fit him best.
Undoubtedly, there have been some cases in
which square pegs have been fitted into round holes,
but, on the whole, it is felt that the adjustments have
been as well as could be expected under the circum-
stances.
Where readjustment is necessary, subsequent action
will be taken.
Sept., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
685
AN ARMY WITHOUT RESERVES
Many letters have been received commenting upon the several
points raised in the editorial "An Army without Reserves"
printed in the July issue of This Journal. In view of these
comments it seemed desirable to make a wider canvass of views
and to present these in the form of excerpts from letters.
Three points were discussed in the editorial : first, the responsi-
bility of the War Department for instructional assistance in
chemistry departments; second, intra-universit'y readjust-
ments; third, material assistance of universities by the chemical
industries.
As the symposium was going to press news was received from
Washington of favorable action by the War Department con-
cerning the detailing of instructors. This is contained in the
announcement below from Major Samuel Avery of the Rela-
tions Section, Chemical Warfare Service, at one time head
of the chemistry department of the University of Nebraska,
and later chancellor of that institution.
In the light of this action universities can now proceed
promptly and effectively to the development of their plans for
the approaching educational year. The action of the War
Department, together with the letter from Major General Sibert,
which leads the symposium, should constitute a powerful,
patriotic appeal to those who have already begun the study of
chemistry in our universities, and to the very brightest minds
among the young men entering this Fall. We are confident
that the response will be a blessing to America both in war and
in peace.
The editorial, Major Avery's announcement, and General
Sibert's letter will be reprinted in combined form. On request
these reprints will be furnished free and in quantity to uni-
versity executives and heads of chemistry departments who may
desire to circulate them. — Editor.
Application for the return of men needed should be addressed
by the heads of institutions affected to the Relations Section,
Chemical Warfare Service, 7th and B Streets, N. W., Wash-
ington, D. C, Attention Major Avery.
(Signed) Samuel Avery, Major,
Relations Section, Chemical Warfare Service
ARMY OFFICERS
It is of fundamental importance for the winning of the war
that the chemical resources, in the shape of man power, be util-
ized at their maximum efficiency. Through the mobilization
of the chemists, chemical supplies are becoming more available
each day, but chemically trained men, necessary to meet the
growing needs of the war, are constantly becoming more diffi-
cult to obtain.
The Chemical Warfare Service realizes to the utmost that men
must be trained in the university laboratories, both for the
necessity of the war and for the furtherance of the growth of
the chemical industries that have been built up in this country
since the European war began. To this end there has been
established in the Chemical Warfare Service itself a division on
University Relations, whose duties are, broadly speaking, to
further the production of chemists for the future, as well as to
supply the immediate demand.
The organization of the industrial and educational resources
of the country is a matter of such import that it must be ap-
proached in a spirit of self sacrifice, each thinking only of securing
the greatest good for all. In this spirit the Chemical Warfare
Service cordially welcomes the cooperation of both the educator
and the manufacturer; and through its divisions of University
Relations and Industrial Relations, is prepared to assist both
in meeting the difficulties in the chemical situation now con-
fronting the country. — Wm. L. Sibert, Chief, Chemical War-
fare Service.
Many of the matters with which this editorial deals are re-
ceiving very careful consideration at our hands, and consider-
able progress has already been recorded along these lines. —
MarsTON T. Bogert, Colonel, Chemical Warfare Service, N. A.
Washington, D. C, August 13, 1918
By recent ruling of the War Department, enlisted men may
now be furloughed to approved institutions for the purpose of
engaging in instruction in chemistry. Upon recommendation
by the Director of Chemical Warfare Service, through the Re-
lations Section, the War Department's Committee on Ed-
ucation and Special Training will administer such furloughs.
The new ruling provides that other enlisted men qualified to
carry on the work of instruction in chemistry may be sent to
approved institutions when these institutions are unable to
secure the return of former instructors already in military
service, or unable to fill vacancies in the teaching staffs from the
ordinary sources of supply. This provision will do much to
assist those institutions whose instructional staffs were very
nearly depleted by the demands for chemists during the early
stages of the war.
The organization of the Chemical Warfare Service has now
progressed to such a stage that assignment of chemists to the
various Bureaus of the War Department may be made without
serious inconvenience to the sources from which these chemists
have been drawn. Industries essential to the prosecution of the
war have already been protected by the return on furlough of
chemists previously employed by them. The provision for the
return of a sufficient number of teachers insures sufficient in-
struction to provide the steady stream of chemical recruits
necessary for war production and research.
PRESIDENT, AMERICAN CHEMICAL SOCIETY
No one realizes more than I do the need of chemists and engi-
neers at the present time, or the anxiety which we all feel as to
filling up the ranks for after-war conditions. The only way to
provide reserves for the army you have in view is to educate men
for the job, and this takes a long time in each case. Our educa-
tional institutions have been sadly drawn upon as regards the
teaching staffs, and I very much fear that our future output of
chemists and engineers will not only be smaller in number than
is needed, but in many cases will not be properly fitted for the
tremendous work they will have to undertake. I sincerely trust
that some means will be devised to keep our educational in-
stitutions going to the fullest extent, as without large successes
in this direction I fear we will find ourselves by and by with a
smaller army and no reserves at all. — Wm. H. Nichols, Presi-
dent, American Chemical Society, New York City.
UNIVERSITY EXECUTIVES
You have put your finger on something that is troubling us
very much here at Columbia. I am sending your editorial to
Dean Pegram in order that he may study and discuss it with
some of our colleagues. — -Nicholas Murray Butler, President,
Columbia University, New York City.
The universities are certainly in a very serious condition in
regard to instruction in chemistry. So many of our instructors
have been taken off into war work that we have barely enough
to go on, and some institutions must be wholly unable to
carry on their instruction. The difficulty is not money but
men. Your article will do good. — A. Lawrence Lowell,
President, Harvard University, Cambridge, Mass.
686
I ill: JOl l-:\ II OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. Xo. 9
I have read with interest your article on "An Army without
Reserves," with its interesting application to the study of
chemistry, and sympathize most heartily with your line of
thought. Of course it is hard to know how to apply it in each
individual case, but of the- general importance of what you say
in be no doubt whatever. Arthur T. Hadley, Presi-
dent, Yale University, New Haven, Conn.
I have read your editorial with care and interest as it discusses
directly the problem that institutions of this kind are facing in
connection with their departments of pure and applied
The problem, as you say, is a difficult one and I know th.it the
authorities at Washington are giving it careful consideration. —
Dexter S. Kimball, Acting President, Cornell University,
Ithaca, N. Y.
We are very much obliged to you for writing the editorial
in behalf of chemistry in the universities. I wish you would
send me a number of the reprints of this article. I shall be very-
much obliged to you indeed and shall use them where they will
help the cause. — Charles W. Dabney, President, University of
Cincinnati, Cincinnati. Ohio.
Your recent editorial is a strong and timely presentation of
the facts of a situation which is fortunately rapidly becoming
better recognized. The first great rush to gather, equip and train
from the most available portion of our population an army
of fighting men has now settled down to steady and effective
procedure. The next step is obviously to look a year or two into
the future and plan to continue the support of the great army in
France, and to overtake and pass our enemy in all measures of
military effectiveness, which at the present time means largely
to beat the Germans in the production and utilization of those
materials and military appliances for the manufacture and
operation of which trained technical men are necessary. There-
fore the training of these men must continue.
It appears that the only effective way in which the resources
and organizations represented by our colleges and universities
can be kept in operation to produce a reserve of trained men is
by enlisting students in colleges and technical schools who are
studying subjects essential to the conduct of the war in a reserve
organization which shall be fully recognized as a part of our
army. Young men of intelligence and vigor are not going to
attend our universities in large numbers in any work that is not
definitely taken over by the War or the Navy Department as
part of their program. Consequently it is most gratifying to
all those concerned with this problem to learn, since the ap-
pearance of your editorial, that through the efforts of the War
Department Committee on Education and Special Training
provision is almost certain to be made at once for an enlisted
reserve of scientific and technical students and for retaining in
the universities the necessary instructors of these men.
The next step which I hope and believe the War Department
Committee on Education and Special Training will, conjointly
with such valuable agencies as your Journal and other general
and technical publications, soon take is to give wide publicity
to the exact facts as to the number of students there will In-
graduated from scientific and technical schools next year and
as to the demand for graduates at the present time and the
prospective demand as the war proceeds by the Army, the Navy,
the Shipping Board, and the civilian concerns.
If the action of the War Department succeeds in filling our
■institutions this Fall it may be necessary still to call upon the
War Department for help in returning instructors to the in-
stitutions if there are any that can be spared from their present
posts. As to the financial support of the universities at this
lime, it appears to be difficult to do very much in the way of
getting contributions until the new Federal Tax Law shall have
been enacted and corporations and individuals shall have learned
where they statu! under the law. After that it should be possible
to count on continued support for our educational institutions
whose value and effectiveness were never so evident as now. —
George H Pegram, Dean. Columbia University, New York
v itj
PROFESSORS OB CHEMISTRY
There can be no question but that the training of chemists
in our universities for positions with the Government or with the
chemical manufacturers is at the present time one of our most
important "wai indu:
***I understand that a plan is now being worked out in Wash-
ington under which adequate NtulYs of instruction in the various
universities will be ensured for the four branches above men
1 ioned [physicians, engineers, physicists and chemists] and
students of good standing in these tour branches will be per-
mitted to continue their university work until the completion
ourses I. M. Dennis. Cornell University, Ithaca, N Y
I have read with interest your editorial which I am heartily
in accord with and congratulate you on writing.
If you have them vet left for distribution, I would like to
have 25 or 30 copies, as I wish to place them in the hands of some
people who have influence and have to do with educational
matters -C. S. Williamson, Jr., Tulanc University, New
' Weans, La.
Your editorial discloses a condition which thoughtful men
have been facing for some time with serious apprehension. It
must be met and the solution found without delay. Otherwise
the injury and loss will be hard to repair. — Francis P. Yenable.
University of North Carolina, Chapel Hill, N. C.
From the reports which have come to my attention, the situa-
tion with regard to instructors in chemistry in many of our col-
leges and universities is almost desperate. I sincerely hope
that the War Department, especially, may come to a realiza-
tion of the need and may authorize the return of some of the
enlisted chemists to.our colleges and universities as assistants
and instructors. In any case, I hope that no further calls for
men of this class will be made upon the depleted chemical staffs
of the institutions of the country. At best, there is a very
great temptation for the young chemists of the country to get
into some form of active service for the prosecution of the war
Some of us believe that an equally important service may now
be rendered in giving instruction to the young men and women
who remain in the universities. Such service may seem rather
tame and unattractive in these stirring times, but it is never-
theless of vital importance for the future. — W. A. Xoves. Uni-
versity of Illinois, Urbana, 111.
It should be of some service to have the seriousness of the
situation so forcibly pointed out. Being myself a university
teacher, I am especially concerned with university conditions.
I am much pleased with some of the suggestions that you
make and hope they may bear fruit. I have seen my own staff
depleted until I have left one assistant professor and two of the
younger instructors. I have been trying in vain all summer to
fill four important positions; so far I have only "prospects."
I think your suggestions in regard to detailing enlisted men
back to the university, is a valuable one, and as far as I can see
this is the only way in which the situation can be handled
Many of the men are leaving because they feel there is some
reflection on their zeal if they remain in university work. Until
university work is given some recognition by the War Depart-
ment, this situation will continue. I, myself, have had a strong
feeling that I ought to be getting into active war work; at the
same time my good judgment tells me the importance of keep-
ing up the supply of trained chemists. Your article has helped
reassure me in this. — Fred W. Upson. University of Nebraska,
Lincoln, Neb.
I have for some time been considering the advisability of
doing an unprecedented thing as a public duty, in view of the
unusual conditions as to our scientific reserve; that is, the
making of an appeal to my most promising students of last year
to continue their scientific work in college the coming year
A little consideration showed that any such appeal should be
enforced by authoritative and official statements as to the need
of the houi and the immediate future. Such statements would
be hud to get or put iii adequate and manifold form.
Two days ago your editorial "An Army without Reserves
reached me. It gave me an idea which I shall dare to place
before you for what it may be worth.
You are the one man in the best strategic position to help us in
the colleges and universities, the sources of the supply. It
seems to me the way is open for you to do a hugely important
thing by taking the leadership in making a wide appeal to the
students themselves
Secretary Baker is much interested in the "scientific reserve."
So is Professoi Bogert. If you could work over that editorial
so as to make it specific for the purpose, the three of you and
perhaps others of great prominence sign it, and rush it in quantity
to tlie colleges and universities in tune for use before the be-
ginning of the academic year I have no doubt that it would
have .1 very great effect.
1 if course you might prefer to start anew, without 1
this editorial, making a statement of the need, and an appeal
to the colleges and universities, students, industries, as mav
seem best
Sept., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
687
If you and the other gentlemen such as I have named are
willing to certify the need, you will strengthen the hands of us
in the colleges in several ways. The need of explanations and
arguments addressed by us to faculties, registrars, students,
would be almost obviated. I, for instance, with such a docu-
ment in hand could with confidence appeal to men of means to
help promising students who are over-burdened by work for
support, and can find little time for laboratory work or money
to pay for the extra expense. It would remove the possibility
of any charge of special pleading. — W. S. Hendrixson, Grinnell
College, Grinnell, Iowa.
Your editorial deals excellently with a number of considerations
which have given me great concern. The need of chemists in
the future is so great that it can hardly be exaggerated; and I
feel very strongly that not only must our all too few chemists
be conserved, but also that young men of chemical promise must
be favored in every possible way, in order to complete their
training. We all agree that every conceivable effort must be
made to win the war and complete the victory of our just cause
— -but it would be indeed short-sighted to put out of the run-
ning our young prospective chemists, upon whom so much
must depend in the future, by assigning to them tasks, however
important, which could be undertaken by others.
If the new draft proposition to lower the age limit (obviously
needed in the present crucial emergency) goes into effect without
any provision for continuing the education of young men who
desire to be chemists, clearly our universities and colleges will
be entirely depleted of able-bodied young chemical students.
The provision for a Chemical Engineer Reserve Corps, excellent
as it is, does not seem to be elastic enough to cover all types of
necessary chemists. If we do not take care, there will be no
more chemists just at a time when chemists are needed more
than ever before in the history of the country. Therefore it
seems to me highly necessary that some provision should be
made for assigning able boys interested in chemistry back to
their universities, after their enrollment in the Army, to con-
tinue their academic work in approved and appropriate studies.
This they should do with the utmost seriousness, realizing
that in this way they are serving their country and civilization
fully as much as if they were in the firing line.
It is because of this conviction that I have continued my
service to the University in spite of intense longing, at times,
to do something more obviously (but perhaps less really) con-
tributing toward our cause. — T. W. Richards, Harvard Uni-
versity, Cambridge, Mass.
I would like to call your attention to two sources of help
in the university teaching situation. The first is the high
school teacher.
Most colleges and universities are located in or near large
cities. Most teachers of chemistry in the high schools of large
cities have taken special courses in the subject; many have one
or more graduate degrees; many are members of the A. C. S.
These teachers have stayed in the high school field preferring
its independence and larger salary.
In these high school teachers, the university and college
can find a corps of enthusiastic men and women, trained in
leaching as well as in chemistry, anxious to do intensive work,
with more or less experience on the executive side as well. They
would be glad to give their free time to the university if programs
can be adjusted. They could take night classes, Saturday
classes, afternoon classes satisfactorily. They should find it
easy to change to a lecture system.
The teacher of chemistry in a city high school knows industrial
chemistry at first hand as well as from a book; he has studied
food chemistry in the school of home experience as well as in the
laboratory. Such teaching can be drafted for the period of the
war, permitting the return of regular instructors after the
Government is through with them. Not least important in this
connection would be the growth in understanding and apprecia-
tion between teachers of college-preparatory chemistry and
directors of university work.
My other suggestion takes in the men who graduated from
schools of chemistry in the "lean years," men who went into
other lines of business, who if residing near their Alma
Mater might 1«- induced to give part time. I should think the
lists of alumni might be worth looking over. — Jessie C.\ri.i\,
West High School, Minneapolis, Minn.
My stafT of eight was cut in two and I have had a very difficult
time indeed to fill the vacancies, in fact, I was 011 the point of
taking women until by good chance I secured enough men to
bring my numbers to normal. It is very certain that if further
ire made upon the staff, it will be practically impossible
at this late day to till their places, and unless we receive aid
from the Government in the shape of returning to us men whom
they have taken, our work will be very seriously crippled.
Naturally, those men who would be returned to us would come
in uniform and serve as detailed men.
It may interest you if I tell you of a small matter that happened
of late and which illustrates the odd way in which some people
look at the matter covered by the editorial. A number of recent
recruits chanced to be in Troy of late and during their progress
around the city were driven through our campus. There they
noticed a number of our students and inquired who they were.
They were told, whereupon they expressed surprise that such
men were not training for the firing line. Upon being informed
that they were getting ready for work behind the lines, of chemical
character, they expressed strong disapproval and requested that
they be driven elsewhere as they didn't care to see any more of
them. In discussing the matter, I had an opportunity to dwell
upon the fact that when our enemies first developed a gas attack
it would have been pretty disastrous if those on our side who
were opposed to them had consisted only of such men as are
technically known as soldiers. Fortunately for us and our
Allies there were available trained chemists who knew what to
do to meet the unexpected procedure of the Germans, and it
was not difficult to persuade those to whom I was speaking that
matters would go pretty seriously for us if specialists, trained
technical men, were not behind the lines ready for emergency
calls. — W. P. Mason, Rensselaer Polytechnic Institute, Troy,
N. Y.
Referring to your timely and interesting editorial, the sug-
gestions therein outlined deserve the thoughtful consideration
of every one of the 15,000 that make up our chemical army.
What is needed mostly to-day to arouse intelligent public
interest in chemistry is a well directed chemical propaganda
that will reach the man in the street as well as the man at the
directors' table. We need more enthusiasts who can interpret
chemistry to the public.
With few exceptions, the backbone of chemical education to-
day is the State University. Unfortunately, its fate is too often
left to legislators of the Siwash breed or the Tammany type.
However, even these worthies may be educated and shown the
light. Granted this, needful appropriations will follow; and
where there are sufficient funds, the right men can always be
found.
Equal in importance to focussing the attention of legislators
on the training places of chemists should come the reminding
of certain corporations of their great debt to these institutions.
There are scores of corporations that can and will follow the
£ne example of the du Pont Company. They will do so not
only out of gratitude for past benefits, but also because their
business foresight will tell them that their future must be pro-
tected.
A general and persistent propaganda, then, should implant
the chemical germ in many hopeful young men, and if a certain
portion of this propaganda could be concentrated upon legislators
and corporations alike, the future would take care of itself,
and the country could be assured of an oncoming and unfailing
supply of chemical reserves. — W. A. WhiTaker, University
of Kansas, Lawrence, Kansas.
I note with gratification your plans for a symposium upon this
vital matter. Naturally, I was most deeply interested in your
comprehensive analysis of the university conditions.
Like many others, I have been confronted with the difficult
task of enlisting and reorganizing a chemistry faculty and have
been successful in filling four out of five important vacancies
with teachers not now subject to draft but who have been drawn
from other universities where their services were also greatly
needed. Truly, something must be done to re-establish the
depleted ranks of the teachers.
It is reported that some of tin- chemists now engaged in
governmental research work are primarily teachers whose past
records do not indicate that they are altogether qualified to
pursue original investigations. Furthermore, mam able
teachers are engaged continuously in governmental routine
laboratory work of such character that it could and should be
delegated to men of undergraduate calibre. I note these re ts
with no intention whatevei of disparagement, but. if they are
correct, it seems to many of us whose faculties have been utlduly
depleted thai men who have already established themselves a
able teachers of chemistry 111 the universities, would undoubted!}
be of greater service to the Government if they could lie offil iaflj
returned to their positions and vocation as teachers
There is another condition connected with the maintenance
of chemistry departments and their courses deserving note,
namely, the indispensable services of clerical help versed in
THE JOURNAL OF INDUSTRIAL AND EXGIXEERIXG CHEMISTRY Vol. 10. No. 9
chemical terminology, chemical stock -keepers, and lecture
assistants. For instance, a lecture assistant, a specialist in the
assembling of lecture experiments, will shortly be removed by the
draft. There are many such men in our universities. They
are not classed as indispensable teachers but their services are
just as indispensable and important as the teachers themselves
Will it be possible to conserve men of this description, as well
as teachers, through the selective draft system, or otherwise? —
H. S. Fry, University of Cincinnati, Cincinnati, Ohio.
Let me use this opportunity to express to you how thoroughly
I agree with you in your plea for the protection of our chemist
reserves. In spite of our efforts of some months with the War
Department, no progress has been made in securing protection
for the students studying chemistry in our universities and
colleges that have no engineering department proper. I under-
stand that the problem is being considered with a larger problem
of utilizing all university men, but it should be consistently and
intelligently pushed the way you are doing it. I should be very
glad to be of assistance in the effort if you see any possibility of
making more rapid progress toward the goal. From the outset
I have foreseen that we should have an extraordinarily severe
shortage of chemists by this autumn, unless we could keep up
the supply from our universities and colleges. With this in
mind, we at Chicago have kept up our full teaching staff, having
lost only one assistant professor and one instructor of draft age.
We have felt that we were doing war service in preparing for
the demand for chemists exactly as others in preparing munitions
and other supplies. It will interest you to know that at our
request the faculty has given us a free hand in regard to the
amount of chemistry which we may require of undergraduate
students, and we intend concentrating their work to such an
extent that in their fourth year they will receive some research
training and will be able to replace men who in normal times
would have had at least two years of graduate training. It is
our plan to include in their work only courses in mathematics,
physics, and English, and such optional courses as demand
chemistry as a prerequisite and which are in fact forms of ap-
plied chemistry- — Julius Stieglitz, University of Chicago,
Chicago, 111.
I find myself in hearty sympathy with your editorial. Its
timeliness is emphasized by the contents of nearly every mail
which comes to my office. There are no young men of ability
with chemical training available to fill positions. The salaries
which are offered to inexperienced men are beyond the dreams
of avarice of a few years ago, and they till their own story.
They also point clearly to increasing perplexities in the future,
unless the problem of training chemists and chemical engineers
is squarely met. Thoroughness must not be sacrificed, but
specialization should be. Courses and subjects of instruction
must be overhauled with courage and a forgetfulness of tradi-
tions. Many so-called "expedients" will be found to be actually
better than the subjects or methods which they replace. It is
often a surprise (not always agreeable; to find how much can
be left out without harm.
All that you say of the difficulties encountered by administra-
tive officers in retaining, to say nothing of securing, instructors
is abundantly true. Even if fairly convinced, in some cases,
that an individual is not the man best qualified for a particular
national service, the administrator must give the instructor the
benefit of the doubt. It seems probable that the time may come
when it will be wise for those connected with the Government to
examine courageously the list of college men in service and return
to college work some who are not needed in the positions they
are occupying because of their specific knowledge or ability.
Some missionary work needs to be done among the freshmen
and sophomores, and especially with their parents, to bring
home the fact that there is a very real need of curbing the natural
tendencies of the youth of eighteen to turn to what he con-
ceives to be the more immediate and certainly the more spectac-
ular forms of service. The better and more virile the lad, the
greater is this tendency. Something needs to be said to them
from sources outside the institutions, to let them know that
there is a very real duty toward the Nation, not for the duration
of the war alone, but for many days after, to persist in the train-
ing for the chemical contests ahead. — H. P. Talbot, Massa-
chusetts Institute of Technology, Cambridge, Mass.
Your editorial calls attention to a matter of very serious im-
port which has doubtless been in the minds of many thoughtful
men for some time.
The chemical situation will be a serious one throughout the
period of the war and, it seems to me, even more serious for
American chemical industry under post-war conditions. To
establish on a permanent basis the vast chemical enterprises
begun during the present emergency will mean that the waste-
ful methods of the past and present must give place to the most
highly developed scientific methods and will require the services
of a very large number of highly trained chemists.
Have we the requisite number of such men5 Are our uni-
versities and technical schools giving the kind of training which
best fits their students for work in the industries? Do the
industries themselves understand fully the kind of training
their chemists should have had in order to be of the highest
value?
These and similar questions are of vital importance at the
present time and I am writing to suggest that steps be taken to
bring about a genera! discussion of the whole subject of the
training and work of the industrial chemist. Is it too late to
arrange for such a discussion at the Cleveland meeting in Septem-
ber? If so, could not the Journal of Industrial and Engi-
neering Chemistry conduct such a symposium as that held by
the Faraday Society about a year ago' An interchange of views
between chemical manufacturers, works managers, industrial
chemists and university professors, under the auspices of the
American Chemical Society or your Journal, it seems to me
would be of very great value at the present time. — B. F. Love-
lace, Johns Hopkins University, Baltimore, Md.
The conditions here at the Worcester Polytechnic Institute
are even more serious than they were in the spring when I
wrote a letter to the Chairman of the National Research Council
urging that immediate action be taken to relieve the situation.
This letter was dated April 17 and was as follows:
"The situation as regards instruction in chemistry in uni-
versities and technical schools is rapidly becoming serious.
The restricted financial resources of educational institutions
in general prevent any increase in the salaries paid to educa-
tors so that with the rapidly increasing cost of living many
of them are being tempted away into the industries where at
the present time there is such a great demand. Numerous
others are volunteering their services to the Government in
various capacities. Ordinarily the places of these older men
would be filled more or less satisfactorily by younger men.
Unfortunately, however, the same causes are at work with them,
but to an even more intensified degree and in addition they are
of draft age. The result is that at the present time there are
almost no. young men entering the graduate schools in chemis-
try and none available for teaching the subject. From our
own department we are losing one full professor, one instruc-
tor, and an assistant, and I am unable to find anyone to take
their places. We have in our institution between fifty and sixty
young men in process of training as future chemists. It seems
to me that something should be done immediately by such organ-
izations as the National Research Council to counteract this
crisis. For example, it would materially help the situation if
all young men desiring to enter the profession of teaching chem-
istry and having the necessary qualifications were given de-
ferred classification. Possibly your Council is now acting on
this question or has already done so."
This was answered by John C. Merriam, who expressed his
gratification at receiving such statements, as the Council was
busy in assembling data regarding the exact situation and hoped
to be useful in working out the proper balance of instruction and
research for educational institutions.
Personally I think this war will be won as quickly, as surely,
and as permanently if we give some time and thought to de-
vising means for keeping our educational institutions running
as nearly as possible along normal lines.
Upon the declaration of war by this country, what do we
find — a universal, and it seems to me somewhat hysterical,
haste to give up scientific research and study and devote this
time and energy to warfare work. This impulse was highly
commendatory' and important results have been achieved.
Necessarily, however, there has been a great deal of wasted
effort and my appeal is to return a part at least of this energy
to normal scientific investigation.
The situation is well stated by Alexander Findlay in the preface
of a recent publication entitled, "The Treasures of Coal Tar,"
in which he calls attention to a quotation of a prominent German
industrial chemist to the effect that "England talks now not
only of holding her own in war, but beating us in our chemical
industries. She cannot do it, because the nation is incapable
of the moral effort to take up an industry like that — which im-
plies study, which implies concentration, which implies patience,
which implies fixing one's eye on the distant consequences and
not considering merely the momentary profit." Commenting
on this, Findlay says, "That is a challenge which this country
cannot refuse to take up, but in taking it up, let us realize that
Sept., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
689
success can be achieved only by a more general appreciation of
science, by the cultivation and encouragement of. chemical re-
search in an enormously higher degree than in the past, and by
the continual cooperation between science and technology.
And it is important, also, to realize that it is not merely science
in its immediate applications to industry that we must culti-
vate and encourage, but also, and more especially, pure science
or experimental research motivated solely by the desire to in-
crease knowledge. The acquisition of knowledge must pre-
cede its application; chemical invention must follow chemical
discovery. All the great discoveries, all the great advances
have been made, not as a result of effort to achieve results of
immediate industrial importance, but as the result of a patient
and persevering pursuit of knowledge."
It strikes me the general public and its representatives in
the Government do not appreciate these facts and even many
of our educators in the higher institutions of learning have
temporarily lost sight of them. What is it that is emptying
our colleges and technical schools? The answer, as given by
the student himself, finds a partial explanation in the resentment
which he feels to some conditions existing in many colleges.
He remarks the great number of college presidents, deans of
colleges, and faculty members who have sought greater emolu-
ment in war service, forsaking the class-room and students.
He believes that the consequent change in faculty members
leads to demoralization of standards, interest, and results, and
a general lowering of scholarship. He will have to be convinced
of a more sincere altruism on the part of educators at Washing-
ton and elsewhere before he will cease enlisting for immediate
active service.
I think this student viewpoint, be it conscious or unconscious,
should be given thoughtful consideration for it depicts the
situation in all the educational institutions with which I am
familiar.
I feel that to save the situation the Government should make
it obligatory on all students, who have the necessary qualifica-
tions, to stay in their respective institutions until their educa-
tion is completed; that measures should be provided to retain
and keep up an ample supply of trained instructors; and, further-
more, provision should be made that will prevent our graduate
schools from atrophy and keep the torch of research alight. —
Walter Louis Jennings, Worcester Polytechnic Institute, Wor-
cester, Mass.
All who teach chemistry throughout the United States are
viewing with alarm the decimation in the ranks of chemistry
teachers and chemistry students which the war has entailed.
This disorganization is going to be more disastrous than it ap-
pears even now. It is well known among the profession that the
men who have just an elementary training in chemistry are
really of minor importance in the industrial world to-day; it
is the men of extensive training and of research ability who are
needed, and who alone can aid and enable our country to do
the high type of industrial work which our modern civiliza-
tion requires. Yet it is particularly the advanced work, even
down into the senior class of the undergraduate college, which
has been disturbed, and in many schools entirely done away
with. Here at the University of Texas we will have two grad-
uate students who have just received their B.A. degree, and
four seniors, where we have had about ten or more graduates
and about fifteen seniors. There is considerable likelihood
that we will lose some of these and, with the new draft age, we
will lose all of these and all of our junior class even. If the war
lasts until January 1, 1920, there will be not only a lack of chem-
ists, due to the absence of advanced students during a period
of three years, but at least four more years will be required for
the students in colleges, who have had only sophomore work,
to be trained sufficiently extensively to do a high quality of
chemical work. Thus a period of seven years will have passed
in which no chemists will have been trained.
If the war should last longer, the present shortage of chemists
will make itself felt even in the conduct of the war.
The seriousness of the situation would be recognized much
more readily if the term 'chemist" were defined somewhat. In
the recent enrolling of the soldiers who had had chemical train-
ing, men who have had only high school training were enrolled
even, and it is likely that, in many instances where so-called
chemists were detailed by the Government to do certain work,
and where firms have tried to secure chemists, men were put in
charge of work which they were wholly unable to do; but, since
mistakes are often covered up as much as possible, the shortage
of competent chemists — that is, of men with sufficient training-
has really not become apparent at present; yet the future is
sure to reveal it.
The draft provisions are not the only causes which are af-
fecting the training of the reserves for our chemical army. Many
of the brainiest men in the teaching profession, impelled by
patriotic motives, have left the colleges to serve the country in
positions in which they were more greatly needed than in teach-
ing. The industrial world has suddenly recognized its great
need for men possessed of the highest type of scientific train-
ing, and by dint of offering large salaries, has drawn many of
the brightest minds out of the teaching profession. While
many good men remain at the post of teaching, yet it must
be admitted that, on the whole, the teaching staffs are de-
cidedly weakened and will be still further weakened by men
leaving the teaching profession to go into governmental or in-
dustrial work, as long as the present great need for chemists
continues. If we are to train a reserve army of chemists, we
must make an effort to retain faculties capable of doing the teach-
ing of, not merely elementary work, but particularly the ad-
vanced work. It should be represented to members of facul-
ties that they can do no more patriotic work than to strive to
do effective teaching, and that they should carry on and stimu-
late work in the advanced courses particularly, even though
the number of students in these courses may be only a small
fraction of those present under normal conditions. Further-
more, presidents and governing boards of colleges should be
urged to meet the high offers of industries by making liberal
increase in salaries to competent men and by urging them to
stay and carry on the work.
I would suggest that your symposium of expressions on the
subject, as well as your original editorial, be printed in a separate
leaflet and sent to the presidents and governing boards as well
as teachers of chemistry throughout the United States. —
E. P. Schoch, University of Texas, Austin, Texas.
Having the responsibility of providing a teaching staff for
chemistry in the University of Pittsburgh, I fully appreciate the
significance of your article. Five of the twelve regular members
of our chemistry staff are at present in the service. A number
of these would have remained at the University had it not
been that they felt they would be called by the draft and could
better serve the country by enlisting in the chemical service.
At the time when our teaching staff was being depleted I wrote
to various officials in Washington and suggested that our men
be drafted in the regular fashion and detailed to instructional
service in the University. This was during the early period
of the war and the request met with no sympathetic response.
I am at present trying to secure three men for assistant pro-
fessorships and one for an instructorship. While I may meet
with success, I am afraid that the salaries offered by our in-
stitution will not be a sufficient inducement, though these are
already far in excess of offers that we have made in past years.
The University suffers from a reduction of available funds
through the loss of a large number of students in the draft. It
is necessary to pay good men from $3,000 to $5,000 per annum,
and I believe it would be wise for the Government to subsidize
this work in universities. Furthermore, I believe it would
be well for the Government to detail men to instructional service,
if necessary placing the chemistry students of our colleges and
universities under the chemical warfare division of the War
Department.
Uncle Sam already has several thousand draftees in the in-
stitutions of higher learning in this district. Why would it not
be appropriate to commission members of a teaching staff
and have them do the regular work in the chemistry de-
partment together with some of the instructional work neces-
sary for the training of the draftees? We have very few students
doing graduate work. It is the graduate student who will have
to look after research problems in Government departments,
industrial plants, and universities after the war. This branch
of the "reserves" will determine our supremacy in the field of
chemistry during the reconstruction period.
As chairman of the Employment Committee, Pittsburgh
Section, American Chemical Society, I realize perhaps more than
any other man in the district what the demand for chemists
really is. I feel certain that there are not less than fifty open-
ings in our own region which cannot be filled by competent
men. Undergraduates are leaving us and going into industrial
laboratories where they arc entitled to industrial exemption.
Such students should be told that they are to remain in educa-
tional institutions and strive for records sufficiently high to
entitle them to deferred enlistment in the Chemical Warfare
Service.
We have already utilized our laboratories to the greatest
possible extent, running sections every morning and every
afternoon. Our universities need greater facilities and I cannot
690
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 0
conceive a better plan than that of sending an official letter
from the American Chemical Society to manufacturers in various
districts, urging them to endow new laboratories and research
funds in the institutions in their district.
I enclose a copy of a letter ( not reprinted) which is being
sent to every chemist in the Pittsburgh district and to all
chemistry alumni of the University of Pittsburgh. This will
show you what we are doing to help build up the chemical
reserves. — Alexander Silverman, University of Pittsburgh,
Pittsburgh, Pa.
I note your reference to the editorial which appeared in the
July issue of the Industrial Journal. Any professional
man who is interested in chemistry would have been stimulated
by that article. I am now taking the opportunity to express
certain views which appear to me very important and give you
liberty to reconstruct them in a manner that is suitable to you
in order to bring before the public the necessary information.
I think it well to remember that, no matter what view may
be held as to the real value of our universities as a national asset,
the young men who are graduates of these institutions are to-
day the rulers of our country, its diplomats, its ju< i
governors, lawyers, professors, scientists, and leaders in almost
every branch of human thought and endeavor. There is no
subject, therefore, in these serious times which deserves more
immediate and earnest consideration than that of the main-
tenance and reconstruction of these institutions to meet the
conditions that prevail at the present time.
. The world has finally awakened to a realization of the real
value of the fundamental sciences and it is the duty of our
educational forces to see to it that our own nation takes full
advantage of opportunities which are unique in the history
of the world. What we need to-day, as never before, in order
to take a prominent lead in the period of reconstruction are
college trained men who have been taught to think for them-
selves. Such men are a valuable asset and it is our duty as
university teachers to see to it that greater emphasis is laid
upon educational methods which will lead to the greater pro-
duction of this type of recruits or reserves.
Never before in the history of our country has the important
and real value of the chemist been so appreciated as at the
present time. The war has created an excessive demand for
men of this profession and if we are to triumph successfully
in the carrying out of principles to which we have dedicated
ourselves, we shall need to organize immediately an educational
program which will provide not only for the present, but also
give serious consideration to the matter of specialized training
in the natural sciences for the future. Under any circumstances
the constructing of reserves from our raw material will be a slow
and difficult process.
In the first place only about 2 per cent of our American youths
of eighteen desire to go to college and, secondly, it takes time and
patience to produce the right kind of finished product. Espe-
cially is this true with respect to the training of chemists. While
the American youth is naturally resourceful, and has courage and
intelligence of a high order, it does require special effort of
enthusiastic and experienced teachers to develop in him that
initiative that is absolutely essential before he, as a chemist, will
ever make a success of his profession.
After this war is over and the reconstruction period commences,
our industries will need technical assistance as never before and
will lie dependent to a large degree upon the product of our
schools of chemistry and chemical engineering. Not only-
will attention be directed by manufacturers and capitalists to old
industries which were successful before the war, but also to the
establishing of new ones. Many such have already been brought
to notice, including particularly those concerned with the manu-
facture of chemicals, drugs, dyes, metals, cements, etc. In all
these developments well trained chemists will be needed in the
organization of more efficient methods of manufacture and in
designing better equipment for successfully carrying on chemical
operations.
In the majority of gainful occupations success requires con-
tinuous and painstaking application of many years. There is no
profession where this is more true than in that dealing with the
application of chemistry to industrial problems. Therefore,
it is essential that every means Ik- provided whereby men can
lie kept in training to meet the exacting demands which neces-
sarily will be made Upon them in the future. Him are We to
provide these reserves and give the necessary instruction if we
are not permitted to operate and continue with what we already
have It would be a sad mistake to curtail at the present time
this educational work, and it is to be hoped that the Government
in its educational policy will in every way provide means
whereby we can retain in our training courses a maximum
number of first-class reserves. — Treat B. Johnson, Sheffield
Scientific School, Xew Haven, Conn.
MELLON INSTITUTE
Your editorial expresses exactly my views and experience as
! nrector of the Mellon Institute of Industrial Research
and Dean of the School of Chemistry of the University of Pitts-
burgh.
This terrible war has demonstrated that there exists for each
large nation a certain number of vital industries which it cannot
neglect without exposing itself to the danger of some day being
at the mercy of its enemies. The nature of the problem changes.
Scientific and technical instruction becomes necessary and this
should be taken up by the universities of the country. Also life
becomes more and more difficult even for the most prosperous
nations such as ours, and the problem becomes singularly com-
plicated when it is no longer simply a question of supplying a
national market, largely open, but of entering into commercial
competition from within and from without, with new industries
strongly organized.
It 1 1' comes necessary then to have a large number of Highly
trained specialists to carry out this work, which means searching
out the most rapid and most economical processes, allowing
no loss of anything which represents any value. We can only
hope to obtain this class of men from the universities that have a
strong teaching staff, therefore, it is absolutely essential that the
universities should be provided with the necessary men of ability,
and in most cases they will not be able to compete for this class
with the industries; therefore, they should receive assistance
both from the industries and the Government if the best results
are to be obtained for the future. — E. R. WErDLErN, Acting
Director.
INDUSTRIALISTS
Your article "An Army without Reserves" should be sub-
mitted to the Secretary of War and to anybody who has anything
to do with the draft. I hope that your warning may be heeded
before it is too late. — L. H. Baekeland. Yonkers. N. Y.
I am, of course, in full sympathy with your desire to ensure
that the forces of the country should be used in the most efficient
manner and that we should not be misled by the fetish of num-
bers, putting every possible man in the army to the sacrifice
of the specialists who must supply the support from the rear. —
C. E. K. Mees, Eastman Kodak Co., Rochester, X Y.
I am too busy repairing a fire damage to our plant to write in
detail, but I am with you on the article, and I hope you can
drive it home — E. Mallinckrodt, Jr., Mallinckrodt Chemical
Works, St. Louis, Mo.
The Panama Canal could not have been built in a hundred
years were it not for the men at home building steam shovels,
locomotives, dump cars, enormous dredges, and the other highly
organized machinery necessary to the work. It would have been
only a small job to have made picks, shovels and wheelbarrows
at home, but the job at the Canal would have been so great under
these circumstances that it would have taken many generations
to complete it.
In all modern great undertakings machinery is becoming
more and more a factor, and in the greatest test of power the
world has ever known, now being made in Europe, the capacity
of our plants at home when strained to the limit will be pitted
against the utmost capacity of the corresponding plants of
Germany and Austria, ami the side that wins will give the men
at the Frout the same advantage that the man with machinery
has over the man with more primitive equipment. — Herbert
H. Dow, The Dow Chemical Company, Midland, Mich.
The editorial is most timely and touches on one of the most
vulnerable points in the situation of the chemical developments
in this country.
The chemist is now an inseparable part of the machinery of
war, but as important as his role is during these times it must
be recognized that his services to the welfare of the country
and to the industries cannot be underestimated when peace
is finally established.
The new chemical industries that have developed in the United
States during the last years must be continued as they arc essen-
tial for our economic independence, and to maintain them suc-
cessfully, among other conditions, we must be prepared with an
army of trained chemists.
The importance of chemistry has been so thoroughly recog-
nized that enrollment in the chemical courses at universities
Sept., 191S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
691
and colleges is continually increasing and it needs no particular
encouragement.
A competent staff of teachers is the most essential require-
ment. In consequence of inadequate compensation at the
educational institutions many of the most able teachers have
resigned for more lucrative industrial positions. As you suggest
in the editorial, it is not only essential that teachers of
chemistry be placed in the deferred list or assigned back to
teaching by the Government, but it is also necessary that the
educational institutions receive financial aid in order to make
the position of the teacher more remunerative.
Uninterrupted progress of the chemical training of young men
must be secured and means to this effect must be coordinated
in an efficient system to obtain the substantial benefits which
must accrue to this country in times to come. — George D.
Rosengarten, Philadelphia, Pa.
Your admirable and timely editorial sounds a warning which
should be emphasized in every possible way. We have only to
turn to Canada for an example of what may happen in this
country if this warning is not heeded. After two or three years
of war, the total number of students graduating in chemistry
in the Dominion had fallen to eight for the year.
The situation which you define involves so many difficulties
that its complete solution will make severe demands upon the
cooperative effort of our educators and industrial leaders.
Certain things may be done at once, however, to relieve the
situation and to serve as initial steps toward the upbuilding
of our chemical reserves. Corporations operating in the chemical
industries have a unique opportunity to combine patriotism,
altruism and self-interest by devoting a proportion of their
war profits to the founding of adequately endowed chairs of
chemistry. They can also do much in the factory itself to de-
velop the latent capacities of subordinates on their chemical
staff by the establishment of classes, reading courses and lectures,
and by arranging the work of the factory in a series of graded
jobs through which the younger chemists have opportunity to
pass.
To relieve the situation in the universities, it should be possible
to recall for temporary courses some of our older chemists of
distinction, now retired. Possibly also some of the eminent
teachers of chemistry now almost without pupils in Canada,
could be persuaded to conduct courses for a time in our own
universities and technical schools, which could at the same time
extend their hospitality to Canadian students. I may even be
permitted to suggest without in any way implying criticism,
that some of our Government laboratories, and especially
those devoted to war research, may possibly be over-manned,
and that their working efficiency, whioh must first of all be main-
tained, might not be impaired by assigning a portion of their
staff to teaching. — A. D. Little, Cambridge, Mass.
Your well-timed article covers a subject to which I have
given considerable thought from the manufacturer's standpoint.
There is no question but the present demand for chemical
help in the army has curtailed laboratory forces in all directions.
In some of our laboratories we are training young women to do
the routine work, but that is not going to help us secure many
chemists. We cannot follow out the practice of the past of
securing promising young graduates from our universities and
technical schools because the Government seems to have first
mortgage on almost every one of them, and from present indica-
tions the next crop is going to be very small.
It has occurred to me that with the present scarcity of in-
structors the only sensible thing to do is to shut down as many
of our smaller institutions as possible and combine the forces
of instructors and professors in a few of our larger institutions
and run them to their full capacity. In that way we can use our
professors and instructors to better advantage than by having
them scattered through many small institutions and be able to
give better training to a much larger number of students than
can be done in a multiplicity of smaller institutions with badly
crippled faculties, I believe the matter is of sufficient importance
to have special legislation, if possible, passed by Congress to see
that the training of chemists is not interfered with by the draft, —
it to be understood, however, that the Government has the first
call on the services of chemists trained under these special
conditions.
It certainly seems illogical for the Government to spend
enormous sums in putting up vast chemical plants for the manu-
facture of explosives, poison gases, and other war materials,
without making ample provision for the training of the men
who are needed to manage and control these plants. T'avih
WESSON, The Southern Cotton Oil Co., New York City.
In Buffalo, on June 22, 1917, I started a discussion al thi
annual meeting of the American Institute of Chemical Engineers,
and the Institute sent a long telegram to President Wilson
asking the exemption of chemists, which speaks for itself. I
had in mind that in the Fall of 1914 when we were still obtaining
German journals, I noticed that among the casualties there
were a large number of chemists, and after each name it simply
stated "Hat den Helden-Tod erworben." In other words,
it took one second to kill a man, but it took anywhere from four
to ten years to make a chemist of him, and by January 1915,
Germany withdrew all her scientific men from trench work!
It took England about fifteen months to learn the same lesson,
and even after the first gas attack at Ypres, England still kept
her engineers and chemists in the front line trenches.
Now comes the appalling situation where the chemical in-
structors of the United States are leaving the colleges for Govern-
ment and commercial work, and if this war keeps on, there will
be no embryo chemists, for the students will have no professors.
Something must be done, and done quickly, to alter the state of
affairs.
You cannot expect a professor of chemistry to work for $3000
or $5000 per year when the industrial fields will pay him much
more than that, and there is at least an outlook for the future.
I have in mind the case of one institution in the city of New
York, where the head professor of chemistry has been receiving
about $5000 per year for the last twenty years, and if it were not for
the fact that all his spare moments are put in on commercial
work, he could not succeed in bringing up his family with any-
thing like the station to which they are entitled, and this brings
to my mind the oft mooted question which nobody has ever
answered satisfactorily to me: "Is a college an altruistic in-
stitution, or is it a business institution?" The nearest answer
I ever got to it was given by the president of one of our very
large universities, who said a university was a little of both,
which to my mind is the equivalent to the answer that it is
"neither flesh nor fowl." If a college is an altruistic institution,
then it must not practice its altruism at the expense of under-
paid professors, and if it is a business institution, I should say
it is very badly managed, if the brilliant heads of its depart-
ments must seek outside work in order to make both ends meet.
I know of one man who for the last fifteen years has given very
liberally of his money and his time to at least three institutions
of learning in order to help the department of chemistry, and of
course, if a large number of men did this, it might solve the prob-
lem partially because poor students could do post graduate work
at the expense of successful manufacturers. But that will not
mend the trouble, as I see it. The first thing that ought to be
done is to conduct the chemical departments on a business
basis, and if quite a number of nonessential studies were elimi-
nated, it would give more money to the college so the professors
could receive higher pay. The second thing that would help
the matter, but it would only tide it over temporarily, is
for a number of institutions, instead of establishing fellowships
entirely, to establish them partially, and give to the pro-
fessors who have charge of the fellows a little share of the money,
for after all, no fellow in science could do much without the
guiding hand, and the guiding hand should at least obtain a
part of the subsidy. The third remedy would be in putting a
number of our institutions on a business basis by having some
active business men take a hand in the affairs of the manage-
ment, and provide additional funds.
Something, of course, must be done. A committee from the
American Chemical Society, the Electrochemical Society, The
American Institute of Chemical Engineers and the Chemists' Club
would make an imposing body, whose advice would carry
weight. — -Maximilian Toch, Toch Brothers, New York City.
I doubt if I can add anything to what has been suggested at
least in your editorial. Even if the machinery were intact and
in good working order a difficulty is met with — the raw material.
Raw material must be taken as we find it. Chemists cannot
be manufactured from imperfect material. The qualities which
are necessary are present when the training begins but cannot
be discovered until later, and therefore teachers of judgment
and experience are necessary, for the right material is limited.
I think perhaps that all teachers of draft age should be placed
in the Service, assigned to the various institutions and paid by
tli. Government. No teacher should be encouraged to enter
the army voluntarily unless with the understanding he might be
assigned to educational work at the discretion of the authorities.
Industrial institutions might be encouraged to use educators
as consultants, the privilege being subject to the approval of
the governing school body.
Boys of draft age, majoring in chemistry, should be put in
uniform and should be kept at school as long is their standing
is satisfactory, otherwise they should be put into service ill some
active capacity.
692
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 9
Chemists in industrial occupations, where the vicinity of
educational institutions permitted, should be selected by the
faculties of such institutions for part time educational work,
this being voluntary or paid for as seemed necessary or advisable.
Technical laboratories are not at present used by the Govern-
ment to such extent as is possible for solving problems of a
technical nature, research or inspection. Inspection and other
technical work of the various war departments might be coordi-
nated to a greater extent, thus economizing ability and personnel.
Many chemists, equipped with experience, ability and train-
ing, discretion and loyalty, are anxious to be employed part
time, at least, on Government problems, or to aid the cause in
some way, if they but knew what the problem or other work
was. If this force could be put to work, economy of ability
and personnel would also result. To give time to build up our
reserves, we must relieve the pressure as much as possible by
fully utilizing our present capacity.
Perhaps our colleges and universities have been too heavily
drawn upon, I sometimes think so at least, and the practicing
technologist has not been utilized to the extent of his possibilities.
• It will certainly be a pity if the country finds itself overstocked
by and by with mediocre chemists. It would be better to
have trained fewer men thoroughly.
There are, no doubt, many women available at least as labora-
tory assistants and there is no good reason why girls should
not be educated as chemists as well as boys, though it may not
be fashionable to recognize the fact and to make allowances
uhtil the novelty of their employment wears off. — -Win. Hoskins,
Chicago, 111.
In my estimation it is much harder for a chemist to stay out
of a uniform than to get into a uniform. The man who gets
into a uniform is right away considered a hero who is doing his
part for his country, while the man who does not enter the uni-
form is easily looked upon as a slacker, whereas in reality he is
in many cases doing much more vital work and accomplishes
much more important work, due to the fact that he is not tied
down by military red tape.
My impression is that many college professors, shortly after
we entered the war and when Washington began to realize the
importance of chemistry, were carried away by their patriotic
enthusiasm and with one of the human weaknesses that is so
apparent in everybody — the desire to do something he is not
doing and feeling that he could do more if he were just doing
something else from what he is doing at present. These pro-
fessors, and there are many of them all over the country, dropped
their work suddenly and disappeared in the maelstrom of khaki
clad men. The result is that the chemical faculties have dis-
integrated. In some cases, I have been told, record registration
to the chemical department has taken place, and no teachers
to teach the students — a condition which is hurtful if not fatal
to our future chemical developments; and in many cases there
is immediate need of chemical skill in large chemical industries.
As I can see it, there are two principal ways by which this
lack of teachers at the universities can be overcome.
Many of the college professors, after the first exhilaration
of appearing in khaki uniform has worn off, have found them-
selves, I am sure, mentally circumscribed; and they have had
assigned to them problems which are not congenial to them and
have found conditions of work which are exceedingly unsatis-
factory; and if a general order was issued by the War Depart-
ment, suggesting that professors could be assigned back to their
universities if they so desired, many of these would certainly
avail themselves, I believe, of this opportunity. It would not
take them out of the immediate field of research, which should
continue. They only transfer their activities from the present
location to their universities. A suitable number of assistants
from the Army could be assigned to them and the professors
would turn out better and quicker work, due to the fact
that they were in home and congenial surroundings.
The equipment necessary for the work has to be assembled
in the new laboratories created, while in the university labora-
tories, the equipment may already be in and standing idle.
Consequently the using of same would be the saving of both
time and money.
A professor would be able to guide his students and give
them the instruction necessary, without materially interfering
with the work he is doing for the Government.
Again, the industries hold in their personnel a very strong
factor in the development of the new generations of chemists
which have to be reared. In these days of cooperation and in
these days when we are planning for the time after the war,
there is no doubt in my mind but that men in practical chemical
work would be pleased to cooperate with the universities in
such a way that they would be willing to give a series of lectures
covering the special field of activity they may be interested in.
As an example, men in the sugar industry would be pleased to
give a series of lectures on sugar manufacture, accompanied by
a visit, in some cases, to a sugar refinery. In other cases, an
expert along sulfuric acid lines would be glad to do the same
thing, and so on. The result would be that the students would
obtain a vastly superior industrial chemical instruction than they
could possibly get through their college professors, who in most
cases never have had any practical experience in the operation
of any of these plants
We might not develop in this way the best theoretical chemists
(and they are badly needed, too) but we would at least develop
a chemical embryo which has good, common-sense chemical
knowledge; and from what I learn, the industries are to-day
clamoring for men who have good, common-sense chemical
knowledge that makes it safe to place them out in the operating
departments of the industries.
It was, I believe, a short-sighted policy on the part of the
Government to permit the large number of college professors
to enter the uniform early in the war; and I think the reassign-
ment of men with their chemical problems to work out to their
universities will help us to train a chemical field army which is
absolutely essential if we want to hold our place in the chemical
industries after the war. — John Woods Beckman. Berkeley,
California.
LFFLCT OF THE. WAR ON AME.RICAN CHLMICAL TRADL
By O. P. Hopkins,
Four years of war have wrought tremendous changes
in American foreign trade. Shipments of foodstuffs
and munitions to Europe and increased sales of manu-
factured articles to countries cut off from accustomed
European supplies have raised export totals from
2,330 million dollars in the fiscal year 1914 to 5,928
million dollars in 1918. A most thorough scouring
of the whole world for raw materials, on the other
hand, has increased the value of imports from 1,894
millions in 1914 to 2,946 millions in 1918.
The increase in exports is 154 per cent; in imports,
55 Per l
For imports, 1918 was the peak year, but for ex-
ports the total for last year was 362 millions below
that of 191 7, the loss of Russia's markets and the ration-
ing of European neutrals accounting for the drop.
The changes wrought in America's chemical trade
by the war are quite as astounding as in any other
Washington, D. C.
line. The Allies would have been much harder
pressed much earlier in the war had it not been for
the American chemist. Explosives and explosive
materials have gone over in enormous quantities.
To other markets, lying outside the fighting zone for
the most part, have gone the finer chemical products
that formerly were more frequently imported from
Europe than from America. To other markets also
have gone increasingly great quantities of such allied
products as paper and glass, foreign trade in which
was not well developed by American manufacturers
•re the war started. Some increases in sales of
heavy chemicals are to be noted in districts outside
of Europe, but this trade is limited by the fact that
such districts are not largely industrial.
To give an approximate idea of how the war has
affected trade in the various chemical branches a
summary table has been especially compiled, revealing
Sept., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
6 93
a jump in imports from about half a billion dollars in
the last normal year to somewhat more than a billion
dollars in 1918, and a leap in exports from half a billion
to a billion and a half. The increase in imports is at-
tributable mainly to heavy purchases of rubber, cop-
per, and mineral and vegetable oils, as will be shown
in later tables. The most spectacular gain in ex-
ports is, naturally, in explosives, the increase being
from a mere 6 million to no# less than 379 million
dollars. This class is followed by metals, principally
copper, by oils, principally mineral, and by heavy
chemicals, principally explosive materials. These are
the showy headliners. From the point of view of
future foreign trade, however, some of the less showy
results are quite as interesting, such as the gains in
exports of drugs and medicines, paints, and paper,
which have been achieved in markets formerly domi-
nated by European competitors.
The summary table follows:
Summary of Foreign Trade in Chemicals and Allied Products
Imports Exports
1914 1918 1914 1918
Million Million Million Million
Classes Dollars Dollars Dollars Dollars
Chemicals 61 97 15 129
Drugs, medicines, etc 9 11 11 21
Dyes, dyestuffs, dyewoods 10 9 (a) 17
Explosives 1 8 6 379
Fertilizers 28 5 12 6
Gums, resins, etc 88 227 20 1 1
Metals, ores, earths 132 286 175 327
Oils, fats, waxes 79 200 194 378
Paints, pigments, etc 2 1 7 17
Tanning materials 5 7 1 4
Paper and pulp 30 66 6 30
MisceUaneous products 120 253 44 132
Miscellaneous materials 8 6 2 3
Total 573 1176 493 1454
(a) $400,000.
These are rough groupings, as such groupings are
bound to be, but will serve the present purpose. A
definite idea of the articles included in each group
can be obtained by a study of the detailed tables oc-
curring later in the article. No perfectly satisfac-
tory grouping can be devised. As an illustration, the
official statistics include under fertilizers only such
materials as are used exclusively for fertilizing. Sodium
nitrate, therefore, goes under chemicals, although the
total for fertilizeis is misleading without it. It is
also puzzling to decide what manufactures should be
included as allied chemical products. The foregoing
table includes in the total some lines that might for
one reason or another have been omitted, and ex-
cludes others that might have been considered. The
importance of the item "Miscellaneous products"
is due to the inclusion of sugar.
A clear enough idea of the changes wrought in our
chemical trade by the war can be obtained from the
detailed analyses of each class that follows. The
statistics are compiled from official bulletins issued
by the Bureau of Foreign and Domestic Commerce,
and cover the fiscal years ended June 30, 1914 and
1918; that is, the last normal year before the war
and the fiscal year just closed.
CHEMICALS
Of all the imports under the heading "Chemicals"
the most valuable is nitrate of soda, the only important
source of which is Chile. Purchases of this material
tripled in quantity in 1918 as compared with 19 14,
while the value was quadrupled. It is Chile's most
vital contribution to Allied success. The practical
cessation of imports of chloride of lime is an inter-
esting feature. England formerly supplied about
three-fourths of the total, Germany being the other
important source. Creosote oil also shows a heavy
falling off. It was imported from the same sources
as was the chloride of lime, in about the same propor-
tions. The drop in the receipts of magnesite is ex-
plained by the fact that it came principally from
Austria-Hungary. The falling off of 14 million
pounds in receipts of nonfertilizer potash needs no
comment. A study of the following table will dis-
close further details as to the import trade in chem-
icals:
Imports of Chemicals
1914 1918
Articles Quantity Value Quantity Value
Acids:
Carbolic, lbs 8,392,995$ 532.211 127,574$ 11.198
Carbolic (phenol), lbs 498,264 58.314
Oxalic, lbs 8.507.850 420,409 792,383 327,785
All other 261,106 1,847.691
Ammonia, muriate, lbs... 9,176,729 465,429 1,120.074 103,534
Argols, lbs 29.793,911 3,228.674 30,267,388 5.443,628
Coal tar and pitch, bbls 25,540 47.645
Coal-tar distillates,
N. E. S. (a) 1.126,400 510,941
Creosote oil, gals 60,900,435 3,839.062 3.857.869 329.846
Fusel oil, lbs 5,802.369 910.759 1,606.528 546.589
Lactarene. lbs 10,798,614 705,264 12,133.855 1.765,653
Lime, chloride, lbs 47,423.651 416,740 4.285 184
Lime, citrate, lbs 3,097,265 493,738 4.253.686 879.199
Magnesite, not purified,
lbs 289,494,316 1,473,207 23,499.789 549,727
Potash (not for fertilizers) :
Carbonate of. lbs 20,603,593 614,926 14,468,211 3,166.043
Cyanide of, lbs 808,721 113,199 144,225 48,323
Hydrate of (containing
not more than 15%
of caustic soda), lbs. 8.450,402 326.668 11,732 4,398
Nitrate of, lbs 3,546,580 115.344 8,820.367 955.018
All other salts of 5,775.588 537,592 1,662.153 803,627
Soda:
Cyanide, lbs 84,652 39,405
Nitrate, tons 564.049 17,950,786 1.607.020 70,129.026
All other salts of 487,038 389,384
Sulfur, or brimstone, tons. 19,389 355,450 282 8,677
AJlother(/.) 8.000,000 9.000,000
(a) Not elsewhere specified.
(fr) Includes all other chemicals, drugs, dyes, and medicines than
those mentioned in this article.
Less than half a million dollars' worth of acids
was exported from this country before the war; in
1918 more than 35 million dollars' worth of picric
acid alone was sent abroad. This, of course, is a war
business. The big increase in the sales of soda prep-
arations, as shown in the next table, may, on the
contrary, be attributed to a wide distribution in
markets that formerly were supplied from Europe.
Fine beginnings of a trade in coal-tar products are
indicated in the exports of "Coal-tar products, N. E. S.,"
which includes such products as are "not elsewhere
specified." (Coal-tar dyes will be found under the
section of this article headed "Dyes, dyestuffs, and
dyewoods.") The destination of the copper sulfate in
1918 is not yet available. In 1917 France was the
principal purchaser, while in 1916 Greece and Spain
took the bulk of the shipments. The comparatively
heavy shipments of acetate of lime in 1914 went
chiefly to Germany, Belgium, and the Netherlands.
The export trade in chloride of lime is new, but the
destination will not be known until more detailed
figures are available. Table of exports follows:
694
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. Xo. 9
Articles
Acids:
Carbolic, lbs.
Nitric, lbs....
Picric, lbs. . . .
Sulfuric, lbs. .
All ot her
Alcohol, wood. gals.
op Chemicals
1914 1918
Quantity Value Quantity Valu
(a) (a) 8,688.554 $4,236,288
961,494 101.040
56.193.952 35.357,010
12,131.750 $ 125,892 67,654.722 1,119,907
357,035 5,673,707
1,598,776 652,486 2.538,001 2,070,026
Calcium carbide, lbs 32.845.649 962,040 28,869.686 1,328,437
Coal tar. bhls 22.150 43, 145 53,955 147, 76^
Coal-tar distillates, X. E. S.:
Benzol, lbs 25,400,852 2.152.315
All other 5,620,851
Copper, sulfate, lbs 7.375,775 330.007 15.164,078 1,431,262
Lime, acetate, lbs 68,160,224 1,560,933 15.490.032 797,996
Lime, chloride, lbs 13,060.401 558.066
Potash:
Chlorate, lbs 1,564,662 681,128
All other salts of 961.989
Soda:
Caustic, lbs 134,729,691 8,629,086
Sal soda, lbs 14,076.264 205,489
Silicate, lbs 26,127,870 375,110
Soda ash, lbs 198,902,457 6.074,879
All other salts of 7.421.521
Sulfur, or brimstone, tons 110,022 2.018,724 140,525 3,842,904
Allother(i) 9,000.000 40,000,000
(a) Some items in this table were not given separately in the official
statistics for 1914, as the trade was not then important enough for particu-
larization.
(b) Includes all other chemicals, drugs, dyes, and medicines than those
mentioned in this article.
DRUGS, MEDICINES, PERFUMERIES, ETC.
The most interesting developments in the foreign
trade in lines included under this broad head are the
decreased receipts of licorice root as the result of
Turkey's stand in the war, the increased sale abroad
of American medicinal preparations, the exportation
of more perfumery and cosmetics than was imported,
the development of a foreign business in infants'
food, and the increase in prices. The persistence of
the Chinese demand for ginseng and the willingness
of Americans to meet it in spite of the questionable
exploitation methods a few years back, are interesting
points. The grouping in the following table is arbi-
trary but convenient:
Imports and Exports of Drugs, Medicines, Perfumeries. Etc
1914 1918
Articles Quantity Value Quantity Value
Imports
Arsenic and sulfide of,
lbs 4,432,793 $ 178,388 9,260,768 SS04.889
Cinchona bark and
products:
Barks, cinchona, or
other, from which
quinine may be ex-
tracted, lbs 3.648.868 464.412 3,273.628 810.775
Quinia, sulfate of.
and all alkaloids or
salts of cinchona
bark.oz 2,879.466 624,125 1.445.702 656.945
Iodine, crude or resub-
limed. lbs 195,087 433,498 268,281 580,538
Licorice root, lbs 115,636,1312,047,182 26,982.932 1.853.927
Medicinal preparations 1,031,054 519.338
Opium, 9% or more
morphia, lbs 455.200 1.810,429 157.834 2.443.228
Perfumeries, cosmetics,
etc 2,309,027 3,497,695
Exports
Formaldehyde (o) (a) 866,038
Infants' food (a) 1.908.141
Medicinal and pharma-
ceutical preparations 6.721,978(5) 10.190,188
Petroleum jelly 661,889 1.278,658
Roots, herbs, barks:
Ginseng 224,605 1,832,681
All other 513.071 784. SI 4
Perfunu-i i
etc 1,620,872 3,965,465
Not stated separately in 1914.
(b) Stated as "medicines, patent or proprietary" in 1914.
DYES, DYESTUFFS, AND DYEWOODS
The establishment of an American dye industry
result of shutting off German supplies has re-
ceived more attention in the public prints than any
other development in the chemical industry, and,
making due allowance for the exaggerations of sen-
sational writers, the general impression gained by the
man in the street is not far wrong; namely, that whereas
formerly we depended almost entirely upon Germany
for dyes, now we are supplying our own needs and
exporting more than we formerly imported.
The following table shows that in 1914 we imported
about 10 million dollars' worth of dyes, dyestuffs, and
dyewoods, but also reveals the surprising informa-
tion that in 19 18 imports still amounted to 9 million
dollars. A second glance, however, will show that in-
creased prices account for this puzzling fact. For in-
nearlv three times as much indigo was im-
ported in 1014 as in 1918, yet the total value was
only about a fourth of what it was last year. The
small consignment of dyes recorded as coming from
Germany in 19 18 was probably a batch ordered be-
fore we entered the war and held up through some
technicality or other in some neutral country.
That exports have increased from less than half a
million dollars' worth in 1914 to nearly 17 million dol-
lars' worth in 1918 is the outstanding fact that has
given so much satisfaction to the American public in
general and the chemist in particular. It is the fact
that shows that the industry has delivered.
Thanks to a new feature in the official statistics, the
destination of the dye exports is now ascertainable.
Japan led in imports of our dyes in 1918 with a total
of more than 3 millions, followed by the United King-
dom. India. France, Canada, Brazil, and Italy, in
the order named.
The following table shows details of both imports
and exports, so far as they are available:
Foreign Trade
Dyes, Dyestuffs, and Dyewoods
1914 1918
Articles
Q
uantity
Value
Quantity
Value
Imports
Alizarin and alizarin dve
lbs
633.414 $ I
\ 29.323
$ 130,722
*
184.467
222.728
21 .273
3,250
Indigo, lbs
8
125.211
1 ,093,221.
3,126.497
3.895.114
2.113.912
3.276.557
Synthetic, lbs
1.012,585
618.557
Colors and dyes. N. E- S. . .
7.241.406
2.507,296
5.965.537
3.048
767 , 783
1 ,675.609
United Kingdom.
239.480
Other countries. .
268.606
268,881
Dvewoods. crude state:
Logwood, tons
30.062
378.064
52.027
1 .066,455
AU other, tons
7.663
108,928
951.667
Exports
Aniline dyes
7.298.298
2.339.480
356.919
16.921 .888
To — France
1.630.131
Italy
1.181.951
785.618
2.569.298
1.419.162
Me\ico
381.488
503.092
Brazil
1.281.758
British India
1 .947.668
1 tpan
Other countries
1 \PI 0SI\ I s
Increased exports of explosives are perhaps the
most spectacular feature of our war trade. Sales to
our associates in the war amounted to almost 379
millions in 191S. as contrasted with total foreign sales
of about 6 millions in 1914. The total for 1018 is
the highest since the war started, showing our ability
to pmvide for our own needs without interfering with
supplies to the Allies. It should be borne in mind
Sept., 1918
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
69 =
that shipments to our expeditionary force are not
entered in our official export returns.
Imports of explosives also show a big percentage of
increase, but the total involved is not large. These
imports originate in Canada.
Such details as are available are shown in the fol-
lowing table:
Foreign Trade in Explosives
Articles
Imports
Fulminates, gunpow-
der, etc
Allother
Total
Exports
Cartridges, loaded.. .
Dynamite, lbs
Quantity
$ 256.379(a)
600,958
857,337
S 7,860,139
437,010
8,297,149
Gunpowder, lbs
Shells and projectiles,
loaded (a)
All other
Total
(a) Not stated separately i
3,521,533
14,464,601 1,587,184
(o) (a)
989,385 247,200
(o)
916,280
6,272,197
1914.
13.672,371
18,911,668 4,991,508
19,346,554
340.516,883 262,201,813
40.130,298
38,559.249
378,901,793
FERTILIZERS
Imports and exports of fertilizers both show a big
falling off according to official figures, but it will be
noticed that the group as given in the following table
does not include sodium nitrate, which, because it
is not used exclusively as a fertilizer, is included under
"Chemicals."
The falling off of potash imports is the serious fact
made plain in the table, for while good work has been
done in developing a domestic industry, it is never-
theless true that the foreign potash is missed.
Exports of phosphate rock to Europe fell off im-
mediately after the war started and have not been
resumed on the old scale, although Spain has continued
to make purchases on something like the scale of pre-war
times. Of the total exports for 1918, four-fifths are
included under the heading "All other fertilizers,"
and there is no way of throwing any further light upon
the subject at present.
Both imports and exports of fertilizers are shown
in the following table:
Foreign Trade in Fertilizers
1914 1918
Articles Quantity Value Quantity Value
Imports
Ammonia, sulfate, tons 83,377 $4,888,563 3 ,983 $ 467 ,999
Bone dust, ash, and meal, tons 41,450 1,034,636 8,511 286.764
Guano, tons 21,887 755,833 10,096 287,446
Kainit, tons 541,846 2,554,567 ...
Manure salts, tons 261.342 2,767,241 190 8,872
Potash, N. E. S.:
Muriate of, tons 237,886 7,915,523 723 195,154
Sulfate of, tons 45,139 1,897,740 135 19,837
All other substances used only
as fertilizers 6,199,554 ... 4.089,989
Total 28,013,657 ... 5.356,061
Exports
Phosphate rock:
High-grade hard rock, tons. . 475,335 4,753,350 25.652 217,650
Land pebble, tons 1,000,630 5,857,969 110,909 456.383
All other, tons 1,906 6,516 25,798 336,880
Superphosphates, tons 6,155 202,268
All other fertilizers, tons 61.601 1,360,903 84,410 4.626.958
TOTAL Tons 1,539,472 11,978,738 252.924 5,840,139
'.I MS. RESINS, ETC. •
Increased imports of India rubber are the most
noteworthy feature of the trade in this class of ma-
terials since the war started, the total receipts jump-
ing from i,3 2 million pounds in 19 14 to ,'i)o million
pounds in 1918. The increase in direct imports
from the East Indies is remarkable and is an encour-
aging circumstance. The tendency to import raw
materials directly from the original source instead of
through European middlemen will probably be an impor-
tant factor in after-the-war trade. It is an interesting
fact that although the quantity of rubber imported
from Brazil has increased slightly the total value has
decreased. The importation of varnish gums and of
camphor has apparently not been affected materially
by the war.
Imports are shown in the following table:
Articles
5orts of Gums and Resins
1914
Quantity Value Qu;
Camphor:
Crude natural, lbs.
Refined and syir
thetic, lbs 566.106
Chicle, lbs... 8,040.891
Copal, kauri, damar,
lbs 32,693.412
Gambier, lbs 14,936.129
India rubber, gutta-percha, etc.:
Balata, lbs 1,533,024
Guayule gum, lbs.. 1,475,804
Gutta joolatong. lbs. 24,926,571
Gutta-percha, lbs-
India rubber, lbs. .
From Belgium. .
France
Germany
NetRerlands. . . .
Portugal
United Kingdon
Central America
Mexico.
3.476.908$ 929,715 3,638,384$ 1.451,050
1,846,109
793,126
607,076
1.155,402
323,567
131,995,742 71,219,851 389,599,015 202
11,005,246 6,481.901
1 ,124,629
3,595,369
1,134,060
176,687
2,629.287
7,052,767
2,016,440
556,560
48.279,674 31.152,336
565,487 297,849
640,448 333,3:
2,449,881
4,307,539
17,475,863
1,151,312
508,017
,610
,095
,816
,323
,392
Brazil 40,641,305 16,319.048
; b East
1 ,016,566
828,856
538,076
21,926,945
736,014
1,033,087
41,277,914
3,565,094
Indies
Dutch East
Indies
Other countries. .
India rubber scrap,
379,886 3,182,605 1,299,.
16.597,105 9,675,709 258,245,724 138,324,
53,663,857
4,921,682
1,504
.913
lbs.
Shellac, lbs.
9, J
America's export trade in the class of gums and
resins is confined to the items included under the
heading "Naval stores," and foreign sales in this
line have been cut nearly in half as a result of the war.
This is to be accounted for by the fact that some of
the best customers under ordinary circumstances
have been entirely cut off and by the fact that the
Ex
Articles
Naval stores:
Rosin, bbls
To Austria-Hungary.. .
Belgium
France
Germany
Italy
Netherlands
Norway
Russia
Sweden
United Kingdom . . .
Canada^
Cuba
Argentina
Brazil
Uruguay
Dutch East Indies. .
1 'l' in
Australia
I Mlicr countries
Tar, turpentine, and
pitch, Mils
Turpentine, spirits of,
To Austria-Hungary...
Belgium
' .. i many
Netherlands
i <1 Kingdom. . . .
I Minrla
Argentina
Brazil
Australia
( ithcr countries
Total Naval
Storks
>orts of Naval Stores
1914 1918
Quantity Value Quantity Value
2.417,950 $11,217,316 1,073,889 $7,876,718
68,158 284,715
111,735 463,464
128 726
799,185 3,465,723
109,380 508.648 10,056 63.570
247,339 1,058,963
2,409 12,490
144,653 584,076
180 980
504,400 2,310,373 274,976 2,021,339
77,064 471,511 132,070 876,077
24,052 127,886 34,455 223.349
102,028 506,260 149,536 1,068,153
99,632 687,480 158,824 1,169,447
18,982 106.295 23.041 181,798
2,252 13,092 27,628 233,092
14,413 94.004 103.081 843.663
61,682 366,561 72,284 561.926
30,278 154,069 87,884 634,304
351.352 568,891 82,030 598.211
18,900.704 8,095,958 5,100,124 2,697,305
7,650 3.3(111
1,027,355 420,595
390 (15
3,275,929 1,368/616
4,393,902 1,870,304
109 851 2,930,570 1 .113.732 659,989
1.114,863 4KH.I38 978,125 424,520
512,544 271,000 321,797 186,661
301.912 154,288 222,339 139,851
499,248 249.935 851,328 528.428
657.060 338,997 1,312,803 757,856
19,882,165 11,172,234
696
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, Xo. 9
belligerents that still have access to supplies do not
need the quantities formerly purchased. Sales to
neutrals outside of Europe and to non-participating
associates of the Allies have increased to some extent,
as will be seen by examining the preceding table.
METALS, ORES, EARTHS, ETC.
Copper is the principal item in both imports and
exports of metals, and purchases and sales of that
essential have increased wonderfully since the war
started. Imports have jumped in value from about
SS millions to more than 122 millions, the augmented
supplies coming largely from Latin- American sources.
Exports have increased in the meantime from 149
to 244 millions as the result of war demands in Europe.
Tin imports have more than doubled, totaling 85
millions in value in 1918. The importation of 10
million dollars' worth of Bolivian ore for smelting in
the United States indicates the importance of one of
our newest industries. There have been increased
importations of all the important metals except iron.
Aside from copper, the only important increases in
metal exports are recorded for iron and lead. A
summary of the foreign trade in the important metals
is contained in the following table, which relates only
to metals in the form of ore, concentrates, pigs, bars,
etc.:
Articles
Imports
Antimony
Chromate of iron
Copper
Ir.
Summary op Trade in Principal Metals
1914 1918
Lead
Manganese.
Nickel
Platinum.. .
Tungsten-bearing ore.
Zinc
Exports
Aluminum
Bauxite concentrates
Copper
Ferrovanadium
Iron
Lead
Nickel
Tungsten and ferrotungsten .
Zinc
Articles
Metals and Orbs:
Antimony:
Ore, regulus, or metal (antimony co
Ore I gross tons
Ure j antimony, lbs
Matte, regulus, or metal, lbs
Cobalt and ore, and zaffer, lbs
Chromate of iron, tons
Copper:
Ore i gross tons
Imports op Metals, Ores, Earths, Etc
1914
( copper, lbs
Concentrates i «ross tons
( copper, lbs
Matte, regulus, etc. j gross to°*
& ' ( copper, lbs
Pigs, bars, etc., lbs
All other
Iron:
Ore, tons
Pig, tons
Iridium, osmium, palladium, etc., and native
thereof with platinum, etc., oz. troy
Lead:
Ore ( gross tons
\ lead , lbs
^"tefc::::::::::::::::::::::::::
Pigs, bars, and old, lbs
All other
Manganese oxide and ore, tons
Monazite sand and thorite, lbs
Nickel ore and matte { Sfoss tons
( nickel, lbs
Platinum:
Unmanufactured, oz. troy ,
Ingots, bars, etc., oz. troy
Retorts, etc., for chemical use
Sulfur ore as pyrites, over 25% sulfur, tons
From — Spain
Canada ,
Other countries
Tin:
Ore, tons
Bars, pigs, etc., lbs \\]
Tungsten-bearing ore, tons
Zinc:
Ore and calamine { f08*'0"5
( zinc, lbs
Pigs and old. lbs
Oust, lbs
All other '..'.'.'.'.'.'.
Clays, Earths, Etc.:
Cement:
Portland, Roman, etc., 100 lbs
All other
Chalk:
Unmanufactured, tons
Ground, etc
Clays or earths:
China, or kaolin, tons
Blue, and bauxite, tons
All other, tons
Fluorspar, tons i ! ! ] !
Gypsum, crude, tons
Mica:
Unmanufactured, lbs
Cut, split, manufactured
Plumbago, tons
Talc, ground or prepared, lbs
Miuerals, crude, n. e. s ,,,,
(a) Covers period from July I to October 3, inclusive.
(6) Covers period from October 4 to June 30, inclusive
(c) Not stated separately in 1914.
2.664.425(a)
555 1 (6)
865,565) (6)
9,633,639(6)
197,009
78.842
444,907)
87,588.730)
(<0
M
33,772)
24,682.744)
281,536,836
• 2.960
55.807)
23,127.210)
37.795.279 1
37,059,518)
236,691
288,706
1,002,300
36,420)
43.549,303)
832,134
638,711
79,141
114,282
18.280 1
14.484.802)
2,145,089
4,807,664
238.802
33.041
73,576
13,655
416,599
i 145
917(a)
24
121(6)
526
115
737
324(6)
038
127
0,137
244
(£)
3.559
740
1,247.567
9.002
60,849
1,841.451
52,329
1,489.208
2.404.364
82.000
3.695.335
2,966,682
312,575
416.078
251.479
90,481
223.010
50,981
1.577.747
228.207
440.853
50.851
482,529
524,454
312,361
1 .846.126
148,523
271.882
$ 696,000
737.000
54.506.000
11 ,879.000
2,057,000
I ,841 ,000
6.110.000
3,976,000
39,422,000
114,000
616.000
1,102,000
616,000
149.480,000
503,000
6.261,000
2,610,000
9,404,000
995.000
I 5.280)
[ 6,526.292 J
33.934,515
161,705
77.781
[ 377,124)
t 104,691.803)
160,998)
39,093.081 I
I 21,658)
[ 22,869,596)
362,494,391
4,759
93,322 1
39,054.690 1
158.509,646
149,575,356)
19,082,922
558,018
4,975,975
58,7761
73,095.770)
810,075
596,583
205.163
8,329
14.816
136.519,310
5,646
102.234)
78,770.011 j
303.505
407.546
194.225
2.292
37,553
10,935
151 ,415
706,706
$ 4.435,000
1,543.000
122.450.000
9,652.000
11,970.000
II .945.000
9.120.000
4,575.000
84.834,000
5,794,000
2.560,000
8.746.000
1.465,000
244.328.000
2.578.000
20,579.000
17,376.000
7.681.000
4,056,000
19,193,000
$ 495,953
3,939,174
306,310
1,542,761
18,318.781
9.492,501
5.279.976
89,221,607
136.927
2,098,045
8,719,554
1,138.757
13,841
11,944,515
329.711
9,120,269
4,308.518
264.096
2.547
4,522.335
3.709.368
765,429
47,538
10.291.261
74.543.006
5.793.698
2,499.468
15.289
44.625
564
1.322.603
11.649
316.407
117.279
256.294
543 , 289
998 . 460
6.127,887
265.979
1.232.613
Sept., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
697
Further details as to the imports will be found in
the foregoing table, which also includes, as a matter
of convenience, such items as cement, chalk, clays,
plumbago, and talc. Imports of these latter arti-
cles are not comparatively important.
Exports of metals, ores, cement, clays, etc., are
shown in detail in the table that follows:
Articles
Metals and Ores:
Aluminum, ingots, etc., lbs
Copper:
Ore, matte, regulus, tons
Ore, tons
Concentrates, matte, regulus, tons.
Unrefined black, etc., lbs
Pigs, bars, etc., lbs
All other
Babbitt metal, lbs
Bauxite concentrates, tons
Ferrovanadium, lbs
German silver
Iron:
Ore, tons
Pig, tons
Lead:
Pigs, bars, etc
From domestic ore, lbs
From foreign ore. lbs
Nickel, oxide and matte, lbs
Platinum :
Unmanufactured, oz. troy
Manufactures of
Quicksilver, lbs
Tin, pigs, bars, etc., lbs
Tungsten and ferrotungsten, lbs
Zinc:
Ore, tons
Dross, lbs
Spelter, etc
Clays, Earths, Etc.:
Cement, hydraulic, bbls
Clays:
Fire, tons
All other, tons
Lime, bbls
Mica and manufactures...
Plumbago:
Unmanufactured, lbs
Manufactures of
and imports of flaxseed mounted from 11 to 34 mil-
lions. This will give some idea of the search Amer-
ican manufacturers have made for food and indus-
trial oils. As is well known, coconut fat has entered
largely into the manufacture of butter substitutes
that have recently appeared in such large quantities
in the market.
of Metals, Orbs,
Earths, Etc.
1914
1918
Quantity i
Value
Quantity
Value
$ 1,101,920
21.256,641
S 8,746.451
77,410
3.257.080
51.545
984 , 709
4.376
216,941
26,550.026
6,920,687
974,791.676
144.895.519
839.904,470
235,717,071
1,327,037
488.837
1,010.651
181,958
2,290,878
610.979
13,792
616,327
21,339
1.464.933
626.641
503,389
2.089,347
2,577.670
38,691
270,703
1.004,547
3.401.156
1.185.769
4,877,380
201,995
2,859,830
377,012
15,701,846
2.610,207
17.377,031
130.303.394
10,411 .539
22,237
1.295
84.260.273
6,965,492
28.895,242
9.403,709
18,818,212
7,680,502
273
12,977
468
50.697
71.172
33,557
64,190
32,241
502.088
679,414
209,391
127.219
2,184,769
4.056,437
14.294
559.785
1.203
64,873
572,477
29,084
31.104.163
2,283,843
406,208
172,333,718
16,844.449
2.391,455
3,382,282
2,575,205
5,898.081
57.581
50,529
310,527
249,335
22.267
188.055
285,749
200,437
142,525
150,197
65,102
71,285
5.376,880
387,075
4,912.730
331,369
269.499
716,538
OILS, FATS, AND WAXES
Exports of mineral oils in 191 8 exceeded the total
for the last normal year by 137 million dollars. That
and the increase in the imports of vegetable oil and oil-
bearing materials are the most interesting changes
wrought by the war in the foreign trade in oils. The
following summary table will show at a glance the
salient features of the trade in this class of ma-
terials:
Summary op Trade in Orts
Articles 1914 1918
Imports
Oils:
Animal $1,034,000 J 3,678,000
Mineral 13,666.000 21,926.000
Fi-ed vegetable 28.829,000 87.986.000
Essential 3.492.000 4.338,000
Oil-bearing materials:
Castor beans 1,139,000 2,641.000
Copra 2.395.000 26.946,000
Flaxseed 10,571,000 33,850.000
Peanuts 1,899.000 4.771,000
Exports
Oils:
Animal 822.000 1,155,000
Mineral 152.174,000 289,037.000
Fixed vegetable 15.624,000 23.930.000
Essential 628.000 1,091.000
Details of the import trade are set forth in the table
on page 698. It will be seen that the increased
imports of mineral oil came almost entirely from
Mexico. The most impressive increases in vege-
table oils are recorded for coconut oil, 7 to 31 millions
in value, and soya bean oil, 1 to 31 millions, while
purchases of copra rose from 2 to 27 millions,
Mineral oil has long been one of America's most
valuable contributions to the world's trade. The
American oil can is recognized affectionately by our
tourists in the most remote corners of the world.
But the war has given a new significance to the ex-
ports, for enormous quantities are now going forward
for war service in Europe. A study of the table of
exports on page 698 will show that the increases have
been restricted to fuel and lubricating oils and to the
light distillates. Illuminating oil has fallen off by half
in quantity.
Exports of cottonseed oil have fallen nearly half in
quantity, but the total value has increased, as is also
the case with oleo oil. Our exports of oil-bearing
seeds and nuts are not of particular importance.
PAINTS, PIGMENTS, VARNISHES, ETC.
American imports of this class of chemical products
have fallen off more than half since the war started,
but never were of much importance. About a mil-
lion dollars' worth came from Germany in 19 14.
Exports have increased from about 7 millions in
value to 1 7 millions, a result of pushing such goods in
markets abandoned by European manufacturers.
It is an interesting departure and one that should be
watched carefully with a view to retention of the
present gains and still further expansion in the
698
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 9
Imports of OrLS, Fats, a
1914
ARTICI.8S Quantity
Oils, animal:
Cod and cod liver, gals 1 .393.706(6)
All other 1 ,488,973
Oils, mineral:
Crude, gals 773 , 052 , 480
From— Mexico 737,712,569
Trinidad and Tobago 14,597,633
Peru 20,710,023
Other countries 32 , 255
Refined:
Benzine, gasoline, naphtha, gals 16, 139,912
All other, gals 1 ,945.007
i »ils, fixed vegetable:
Chinese nut, gals 4,932,444
Cocoa butter or butterine, lbs 2,838,761
Coconut, lbs 74.386.213
Cottonseed, lbs ' 17.293,201
I.inseed, gals 192,282
Olive, non-edible, gals 763,924
Olive, edible, gals 6,217,560
From— France 949,858
Italy 4.319,567
Spain : 362,483
Other countries 589.652
Palm, lbs 58,040,202
Palm kernel, lbs 34,327,600
Peanut, gals 1,337,136
Rape-seed, gals 1 , 464 , 265
Soyabean, lbs 16,362.452
From — China 5,983
Japanese China 6.150.000
Japan 6.427.307
Other countries 3 , 7 79 . 1 62
All other
Oils, distilled and essential:
Birch tar and caj put
Lemon, lbs 385,959
All other
Glycerin, lbs 36,409.619
Oleostearin, lbs 5,243,553
Paraffin (except oil), lbs 7,495,459
Wax:
Beeswax, lbs 1,412,200
Mineral, lbs 8,086,422
Vegetable, lbs 4.255,686
Grease and oils, N. E. S 22,322,492*
Oil seeds and nuts:
Castor beans, bu 1 , 030 , 543
Coconuts in shell
Copra, lbs 45.437,155
From — Australia 1 , 85 1 , 74 1
Other British Oceania
Philippines 27,542,443
Other countries 1 6 , 042 , 97 1
Flaxseed, bu 8,653,235
From — Canada 8,647.168
Argentina
Other countries 6,067
Peanuts:
Not shelled, lbs 17,472,631
Shelled, lbs 27.077 158
d Waxes
1918
Value
Quantity
Value
$ 563.600(6)
2.. 021, 656
$2,111,489
470.251
2.906,473
1.566.366
11,776,737
1.347,543,144
17,916.737
10,971.613
1,346,666.866
17.901 ,639
297.603
506,535
907
77
986
875,371
15,021
1.400.740
11 .069,899
1.473.033
488,463
45.114,581
2,536,600
1,962,389
4.815,740
4,038.072
793,451
405
74
6.703,942
259,194,853
30.919,783
1,044,834
14,291,313
1 .629.111
91 ,555
50,827
32,203
477.210
114,324
94.629
7,916,980
2,537,512
1,512,324
227,617
576.602
5,552,098
200.403
467,692
370,053
2,091.400
2,783,691
482,505
18.092
45,226
3.858.001
27,405.231
2.527,301
3.087.343
18,618
2.583
918,614
8,288,756
7.311,824
704,655
3,056,438
2 , 702 , 920
830.790
336.824,646
32.827.460
363
12.470,720
1 ,456.172
288.320
237,442,917
23.104.484
313.795
86,830,583
8.255,001
228.312
80,426
1 1 , 803
439,009
2,027,137
25,981
858.220
628,057
427,318
2,633.789
3,884.287
4,486.415
1 .875,531
804.618
459,989
6.575,379
1.118.422
326,966
8,997,023
672,518
476.364
1,826,618
632.356
543,103
1.708,514
135.920
1.049,126
8,707,396
2.693.258
1,251,997
28,000,428
3.343.565
1,139,311
1.222.934
2.640.902
2.133.416
2.788.635
2,395,013
486,996,112
26.945.569
86,473
96.397,324
6.104.493
46 , 206 , 768
1,497,358
219.555.171
9,949,785
811,202
124.836.849
7,671 ,064
10,571,410
13.187,609
33,8S0,054
10,561.662
5,501 .391
16,375.622
7.253,501
16,471.798
9.748
4 '. : . : i 7
1.002.634
660,010
3, ISO, 747
153.054
1,239,227
162,215
4.617.560
Oils, Fats, an-d Waxes
Articles
Oils, animal:
Fish, gals
Lard, gals
All other, gals
Crude, gals
Refined or manufactured:
Fuel and gas, gals
Illuminating, gals •. . . I
Lubricating, gals
Gasoline, gals
< Ither naphthas, gals
Residium, gals
Oils, fixed vegetable:
Corn, lbs
i ed, lbs
Linseed, gals
All other
Oils, volatile or essential:
Peppermint, lbs
All other
Glycerin, lbs
Greas.
Lubricating
Soap stock, etc
Olco oil. lbs
Oleomargarine, lbs
Paraffin:
L^nrefined. lbs
Refined, lbs
Stearin:
Animal, lbs
Vegetable, lbs
W«:
Beeswax, lbs
Manufactures of
Oil seeds and nuts:
eed, lbs
d 'in
Peanuts, lbs
(o) Not stated separately in 1914.
448.366
110.199
891,035
146,477,342
475,143.205
157,283,310
196.884.h96
151,611 ,537
40,840,730
[13,370,245
18,281,576
192,963,079
239,198
16,342.384
ins, 546
I
87.364
609 . 294
6,812,672
13,747.863
74.500.162
27,852.959
21,699.475
5,653.210
1.907.715
1.307.204
13.343.179
M4.54H
117,809
397,050
230.55 7
97.017,065
2.532.821
2,394.918
5.046,959
10,156.665
263,453
186.357.728(a)
6.516,338(0)
2,724.182
(<■)
234 .121
(»)
96,215
112,193
215.115
436.874
421.367
Quantity
Value
464.936
91,585
442,496
$ 448.710
126.672
579.631
186,672.778
9. 107.519
224.807.4iH
328,805,501
269.667, 145
260.300.337
207.905,009
1.879.475
61.339.504
4 -.488. 425
66.146.827
61.447.382
52,408.330
206,940
1 .831 . 114
10(1.005.074
1 .187.850
306.219
18,142,938
1.532.307
3.948.483
76,247
21.(145.991
233.899
10, 587,531
56.648,102
6.404.896
2.986,815
12, 166.482
1 .631.267
84.657.140
162.003,480
4.857.931
13.683.597
10.252,522
1.293.327
2.180.485
293.591
189.871
68.117
717.181
1.565,052
21.481
12.488.209
57,693
101.165
1,517.831
Sept., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
699
Value
.125.22
Value
$ 961.047
future. Available details are shown in the following
table:
Foreign Trade in Paints, Pigments, Etc.
1914 1918
Articles Quantity
Imports
Paints, pigments, etc $2
Exports
Dry colors:
Carbon, bone, and
lampblack
All other
Lead:
Red, lbs (o)
White, lbs 16,845.154
Ready-mixed paints, gals. 852,910
Varnish, gals 1.069,501
Zinc, oxide, lbs 29,197,790
All other
Total
(a) Not stated separately in 1914.
Articles
Imports
Trade in Tanning Materials
1914
Quantity Value Quae
All other, lb:
Materials:
Mangrove bark, tons. 7,689
Quebracho wood, tons 73,956
Sumac, lbs 10.770.540
8,710.040 306,934 4.573,925
All other.
(a)
1,013,506 18,235,783
1,096,335 1,521,588
1,038,864 736,949
1,215,360 25.862,063
1,779,863
7,256.312
4,792,330 567.854
2,072,352
2 , 399 . 638
1,209,762
2.750,610
4,875,006
16,894,154
Exports
Bark, tons (a
Extracts
Germany
Netherlands
Norway
Sweden
United Kingdom
Canada
Japan
Other countries
(a) Not stated separately i
196.891
900,880
258.738
468.230
(a)
639,941
11,776
1,474
1.874
909
214,151
353.833
19,561
36,363
3,529
45,440
14,046.662
72,956
718.567
467,663
496,070
,357.272
.094.330
750
334.401
TANNING MATERIALS
Quebracho is the only important tanning material
imported into the United States, and the war seems
to have stimulated this trade to a slight extent. Ar-
gentina and Paraguay are getting an important share
of the business.
Exports of tanning extract have increased from less
than 1 million to nearly 4 millions since the1 war started,
practically all of the consignments going to England
and Canada, as will be seen in the table entitled
"Foreign Trade in Tanning Materials."
PAPER AND PULP
Imports of printing paper have doubled in quan-
tity and tripled in value since the war started, and at
the same time exports have increased threefold in
quantity and nearly fivefold in value, although the
import trade is the more important. Probably recent
restrictions will effect some changes in the trade for
1919.
Imports of pulp fell off 65,000 tons in 1918 as com-
pared with the receipts in 19 14, but the value of the
imports nearly doubled. Canada made up for the
failing supplies from Scandinavia, but at greatly en-
hanced prices. More pulp was exported than in 1914,
but this trade is not important.
Details of the trade will be found in the table
given below:
MISCELLANEOUS PRODUCTS
Under this heading has been included sugar, which
perhaps could just as well have been excluded from
Foreign Trade in Paper and Puli
Articles . Quantity
Imports
Printing paper:
Not over 5 cents lb., lbs 536.815.288(a)
All other, lbs 6,053.429
Surface-coated paper, lbs 6,925 , 505
Wrapping paper, lbs 36 , 5 1 5 , 554
Wood pulp :
Mechanically ground, tons 177 ,484
From— Canada 176,169
Other countries 1,315
Chemical, unbleached, tons 302,963
From — Germany 55,844
Norway 43.970
Sweden 117.914
Canada 79.327
Other countries 5.908
Chemical, bleached, tons 88.917
From — Germany 18.638
Norwav 46 . 292
Sweden 14.165
Canada 6.630
Other countries 3 . 192
Total Pulp, Tons 569.364
Exports
Printing paper:
Newsprint, lbs 88.966.738
To— United Kingdom 4,017,01 1
Canada 7,544,600
Mexico 417.401
Cuba 11 .955,505
Argentina 17,688,296
Chile 1 .493 ,973
Australia 36,583,363
Other countries 9.266.589
All other printing paper, lbs 28,602, 134
To— United Kingdom 4,014.625
Canada 10.379,029
Mexico 522,388
Cuba 5,104,725
Argentina 356. 150
lirazil 45,534
Chile 913,419
Japan 855,960
Australia 2.828,669
< >ther countries 3 , 58 1 , 635
Total Printing 1 1 7 . 568 . 872
Wrapping paper, lbs 14i 133,097
Writing paper and envelopes
Wood pulp, tons H.481
o) Not over 4 cents per pound.
1914
1918
Value
Quantity
Value
$10,785,129
1,203,762,118
S34. 192.845
290,530
278.367
41,377
620.061
380.153
85.675
1,028,500
6,150.942
375,592
2,733,595
189,599
6,138,831
2,704,901
178,130
5.814.419
28,694
11,469
324.412
10,136,707
296,465
23,314,875
1,035,267
1,538,788
3,235
287,046
3,761,637
40,420
3,900,494
2,862,943
251,265
18,949,696
938.072
1,545
177.639
4,153,036
18,044
2,135,384
886,604
2,168,173
4,316
627,248
614,227
1,368
172,202
340,673
11,464
1.225,492
143,359
896
110,442
17,023,338
504.108
31,589.090
2.177.483
220,080,301
9,559,849
90,901
8,274,963
468,719
151.783
453,611
27,244
13,218
8.230,196
343, 177
266, !S7
19,667,822
708 . 298
447,908
48,177,451
1,983.472
37, 141
15.593,731
626,429
947. 185
20,520,633
839.342
223,090
99,161,894
4,563,168
1,612,370
90,353,235
7,702.090
296,731
1.750.864
146,897
601,909
8,334,122
722,944
32,111
3,192,276
'.SK.'X.l
263,157
9,521,768
885.907
25.618
10,037,691
870,846
2,724
10,361 ,919
872.320
40,665
4,442.904
388.369
33.651
9.751.534
816,946
132,498
13,041,834
1,084,481
183.306
19,918,323
1,654,419
3,789.853
310,433,536
17,261 ,939
532.657
59.350.946
4,489,287
1,179
4,560.084
529.741
34,805
3,531,639
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. N'o. 9
Articles
Imports
Collodion, and manufactures of
Glass and glassware
Glue and glue size, Lbs
Matches
Oilcloth and linoleum for floors:
Linoleum, sq. yds
Oilcloth, sq. yds
Photographic goods:
Dry plates
Motion picture films:
Sensitized, not exposed, lin. ft
Negatives, tin. ft
Positives, lin. ft
All other films and plates
Soap-
Castile, lbs
All other
Sugar and molasses:
Molasses, gals
Sugar:
Beet, lbs
Cane, lbs.
Exports
Baking powder, lbs
Blacking and polishes
Candles, lbs
Celluloid and manufactures of
Chewing gum
Flavoring extracts and fruit juices
Glass and glassware
Glucose and grape sugar:
Glucose, lbs
Grape sugar, lbs
Glue, lbs
India-rubber manufactures:
Belting, hose, and packing
Boots and shoes, pairs
Tires
All other
Ink:
Printers'
All other
Matches
Metal polish
Mucilage and paste
Oilcloth and linoleum:
For floors, sq. yds
AU other
Photographic goods:
Motion-picture films:
Not exposed, lin. ft
Exposed, lin. ft
Other sensitized goods
Soap:
Toilet or fancy
All other, lbs
Sugar and molasses:
Molasses, gals. .
Sirup, gals
Sugar, refined, lbs
Vulcanized fiber and manufactures of . . .
Washing powder and fluids, lbs
(a) Not stated separately in 1914.
(6) From October 3. 1913, to June 30, 1914.
(c) Stated as "All other" motion-picture films in 1914
Foreign Trade in Miscellaneous P
Quantity
KODUCTS
1914
Value
$ 569,763
8.191,833
1 , 805 , 543
882,812
1,762.896
66,700
889.560(6)
402. 704 U)
1,009.469
264.655
360,128
460.485
1,744.719
70,829
101,365,561
790.274
649.395
283.018
1,387,541
178,630
3,729.623
3 . 766 , 284
799,635
258.611
2.372.887
1.113.495
4,068.639
4,886,199
443,377
181,697
77.736
162.504
95.013
60.608
666.479
4.264,722
2,282,924
1,348.216
2,141.633
2,797.369
175.498
1.491 .639
1.839.983
854,642
53S.635
Quantity
2.048.543
38.584
5,060
47,462,715
713.363
3.374.497
1.016.399
130.730.861
750
4,898.277.025
6.046.455
6.761.767
80,970.744
16,887,557
4,935.250
2 , 803 . 768
1,259,805
57,995.064
84,557,376
82.726,757
3.811,341
7,690,074
576,415,850
4.754.084
1918
Value
$ 53.637
1.723,014
22,714.877
348,241
3.856.961
3,724,086
28.080
340,288
1.934
(a)
33.857
739.135
166.033
20,057,144
177.148
203.719
4,622.082
147.149
211.149
51.410,271
9,177,833
2.367,708
73
5.061.564,621
236.105.886
2,725,964
1.840.251
1,009.100
3,047,756
1.031 .184
3.744,745
1.896.135
1 .018,102
14,012,656
162,680,378
4,949.159
36,850.496
1.045.512
2.351,770
839,197
4,578.396
1,735.619
5.774,341
15,128.294
6.194.816
882.062
407.093
471.385
192,691
399 , 295
163,214
655.175
1.277,777
155.359.550
32,690.104
1,385.291
5.132,528
2,938,756
2,246.258
58.547.763
6.894,454
1.002,441
847,692
11,630,528
4,823.912
38.756.680
950.029
12.761,958
243,184
consideration entirely. Sugar imports were not quite so
high in 1918 as in 1914, considering quantities, but
the value was more than doubled. Exports, on the
other hand, increased from 51 to 576 million pounds,
the values increasing from 2 to 29 million dollars.
The refining of Cuban sugar for export to Europe is
a war development.
Exports of rubber goods have increased from 12
to 32 millions in value, although what percentage of
increase has been due to high prices would be diffi-
cult to determine.
Imports of matches have increased in value, as, to
a lesser extent, have the exports. Japan has built
up a good business in matches as a result of difficul-
ties in Sweden.
In the above table will be found a number of
export increases that, while comparatively unim-
portant, are significant because they represent new
business in non-fighting countries, business that may
possibly be retained when the war is over.
MISCELLANEOUS MATERIALS
Grouped under this head will be found a number
of materials that will interest some branches of the
chemical industry, but which could not well be in-
cluded in any of the previous groupings and are not
important enough to be treated individually. '
Foreicn Trade in Miscellaneous Materials
Articles
Imports
Asphaltum and bitumen..
Hlood, dried
Bones, hoofs, and horns. .
Fish sounds, lbs
Gelatin, unmanufactured,
lbs
Hide cuttings, raw. and
other glue stock, lbs . .
Moss and seaweed:
Crude
All other
Rennets, raw or prepared
Salt, 100 lbs
Vanilla beans, lbs
Exports
Asphaltum
I nmanufactured. tons 49.831
Manufactures of
Moss
Salt, lbs 148.931.265
(a) Not stated separately in 1914.
80.689 $ 918,387
391.816
1.061.466
(o)
(a)
2.341 .317
3.076.071
139.899 863.476
462 , 703
1.374,546
77.499
738.731
2.158.514
301.259
54.3 7'.
129,720
423.322
331,248
365.586
21.710.205
133,057
936.393
230.163
8.514
62,173
307.036
897.100 2.277.675 914.668 1.475.676
.131.086 22,052
362.347
51.006
542.783 267,045.840
Sept., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
THE CHLMICAL MARKETS OF SOUTH AMERICA^
By O. P. Hopkins,
THE CHEMICAL MARKETS OF ARGENTINA, BRAZIL AND
URUGUAY
Received July 29, 1918
The region in South America which embraces
Argentina, Brazil, and Uruguay is famed chiefly for
its agricultural and pastoral products. Brazilian
rubber is a forest product, but as a whole the forests
of the region, although rich in material, have been
little exploited. The mineral resources of some
parts of the district are beyond calculation, but they
have been worked only very superficially.
The lack of one mineral, however, is the factor that
keeps the region definitely pastoral and agricultural
rather than industrial — there is very little coal. It
is the lack of fuel that holds in check the present
tendency to manufacture at home the articles that
formerly were imported from Europe and the United
States, but which now are almost unobtainable on
account of the scarcity of tonnage and the disloca-
tion of trade caused by the export restrictions of the
belligerent countries.
As would be expected, chemicals and allied prod-
ucts are not imported in comparatively important
quantities. The finer chemical products, however,
such as pharmaceutical products, perfumes, patent
medicines, and soaps are in demand and are purchased
to a large extent from foreign manufacturers. Such
products as paper and glassware are imported also.
Before the war Germany had the lion's share of the
trade in most of the imported articles, but American
manufacturers have not been slow to take advantage
of the German's absence and have learned so much
about the business that they never knew before that
it is very unlikely they will ever lose their grip. Lack
of shipping and export restrictions stand between
them and a complete conquest of the markets.
The statistics contained in this article have been
compiled with the primary object of showing the ex-
tent of the market for chemicals and allied products
which exists in the three countries treated. The
principal table in each case shows details of imports,
including the chief sources of origin, and is a com-
pilation from the original official statistics, published
in Spanish or Portuguese. Official detailed statis-
tics in most of the South American countries are always
several years behind time, but these figures will give
an adequate idea of the demand for imported goods.
Tables are also given showing the trade of each coun-
try with the United States for the fiscal years 1914
and 191 7, based on statistics published by our own
Bureau of Foreign and Domestic Commerce. These
will show how the war has affected our trade with
the three countries, and will also indicate what those
countries have to export in the way of raw and manu-
factured chemical products.
It should be borne in mind that South America was
at first much harder hit by the war than we were and
that the period of depression lasted much longer. Re-
(») First of a series of articles on South American Chemical Markets.
Washington, D. C.
covery was finally effected through the European
demand for foodstuffs and other raw materials and a
period of unexampled prosperity has now set in.
ARGENTINA
Cereals and meat products in mighty volume have
given Argentina her rank among South American
nations and are almost the sole cause of her present
prosperity. Manufacturing industries have never
thrived in the face of such obstacles as the lack of
coal and iron and the high price of labor. Mineral
resources are comparatively unimportant and the
forests have not been extensively exploited.
A variety of chemicals are imported, but only a few
in anything like important quantities. Sheep dip
is not manufactured at home and foreign purchases
of this Argentine essential amount to more than
$2,000,000 a year. Since the Uruguayan Govern-
ment established its domestic sheep-dip industry,
some imports have come from that source, but nor-
mally England gets the bulk of the business.
Tartaric acid, an essential in Argentina's rapidly
developing wine industry, was formerly imported
from Europe, but short supplies have resulted in es-
tablishing the industry at home, which in turn has
cut down Argentine exports of argols and wine lees.
American firms have taken an active part in stimulat-
ing the new industry. The largest wine producers
have installed apparatus for making the high-priced
crystallized acid from their own raw materials.
Aluminum sulfate, formerly imported largely from
Germany, and used in water-purification plants, is
now being manufactured at home to some extent with
the assistance of the Government. Eight thousand
tons were required in 1917. The kaolin used is found
in the Sierra Chica, Province of Buenos Aires.
The ammonia required in the meat-freezing plants
was formerly imported from Austria and the United
States, but now American exporters do all of the
business.
The Argentine paper market is an important one
and will continue to be so, as there is no prospect of
formidable competition from domestic producers. It
is one of the markets that Germany cultivated most
carefully, but American exporters have recently taken
over the best of the business. Germany's success,
apart from price considerations, was due largely to
the fact that the wholesale houses were controlled by
Europeans who were not keen about pushing American
products. Now there are at least two wholesale
houses controlled by Americans and they are doing
a big business. Other things being equal, these houses
will favor American goods after the war.
Paints and glass are two other lines that have been
developed by American exporters since the war started,
as will be seen more clearly in the second table, which
is based on American statistics.
The following table, based upon official Argentine
statistics, shows chemical imports in considerable de-
702
THE JOURNAL Of INDUSTRIAL AND ENGINEERING CHEMISTRY Vol.
No.
tail. It should be used only as a general guide, how-
ever, as the Argentine customs returns are based upon
arbitrary valuations that are seldom changed. They
are lower i! . X. E. *S. is an
abbreviation for "Not elsewhere specific <:
Argentine Imports op Chemicals and Allied Products
CHEMICALS. JlRUGS,
Dybs, Medicines
Acids:
Acetic, diluted S
Germany
Netherlands
United States
Jloric
France
Germany
United Kingdom
Carbonic
France
Germany
United Kingdom
Citric
France
Germany
Italy
United Kingdom
Hydrochloric
France
Germany
United Kingdom
United States
Hydrofluoric
France
Germany
Nitric
France
Germany
United States
Phenol
Germany
United Kingdom
United States
Sulfuric
Germany
Netherlands
United Kingdom
United States
Tannic
France
Germany
United States
Tartaric 1
France
Germany
Italy
United Kingdom
United States
All other acids
Germany
United Kingdom
United States
Alum
Belgium
United Kingdom. . .
United States
Al.UMlNH M SULFATE.
Belgi
Gem
Un
my
ed States .
Anhydrous
Austria-Hungary
United States
Carbonate of
Germany
km. dom
Liquid
Germany
United Kingdom
1 nited Mates
Muriate of
I '.iTIllilllV
i mi . .1 States
Other
United Stales
Aniline Dybs
it .1.1. i
• in
Switzei
United States
Arsenic fuk Indi str]
Germany. ...
1 iiiu-d Kingdom
I nited States
•i Casbidh.
Norway
.Sweden
United States
9 with Carbonic Acid
United Kingdom
68,694
26,262
31.332
9,720
8.868
3,940
6,593
268
5,252
363
79,310
1 7 , 806
31,264
207
23.367
21,346
15,208
4,425
3.351
1,074
6.671
3,952
2,555
27,911
1.341
24,747
418,579
399,502
121,052
32,964
27.551
985
1.678
246.787
188.917
53,113
1.861
107,475
37,191
55,993
122,982
35,556
56,654
18,061
4,004
13.110
14,744
209.723
15.104
174,728
10.392
327
10,687
7.718
2.303
521.668
242,204
40.808
13
18,159
17,939
13.072
6,552
1 , 307
4.323
5 . 207
2.260
1.977
970
65,627
24,035
1,252
17,722
15.97!
3 . 693
1.478
2,535
' 1 ,683
694
11.484
2.264
773
749,098
70.788
148.719
461,259
66.967
1,353
14,542
988
1.697
5.873
253,960
61,701
129.364
54,626
232
13,037
37.090
156,317
IV J47
14,986
209
13.276
7,840
5,'6oi
2 . 1 58
9.306
715
2,616
9,089
174
7.679
29,956
2.016
15,965
5 . 769
17 .347
9.775
6.711
452,894
156.017
27.761
5.500
5.481
Argentine Imports op Cbb
Dyes. Medicines
in Sulfide
Fr.iiu e
United Kingdom
c sbmti u. Prodi i rs, N. F.. S.
Prance
man y
United St.il. s .
C HI...RAL
Cblobi bbb
Germany
United States
i Si LPAT8
I tilled Kingdom
I nited States
U '•
United Kingdom
Cyancrates
Germany
United States
Cream of Tartar
Extract of Tannin
France
United Slates
Extracts, Medicinal
Extracts, Industriai
Formalin
Germany
United States
Glycerin
Germany
United States
Gums
Adhesive
I nited Kingdom
United Stales
Camphor
Japan
other
France
United States
Hydrogen, Peroxide of
France
United States
Iodoform
Iron. Sulfate of
United States
I.ime. Chloride of
France
United States
I.IML. HYPOCHLORIDE OF
L.YSOL
Magnesia. Sulfate of
Manganese Peroxide
Germany
United States
Medicines. Prepared
France
United States
Morphia and its Salts
Pharmaceutical Products,
N E. S
Germany
United States
Perfumery
France
United States
Pliosr
[icals and Allied Products (Continued)
Phosphorus Sesq.uisui.fide. . .
Switzerland
United Kingdom
Potash
Bicarbonate
Bichromate
Carbonate
Caustic
Chlorate
Nitrate
United States
Permanganate
I'russiate
Potassium Iodide
Qutni \. Sulfate op.
Roots Leaves. Bakes, Etc.,
MAI
Germany
United States
I HP. .
United Kingdom
United States
Soda Ash
United Kingdom
United Slates
Soda:
Bicarbonate
United Kingdom
United States
1913
1915
1916
$ 170.238
80.758
59.400
$ 27,698
3,792
17.042
* 9.627
809 . 889
176.558
620,753
134,165
. 28,940
299,637
1.349
933
679
14.304
8.897
93
18,811
1.340
11.997
9,528
206,856
180.994
190.132
172.462
19.878
17.079
3.536
1,214
4,072
13.219
7.481
4.851
1 ,064
2.013
6,981
3.170
5.719
140.935
82,133
10.131
5 , 24 1
Not shown
36.569
Not shown
25.063
13,207
7.771
7,569
695
4.560
17.387
43 , 229
25.035
9.616
263
3,283
15.643
11.787
4.650
19,615
7 . 854
141.827
31,885
1,853
5.059
; -'4
978
12.765
5.603
134.305
32.642
9.511
5.191
27,101
113,620
29,170
22 . 536
1,503
14.497
8,657
2,741
24.279
8.940
2.810
2.810
11,083
8,584
3,111
725
1.645
41.112
18.903
25,208
1,264
8.711
17.544
14,304
18.527
9.361
9.096
2.878
597
3.865
7.167
6.391
124.433
16
8.500
6.096
9,391
1 .9J4. 7 16
1,080,402
220.073
1 ,416,500
791.138
-
1 .621 .444
6,128
4.005
323.673
-
208,100
14,143
51,932
164. 2~4
1.238.850
948.987
765.620
544,873
30,055
Not shown
5 . '02
1.438
178
46,487
44.470
6.076
1.583
•
23,302
301
9.661
34.091
2 . 289
-
■
9.194
1.092
18.992
3.217
1.726
29.507
-
2.169
1.018
13.941
44
4.586
1.107
-
-
698
497
22.190
J7.707
12.603
9.646
6,612
4.632
115. 008
404
68.952
966
2,040.643
1 ,891 . 143
97.044
2.301,094
2.234,127
47.632
un. 7m
136.139
128.156
5.848
76.370
•
1.784
Sept., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
703
Argentine Imports of Chemicals and Allied Products (Concluded)
Chemicals, Drugs,
Dyes, Medicines 1913 1915 1916
Bisulfite $ 9,843 $ 12,114 $ 3,479
Borate 4,225 2,928 2,571
Carbonate, crystals 152,403 83,890 41,129
United Kingdom 140,339 79,759
United States 2,797
Caustic 375,768 308,987 336,590
United Kingdom 325,717 151,133
United States 14,375 155,596
Hyposulfite 17,151 8,790 13,050
Nitrate of 18,776 47,352 17,365
Salicylate 24,582 1,503 6.232
United States 10 1,063
Solvay 186,500 180,787 145,453
United Kingdom 177,161 170,441
United States 838 2,326
Silicate 143,711 134,983 83,486
United Kingdom 136,661 131,262
United States 1,073 1,859
Sulfide 36,608 49,227 20,768
Germany 28,945 843
United States 39,951
Sulfur 97,067 85,975 135,181
Italy 91,000 78,213
United States 693 .6,040
Sumac 360 510 1,049
Oils and Greases:
Total Imports 22,946,654 34,875.377 18.527,909
Italy 2,664,495 2,120,068
Mexico 1,285.227 14,544,651
United States 15,188,993 15,856,670
Cottonseed Oil 1,141,668 1,480,186 432,256
United States 1.129,282 1,459,560
OliveOil 4,153,451 3,753,360 3,394,291
Italy 2,577,166 2,050,663
United States 171,271 182,901
Kerosene 1,975,220 1,361,990 1,247,453
United States 1,974,446 1,361,964
Lubricating oils 2,465,213 1,824,438
United States 1,400,894 1,472,266
Naphtha; raw petroleum 11,514,226 24,706,323 8,280,672
Mexico 1,280,160 14,544,651 (incomplete)
United States 9,857,766 10,145,593
Paraffin 93,018 837,363 453,983
United States 36,248 802,572
Vaseline 48,082 51,214 59,393
United States 35,432 48,393
Miscellaneous :
Explosives:
Blasting powder 52,559 16,768 8.939
United States 7,634 5,744
Dynamite 55,776 26,128 41.363
United States 3,939 272
Gunpowder 670,703 243,733
United States 303,629 166,411
Glass:
Sheet and plate 2,037,529 725,730 734,442
United States 17,478 190,734
Other manufactures 2,603,046 495,493 462,012
United States 142,531 77,878
Paints, Etc.:
Varnishes 461,164 307,259 392,045
United States 71,695 65,258
Paints, colors, dyes, lacs.
inks, varnishes:' 2,446,697 1,392,897 1.658,371
United Kingdom 1,047,723 727,070
United States 276,638 388,720
Paper:
Paper and cardboard 5,800,948 3,800,475 5,006,201
Germany 2,792,937 499,523
United States 828,488 1,324,426
Manufactures of paper... . 3,754,468 1,818,987 1,977,645
Germany 1,140,869 209,117
United States 164,213 195,628
Soap:
Common 225,218 203,541 221,077
United States 25,540 21,664
Medicated 312,608 127,382 140,583
United States 223,654 116,101
Perfumed 98,855 75,485 116,049
United States 8,099 17,247
1 This confusing total includes aniline dyes, indigo and varnishes
stated separately above.
The progress made by American exporters in the
Argentine chemical markets can be traced readily
enough in the following table, which is compiled from
official American statistics. These are based upon
wholesale values in this country at time of shipment,
which means, of course, that the increases shown are
due in part to advanced prices. The most striking
increase has been in paper. While the sales of soda
were encouraging in 1017, it should be noted that this
item was not stated separately in 1014. These figures
are for the fiscal years 1914 and 191 7:
American Products Sold in Argentina
Articles
Asphaltum:
Unmanufactured
Manufactures of
Blacking, shoe paste, etc
Candles
Celluloid, and manufactures of
Chemicals, drugs, dyes, medicines:
Acids:
Sulfuric
All other
Alcohol, wood
Baking powder
Bark, extract for tanning
Calcium carbide
Copper sulfate
Dyes and dyestuffs
Lime, acetate of
Medicines, patent or proprietary. . .
Petroleum jelly
Roots, herbs, etc
Soda salts and preparations of '
Sulfur (brimstone)
All other
Chewing gum
Explosives:
Cartridges
Dynamite
Gunpowder
All other
Fertilizers
Glass and glassware
Glucose and grape sugar
Glue
Grease :
Lubricating
Soap stock and other
India rubber, manufactures of
Ink:
Printers'
All other
Leather, patent
Metal polish
Naval stores:
Rosin
Turpentine, spirits of
Oilcloth and linoleum
Oils:
Animal
Mineral:
Crude (including all natural oils) .
Refined or manufactured:
Gas oil and fuel oil
Illuminating
Lubricating and heavy paraffin
Naphthas:
Gasoline
All other
Residuum (including tar)
Vegetable:
Corn
Cottonseed
Linseed
All other
Volatile:
Peppermint
All other
Paints, pigments, colors, varnishes:
Dry color
Ready-mixed paints
Varnish
White lead
Zinc , oxide of
All other
Paper and manufactures
Paraffin and paraffin wax
Perfumeries, cosmetics, etc
Photographic goods:
Motion-picture films
Other sensitized goods
Soap:
Toilet
All other
Wax, manufactures of
1 Not stated separately in 1914.
The only Argentine contributions of prime im-
portance to America's present chemical needs are
quebracho and flaxseed. About 117,000 metric tons
of tanning extract were produced in Argentina and
Paraguay during the calendar year 19 17, practically
all of which was exported. The potential output
was estimated at 230,000 tons, shipping difficulties
and low prices being assigned as the reasons for low
actual production. One company exported 102,000
tons of extract. Ninety-five thousand tons of logs,
equal to 25,000 to 30,000 tons of extract, were shipped
90,043
$ 16,453
1,148
9,698
49,187
86,893
21,772
7,836
74,575
1,035
271
180,905
109
40,819
54.309
17.032
242,784
197.986
73,244
124,128
262,563
4.500
382,135
502,705
36.127
39,108
15,719
16,326
684,905
1,176
53,007
257,734
1,853,017
4,068
6.839
194,555
265,445
10,671
1 1 , 664
2,656
82,600
12,573
86,153
210
91,173
605,476
140,998
93,170
392
5,490
102,345
57,231
17,789
21,330
120,520
1,818,511
17,506
166,282
2,790
20,921
338,805
336,128
23,833
8,715
506 , 260
808,809
271,000
200,271
39,668
109,686
934
4,852
593,594
542,012
102,442
253,865
687,358
1 ,559,989
789,185
1,266,175
337,647
720,118
310,889
2,479,760
7,035
4,372
9,412
38,336
168,127
404,782
718
5,599
104,460
62.339
632
25,143
9,301
165,949
78,024
35.492
22,253
55.902
5,945
148,118
21,222
54,896
203,581
584 , 669
3,331,254
21,483
186,469
67,239
111,382
19,492
373,472
35,033
174,751
261,712
183,369
58.377
94,339
1,611
47,832
7°4
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol.
No.
to the United States during the calendar year 191 7,
according to advices from Argentina.
A recent attempt, originating in the United States,
to stimulate the production of linseed oil in Argentina
and thus economize in the tonnage now required for
flaxseed, has apparently failed. Several reasons are
assigned for the inability to increase the oil output, the
most important of which are lack of machinery, lack
of containers, and the absence of any important local
demand for the cake. The small quantity of oil now
produced is sold most profitably in Argentina, Brazil,
Chile, and South Africa. Some of the small mills
prefer to take advantage of the present demand for
edible oil. These reasons seem conclusive enough.
The following table of imports from Argentina
covers the fiscal years 19 14 and 191 7:
Argentine Products Sold in the United States
Akticlbs 1914 1917
Antimony ore
Bismuth
Blood, dried
Bones, hoofs, and horns
Chemicals, drugs, dyes, medicines:
Argols
Extracts for tanning:
Quebracho
All other
Glycerin, crude
Lactarene, or casein
All other
Copper ore
Dyewoods in crude state
Fertilizers
Hide cuttings and other glue stock.
India rubber
Mica
Oils, essential
Oleo stearin
Oil seeds:
Castor beans
Flaxseed
Tanning materials, crude:
Quebracho wood
All other
Wax, beeswax
96
469
373
077
313,785
398 , 893
.441
083
5,198.667
39
129
6
811
538
63
126
289,476
948.635
3,943
26,416
330
116
040
545
346,159
234.101
185
596
82,269
26,282
899
603
840
1 ,180,447
817
17.968
The great wealth of Brazil lies principally in her
coffee and rubber, although cotton, sugar, tobacco,
matte, rice, cacao, cereals, nuts, gold, diamonds, iron,
manganese, monazite sand, marble, and live stock all
represent industries that have an important part in
the economy of the nation. The mineral resources
are apparently without limit but have barely been
scratched.
There are no great manufacturing industries in
the sense that we know them, but the war has greatly
stimulated the domestic production of textiles, soap,
sugar, and a number of other products. Water
power seems in some districts to have solved the fuel
problem, and has even made possible a rather im-
portant calcium carbide industry. The impossi-
bility of getting supplies of caustic soda has recently
threatened some of the growing industries and the
Government has come to the rescue by subsidizing
the production of that chemical. Factories will
probably be operated in Rio de Janeiro, Bahia, and
Santos, where electric power and ample supplies of
salt are available.
A study of the following table will reveal the more
ting facts about the Brazilian demand for chem-
icals and allied products and about the normal sources
of the supplies imported. The insignificant part
played by the United States before the war is at once
apparent.
Of the articles usually classified as chemicals, soda
in various forms, but particularly caustic soda, is
the most important import. It is used in a number
of growing industries, especially in soap making, and
was formerly imported chiefly from England. Re-
cently it has been purchased almost exclusively from
the United States, but export restrictions and other
difficulties have interfered with supplies to such an
extent that the Government is endeavoring to estab-
lish a domestic industry, as already stated.
Imports described as "Chemical Products and
Medicines Unenumerated" were valued at nearly
$5, 000, 000 in 1913 and at considerably more than
$6,000,000 in 1916, but there is no way of finding out
just what items make up the class. Patent and pro-
prietary medicines are undoubtedly the most im-
portant item, and the United States has obtained a
fair share of that business.
Brazil followed the lead of other countries in pur-
chasing dyestuffs from Germany before the war, but
now depends upon the United States. As the second
table shows, more than $1,200,000 worth of dyes were
purchased from the United States during the fiscal
year 191 7. This demand will grow as the dye-
using industries, especially the textile industry, ex-
pand.
More than a million dollars worth of perfumes was
purchased in 19 1,5, practically all from France, but
in this connection there is a most interesting item
entitled ''Perfumery for Carnivals," purchases of
which amounted to more than $400,000 in 1913.
Swiss manufacturers had a monopoly on the business,
but inability to deliver cut down the imports to
$41,000 in 1916. Can "carnival perfumes" be made
in America?
Brazil needs important quantities of paper and
this is one line in which the United States has ef-
fectively supplanted the German business, for the
time being at any rate. It is gratifying to state that
American exporters have on the whole made a good
impression and have rapidly adapted themselves to
the conditions of the market. It is to be hoped that
circumstances will permit their carrying on the busi-
ness throughout the war so that they will be in an
advantageous position when the old competition re-
turns.
Mineral oils are imported in considerable quantities.
and in that line America, as usual, is supreme.
In studying the accompanying table it should be
borne in mind that the Brazilian Government does
not compute import values on the same basis on which
we compute export values: hence there will be dis-
crepancies between values in the first and second
tables. The first table should be used as a guide for
determining the relative importance of imports and
of the principal sources of supply.
Sept., 191S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
705
Brazilian Imports of Chemicals and Allied Products
Chemicals, Drugs, Dyes,
Medicines 1913 1914 1
Acids:
Acetic , $ 53,823 $ 33,440 $ 12
Germany 24,193 15,702
United States 141 303
Brazilian Imports of Chemicals and Allied Products {Concluded)
Nitric
Germany
United States.
Sulfuric...".
Germany
United States..
Tannic
Germany
United States.
All other
France
Germany
United States..
Aniline Dyes
Germany
United States.
Calcium Carbide.. .
Norway...
United States. .
Capsules, Pills. Globules, Med-
ical
France
United States
Chemical Products and Medicines.
Unenumerated
France
United States
Chloride of Lime
United Kingdom
United States
Essences and Oils, N. E- S. , Fixed
Liquid, Volatile
Germany
United States
Ethyl Chloride
France
Germany
United States
Extracts, Vegetable, N. E. S..
Italy
United States
us, Resins, Natural Balsams.
Germany
United States
Glycerin
United Kingdom
United States 1
Indigo and Ultramarine Blue.
Germany
United States
Perfumery. Other. . . .
France
United States . . .
Potash, Caustic
Germany
United States...
Soda Ash
United Kingdom
United States
Soda, Caustic
United Kingdom.
United States. . . .
Soda, Nitrate of
United Kingdom.
United States... .
Oils and
Benzine
France
United States.
Cod-liver oil and
Norway
United States
inseed oil
United Kingdom
United States
137,534
33,372
57,600
1,364
426,568
235,586
35.801
50,931
14,899
26,658
4,903,654
1,706,481
427,919
59,500
41,563
525
3,804
1,520
2,247
36
119,090
79,455
299
136,704
42,448
3,032
5,646
2,331
789
90,015
37,971
105
1 .141 ,553
928,979
55,296
250,448
236,989
662
512,402
491 .820
3,437
18.537
4.603
5,586
24,984
1 0 , 099
7,413
829,670
730,296
1 . 863
23,171
1 2 , 007
393
4,781
2,285
119
74,639
7,682
29,132
6 . 235
335,777
158.404
58.308
29,377
7,902
13,171
3,087,189
1,098,884
314.097
26,689
17,514
1,115
91,074
50,272
790
48,827
27,326
2,266
89,579
23,585
1,330
570.844
484,512
25,328
64.356
49,171
606
3,994
2,642
244
13,588
3,413
6,242
462.390
403,74(1
5,445
44 . 366
183,681
,646.549
.838,493
712,825
Oils and Waxes
Lubricating oils, mineral
vegetable
United States
M
1 fuel oil. .
United States
Olive oil
Italy
United States.
Palm oil
British India..
United States.
Paraffin
United Kingdo
United States.
Vaseline
Germany
United States
Glass and Glassware
Sheet and plate glass
Belgium
United States
lanufactures of gla
Germany
United States . . .
Paper and Ma;
Total imports ...
Germany
United States
SI, 591, 470
1,065.144
$1,065,488
803,242
$1,851
.751
208,646
114,789
89.907
451,785
322,316
128,597
1,370
659
1 .788,941
638,950
80
1 .585,747
692,525
9
1.794
,890
201 ,968
56,464
812
149,598
42,243
1,264
105
,618
79,266
35,460
15,628
64,997
33,815
16,478
142
374
48,102
13,145
13,134
27,688
6,595
9,482
55
604
750,662
437,416
6.490
292,687
154,380
2,456
771,
692
1 .995,800
1 ,083,064
120.602
727,913
327,890
56,942
511,
154
7,342.182
2,540,920
516.933
4,321,000
1,469.808
283.296
8,062,
971
The principal chemicals exported to Brazil by the
United States are dyes, soda, medicines, acids, and
copper sulfate. Only time can tell whether our present
hold on the market for these products is to be perma-
nent. Of the products sometimes classed as "allied
chemical products," the United States is at present
supplying in considerable quantities mineral oils, paper,
naval stores, india-rubber manufactures, explosives,
and glass.
The following table, compiled from official American
statistics for the fiscal years 1914 and 1917, will give
an idea of how the war has affected the chemical trade
between the United States and Brazil. Some of the
increases may be ascribed to the present prosperity
of Brazil, but for the most part they represent gains
that have been made as the result of the withdrawal
of European competitors.
American Products Sold in Brazil
Articles 1914 1917
Aluminum and manufactures
Asphaltum and manufactures
Babbitt metal
Blacking, shoe paste, etc
Celluloid and manufactures
Cement, hydraulic
Chemicals, drugs, dves, etc.:
Acids:
Sulfuric
All other
Baking Powder
Bark extracts, tanning
Calcium carbide
Copper sulfate
Dyes and dyestuffs
Lime, acetate
Medicines, patent or proprietary
Petroleum jelly
Roots, herbs, barks
Soda salts and preparations1 . . .
Sulfur (brimstone)
All other
Explosives:
Cartridges, loaded
Dynamite
Gunpowder
All other
Flavoring extracts and fruit juices
German silver
Glass and glassware
( -lucose
Glue
5.595
$ 106.227
80,291
11,612
21,413
19,093
25,235
41,330
5.498
5 1 , 800
200.337
426,166
1,363
17,437
4 . 569
144,497
6,456
19,913
8,136
32,236
31,743
2.448
126,254
65
1,203,140
4,600
248.617
315.392
9,595
42,191
10,569
1,063,476
53,273
84,579
2.519,396
287,600
570.824
14,835
45.944
51,730
3,726
304 , 803
1 .634
14.413
4.695
0,492
455 , 872
498
18,248
731
8,173
1,903
<,, ,04 1
1 ,120
9,990
Not stated separately in 1914.
706
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 9
American Products Sold in Brazil (Concluded)
Articles 1914 1917
India rubber, manufactures of $ 119,272 $1,154,381
Ink: 14,743 69,501
Leather, patent 41.612 352,318
Metal polish 26.925 13.357
Naval stores:
Rosin 673,687 975,044
Tar, turpentine, pitch 3,302 3,153
Turpentine, spirits 154,288 165.523
i >i! doth and linoleum:
For floors 142 10.597
All other 5,644 30.155
Oils:
Animal 2,216 2,613
Mineral:
Gas and fuel 54,412 95,451
Gasoline, etc 1,311,024 1,429,143
Illuminating 3,231,668 2,942,326
Lubricating, etc 659 , 352 886 , 542
All other 2,630 2.214
Vegetable:
Cottonseed 191,781 70,080
Linseed 2,793 154,272
Volatile or essential 3,108 31,593
Allother 601 59,687
Paints, pigments, etc.:
Dry color 5,642 35.001
Ready-mixed paints 44 , 679 85 , 393
Varnish 30.057 82.738
Zinc, oxide 64 . 522
All other (including crayons) 45.641 197,322
Paper and manufactures 499,393 2,419,287
Paraffin and paraffin wax 18,498 72,213
Perfumery 15,818 133,350
Photographic goods:
Motion-picture films:
Exposed 1.900 122,006
Unexposed 10,575 5,533
Other sensitized goods 32,417 110,229
Plumbago and manufactures 1,259 21,475
Salt 1.050 77
Soap:
Toilet 37,322 22,637
Allother 3,728 12,573
Sugar and molasses:
Sirup 65 405
Refined sugar 284 159.207
Vulcanized fiber and manufactures 109 8,082
Wax and manufactures 4,043 5,777
Brazil is making only two important contributions
to our war-time industries — rubber and manganese —
but they are vital. The demand for rubber has meant
a great deal to Brazilian prosperity, as pre-war com-
petition from the cultivated East Indian rubber had
placed the Brazilian industry in a precarious posi-
tion. The active demand for rubber has counter-
acted to some extent the depression resulting from
the diminishing demand for coffee.
Brazilian Products Sold in ti:e United States
Articles
Aluminum, crude
Chemicals, drugs, dyes, etc.:
Glycerin, crude
Gums
Lactarene
Soda, cyanide of
All other
Copper
Dyewoods in crude state:
Logwood
Other
Clue and glue size
Hide cuttings and other glue stock
India rubber, etc.:
Balata
India rubber
India rubber scrap
Manganese oxide and ore
Mica:
Unmanufactured
Cut . split, etc
Monazite sand and thorite
Oils, vegetable
Paper and manufactures
Platinum and manufactures
Seeds:
Castor beans
Allother
Wax:
Beeswax
ii'lc
4,382
16,3i9]048
466 \ 125
410
54 ! 329
94
292,597
594
10,248
38,059
14S.390
164.941
7.339
356
49,467
4,381
4,296
25.654,924
11.802
8,965,110
44,164
10,468
54,519
120.387
1,234
9.097
The preceding table shows in some detail the ex-
ports of chemicals and allied products from Brazil
to the United States for the fiscal years 19 14 and
1917.
URUGUAY
In size, Uruguay is the least of the South American
republics, but it is prosperous and progressive, for
the population is intelligent and wide awake. The
country is pastoral, however, with a recent leaning
toward wheat growing, and offers a limited market
for chemicals and allied products, as the following
table will show.
Must of the fluctuations noted in the table can be
traced readily enough to the war, but the falling off
in foreign purchases of sheep dip must be attributed
to the establishment of a local industry and the setting
up of standards that are rather difficult for outsiders
to attain. The Government is lending every en-
couragement to the domestic industry, as the product
is a very important one in a country that depends so
largely upon stock raising.
Statistics are given for the latest normal year for
which official Uruguayan figures happen to be avail-
able in this country and for the latest war year. The
valuations for these years are purely arbitrary and
should be used only as a general guide. The statis-
tics now being compiled for 191 7 are based upon
actual values and are said to be 30 to 150 per cent
higher than the arbitrary values heretofore used.
Uruguayan Imports of Chemical and Allied Products
Articles and Principal
Sources 1911 1915
Alcohol $ 1.934 $ 141.605
Argentina 1,448 140.939
Germany 276
Chemicals, Drugs, Explosives.. 752,490 823.548
Argentina 55.600 64,322
France 128,768 101.182
Germany 175.759 17,033
United Kingdom 228,948 205.979
United States 40.671 314.557
Glass and Glassware 494,459 156.426
Belgium 203,590 12.232
France 37.986 12.450
Germany 162,768 14.469
United Kingdom 56.530 40.829
United States 10,123 22.817
Oils. Edible 733,670 965,322
Italy 332.467 256.517
Spain 191,181 463.951
United States 158.375 198.751
Oils. Industrial (Not Including
Kerosene) 544.566 1.260.239
United Kingdom 43,308 63.360
United States 405,057 1,065.682
Kerosene 902.150 1.132.163
United States 887,019 1,094,275
Paper and Paper Wares 1.023.028 808.849
Belgium 220,389 27.381
Germany 317,255 35,238
■ i Kingdom 156,462 100.674
United States 98.468 189,850
Medicines. Proprietary 76.595 91 ,335
France 22.657 38.673
United States 21,794 19.857
Perfumery 153.696 86.681
France 98.515 5!
Germany 13.646 2.060
United King, loin 29,831 11,105
Sheep Dip 844.710 125.785
Argentina 60.485 17.778
United Kingdom 669.681 S9.356
United States 36.330 8.400
American statistics show that the sales of certain
chemical lines to Uruguay have increased since the
war started, but comparatively they are unimportant,
as a glance at the following figures for the fiscal years
1914 and 191 7 will show:
Sept., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
American Products Sold in Uruguay
Articles
Asphalt 11 m
Blacking, shoe paste, etc
Celluloid and manufactures
Cement, hydraulic
Chemicals, drugs, dyes, etc.:
Alcohol , wood
Baking powder
Bark extract for tanning
Calcium carbide
Copper sulfate
Dyes and dyestuffs
Medicines, patent or proprietary.
Petroleum jelly, etc
Soda salts and preparations1
Sulfur (brimstone)
All other
Explosives:
Cartridges, loaded
Dynamite
All other
Glass and glassware
Glucose
Grease :
Lubricating
Soap stock, and other
India rubber manufactures
Ink
Leather, patent
Metal polish
Naval stores:
9,003
286
3,632
Ko
Tar, turpentine, pitch
Turpentine, spirits
Oils:
Animal
Mineral:
Gas and fuel
Illuminating
Lubricating, etc
Gasoline
Other light
1 Not stated separately i
1917
$ 66,290
17,014
14,018
8,966
22,598
5,413
9,013
23,639
8,538
39,367
52,647
107,022
5,592
163,935 '
7,600
269,372
50,209
5^731
81,271
42,965
19,201
1,462
188,096
9,914
15,432
3,853
106,295 157,100
707
$ 62,416
147,425
6,806
3,011
14,954
32,612
25,839
13,112
35,316
56,610
40,067
10,946
2,612
10,948
17,796
1 1 . 240
15,824
809,056
48,651
291,828
20,675
467
4,976
713,945
92,978
47,253
413,774
American Products Sold in Uruguay (Concluded)
Articles 1914
Vegetable:
Corn J 13,978
Cottonseed 334,381
Other fixed , ' , ,
Volatile ! ! 388
Paints, pigments, etc.:
Dry colors 1 1 ,225
Ready-mixed paints 1 8 ' 750
Varnish 5|678
White lead 426
All other 103
Paper and manufactures:
Paraffin and paraffin wax 18,505
Perfumery, cosmetics, etc 12,240
Soap:
Toilet 6 .021
All other 8.783
In chemical lines Uruguay makes no important con-
tribution to the United States, as the following figures
for the fiscal years 19 14 and 191 7 show:
Uruguayan Products Sold in the United States
Articles
Bismuth
Blood, dried
Bones, hoofs, and horns
Fertilizers
Flaxseed
Glycerin
Grease and oils
Hide cuttings, and other glue stock
India rubber
Oleo stearin
Tin ore
4
1917
$ 4,067
751
50,803
304
110,401
141
124,684
24,032
8,520
16,520
748
83,851
53,015
28.705
70.078
ORIGINAL PAPERS
"JELLY VALUE" OF GELATIN AND GLUE
By A. Wayne Clark and Louis DuBois
Received April 23, 1918
The examination of samples of glues and gelatins
in this laboratory during the past ten or twelve years
has included a test which we have designated as
"jelly value." In making this test we have not fol-
lowed the common practice of the makers of these
products but have endeavored to improve upon it by
following a procedure which produces results that
can be expressed in absolute figures.
The system apparently in common use among the
makers seems to be to make up a jelly of definite con-
centration and compare its physical strength with
that of a standard sample.
The literature is exceedingly scant. Alexander1
in an excellent paper has fully explained his methods
and Fernbach2 also goes into the subject in consider-
able detail. It seems to us, however, that our meth-
ods result in a more scientific presentation of the
jelly-forming characteristics of these materials in
that they can be expressed in per cent figures. Our
practice has been to make up a series of glue or gela-
tin solutions of various known concentrations, cool
them until well set, and then slowly warm them to a
predetermined temperature and at that point note
which concentrations are solid and which are liquid.
We are then able to state that at a given tempera-
ture, the sample tested has a jelly value of, for in-
stance, 6 per cent, meaning that the 3 per cent, 4
per cent, and 5 per cent trials were fluid, whereas the
' "The Grading and Use of Glues and Gelatin," Jerome Alexander,
J. Soc. Chem. lnd., 26 (1906).
1 "Glues and Gelatin," Fernbach, D. Van Nostrand Co., 1907.
6 per cent, 7 per cent, and 8 per cent trials were solid.
This procedure obviates the use of all "shot tests"
or weighed devices for testing the physical strength
of a given jelly.
During the course of years in which these tests have
regularly been made, we have used different tempera-
tures for observing the setting of the water solution
of the various percentages tried. The results have in
many respects been quite unsatisfactory, until recently
we have been able to carry out a considerable number
of experiments to determine whether there might
exist a trial temperature at which such mixtures
show the best results. Our efforts have been re-
warded by the discovery that there is in such mix-
tures a very plainly indicated temperature-range
through which the "set" or "gel" of a definite con-
centration of solution is not changed. Our results,
in general, as might be expected, are more satisfac-
tory with gelatins than with glues and they are prob-
ably not as definitely useful in judging the strength
of glues as in judging the quality of gelatin.
10 a »■ 16 is zo zz z+ tie is Jo
As to the character and sources of the samples used
in obtaining the curves shown herewith, it will be
necessary to state as follows:
The material designated "Gelatin" is a product
708
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 9
i * t 8
10 a /■* it m zo zz z* zt ze jo
7emjotr*ri*re Cenltyrade
Ge/ol,n-Ed,b/c
Piles Coopers
J
S^ 'V.
~~
0 2 + 6 6 10 IZ 14- /C 18 ZO ZZ Z+ Zt Z8 JO
Ttrrtperoturt Ceit/yac/e
e
t<
MifeG/ue
f*
— " f%
j-jj
C5
z
far.
0
fi7.
OvBcs
0 Z f- 6 8 10 IZ I* It /« Zo ZZ
Temperature Centigrade
regularly used in manufacturing processes and, as
far as we have been able to ascertain, is of American
manufacture. It is purchased from one of the most
reputable of American manufacturers.
The "Gelatin Edible, Knox's," the "Gelatin Edible,
Cox's," and the "Gelatin Edible, Peter Cooper's"
were purchased in grocery stores for purposes of ex-
amination, as being reputable brands regularly on sale
for household use.
The so-called "White Glue" is simply a gelatin
which might be called gelatin-glue, carrying a cer-
tain amount of white pigment.
The "Brown Flake Glue" is a common commercial
variety used chiefly for the manufacture of paper
boxes and other similar purposes where strength is not
especially required.
The "Fish Glue" is a product about which wc have
complete information, as it is made in one of our own
departments for use in coating court plaster and corn
plasters where we are desirous of using a thoroughly
standardized product well boiled for purposes of de-
stroying pathogenic bacteria, etc. It is made from
fish-sounds by thorough extraction with boiling water
Followed by protracted boiling in the steam kettle.
This is then made into sheets and dried; in other words,
it is straight first-class fish glue.
The method of procedure is to have on hand a
sufficient number of ordinary 6-in. test tubes to in-
clude the range of percentages to be tried, each fitted
with a cork and graduated for 10 cc. Into each tube
is put a weighed amount of the granulated glue or
gelatin sample and to these cool water is added up to
■30
Brown Flake G/ue
r Jo%
Zt,
«
Jr z*7.
2f
ZZ
Z>
* **%
18
It
t
5'*
f I* 7.
,.
^_^r1o%
8
t
+
z
f'7.
fs-%
"7.
o^ 0ma
0 Z 4 ' 8 /0 IZ 14- IC /8 £0 11
"Temperature Cerrriorad&
the 10 cc. mark. A glass rod is now put into each tube
and the contents stirred occasionally during several
hours, after which the tubes are allowed to stand in
boiling water until the sample is completely dissolved.
The rod is now removed and the tubes tightly corked
so as to avoid the formation of a skin on the surface
of the solution when it cools. These tubes are then
cooled considerably below the temperature at which
the observation is to be made. They are then stood
in water, which is allowed very gradually to come
up to the desired temperature. Observation of the
"set" is now made by tilting the tube to observe
whether or not the jelly is solid. Naturally, this point
is not absolutely accurate, but with tubes of uniform
diameter the judgment of the "set" or "gel" is reason-
ably easy to make. It will be observed that this
per cent is based on the weight of the solid and the
volume of the liquid, as is usual under such conditions.
As a result of this investigation, it is evident that
for practically all of this work a temperature of 10 ° C.
iZ
Fish Glue
Inf.
iff
10
Johnson I Johnson's
f ie%
e
— Ice*.
N
X™
u
/tf.
cf>
z
/^*3&
■ *"5x
A«w.
>o tz # /* a zs zz £f zt z* -»
Sept., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
709
is the most valuable for comparative purposes. For
instance, on the sample represented by the curve
marked "Gelatin," it will be observed that the range
of temperature between the points of liquefaction of
the 1 per cent and the 2 per cent mixture is about one
degree; also, that between 4 per cent and 6 per cent
concentration it is about one degree, while between
2 per cent and 3 per cent the temperature range is
about 180. While in this particular instance the 10°
point is no more valuable than the 16 ° poirit for a
standard jelly-value temperature, yet taking this
curve in conjunction with the others illustrated here-
with, it will be seen that io° C. is a good average work-
ing temperature-point for observation of the entire
line of glues and gelatins.
Rssearch Laboratory
Johnson & Johnson
New Brunswick, N. J.
A NEW METHOD FOR THE QUANTITATIVE ESTIMATION
OF VAPORS IN GASES
A DIFFERENTIAL PRESSURE METHOD
By Harold S. Davis and Mary Davidson Davis
Received March 27. 1918
INTRODUCTION
In a former paper1 a new form of tensimeter was
described for measuring the partial pressure, in a
mixture of inert gases, from any liquid or from its
solution in a nonvolatile substance.
The ease with which these experiments could be
carried out led us to experiment with modified forms
of this apparatus, having in view the development
of a method for the estimation of small quantities of
vapors in inert gas mixtures.'2
THEORY OF METHOD
According to the principle often referred to as Dal-
ton's Law of Partial Pressures, the vapor pressure
from a liquid is independent of the kind of gas above
it, provided the gas is inert. Deviations from this
law are well known, but it holds with surprising ac-
curacy in the case of a mixture of benzene and air
at atmospheric pressure, as has already been shown
by one of us.1
Consider two closed flasks connected, as in Fig. I,
by a manometer and filled with air at atmospheric
pressure. If now a small sealed bulb containing a
volatile liquid be broken in each, the liquid will partially
evaporate, and if the temperatures of the flasks re-
main the same, the same additional pressure will be
developed in each, so that the manometer connecting
them will register no difference in pressure. Even if
the temperatures of the flasks do vary, no difference
in pressure will be recorded until there is a relative
difference in temperature between them.
Now suppose that one of the flasks had contained
a certain quantity of the vapor of the volatile liquid
corresponding to a pressure less than the saturation
1 "The Extraction of Aromatic Hydrocarbons from Gases by Means of
Liquid Absorbents." Harold S. Davis, University of Manitoba Publications,
February, 1917.
J Most of the work was done during the early part of the summer of
1917 and the results under the same heading as that of this paper were
given to the Canadian Advisory Council and to the Imperial Munitions
Board of Canada. United States Patent No. 1,272,922 on this method
was issued July 16, 1918.
pressure. When the small bulb of liquid was broken
in this one, the liquid would not add all its vapor
pressure to the pressure already in the flask, for part
of that was already due to its vapor. It would add
only the amount of pressure necessary to bring its
pressure up to saturation; and since the total satura-
tion pressure was added to the pure air in the other
flask, the manometer connecting the two would regis-
ter a pressure equal to the pressure of vapor in the
original gas.
Two important points should be noted here:
i — The partial pressure of any particular vapor in
a sample of gas is independent of the temperature
of the gas, provided that the total pressure on the
gas remains constant while the volume can change
with the temperature, and provided the vapor remains
always unsaturated and obeys the simple gas laws.
2 — The difference in pressure developed between
the two flasks, one of which contains air and vapor,
and the other air free from vapor, will vary as the
absolute temperature, provided the relative tempera-
tures of the flasks remain the same ; that is, for prac-
tical purposes, the difference in the pressure is inde-
pendent of variations of temperature.
An apparatus constructed on this principle will,
therefore, measure a definite quantity, viz., the pressure
of the vapor in a gas at any particular gas pressure.
The differential pressure which develops between
the two flasks is equal to the original partial pressure
of the vapor in the gas, when the total pressure on
the gas is equal to the atmospheric pressure at the time
of the experiment. This can be reduced to standard
conditions in the following way:
Let P be the atmospheric pressure at the time of
the experiment.
Let P0 be normal atmospheric pressure = 76 cm. of
mercury.
Let X be the differential pressure developed be-
tween the flasks.
XP
Then ° is equal to the partial pressure of the
vapor in the gas when the total pressure of the gas is
XP
P0. As was pointed out before, the value — — is
independent of the temperature provided every com-
ponent of the gas remains unsaturated.
In a similar way the total of the partial pressures
of two or more vapors may be reduced to its value
for a total standard pressure on the gas.
However, though this partial pressure of a vapor is
independent of the temperature, the actual weight
of the vapor contained in unit volume of the gas de-
pends on the temperature. For one vapor this may
be calculated from the partial pressure on the assump-
tion that the vapor gives the same partial pressure
as it would if it were a true gas at that temperature
and molecular concentration.
SOURCES OF ERROR
1 — The permanent gases in one of the flasks may
dissolve in the liquid to a greater extent than those
in the other flask and thus lower the pressure on that
side.
7io
THE JOURNAL OF INDUSTRIAL AN D'liNGI N EERINC CHEMISTRY Vol. 10, No. 9
2 — The dissolved gases may lower the vapor pressure
of the liquid to a greater extent in one flask than in
the other and thus decrease the additional pressure
developed in the former.
3 — If there are other vapors present, these will
partially dissolve in the liquid in the bottom of the
flask, and thus their own partial pressure in the gas
will be less, while, in addition, the vapor pressure
from the liquid will be lowered.
If the gases in the two flasks are the same, these
errors are negligible, for the only error is caused by
the gas in one flask being at a slightly higher pressure
than the gas in the other so that more of it will dis-
solve in the liquid. If, however, the gases are not the
same, only careful experimentation will show the
magnitude of the errors.
It is not necessary that the substance in the sealed
glass bulbs should be in the liquid state, for, in the
case of a substance which can exist as a solid under
the conditions of the experiment, it is of course possi-
ble to estimate the amount of its vapor present in
the gas by the same method. We have actually
estimated quantities of benzene in gases at tempera-
tures lower than 5°, using bulbs filled with frozen
benzene. This will be described in another paper.
A solution which has a vapor pressure of the particu-
lar substance to be estimated greater than that actually
in the gas could be used under certain conditions.
EXPERIMENTAL PART
The apparatus used is of the form shown in Fig. I.
Into the ground glass stopper of each of the flasks
tubes are sealed; one of these terminates about 1 cm.
above the stopper and through it a metal rod passes
to the bottom of the flask, projecting above the stopper
to a distance of 10 cm. The upper end of this rod is
screwed into a short piece of metal rod of larger diam-
eter. Over this rod, and extending down over the tub-
ing which projects above the stopper, is slipped a
piece of tightly fitting, rubber pressure tubing. The
rubber joints are made tight by means of vacuum
grease and wire. The second tube passing through
the stopper is closed at the upper end by a stopcock.
It simply provides a means for the passage of gases
into or out of the flask and can as well be sealed into
the side of the neck of the flask or the upper part of
the manometer tube. In later work we have used it
sealed into the manometer. To the bottom of the
metal rod a small glass bulb is attached by means of
small soldered supports and fine copper wire. This
bulb, which has a thin bottom, contains sealed up
inside some of the liquid whose vapor is to be esti-
mated. By pushing down the rod at the proper time,
or giving it a slight tap, the bulb at the end can be
broken, thus liberating the liquid it contains. The
rubber tubing then draws the rod back into place.
The left flask is filled with the gas to be examined,
at a pressure slightly above atmospheric. When the
temperatures of the gases in the two flasks become the
same, their pressures are equalized to that of the atmos-
phere by opening the stopcocks, which are then
closed. This step is necessary if the temperature of
the room or thermostat in which the experiment is
being done varies to any extent.
Next, the small sealed bulbs containing the liquid
are broken by pushing on the rods and the ap-
paratus is allowed to stand, with an occasional shak-
ing, until the manometer levels cease changing. The
time required to reach equilibrium is 10 to 15 min.
and 30 to 60 min. for flasks of 140 cc. and 340 cc.
capacity, respectively. In routine work it is possi-
ble to hasten the evaporation of the liquid by heating
the flasks, either gently with a flame or by immersion
in a warm bath. In such a case it is necessary to guard
against a leak through the extra pressure developed.
Two corrections must be applied to the difference
in the mercury levels to obtain the true difference in
pressure:
1 — Reduction of the mercury height to 0° C. This
can usually be neglected.
2 — Correction for the increase in volume in the
right-hand flask and the decrease in volume in the
left-hand one, due to the movement of the liquid in
the manometer tube. If, however, the flasks are
fairly large and the bore of the manometer tube small,
this correction can also be generally neglected.
Unfortunately it was impossible, at first, to obtain
satisfactory apparatus and much of the following ex-
perimental work had to be done with flasks closed by
corks instead of glass stoppers. Rubber stoppers can-
not be used as they rapidly absorb benzene vapor
and so cause serious errors. If the corks are boiled in
soft paraffin they will hold a vacuum fairly well but
arc much inferior to glass stoppers. A little soft
paraffin on the stoppers makes gas-tight joints, and to
hold them securely in place thick rubber bands are
slipped over their tops and fixed to small catches on
the necks of the flasks.
Sept., 1018 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
In the first part of this work we introduced the gases
into the flasks by simple displacement, but it is sur-
prising how much gas is needed to completely dis-
place the air from even a small flask and most of our
troubles arose from overlooking this fact. About 5
liters will displace nearly all the air from a 300 cc.
flask. We have since devised a slightly modified
form of apparatus (Fig. II) which is filled by first
evacuating the flask and then attaching to the gas
supply. As will be seen,
in this form the two
flasks are close to-
gether, and the manom-
eter tube is led out
in front from them, so
that the flasks may be
placed in a bath of
any kind while the
manometer remains
outside. Further, there
is a stopcock above the
mercury in the manom-
eter tube on the side
nearest the flask to be
filled with the gas to
be analyzed. This
stopcock is closed be-
fore evacuating the ^
flask. It allows the
whole apparatus to be
inverted without losing the mercury in the manometer
tube.
The evacuation is carried out by a water pump
which rapidly reduces the pressure to less than 1 cm.
of mercury. The residual pressure is measured by a
manometer in series with the pump. With this form
of apparatus only a small quantity of gas need be col-
lected for analysis. It can be kept, until required,
in a small gas holder from which it is displaced into
the apparatus by mercury. We have used gas hold-
ers of 300 cc. capacity with stopcocks at both ends.
When one experiment is completed, the apparatus can
easily and rapidly be cleaned for the next by drawing
hot air through it.
Fig. II— Side View Modified Form of
o
=0
o
=0
Fie. Ill
Naturally, in order to avoid fracture, the determina-
tion flasks should be of good uniform thickness, espe-
cially near the bottom where the little bulbs are broken.
We have also lessened the danger of breakage by
placing a thin piece of lead in the bottom of each
flask. These precautions are useful when the bulb
contains a solid, but when dealing with a liquid one
need never break the bottom of a flask if the little
sealed bulbs containing the liquid are made as shown in
Fig. III.
The bulb is blown from a piece of glass tubing,
preferably of a diameter not less than 0.8 cm. Our
experience has been that if smaller tubing is used,
bubbles form in the glass when it is blown; this may,
however, be due to incorrect methods of procedure.
This tubing, 1, is first drawn out as in 2 and a slight
constriction made on each side, 3, for convenience
later in tying the bulb to the bottom of the rod (see
Fig. I). From 4 the round bulb 5 is blown and at
once its bottom is heated in a mild flame and blown
out in the form 6. Bulbs of this type will stand a
wonderful amount of usage but can be broken on the
bottom by a gentle pressure against any surface.
For filling, the neck of the bulb is bent in the form
7 and immersed in a narrow-mouthed vessel full of
the desired liquid. On heating gently at intervals,
the air is soon driven out, some liquid drawn over,
vaporized, and the whole bulb filled with liquid.
The liquid is now driven out from the capillary
and the bulb full of liquid is sealed off with
a small pointed flame at the point 7. In the
case of benzene and toluene we have used a small
naked flame for heating, and protected the flask by
wrapping with asbestos paper. In this way a bulb
can be filled in a few moments. Occasionally, one
explodes and takes fire without serious results. If de-
sired, one can work behind a glass screen. In the case
of more volatile substances a liquid bath for heating
and other such precautions could be used.
Another satisfactory method for filling the bulbs is as
follows: The vessel containing the desired liquid to-
gether with a number of bulbs immersed in it, as
shown in 7, are placed in a closed glass dish with a
removable top, such as a desiccator. Next the air
pressure in the desiccator is lowered by pumping out
the air and is again brought to atmospheric by opening
a stopcock. If this process is repeated a few times
the bulbs will be completely filled with liquid.
We have given this description in detail, but when
once mastered the manipulation is easy and two per-
sons with only moderate experience in glassblowing
can easily prepare twenty complete bulbs filled and
sealed in an hour, casualties not being counted.
At first, we performed all the experiments in a thermo-
stat with glass sides, the temperature of which re-
mained constant to a few hundredths of a degree;
but this is unnecessary. We have found it quite
easy to obtain accurate results in a room where the
temperature varied over several degrees.
Several samples of benzene obtained from well-
known firms were used; on being distilled they boiled
over constant to less than a tenth of a degree. Many
of the preliminary results are omitted.
We attempted to check the benzene content in
samples of air, containing known quantities of benzene,
made up in the following way: Measured volumes
of air, saturated with benzene vapor at a known tem-
perature, were drawn from a 500 cc. flask and diluted
with air over mercury. In the first 5 experiments
given below, a 140 cc. determination flask was filled
712
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. o
by displacement of air with about 500 cc. of the sam-
ple of air and benzene vapor. This was a quantity
far from sufficient to displace all the original air, and
the results are low.
In Expt. 6, the flask was filled by displacement
of mercury and the result is much better. In No. 7,
a bulb containing a known weight of benzene was
broken in a 5 liter flask slightly evacuated. Air was
then admitted and the whole shaken up well by means
of a small quantity of mercury in the bottom of the
flask. After this, a 340 cc. determination flask was
filled by displacement of air with the 5 liters of air
and benzene vapor which were driven over by dis-
placement with water.
PRELIMINARY RESULTS
Experimentally
determined
Cm. He
0.67
0.94
2.40
2.30
2.00
1.38
2.31
Calculated
Cm. Hg
0.85
1.06
3.00
3.00
2.60
1 .50
2.45
In the final series of determinations a weighed
quantity of benzene, less than that required for satura-
tion, was introduced directly into
the determination flask. This was
accomplished by means of a second
small, sealed bulb (Fig. IV) which
contained a weighed amount of ben-
zene. Its position could be regu-
lated by means of the attachment
screw A, so that on pushing on the
rod the small bulb broke, leaving
Fig iv tli,- larger one above it intact, to
be broken later.
In this way the actual pressure developed by the
weighed amount of benzene could be measured, and
the pressure could be checked by breaking the large
bulbs according to the method already described.
F1NAI RESULTS
A
1!
C
D
'crcentage
Pressure
difference
Pressure
measured
between
Percentage
Wt.
calc. from
Pressure
by new
B and
difference
of benzene
gas laws
developed
method
average
between
No.
G.
Cm.
Cm
Cm.
C and D
C and D
.. 0.0140
1.01
0.95
1.00
4.0
5.0
2..
.. 0.0204
1.43
1.46
1.46
2.0
0.0
3..
.. 0.0344
2.40
2.20
2.28
7.0
4.0
4..
.. 0.0618
4.32
3.79
3.80
12.0
0.2
5..
.. 0.0726
5.12
4.50
4.56
11.0
1.3
6..
.. 0.0763
5.34
4.48
4.54
16.0
1.3
7..
.. 0.0815
5.63
5.65
5.66
0.3
0.2
8..
.. 0.0819
5.64
5.11
5.29
8.0
3.6
9..
.. 0.0824
5.59
5.21
5.21
7.0
0.0
10..
.. 0.0839
5.91
5.50
5.41
8.0
1.7
11..
.. 0.0868
6.04
5.67
5.69
6.0
0.4
12..
. . 0.1015
7.02
6.42
6.41
8.0
1 .4
13..
.. 0.1175
8.20
6.73
6.74
18.0
0.3
Av.. 7.4 Av., 1 .5
DISCUSSION OF RESULTS
The agreement between the pressures of benzene
actually developed and those determined by tin new
method is satisfactory. The average deviation is
1.5 per cent, but bitter agreement could undoubtedly
have been secured by working in a thermostat, as the
temperature of the room varied considerably.
The differences between the pressures actually de-
veloped and those calculated from the weights of ben-
zene, the volume of the flasks being known, are fairly
large; mean deviation, 7 per cent. In each case the
pressure developed was less than the calculated.
These deviations maybe attributed to two causes:
1 — Impurities in the benzene and impurities col-
lected from the interior surface of the flask. These
impurities when dissolved in the last traces of benzane
might lower its vapor pressure until it would cease
to evaporate, being in equilibrium with the pressure
in the flask. Naturally this tendency would in-
crease as the amount of benzene pressure in the flask
increased.
2 — Divergence of the benzene vapor from the sim-
ple gas laws caused perhaps by polymerization, but
the results show that this effect is not very large for
pressures approaching saturation.
SUMMARY
I — A differential pressure method for the quantita-
tive estimation of vapors in gases has been described.
II — Experimental results are given of the trial of
this method for the estimation of quantities of ben-
zene vapor in air.
i ihi'artment op chemistry. i'niversity of manitoba
Winnipeg. Canada
THE APPLICATION OF THE DIFFERENTIAL PRESSURE
METHOD TO THE ESTIMATION OF THE BENZENE
AND THE TOTAL LIGHT OIL CONTENT
OF GASES
By Harold S. Davis, Mary Davidson Davis and Donald G
MacGregor
Received March 27, 1918
INTRODUCTION
It is unnecessary to dwell on the importance of
the aromatic hydrocarbons, particularly benzene and
toluene, at the present time, and on the necessity of
increasing their output in every possible way.
A great need has been felt, by those engaged in
the commercial production of these substances, for
methods of analysis requiring only small samples of
gas and giving a rapid estimation of the content of
these vapors either collectively or individually. Such
methods would make it possible to find the conditions
of production necessary to obtain the maximum con-
centration of each aromatic substance and would also
permit the efficiency of absorption processes to be
at every point.
A method widely used at present for the estimation
of these vapors requires the following steps:
i — Their absorption from a large measured quan-
tity of the gas by means of a suitable solvent.
2 — The distilling and fractionating of the solution
thus obtained according to a definite scheme of opera-
tion.1
The absorption process most widely adopted for
works purposes is the passage of the gas through a
train of wash bottles filled with absorbing oils.5
The technique of this process as widely used in the
United States has been fully described by F. W. Sperr.3
■ H. G. Coltnan, J. Gas Lishtins. 189 (1915). 314-315; H. W. James.
J. Soc. Chem. lnd.. SB (1"1
' R. Lessing. J. Sor Chtm. Ind.. SS (1917). 103.
> it*, and Chtm. E«f., 17 (19m. 548, 586. 642.
Sept., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Absorption processes of a different kind have been
proposed by R. Lessing1 and H. H. Gray.2
Other methods3 for the estimation of these vapors
in gases are based on the fact that the vapors condense
to liquids with negligible vapor pressures at low tem-
peratures, while the permanent gases do not.
In the preceding paper there is described a differ-
ential pressure method for the estimation of a vapor
in a mixture of inert gases.
The present paper4 embodies the results of investiga-
tions on the application of this method to the estima-
tion of a vapor in a mixture of other vapors and inert
gases. In particular, we have studied the applica-
tion of this process to the estimation of benzene and
of the total light oil content in coal gas or coke oven
gases.
RATE OF DEVELOPMENT OF THE DIFFERENTIAL
PRESSURE
We have investigated more carefully the rates at
which the vapor pressures are developed in the sepa-
rate flasks, after the bulbs containing the liquid or
solid are broken.
The rates of development of the vapor pressure from
liquid benzene at 18° and from solid benzene at 0°
were measured, with the results given below. About
1 g. of benzene was used in each case, in a 300 cc.
determination flask, without shaking.
Benzene
0iqu
id) 18.6°
Benzene
(solid) 0°
Time Pressure
Time
Pressure
Min. Cm. Hg
K
Min.
Cm. Hg
K
0 0
0
0
2 1.6
— o!o54
5
0.67
— o'.bh
5 3.5
—0.058
10
1.23
—0.035
9 4.9
—0.055
15
1.54
—0.035
23 6.85
— 0.056
25
1.90
—0.034
49 7.18(Pc
e) to
1
35
1.99
2.21(Pa
—0.028
0)
(fl) Px = saturation pressure at / = 00.
If the rate of development of the pressure is pro-
portional, at each instant, to the undeveloped pressure
in the flask, and if we represent the time in minutes
by / and the pressure in centimeters of mercury by p,
then:
dp
dt
stant).
-K(Pcc
/>)and-log (J — p )
K (a con-
1 J. Soc. Chem. Ind., 36 (1917), 103.
I J. Chem. Soc, 111 and 112 (1917), 179.
» St. Claire DeviUe, J. des Usints a Gaz, 1889; Lebeau and Damiens,
Compl. Rend., 156 (1913), 144, 325; Burrell, Seibert and Robertson,
U. S. Bureau of Mines, Technical Paper 104 (1915); Burrell and Robertson,
This Journal, 1 (1915), 669; H. F. Coward and F. Bailey, Manchester Lit.
and Phil. Soc, 24 (1916)
* After the work on the present paper was completed, the comprehensive
article from the U. S. Bureau of Standards on the "Recovery of Light
Oils and the Refining of Toluol" appeared in This Journal. 10 (1918),
51. In the same number of This Journal, p. 25, is an article by R. P.
Anderson on the "Determination of Benzene Vapor." This contains a
summary of the various methods which have been employed for the esti-
mation of benzene vapor in gases and proposes a method on which he has
done preliminary work. In this method the benzene content is to be es-
timated by measuring the increase in volume of the gas mixture when
placed in contact with liquid benzene. He also points out that fl sirn
ilar method differing only in detail had been developed by the Societe
Rouhaisiennc d'Eclairage par le Gaz and R R I. H. Fonicres For an
account of the specifications of the German patent on this method sec
J. Soc-Chem. Ind., 38 (1914), 129.
The actual value of K would depend on the condi-
tions of temperature, the surface of benzene exposed,
the volume of the flask, etc., which conditions must
approach constancy for any given determination.
As will be seen from the tables given above, the
values of K calculated in each case from the experi-
mental results are sensibly constant. It thus appears
that the pressure is an exponential function of the
time.
Consider a differential pressure apparatus contain-
ing air in each side, in which bulbs of benzene are
broken at the same time. The pressures will de-
velop exactly alike so that at no time is there any
difference of pressure indicated. Now suppose, on
one side, there is an original pressure of benzene.
Then a difference of pressure slowly develops. This
can be demonstrated to be an exponential function
of the time similar to that of the pressure in either
flask and it can be shown that at any time
Difference in pressures
Maximum difference in pressures
Pressure developed in either flask
Maximum pressure developed in that flask
This important result shows the great advantage
of the differential pressure method. Consider the
determination, at ordinary temperature, of the ben-
zene pressure in a sample of gas containing i cm.
pressure of benzene. When the benzene pressure on
each side is 95 per cent developed, the differential
pressure reading will be 0.95 cm. instead of the cor-
rect 1 . 00 cm., an error of 5 per cent. On the other
hand, if instead of the differential pressure method, a
method is used in which only one flask is employed,
and the pressure obtained by breaking the benzene
bulb is subtracted from the saturation pressure at that
temperature, the error is much greater. For now at
95 per cent saturation, the numerical value of the
error in the result is 5 per cent of the saturation pressure
(about 10 cm.) or about 50 per cent of the original
vapor pressure in the gas.
ESTIMATION OF BENZENE VAPOR IN THE PRESENCE OF
TOLUENE VAPOR
Our next work on this subject concerns the estimation
of benzene when toluene vapor is also present. A
known amount of toluene vapor was introduced into
the air of one of the flasks. Bulbs of benzene were
afterwards broken on each side. If now the toluene
did not dissolve in the benzene, the same benzene
pressure would be developed in each flask and the
manometer reading would not change. On the other
hand, if the toluene dissolved in the benzene to any
extent, the pressure developed in the flask containing
the toluene would be less than in the other.
We were well aware that the toluene would dissolve
in the benzene to some extent, but as the flasks used
had a capacity of 150 cc. to 350 cc. and as the quantity
of benzene used was less than 1 g. in each case, it
7i4
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. o
seemed probable that the toluene would not apprecia- this pressure, however, was developed in the first
bly dissolve out from the gas before equilibrium had 15 min., yet the flasks had not been shaken and the
been reached by the evaporating benzene. Other- liquid benzene lay undisturbed on the bottom. When
wise, the toluene would first have to diffuse from all it is considered that the difference in pressure was due
parts of the flask into the outer layer of liquid benzene to toluene dissolved in the benzene and that this
and then from this layer through the main body of toluene had to be absorbed out of the gas in a 300
the liquid itself. cc. flask into about 1 cc. of liquid benzene on the
Experiment has shown that these ideas were er- bottom, one cannot but be struck by the comparative
roneous; the toluene rapidly dissolved out from the speed of the process of absorption. It may well be
gas in the flask into the liquid benzene. It seems im- that it is not so difficult to wash these aromatic hydro-
possible that this should be due to simrile gas diffusion; carbons from gases as has often been supposed, a
it must rather be caused by convection currents in conclusion of great importance for industrial absorp-
the gas. We attempted to prevent such currents by tion plants,
surrounding the liquid benzene with fine copper
gauze, but without success. variations in the differential pressure, de-
„ , . r , c ., pending on the quantity of liquid used
Below are given summaries of a few of these experi-
ments, some performed at ordinary temperatures If the gas to be analyzed contains only one vapor,
and others at the temperature of melting ice. together with inert gases which are insoluble in liquid
The following points are to be noted in interpreting of the same composition as the vapor, the differential
f-jjg resi pressure developed will not vary with the amounts of
. . liquid used. On the other hand, suppose the vapors
1— The benzene bulb in the flask containing the of twQ completely miscible liquids are present_ If an
toluene was always broken first, so that the benzene attcmpt is made t0 estimate one of these vapors by
pressure was always a little higher on that side at the differential pressure methodi with bulbs containing
first. Accordingly, the toluene really dissolved out .^ ^^ the actual difference in pressurc developed
more quickly than would appear from the table. between the twQ flaskg ^ depend Qn thg amQunt
2 — The rates at which the difference in pressures of liquid used, as the following considerations show:
d( -eloped in the several experiments are not strictly _ ., . . . , , _
H v ...... Consider a mixture containing inert gases and two
comparable, because it was impossible that the in- , , . . . ,_. T _ . _
F ' * , ,, . vapors, benzene and toluene, for example. Let a
terval between the breaking of the bulbs should be ... , , u u 1 • u e *i a t_
s bulb of pure benzene be broken in each of the flasks
the same in each case, and that the contents of the , , _,, . , . »„:_:__
., ' ,. . . , . of the apparatus. Then in the one, A, containing
bulbs should be uniformly distributed on breaking. . .. , ,, ,.„„.„ ,„. ... +„^„„,0
' pure air, the full pressure of benzene for that tempera-
3 — In comparing the final differences in pressure, it ture is developed.
must be remembered that the magnitude of these de- In lhe flask B> containing the vapors and inert
pended on the amount of liquid benzene left in the gaseSj the following conditions exist at equilibrium:
flask. If this was large, the lowering of its pressure
caused by the dissolved toluene was small, and vice J-The toluene has dissolved in the benzene until
versa. This effect is discussed in detail later in the lts solution in the benzene gives a vapor pressure of
toluene equal to the residual vapor pressure of toluene
... .. , . in the gas.
4 — In the experiments in which solid benzene was
used, there was sufficient toluene present in the flask *~ The dissolved toluene has lowered the vapor
to cause the benzene in that flask to melt. pressure of the benzene.
Consequently a difference in pressure has been de-
v. p. of Developed between Flasks veloped between flasks A and B, made up of the fol-
Kind of Toluene Time in Minutes i„„.;„„ <•„„+„,,..
Material in Flask 1-3 3-6 7-10 10-15 20-30 60 80 lowing tactors.
No. Temp in Bulbs Cm. Cm. Cm. Cm. Cm. Cm. Cm. Cm. , . _,. . . , , . , ,. ,
1 22» Liquid benzene 2:37 o.30 0.74 1.54 i .90 2.41 .. .. (a) The original vapor pressure (unsaturated) of
2 24° Liquid benzene benzene in B.
surrounded by
3 B-uSaTiSi 2:05 0.80 .:20°:222:oo°:39 :: 2:ii (») The original pressure of the toluene vapor which
5 a'uSuWb™ °:45 :: o:i6°:39 :: o^oi'siloo is now dissolved in the benzene in B.
6 o° Solid benzene U) The lowering of the vapor pressure of the
0.075 G. 0.22 .. 0.04 0.12 0.15 .. 0.32 0.34 ,. ., , . ' * _ . ^, j. , . . ,
Toluene 0.006 g liquid benzene in flask B by the dissolved toluene.
o.o°o G."ne 0.32 .. 0.33 .. .. 0.62 .. .. Pressure developed between A and B = a + b + c.
Toluene 0.009 G. _ ., , . . . .. - , ,._ .. .
8 o° Solid benzene Consider now the variations in the final differential
9 o° solid benzene °'24 " " °'27 pressurt.' between A and B, caused by using different
•S$}£ 0.008 G. 0.24 •.". o.i. '.: :: 0:240:27 :: Quantities of liquid in flask B. As these quantities are
10 0° Air saturated incn i or (6) becomes larger, and approaches
with toluene 0.23 0.41 .. , \' ... j- i •
a limiting value, which would represent the dissolving
In most of the observations recorded in this table, of all the toluene in the liquid benzene. At the same
difference in pressure had ceased to increase at time, Factor (c) approaches a value infinitely small.
the time of the last observation. The greater part of The difference" in pressure developed between the two
Sept., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
715
flasks at this limiting value P^ is equal to the sum
of the original vapor pressures of benzene and toluene
in the gas.
If now the quantities of liquid benzene are decreased,
Factor (b) approaches a value infinitely small, which
would exist if the quantity of liquid benzene used were
so minute that only an infinitely small quantity of
toluene could be dissolved from the gas. In this case,
Factor (c) increases to a limiting value, equal to the
lowering of the vapor pressure of benzene caused by
the dissolving of sufficient toluene to give a vapor
pressures of toluene from the solution equal to that
originally present in the gas. The difference in pres-
sure developed between the two flasks at this limiting
value, P0, is equal to the sum of the original vapor
pressure of benzene in the gas and the lowering of the
vapor pressure of benzene from a solution of toluene
which gives a vapor pressure of toluene equal to that
in the original gas.
The approximate form of this curve is shown in
Fig. I.
Po
= AB
-<-)
At 25 ° the ratio of the vapor pressure of benzene
to that of toluene is about 10 : 3, so that
7
AB
-fr-)
or about - T
3
Weight oFLi<juid Re77ia.inLng in Flask 3
Thus AB represents the vapor pressure of toluene
7 •
originally present in the gas, magnified about - times.
3
Suppose that instead of toluene, the original mixture
had contained the vapor of some less volatile liquid,
a xylene for example. Then AB would represent the
original vapor pressure of the xylene magnified to a
still greater extent than was that of toluene. It is
therefore evident that when the differential pressure
method, employing bulbs of liquid benzene, is used for a
gas mixture containing benzene vapor and the vapors of
high boiling compounds, the vapors of these compounds
will cause a sharp increase in the differential pressure
in those cases in which minute quantities of benzene
remain in Flask B.
We have tested these conclusions experimentally
on a sample of illuminating gas collected in small gas
holders. The gas was passed through them in series
for a time sufficiently long to ensure a uniform sample.
The apparatus used was of the modified type de-
scribed in a previous paper. In an apparatus of this
form one of the flasks can first be evacuated and
then filled with the gas to be analyzed. The flasks
were of about 150 cc. capacity each. The results
of these experiments are given in the table. The
high values obtained in Nos. 6 and 9 are undoubtedly
due to experimental error.
Po — Poo = AB = Limiting value of lowering of
v. p. of benzene — Original v. p. of toluene in gas.
It is now necessary to obtain a relation between the
two factors on the right-hand side of the equation,
that is, a relation between the original pressure of
toluene in the gas and the lowering of the vapor pressure
of benzene in a solution of benzene and toluene which
gives a vapor pressure of toluene equal to that in the
original gas.
Let there be Ni molecules of benzene and N2 molecules
of toluene in the solution
Let P4 be the saturation pressure of pure benzene at
that temperature
. Pi, the saturation pressure of pure toluene at that
temperature
T, the original vapor pressure of toluene in the gas
N2
Lowering of v. p. of benzene = — 1 m~ ^b
Ni
Lowering of v. p. of toluene
N, + N,
P<
Or, v. p. of toluene from solution =
Pi
Therefore,
Lowering of v. p. of benzene _ P;,
v. p. of toluene from solution P/
Or substituting in the relation obtained above :
Expt. Benzene1
No. Grams
1 0.0586
2 0.0617
3 0.0707
4 0.0978
5 0.1092
6 0.129
7 0.140
8 0.214
9 0.314
10 0.957
I I
.20
0.0066
0.0087
0.0177
0.0448
0.104
0.124
0. 139
0.209
0.309
0.948
1.20
2.83
2.34
2.33
1.20
1.00
(1.29)
0.97
0.96
(1.11)
1.04
1.39
' Represents the weight of liquid benzen
2 The calculated weights of benzene wl
some having evaporated into the flask.
" The pressure difference between the tv
initial difference and manometer movement.
broken into Flask B.
ich remained at equilibrium
ith corrections for
These results are plotted in Fig. II. It seems reason-
able to suppose that the elevation of the curve from
H-lHIlllr+tf
Weight of liquid Remaimnq in Flask in Grams
Vic. II
B to A is mainly due to toluene. This curve projected
would meet the axis at a point corresponding to a
vapor pressure of 1.4 cm. The constancy of the
pressures in Nos. 7 and 8 would indicate that under
these conditions all the toluene and other vapors had
7i6
THE JOURNAL OF INDUSTRIAL A X D ENGINEERING CHEMISTRY Vol. 10, No. 9
dissolved in the liquid benzene. The average value
of these pressures is about 0.97 cm.; or the limiting
value of the elevation AB due to toluene is 1.35 —
0.97 = 0.38 cm.; that is, the original vapor pressure
11I toluene in the gas was about o. 15 cm.
The gradual elevation of the curve from C to D is
undoubtedly due to increasing absorption into the
liquid benzene of some constituents of the gas other
than the light oils. As this effect was not very pro-
nounced, it seems probable that in experiments done
in this way when the volume of liquid benzene used is
about 0.2 to 0.5 per cent of the volume of the flask,
the difference in pressure developed represents the
total pressure of the light oils in the gas.
The following experiment was carried out on il-
luminating gas, in order to test the solubility of the
permanent gases in benzene:
A sample of illuminating gas was shaken up for a
long time with two successive portions of straw oil
(sp. gr. 0.87), such as is used in commercial works
to remove the light oils from gases, until it seemed
probable that these hydrocarbons had been removed
from the gas. The left flask contained gas with the
benzene, etc., removed by oil washing; the right, air.
The pressure developed was 0.02 cm. less in the
left than in the right. This result indicates that the
errors, caused by the permanent gases in coal gas dis-
solving in the benzene, are small. The experiment,
however, should be repeated with more detail.
NEW METHOD FOR THE ESTIMATION OF BENZENE IN A
GAS CONTAINING ALSO TOLUENE AND OTHER
VAPORS
In a former paper it has been shown that the amount
of benzene in an inert gas can be accurately estimated
by the differential pressure method, using bulbs of
liquid benzene. It has been shown above, however,
that when the gas also contains toluene and other
light oils, the following factors must be considered:
1 — The toluene and other light oils dissolve in the
liquid benzene so that their pressures are almost
entirely removed from the gas, while at the same
time these dissolved substances lower the vapor pres-
sure of the benzene.
2 — A less serious error is caused by the gases other
than the light oils dissolving in the liquid benzene.
In order to eliminate these sources of error, we have
conducted investigations on gases by the differential
pressure method, using bulbs filled with solid benzene
and immersing the apparatus in a bath below the
freezing point of benzene, 5.48°. It is well known
that the solubility of permanent gases in a solid, such
as frozen benzene, is vanishingly small, so that the
second source of error mentioned above is completely
eliminated.
Again, the vapor pressure imm the solid benzene,
at any fixed temperature, is independent of the solu-
tion by which it is surrounded, so that while the solid
benzene is present at equilibrium there can be no
lowering of its vapor pressure.
Moreover, there are certain definite pressures of
the light oil vapors which, at definite temperatures,
can be in equilibrium with solid benzene. Any smaller
pressures of these vapors will not be affected by the
breaking of the bulb containing solid benzene. The
following considerations make this clear:
Suppose that the light oil in the gas, besides ben-
zene, is toluene. We are then to calculate the maxi-
mum quantity of toluene that can be in equilibrium
with solid benzene, the temperature being known.
For each temperature there is a solution of toluene
in benzene which would be in equilibrium with solid
benzene. Its concentration can be calculated from
the formula for the depression of the freezing point :
T = Wl X 5-
Where T = depression of freezing point of solvent
(benzene)
Wj = weight of dissolved substance (toluene)
M = molecular weight of dissolved sub-
stance (92)
W2 = weight of solvent (benzene)
K = molecular depression constant of sol-
vent (4900)
so that
W, T X M 92 T _ T
Wi K 4900 S3
If the weight of benzene (W:) be 78, or 1 gram-mole-
78 X T
cule. then the weight of toluene (W,) is =
53 X 92
0.017 T gram-molecules. But the solution in equilib-
rium with the solid benzene may be considered as a
solution of benzene in toluene. Knowing its concen-
tration, the vapor pressure of toluene from this so-
lution can be calculated in terms of the vapor pressure
of pure toluene at that temperature, by the modified
equation of Raoult:
AP _ w.
P ~ N, + NS
Where N| = number of gram-molecules of benzene
X; = number of gram-molecules of toluene
AP
P
pressure
AP _ 1
P 1 + 0.017 T
At o° C, T =5-5°
AP 100
fractional lowering of toluene vapor
Therefore.
109
Or, the vaporpressure of toluene from the solution is
109
of the vapor pressure of pure toluene at that tempera-
ture (about 6 mm.) =0.5 mm. This, then, repre-
sents the possible concentration of toluene vapor in
equilibrium with solid benzene at 0° C.
In these calculations we have assumed that the
simple law for the depression of the freezing point
given above holds good over the range of tempera-
tures considered. We intend to test this experi-
mentally. If there are deviations they will probably
tend to make the concentrations of toluene vapor
Sept., 1918 TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
717
which can be in equilibrium with solid benzene greater
than those calculated above. We also expected that
the method for the estimation of benzene could be
used in the presence of still larger quantities of toluene
vapor on account of metastability of the benzene
crystals, provided they were well frozen.
Similar reasoning will apply to a gas mixture con-
taining benzene with xylene or other vapors.
In order to test these conclusions a series of experi-
ments was carried out in the following way:
Air saturated with toluene vapor by bubbling it
through toluene in a Geissler absorption tube was col-
lected in a eudiometer. From this a measured quan-
tity was drawn into the left flask of the differential
pressure apparatus evacuated sufficiently to receive it.
Determinations were also made with both toluene
and xylene vapors present. In this case quantities
of air separately saturated with the vapors were drawn
into the eudiometer. These quantities were meas-
ured, so that the pressure of each vapor in the flask
could be calculated for the temperature of the experi-
ment.
The apparatus was then packed in snow, or snow
and brine, which was kept well stirred, and the de-
termination carried out in the usual way. Special
care must be taken in breaking the bulbs of solid ben-
zene in order not to fracture the bottoms of the flasks.
The rod should be hit, not a hard blow, but a series
of taps with a light object (we used the handle of a
small screw driver). The bulb soon breaks and the
solid benzene settles down in small pieces.
Pressure
Developed
Cm.
— 0.035
— 0.085
—0.021
—0.055
-5.8°
-5.0°
Toluene 0.078
Toluene 0.122
Toluene 0.155
( Toluene 0. 167
(Xylene 0.023
(Toluene 0.122
I Xylene 0.034
Toluene 0.237
(Xylene 0.067
—0.218
—0.011
In not a single case was the differential pressure de-
veloped towards the flask containing the vapors. This
indicates that these vapors did not dissolve in the
solid benzene. On the other hand, a small variable
pressure was developed the other way. We are un-
able to say whether this was due to some source of ex-
perimental error in the particular apparatus used or
whether it was actually caused by the presence of
the toluene and xylene. We intend to investigate
this phenomenon further.
Tests of this method for the estimation of the ben-
zene and of the light oil content were carried out on a
sample of illuminating gas collected in small gas
holders.
The following results were obtained:
Difference in
Pressure Developed
emperature
Cm.
— 17°
0.61
—18°
0.61
0°
0.58
0°
0.62
0°
0.60
4.5°
0.88
6.5°
1 . 12
4.5°
0.91
5.1"
0.98
5.6"
1.12
22°
0.94
20"
1.01
The following points are to be noted:
1 — The pressure developed was practically constant
from — 170 to o° C. This value (0.60 cm.) probably
corresponds to the pressure of benzene vapor in the
gas.
2 — The first part of Expts. 6 and 7 was in each case
carried out in a water bath at a temperature below
the melting point of benzene. The result, 0.98 cm.,
obtained at 5.1°, when some solid benzene was pres-
ent on both sides, probably represents the total pres-
sure of the benzene and the light oils, for at a tem-
perature so near the melting point of benzene the lat-
ter must have nearly all dissolved out.
3 — The latter parts of Expts. 6 and 7 were done
at a temperature slightly above the melting point of
benzene and the difference in pressure read after all
the solid benzene had disappeared. The high value
1. ia cm. obtained for the differential pressure is
probably caused by solution in the liquid benzene
of constituents from the gas other than the light oils.
4 — The mean of the values obtained at room tem-
perature (0.97 cm.), bulbs of moderate size being
used, probably represents the total light oil content
in the gas as has already been shown in this paper.
To sum up, determinations made at 0°, that is, in
melting ice, gave the benzene content in the gas;
and those done at ordinary temperatures with the
proper proportions of liquid benzene gave the total
light oil content.
Samples of illuminating gas, collected in small gas
holders, were also analyzed by the method outlined
above, at 23°. the following liquids being used in the
bulbs:
1 — Benzene only.
2 — A solution of equal volumes of benzene and
toluene.
3 — A solution of equal volumes of benzene, toluene,
and xylene.
The following results were obtained:
Benzene Benzene
Differential Pressured) - 1 .03
(2)
Mea
Total Pressure Developed 9.0
In the first case, the toluene and xylene from the
gas dissolve in the benzene. In the second case, the
pressures of both the benzene and toluene from the
solution in the bulbs are greater than their original
pressures in the gas; they are estimated by the same
principle. In the third case, all three vapors are
estimated in this way. It is seen that the mean values
of the results are about the same in every case, which
confirms the conclusion given above, that when ben-
zene is used in the bulbs at ordinary temperature,
the differential pressure represents the total light oil
pressure in the gas.
The advantage of using one of the solutions rather
than pure benzene in the bulbs is seen in the figures
representing the total pressures developed, for in
these cases the pressures developed are much smaller,
so that the danger of leakage is greatly decreased.
and
Toluene
enzene
Toluene
Xylene
Cm.
Cm.
Cm.
1 .03
0.99
0.99
1 .00
1.06
1.14
1.02
1.03
1.06
9.0
5.0
4.0
7i8
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 9
PRELIMINARY WORK ON THE VARIATION IN THE CON-
CENTRATION OF LIGHT OILS IN THE COAL GAS
PRODUCED AT VARIOUS STAGES OF
CARBONIZATION
We have shown above that the differential pressure
method, bulbs of liquid benzene being used, gives an
easy and fairly accurate method for the estimation
of the light oil content of a gas mixture.
In order to obtain some idea of the change in the
light oil content of coal gas as carbonization proceeds,
we carried out the following experiments on one of the
retorts of the Winnipeg Electric Railway Gas Plant:
Through a hole drilled in the door of the retort, sam-
ples of gas were drawn off from time to time, washed
with water, and the light oil content estimated. A
340 cc. estimation flask was filled by displacement of
air with 2 to 3 liters of gas. This was not sufficient
and the results are probably low, though they are
comparable with each other, as the treatment was uni-
form throughout.
Time
Light Oil Content of Gas
Mm.
Cm. Hg
0(a)
0.94
13
0.70
52
0.56
102
0.29
186
0.21
227
240(6)
(a) Retort charged with coa
1.
(6) Carbonization complete.
retort emptied.
It will be seen that the gas which came over the first
hour was rich in light oil; after that the content steadily
declined.
COMMERCIAL POSSIBILITIES OF THE METHOD PARTICU-
LARLY IN CONTROLLING THE PROCESS OF AB-
SORPTION OF LIGHT OILS AT
RECOVERY PLANTS
Before the complete development of the apparatus
and methods outlined above, we carried out, with
considerable success, a series of tests on the absorption
plant of the Toronto Chemical Co., at Sault Ste.
Marie.
There seems to be no doubt that the methods of
analysis outlined in this paper will be of great assis-
tance in the control of the washing processes and in
the development of more economical methods of light
oil recovery. This will be taken up in more detail in
a subsequent pa_per.
SUMMARY
I — The rate of development of the differential pres-
sure in the new method for the estimation of vapors
in gases has been investigated.
II — Theoretical considerations and experimental
data are given concerning the estimation of one vapor
in the presence of other vapors by the differential
pressure method.
1 1 1 Theoretical considerations and experimental
data arr given concerning the variations in the differ-
ential pressures obtained according to the quantity
of liquid used.
IV — A new method for the estimation of the ben-
zene and of the total light oil content of gases has
been developed.
V — A brief account is given of preliminary investiga-
tions, by this process, on the production of light oils
during carbonization of coal. The utility of the
methods developed in this paper for commercial
processes is discussed.
We gratefully acknowledge the aid of the Honorary
Advisory Council for Scientific and Industrial Re-
search in Canada, which has made possible the as-
sistance of Mr. MacGregor in this work.
Department op Chemistry, University op Manitoba
Winnipeg. Canada
STUDIES ON THE ABSORPTION OF LIGHT OILS FROM
GASES
By Harold S. Davis and Mary Davidson Davis
Received March 27. 1918
INTRODUCTION
The physico-chemical aspects of the processes by
which "light oils" are absorbed from gases are con-
stantly receiving more attention by those concerned
with their production at recovery plants. It is now
recognized that the light oil vapors are not simply
washed out of the gas mechanically, but are dissolved
by the wash oil to form a true solution. At the same
time, ideas as to what actually occurs in the process
of absorption are not very definite. Two causes
might be given for this:
i^The light oil mixture is considered to behave
as a single compound, whereas the different chemical
substances of which it is composed act independently
of each other to a large extent, particularly as they
are in the vapor state.
2 — There is much confusion as to when an oil is
to be considered saturated with respect to the light
oils. This can be attributed partly to the reason given
above and partly to a lack of clear understanding of
the principles governing the dissolving of the vapors
by the wash oil. Statements to the effect that the
washing oil must exert a good solvent action on the
light oils illustrate this lack of clearness.1
THEORY OF WASHING PROCESS FOR THE ABSORPTION
OF BENZENE VAPOR
Consider a bubble of gas at a definite pressure and
temperature, surrounded by the pure washing liquid.
Suppose, further, that benzene is the only light oil
vapor present in the gas, then benzene will dissolve
in the oil until the vapor pressure of benzene from
the surrounding oil is equal to that in the gas. It
follows that the maximum content of benzene which
can be absorbed by the oil from the gas is that which
gives a vapor pressure of benzene from the solution
equal to the vapor pressure of benzene in the gas.
Consider a scheme such as is given in Fig. I for
washing the gas continuously with oil. The gas pass-
ing from A to B meets the oil travelling in the opposite
direction. At B, fresh oil takes out the last traces
of benzene from the gas, since such oil has no vapor
pressure of benzene. The oil thereby acquires a vapor
pressure of benzene proportional to its benzene con-
tent, and in passing from B to A it continuously
' Tins Journal. 10 (1918). 5.1 Trans. Am. lost. Chem. Eng.. 9
Sept., 1018 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY 719
meets gas with a higher vapor pressure of benzene, Smith, manager of the Dominion Tar and Chemical
until at A it should leave with a vapor pressure of Company, who supplied the following details concern-
benzene equal to that in the gas entering at A. The ing its properties:
benzene is separated by distillation from the oil at C Distillation— First drop 278° c
and the debenzolized oil re-enters the absorotion 1 per cent 280° c.
^ 0/ per cent 360 C.
Column at B. Specific Gravity — 0.870 at 15 . 5° C.
Still to extract Benzene We found the sp_ gf_ to be 0 86?7 at 23.10 C.
An approximate estimation of the vapor pressure
"*£x\ of the oil at ioo° C. was made by introducing it into
a Torricelli vacuum. The result showed that the
vapor pressure was small, certainly not more than
Gas charged* A -* Oil B L Gas free „ , ., ' , ,,
mthBente-^ - Gas — ► r>,„ Benzene x cm' at IO° ' and therefore probably negligible at
' room temperature. The benzene and oil were misci-
ble with each other in all proportions at ordinary
To ensure complete removal of the benzene from the temperatures. A 50 per cent solution deposited crys-
gas the following conditions are necessary: tals of benzene at about — 10° C.
(1) The contact between gas and oil in the space The apparatus used was a simple form of the differ-
A to B must be sufficiently good to nearly maintain ential pressure apparatus described in the previous
equilibrium at every point. The amount of oil which papers. However, only one of the flasks was pro-
needs to be actually in contact with the gas at any vided with the special device by which a small sealed
time is determined by the rate at which the benzene bulb of liquid could be broken inside it. The other
vapor is absorbed into the oil, that is, by the efficiency flask, which was simply used to compensate for changes
of the washers. in temperature and atmospheric pressure contained
(2) The rate of flow of the oil must be so regu- only air.
lated that the quantity of benzene, carried from the By breaking a bulb of benzene in the first flask the
washers per second, shall be equal to the quantity saturation vapor pressure of benzene in air was meas-
brought in by the gas. It has been shown above ured. When the vapor pressure from a solution in
that the washing oil can absorb only a definite propor- the oil was desired, the bulb containing a known weight
tion of benzene. If this proportion is known and the 0f benzene was broken in a known amount of oil in the
rate of passage through the washers, then the rate of bottom of the flask and a solution of the benzene was
flow of the oil necessary to completely remove the formed in the oil.
benzene from the gas can be readily calculated. Collected experimental Results
(3) The poor oil which enters the washers must be v. p.
completely free from benzene for no amount of washing v. p. of enzene
r J J j a Benzene Per cent
will ever lower the vapor pressure ill the poor gas below Solution Temperature Cm. Hg Solution
that from the poor oil with which it is finally washed. s"™ pwcent'benzene'in'oii'!'!! 23l2°c' K99 0.229
The presence of benzene in the poor oil means that the \0]tsP"JZltllfzll'^\ \ \ \ m.I* C. silo o.lll
steam distillation is inefficient and does not completely
separate the benzene from the washing oil. Such in- discussion of results
efficiency may cause a very serious loss to the plant, for According to the experimental results, the vapor
the fraction of benzene lost will be the ratio of the pressure of benzene at 23. 2 ° C. from two solutions in
vapor pressure of benzene from the poor oil to that in oil, one of approximately double the concentration
the rich gas. of the other, was directly proportional to the concen-
In the previous paper, methods for measuring this tration; that is to say, the vapor pressure of benzene
ratio were described by means of which a check can be from a solution in oil and the concentration of ben-
kept on the efficiency of the washing system and the still, zene in the oil are related according to Henry's Law
The following experimental work was undertaken for the solubility of gases in liquids — a result of great
to examine the conditions which determine the maxi- theoretical and practical importance,
mum benzene content which the oil can absorb from A further important principle can be deduced from
the gas. the following table:
v p
THE DETERMINATION OF THE VAPOR PRESSURE OF of Benzene Ratl°
(rom a V P V. P. of 1
BENZENE FROM ITS SOLUTION IN HIGH-BOILING 1 per cent Solu- of Pure per cent Solution
AMERICAN PETROLEUM OIL Temp tlonta Oil Benzene ^^^
The benzene used in these experiments was ob- 23"2oc o 488 i9-2 0025
tained from a well-known firm. It was of high quality
and when freshly distilled, the greater part boiled That is to say, the ratio of the vapor pressure of
over at a temperature constant to much less than a benzene from a solution of definite concentration to
tenth of a degree. It was then boiled in vacuum to the vapor pressure of the pure solvent is independent
expel dissolved air. of the temperature (Von Babo's Law).
The oil used in these experiments had been refined It is now possible to calculate the vapor pressure
from a mixture of American crude petroleums. It of benzene from a solution of any particular concen-
was obtained through the kindness of Mr. E. Bernard tration at any temperature, since the vapor pressure of
720
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. 9
pure benzene is known at that temperature, and also
the ratio borne to it by the vapor pressure of benzene
from a 1 per cent solution in oil.
The following table is calculated, on the assumption
that the two laws given above hold over the ranges of
conditions concerned, for a gas containing 1 mm.
vapor pressure of benzene.
Maximum
Concen-
V. P. of
tration
,— Fresh Oil
Required-
Benzene
Grams
Gals. Oil
from a
Absorb-
(HI per
(U. S. A.)
V. P. of
1 per cent
able
cu. m.
per 1000
Benzene
Solution
by Oil
of
cu. ft.
Temp
Mm.
Mm.
Per cent
Gas
of Gas
—20" C.
5.8
0.15
6.6
70
0.53
—10° C.
12.9
0.33
3.0
150
1.15
0° C.
25.3
0.66
1.5
300
2.17
10° C.
45.3
1.18
0.85
540
3.74
20° C.
75.7
1.97
0.50
920
6.04
30° C.
120
3.12
0.32
1400
9.22
40° C.
183
4.76
0.21
2200
13.62
The amount of fresh washing oil required for any
particular rate of flow of gas depends only on the tem-
perature of washing. At first we thought that, if
the benzene content of the rich gas varied, the rate of
flow of oil necessary to completely absorb it from the
gas must vary too. Consideration shows that this is
not the case. Suppose the benzene content in the
rich gas is doubled; then the maximum benzene con-
tent in the rich oil is also doubled; for, according to
Henry's Law, the vapor pressure from the oil is pro-
portional to the benzene content. Hence the same
rate of flow of oil as before will suffice to remove all
the benzene from the gas.
THE DETERMINATION OF THE AVERAGE MOLECULAR
WEIGHT OF THE OIL WHEN DISSOLVED IN BENZENE
BY THE METHOD OF THE LOWERING OF THE
FREEZING POINT
It is evident from the experimental data given above
that the efficiency of a medium for absorbing benzene
from gases is determined by its power to lower the
vapor pressure of benzene when dissolved in it. For
dilute solutions in common solvents this power of
lowering the vapor pressure is inversely proportional to
the molecular weight of the dissolved substance. We
suspected that this relation might hold for very concen-
trated solutions of washing oil in benzene.
The molecular weight of the oil when dissolved in
benzene was determined in the ordinary way by Beck-
mann's method, using 19.88 g. benzene.
Calculated Lowering
Weight of Lowering, of Freezing of the Freezing Point
Oil Added Point Produced per Gram of Oil
0.3813 0.450° C. 1.181° C.
0.4566 0.500° C. . 1.095° C.
1.2617 1.180° C. 0.935° C.
It will be seen from the right-hand column that the
proportional amounts of lowering caused by the
weights of oil grew continually less. Extrapolation
give about 1.2° as the amount of lowering per gram
of oil, when a small amount of oil was added. This
corresponds to a value of 205 for the average molecu-
lar weight of the oil when dissolved in benzene.
The proportional lowering of the vapor pressure of
benzene caused by the addition of 99 per cent of oil
can now be calculated from the equation of Raoult:
AP _ H
P n + N
Where AP = Lowering of the vapor pressure
P = Vapor pressure
h = Gram-molecules of dissolved substance
N = Gram-molecules of solvent
99 g. of oil =0. 48 gram-molecules of oil.
1 g. of benzene = 0.0128 gram-molecules of benzene
So that for a 99 per cent solution of oil in benzene
Fractional lowering of vapor pressure =
AP 0.4S
P ~ 0.48 + 0.0128 "" °'9'4
And the fraction of vapor pressure left is 0.026, in ex-
cellent agreement with the experimental result 0.026.
The determination of the molecular weight of an
oil when dissolved in benzene seems therefore to af-
ford a good method for testing the efficiency of the oil
for absorbing benzene or other vapors from gases.
THEORY OF WASHING PROCESSES FOR THE ABSORPTION
OF LIGHT OIL VAPORS
We shall base the following discussion of the process
of absorption of light oils into washing oils on two
premises, both of which are supported by the experi-
mental data given later in this paper:
1 — That each separate vapor contained in the gas
dissolves in the washing oil, independently of the other
vapors present, until equilibrium is reached between
its vapor pressure in the gas and its vapor pressure
from the oil solution.
2 — That when washing of moderate efficiency is
employed, equilibrium between the oil and each of
the light oil vapors is reached much more quickly
than has often been supposed.
Of course, each of the constituents of the gas, other
than the light oils, also dissolves in the washing medium,
until corresponding equilibrium is reached, but as
only a small amount of these substances need dissolve
to secure equilibrium with the gas, their effect may be
neglected.
Although it is necessary that the washing medium.
be able to dissolve the liquid light oils in fairly large
quantities, it must not be supposed that the ability
to dissolve these liquids is a measure of the efficiency
of the oil as an absorbing medium. As a matter of
fact, all the high boiling oils usually employed for
scrubbing purposes are largely or completely misci-
ble with the liquid light oils.
It has been pointed out above that the efficiency
of an oil for absorption purposes depends on its power
to lower the vapor pressures of the light oils when they
are dissolved in it. and that this power depends on
the average molecular weight. Other properties of
the washing medium, such as viscosity, boiling point,
tendency to froth, etc., may affect its usefulness as a
washing medium, but they do not determine its ability
to absorb the various vapors, if equilibrium is nearly
reached at each stage of the washing. For. according
to our first assumption, given above, each vapor can
be absorbed into the washing medium until its vapor
pressure from the solution is equal to its vapor pressure
in the gas at that point.
In a washing process on the counter-current princi-
ple, the oil flowing in one direction meets the gas.
Sept., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
passing in the other direction. The oil constantly
absorbs vapors from the gas, equilibrium between the
vapor pressure of each substance in the gas and its
vapor pressure from the oil being nearly maintained
at every stage. But the oil does not become saturated
with every vapor at the same stage of the washing,
rather, the stage at which the oil becomes saturated
with respect to any one vapor is determined by the
saturation vapor pressure from the pure liquid of the
same composition as the vapor in question.
Consider the absorption of benzene and toluene
vapors from the gas into the oil. As long as the process
of washing is so regulated that all these vapors are
removed from the gas, then the number of gram-
molecules of each of these substances in a definite
quantity of rich oil is proportional to its original
pressure in the rich gas. These dissolved quantities
of the hydrocarbons, however, do not give vapor
pressures from the solution proportional to their
original vapor pressures in the rich gas.
For instance, the benzene content in the rich oil
has reached its maximum when it gives a vapor pres-
sure of benzene equal to that in the rich gas. Yet
at this stage the dissolved toluene only gives a pressure
from the oil equal to a fraction of the toluene pressure
in the rich gas. This fraction is equal to the ratio
of the saturation pressure of pure toluene to that of
pure benzene, as may be proved from the following
considerations:
Let X(, = original vapor pressure of benzene in the
rich gas
X( = original vapor pressure of toluene in the
rich gas
N] = gram-molecules of benzene and Ns,
gram-molecules of toluene contained in
a definite quantity of rich gas
X = number of gram-molecules of washing
oil necessary to completely remove all
the benzene from the quantity of gas
considered on a counter-current process
P& = saturation pressure of pure benzene
P( = saturation pressure of pure toluene
Yj, and Y 1 = vapor pressure of benzene and
of toluene, respectively, from the oil
solution
"*■■ N2 , .
and applying Raoult's equation,
Then
X,
Vt =
Y, =
Ni
+ (N + Nt)
N,
Pi
< )r
Oi
Y,
Yj
v,
X2 + (N + N,)
X2P,
N,P4
Y,X,P,
xtp4 •
When the oil is saturated with benzene Xj = Yj,
and Y, = X« l1.
* b
At 25° the vapor pressure of benzene is about 10 cm.,
of toluene aboul 3 cm., and of w-xylene about 0.9 cm.,
so that when the rich oil is saturated with benzene
it is only 3/io saturated with toluene and 9 10o saturated
with xylene. Any attempt to obtain a higher per-
centage of toluene or xylene in the rich oil will result
in loss of benzene, for some will now pass through
without being absorbed.
It is evident that such terms as "saturation con-
tent of the oil" or "maximum enrichment of benzol,"
where benzol means light oils, have no concrete mean-
ing.
If by the maximum enrichment of the washing oil
is meant the maximum quantity of light oil which it
can contain, without any light oil passing through
the washing process unabsorbed, then it is reached
when the vapor pressure from the washing medium
of the lowest boiling compound in the light oil, in
this case benzene, is equal to its pressure in the rich
gas.
SATURATION OF THE RICH OIL
Confusion in regard to the principles outlined above
is shown by a method in use for determining whether
sufficient washing oil to remove all the light oil vapors
is being brought in contact with the gas. In this
method, fresh gas is passed through the rich oil; if
the oil is found to take up additional quantities of
hydrocarbons from the gas, as evidenced by an in-
crease in weight, it is considered as having been un-
saturated. To obtain the saturation content, gas is
passed through the rich oil until it ceases to increase
in weight, at which point it is considered saturated,
all lower concentrations being considered unsaturated.
If the gas contained but one vapor, or several vapors
dissolving as a single component, this conclusion
would be correct. But in the case of a gas contain-
ing several vapors acting independency, as does the
coal gas in question, the problem is very different.
Consider what happens when such a method is
used on the coal gas of our experimental work, with an
average benzene content of 6 mm. and an average
toluene content of 1 . 5 mm.
Consider a typical absorbing oil (sp. gr. 0.87) with
an average molecular weight of 205.
It has been shown above that the proportional
lowering of the vapor pressure of benzene caused by
the addition of 99 parts of oil is 0.9737, and tne frac-
tion of vapor pressure left is 0.0263. Similarly for
toluene, it can be shown that the fraction of vapor
pressure left is 0.0222.
The following table can then be calculated for any
temperature, e. g., 26 ° C.
Substance
Bi ozene
Toluene . . .
V. P. Possilik-
1 per cent Concentration
Solution in Oil at 26° C.
Cm. Per cent
0.26 2.3
0.066 2.3
As the amount of toluene in the rich gas is to the
i; 6o
amount of benzene in the rich gas in the ratio — : — ,
78 92
it follows ilia! when the oil lias taken up 2.3 per cent
of benzene, it will have taken up only 0.68 per cent
of toluene, which is about ' ,; of the possible amount.
Or, toluene can Still be taken up to the amount of 30
pei cenl oi the total possible hydrocarbon content.
722
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. lo, No. o
/7 10 19 2021 2? 23 2-4 25 2*21 28 29 30 3/
M 31 33394041 42 41 44 45 46 4 7 4S 49 SO H S7 S3 S4 SS S6S7J3J36061 62 63
Time in Dac/s
Similar considerations apply to the small quantities of
high boiling compounds which exist in the gas and which
are soluble in the oil. Each of these compounds will
continue to be absorbed until the vapor pressure
from the oil equals its vapor pressure in the gas. At
the same time, the constitution of the oil solution will
slowly change, and its absorbing power will be gradually
modified. These factors would result in a steady,
slow increase in the amount of the total hydrocar-
bons absorbed over a comparatively long period.
EXPERIMENTAL PART
experiment i — In the first experiment, two conical
flasks, A and B, of 125 cc. capacity, were used, con-
taining, respectively, 103.8 g. and 101.8 g. of a typical
straw oil (sp. gr. 0.87; average molecular weight,
203). Illuminating gas from a gas jet was bubbled
through each, the pressure being regulated by stop-
cocks in the inlet tubes. At first the gas passed through
at an average rate of 2 liters per hour, being some-
what faster in the case of B. Later, however, the gas
was passing through A at a considerably faster rate
than through B. This accounts for the curves of
A and B crossing each other.
Both the ingoing and the outgoing gas passed through
cotton wool, to prevent loss of weight from the oil
passing over. The outgoing gas led to a Bunsen
burner. In this and subsequent experiments the
gas flasks were packed with wool in a copper con-
tainer which was immersed in the water of a thermo-
stat regulated at 26 °.
The experiment ran from October 20 to December 26,
the flasks being weighed every one or two days. There
was trouble at the last, due to loss (if weight by the
passing over of the oil, particularly in B, so that the
final results arc somewhat lew.
A few of the results are given below; they are shown
completely in the curves plotted in Fig. II.
-Gain in Weight-
Time
A
B
Days
Grams
Grams
1
0.67S
0.917
8
3.192(a)
12
2.998(c
19
4.687(6)
31
4.973
3.731
67
5.613
4.318
(a) At 2.98 per cent the oil should be nearly saturated with benzene
(see above).
(6) At 4.6 per cent the oil should be nearly saturated with benzene and
toluene if nothing else be present. As it is, the percentage will be some-
what higher.
experiment ii — A second series of determinations
was carried out, this time using as absorbing flasks
Bender and Holbein's potash bulbs, C and D, which
contained 7. 95 g. and 9.93 g. oil, respectively. Gas
bubbled through C at the rate of one liter in 32 min.,
and through D at the rate of 1 liter in 1 7 min. The
experiment was run from December 19 to 22. when it
was found necessary to discontinue on account of
the oil passing over.
Gram
0.358
Weights
D
Gram
0.479
0.541
Per cen
5!68
i Weight--
D
Per cent
s'.is
experiment hi — In the next experiment the bulbs
C and D were connected in series, and gas from the
mains bubbled through at the rate of 2 liters per
hour, being washed first by D and then by C. It
was found necessary to use an aspirator in order to
obtain a flow of gas. C contained 10.6 g. and D, 10.4
g. oil. About 73 liters of gas passed through; the
bulbs were weighed every hour. The experiment
was run from January 1 to 18, at the end of which
time D had gained 0.371 g. and C, 0.324 g. The
complete results are plotted in Fig. III.
experiment iv — In order to have a constant gas
supply for this experiment, a 100 liter tank was filled
with illuminating gas, by displacing water from it. It
was so arranged that the pressure could be regulated
as desired. The gas drawn from the tank was re-
Sept., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
723
placed by water, which was first saturated with illumi-
nating gas.
/
3
»--* to 20 30 40 SO 60
Amt of Gas in Liters
Fig. Ill
■ The expt. itself was substantially the same as
Expt. III. The same bulbs were used, C con-
taining 10.2 g. and D, 9. 2 g. of oil; C was connected
to the gas supply. The gas, as before, was drawn
through by means of an aspirator at the rate of 2
liters per hour, 40 liters being drawn through alto-
gether. The weights of the bulbs were taken every
hour. The experiment was carried on from January
21 to January 25, when C had gained o. 293 g. and D,
0.215 g- The results are plotted in Fig. IV.
DISCUSSION OF EXPERIMENTAL RESULTS
The general form of the absorption curves in Fig. II
is clear. There is first a fairly rapid, steady increase of
weight (1 to 2), then a slower increase of weight (2 to 3),
and finally a very slow increase (3 to 4) extending over
a long period. We believe that the first rapid in-
crease is due to the absorption of the benzene vapor
from the gas, equilibrium being quickly attained.
The next increase (2 to 3) is caused by the toluene and
the xylenes, while the final slow increase (3 to 4) is
caused by the absorption of the high boiling com-
pounds existing in the gas in minute quantities.
If this explanation is correct, the following conclu-
sion may be drawn :
When the oil has once become saturated with ben-
zene and toluene, which form the greater part of the
light oils absorbed from the gas, a lowering of the gas
pressure will cause their concentrations in the oil to
decrease, for some of the benzene and toluene will be
lost. At the same time the other vapors will continue
to be absorbed, but in such small quantities that the
net result will be a loss of weight. The theory is
pretty well substantiated by the curves of the first
experiment, for after the point 2 has been reached, a
great many fluctuations appear. Changes in atmos-
pheric pressure which amounted to 25 mm. during
the course of the experiment, variations in gas pres-
sure, and possibly small changes in the concentration
of light oil vapors in the gas, are undoubtedly responsi-
ble for these fluctuations.
In Fig. Ill, the curve, representing the gain in weight
of the first bulb, is of the same form as the curves of
Fig. II, and the same considerations apply to it. In
regard to the curve representing the gain in weight
of the second bulb, the following points should be noted:
At first there is a very slight increase in weight,
then a rapid increase, so that the curve at 1 is convex
towards the " x" axis. In the region of 2 the slope of
the curve decreases, there being possibly a further
decrease later on at 3.
If our explanation of the first curves is correct, and
if equilibrium is really closely maintained at every
stage, so that the gas coming into the second absorp-
tion bulb contains that amount of each vapor which
is in equilibrium with its solution in the oil of the first
bulb, the following argument holds:
Since it is the benzene pressure in the oil of the first
bulb which grows most quickly, the toluene next,
etc., one would expect the increase in weight of the
second bulb to grow slowly at first, then rapidly until
the oil approaches saturation with benzene, when it
would fall off. As it approaches saturation with
benzene and toluene, it should fall off still more.
The absorption of the other substances from the gas
would continue slowly, but a very long time would be
necessary for the oil in the second bulb to become
saturated with them, particularly with the high boil-
ing compounds. Hence the percentage increase in
weight of the second bulb would take a very long time
to reach thafof the first.
As shown in Fig. Ill, the curve was of the general
form which we had anticipated.
Another factor tending to make the gain in weight
of the second bulb always lower than that of the first
was the necessity of using considerable aspiration in
order to maintain a flow of gas, so that the pressure
on the gas was always less in the second bulb than in
the first.
Amt of (ras in Liters
Fig. IV
At the point 1 in Fig. IV we put considerable pressure
on the gas and regulated its outflow from the second
bulb by a stopcock. The pressure on the gas in the
second bulb being thus increased, there was a sudden
gain in weight. When the pressure was decreased to
its original value, the increase in weight dropped corre-
spondingly, as indicated at the point 2 in the figure.
EXTRACTION OF TOLUENE FROM GASES
We have pointed out above that if the rate of flow
of the wash oil is just sufficient to extract all the ben-
zene from the gas, all the toluene is also extracted
at the same time, but the oil never becomes saturated
with respect to toluene. If the aim of the washing is
to extract toluene only, a method of procedure much
desired at the present time, then much less oil need be
724
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 9
or washing. It has already been shown that
only one-third as much oil is theoretically necessary
to completely absorb all the toluene, as to com-
pletely absorb all the benzene.1 It follows that if just
this quantity of oil is used, about two-thirds of the
benzene will pass through unabsorbed. Of course, in
addition to the toluene, all the higher boiling com-
pounds will be completely extracted from the gas.
In most commercial processes for the extraction of
light oils, the gas is passed through several towers in
series. Evidently the only advantage that several
towers have over a single one is that they prolong the
contact between gas and oil, so that equilibrium is
more nearly reached at every stage. If this equi-
librium is actually nearly maintained and if the rate
of flow of oil is just sufficient to remove all the light
oils from the gas, it follows that practically all the
toluene will be absorbed in the first third of the tower
system.
Confirmation of this tendency of the toluene to be
absorbed in the first towers is obtained by a considera-
tion of the relative proportions of benzene and toluene
in the gas and in the tar formed at the same time.
This tar may be considered as the first washing medium
for light oils through which the gas has passed. The
ratio of the toluene to the benzene in samples of
English tar was 0.9 to 1.1; in samples of German
tar, 0.4 to o.6;! that is, the toluene content is about
70 to 80 per cent of the benzene content, whereas in
coal gas the toluene content is only about 25 to 30
per cent of the benzene content.
This tendency of the toluene to be absorbed into the
first towers can, perhaps, be utilized in a system of
washing such as that illustrated in Fig. V, so that all
the toluene could be obtained in a relatively small
amount of washing oil and benzene. The greater
part of the expense and difficulty in a commercial
plant comes, not in the washing of the gases, but in
the separation of the light oils from the wash oil by
Steam distillation and in the fractionation of the light
oils. The separation into the fractions is never com-
plete, the large quantity of benzene always contain-
ing a small quantity of the more valuable toluene. It
seems rational then to avoid as far as possible the
mixing of the toluene with the benzene and to collect
and distil the rich oil collected in the first part of the
washing system separately from the rest of the oil.
ABSORBING MEDIA
We have already shown that, for the oil of our
experiments, with an av< ilar weight of 205.
1 The use of prcbenzolized wash oil for the i
ed at a conference on coal suppl:
1915. This Journal, 7 (1915). -138.
c. "Coal Tar and Ammonia." 1916). 1
avery of toluene from
held at Manchester in
the maximum benzene content obtainable at 26 ° C.
from a gas with a benzene content of 6 mm., is about
2.3 per cent, while the maximum light oil content is
about 3 per cent. This result of course could be ob-
tained only if there were perfect washing, *". e., if
equilibrium were exactly maintained at every point.
In actual practice this maximum content would neces-
sarily be somewhat lower.
These results agree with the statement of Sperr1
that "in best practice, the amount of benzol absorbed
(technically, the 'enrichment') is kept between 2
and 3 per cent of the absorbing oil."
Lunge,2 however, states that one observer obtained
an increase of weight in an oil of 20 per cent, and that
another observer records an increase in weight of 10 per
cent caused by the absorption of benzol. It is difficult to
interpret these results without more specific data, as
will be clear from the discussion of "saturation''
given above. Still, unless these high results were due
to the pressure on the gas being greater than atmos-
pheric, they could be due only to the following causes:
1 — High content of light oil in the gas.
2— An absorbing oil of low molecular weight.
If the results quoted above are correct they indicate
great possibilities from the study of conditions neces-
sary to produce the maximum content of light oil dur-
ing carbonization. They also indicate that research,
may lead to the development of washing media with
all the desired qualities of boiling point, fluidity, etc.,
having at the same time a comparatively low molecu-
lar weight. While to a certain extent the molecular
weight of a compound determines its physical proper-
ties, such as the boiling point, still, exceptions to the
general rule may be turned to good account in the de-
velopment of new washing media.
Such media could absorb much larger quantities
of the light oils than is possible for the washing oils
at present employed.
s 1 M M A R Y
I — It has been shown, experimentally, that two
important laws can be applied to the vapor pressure
of benzene from its solution in oil: (1) Henry's
Law for the solubility of gases in liquids; (2) Von
Babo's Law for the constancy of the fractional lower-
ing of the vapor pressure from a solution over varia-
tions of temperature.
II — These principles have been applied to calculate
the flow of oil necessary to completely remove the
benzene from a gas.
Ill— The molecular weight of a typical washing
oil when dissolved in benzene has been found and a
calculation made of the fractional lowering of the
vapor pressure of benzene by the addition of 99 per
cent oil. A method based on these results is suggested
for standardizing oils in regard to their efficiency for
absorbing vapors from gases.
IV — The theory of washing processes for the re-
moval of a mixture o\ light oil vapors completely from
a gas is discussed.
> Mtt. and Chem. /■>«-. IS 19
1 Loc. iit., t>: . 72.
Sept.. 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
725
V — The "saturation" of the rich oil is considered.
VI — Experimental data are given of the rates of
gain in weight of absorbing vessels filled with wash
oil when illuminating gas was passed through them.
VII — The extraction of toluene from gases is dis-
cussed and suggestion made for a more efficient scheme
of washing in order to increase the yield of pure toluene.
VIII — The possibility of obtaining better washing
media, through research, is suggested.
Department of Chemistry
University op Manitoba
Winnipeg, Canada
THE EFFECT OF FROST AND DECAY UPON THE STARCH
IN POTATOES
By H. A. Edson
Received June 18, 1918
Severely chilled, frosted, and decayed potatoes are
regarded by the trade, the grower, and the general
public as worthless. On theoretical grounds, however,
such material would seem to possess a potential value
for starch production nearly or quite equal to that
of sound stock. It is a matter of common knowledge
among potato pathologists that the starch granules
of frozen potatoes, and of most decayed stock as well,
present a normal appearance under the microscope.
Decay in potatoes is initiated in most cases either
by frost or by fungi, followed of course by bacteria,
but often the bacteria play a relatively unimportant
part in the process, except perhaps in the final stages.
Southern bacterial rot, black-leg decay, and bacterial
decay following flooding accompanied by high tem-
peratures, constitute the most important exceptions
to this general rule. The total amount of destruction
from these three last -mentioned causes, however, is
relatively small. In New York and New England,
and in a few other regions, late blight decay is quite
destructive certain seasons on stock from unsprayed
or improperly sprayed fields. In these cases the
destruction is accomplished largely through the action
of so-called secondary organisms to which the
Phylophthora gives entrance. Among these secondary
invaders, Fusaria of various species are frequently
encountered. Powdery dry rot, jelly-end rot, numerous
types of dry rot as well as several soft or wet rots are
caused by one or another species of Fusaria. Potato
leak in California is caused by Pythium. Taking the
country as a whole, parasitic Fusaroa, and frost in
field, storage, or transit, combined with the parasitic
and saprophytic Fusaria which usually follow frost, are
responsible for the destruction of enormous amounts of
potatoes. Shippers have expressed the opinion that
frost is the most important single cause of loss en-
countered after the crop is harvested.
Since much of this injury seems more or less inevi-
table and is likely to continue, the question of possible
salvage is worthy of consideration and one who is not
primarily concerned with problems of potato utiliza-
tion may be permitted to bring to the attention of
those interested certain facts regarding this neglected
source of starch supply with which he has become
familiar during the prosecution of his duties as a
potato pathologist. As already stated, the micro-
scope indicates that the starch in frozen and in most
decaying stock is normal. The action of frost and the
results of invasion by organisms of decay appear to
be exercised upon the lamellae of the walls and the
protoplasmic contents of the cells rather than upon
the starch. Such physiological studies as have been
conducted upon the organisms under consideration
indicate that most of them are either entirely incapable
of cleaving starch or that their amylolytic power is
weak. This is especially true of the filamentous fungi
involved, but it also applies to many of the bacterial
species associated in the decay of potatoes. This
explains why the starch granules often remain free
from corrosion even in cases of advanced decomposi-
tion.
With these facts in mind, preliminary trials were
undertaken to further establish the action of decay-
producing organisms upon potato starch, and the
possibility of its recovery from frozen and from de-
cayed material. The first tests were conducted upon
frosted and decayed potatoes obtained during routine
examination in connection with the service of the
Bureau of Markets for inspection at destinations.
Four types of material were included:
1 — Frozen potatoes which had not been allowed to
thaw.
2 — Frozen potatoes subsequently thawed and
softened, but not materially decayed.
3 — Fusarium decayed stock in which the indications
were that slight field frost undetected at the shipping
point probably predisposed the material to decay.
4 — Decayed portions only of the material described
in 3.
The potatoes were pulped by grinding in a small
hand corn mill and the starch recovered by repeated,
successive shakings with 10 or 15 volumes of water,
sedimenting the pulp, and decanting the supernatant
liquid. For the final purification only 1 or 2 volumes
of water were used.
Since the original weight of the samples before
injury could be determined only for 1, the per-
centage yields could not be calculated, but they ap-
peared to be normal in amount and they were certainly
of good quality and free from odors. That from 4
(decayed portions only), while a good white starch,
was not so clear as that from the other three classes of
material. This was due in part to the fact that the
sample was not washed before pulping and particles
of earth sedimented with the starch. The micro-
scope revealed also a considerable number of free,
unbroken cells with their starch content intact em-
bedded in the pure material. The brownish cellulose
walls of these cells doubtless contributed to the dis-
coloration.
In another series of experiments Green Mountain
potatoes from the same sack were employed. Eleven
samples of equal weight were washed and treated as
indicated below:
1 — Normal; extracted at once for a control.
2 — Frozen solidly; thawed and extracted after an
interval of one day.
726
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 9
3 — Frozen solidly; thawed, heavily inoculated with
a mixed spore suspension of potato-destroying Fusaria,
held in the laboratory 4 days at about 70° F., and ex-
tracted.
4 — Same treatment as 3, but held for 16 days.
5 — Same treatment as 3, but held for 20 days.
6 — Normal; extracted at close of experiment as
control.
7 — Inoculated with Fusarium oxysporum and held
in a moist incubator at 25 ° C. until completely de-
cayed.
8 — Inoculated with Fusarium radiciola and held in
a moist incubator at 300 C. until the greater portion
of each of the tubers decayed. The rot obtained was
in some cases dry, in others wet.
9 — Inoculated with Fusarium radiciola and held in
a moist incubator at 30 ° C. with abundant aeration
until completely decayed. The rot obtained was al-
together very wet and soft.
10 — Inoculated with Rhizopus and held in a moist
chamber in the laboratory until most of the tissue was
involved in decay. The rot was dry and apparently
due in part to Rhizopus and in part to other fungi and
bacteria present.
11 — Inoculated with Pythium deharayanum and held
at room temperature, approximately 700 F., until de-
cay resulted.
The results are briefly presented in tabular form be-
low:
Table I — YrBLDS op Starch prom Decayed Potatoes
Yield
No. Treatment Per cent Grade
1 Control 10.29 1
2 Frozen, held 1 day 10.30 2
3 Frozen, inoculated, held 4 days 9.93 2
4 Frozen, inoculated, held 16 days 9.53 1
5 Frozen, inoculated, held 20 days 6.83 4
6 Control 12.13 1
7 Decayed by F. oxysporum 1 1 . 43 3
8 Decayed by F. radiciola 9.19 3
9 Decayed by F. radiciola 1 2 . 88 1
10 Decayed by Rhizopus 6.04 3
11 Decayed by Pythium debarayanum 5.76 2
Microscopic examination of the starch from these
samples revealed no indications of injury to the grains
from any of the treatments employed except in the
case of Pythium, which exerted a solvent action on the
granules. Macroscopically all were of good quality.
The washed samples were free from the odor of decay.
According to color they could be separated into four
grades as indicated in the table but the difference in
clarity between Grade i, the lightest, and Grade
4, the darkest, was by no means striking. Under
the microscope it could be determined that the degree
of variation from pure white was proportional to the
quantity of free, unbroken, starch-laden cells in the
sample. This in turn seemed to depend upon the type
and degree of decay. The low yields from Sample
1 1 appear to be due in part to the solvent action
of the organism on the starch, but the outcome in the
case of Samples 5 and 10 was not the result of
starch destruction during decay but of excessive loss
during recovery. At least the examinations made of
the discarded pulp and the recovered starch point to
that conclusion. The mechanical condition of the
pulp obtained on grinding the samples varied ma-
terially according to the type of decomposition. In
some, the middle lamellae of the cells were quite com-
pletely dissolved, leaving the cellulose lamellae intact
and the cells detached. Many such free starch-
bearing cells were not ruptured during the process of
pulping and more or less difficulty was experienced
in separating them from the free starch. As already
indicated they discolored the samples more or less
when they were retained; and as they were filled with
starch, the yield was lowered when they were washed
away. The difficulty of complete separation was con-
siderably increased in Samples 5 and 10 where
practically all the tissue was involved in a dry rot.
The pulp contained many free cells and many small
aggregates of cells surrounded by a mat of radiating
mycelial strands by which they became entangled in
sedimentation.
The highest yield was obtained from Sample 9
which underwent very complete wet decay involving
the cellulose lamellae of the walls as well as the middle
lamella. The semifluid obtained on breaking the
skins of the potatoes of this lot consisted of free starch
grains floating in a matrix of residual material. Much
of the tissue was sufficiently disintegrated to pass
readily through cheesecloth without pressure or the
use of additional water. Two-thirds of the entire
yield secured came from washing this portion without
grinding and the balance from the remainder after
it was pulped. The behavior of this sample suggests
the possibility of employing Fusarium radiciola for
the destruction of the pulp in the preparation of special
potato starch for use in biological work where a high
degree of purity is essential. Before a practical
method of this sort could be established it would of
course be necessary to standardize the procedure so
as to secure the condition of temperature, humidity,
and aeration affording a maximum cellulose destruc-
tion.
Frosted and decayed potatoes have been found in
these trials to be entirely capable of producing accept-
able and frequently normal yields of clean, white
starch of good quality. Much of this material appears
to possess a potential value for the production of sizing
starch approximating that of the stock at present used
for this purpose. The mechanical difficulties in re-
covery from decayed pulp are sometimes greater
and sometimes less than from normal. Modified
procedure better adapted to these abnormal pulps
could doubtless be devised, but there seems to be no
reason why thi present methods might not be applied
profitably in the meantime in the production of sizing
starch in factories at thi largi shipping centers installed
to utilize the great quantities of frozen and decayed
potatoes- arriving during the fall and winter. This
would turn to profitable account large supplies at
present without value, but which are a serious burden
of expense, since to their cost of production must be
added transportation and dumping charges.
Bureau of Plant Inih-stry
U. S Department op Agriculture
Washington, D. C.
Sept., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
THE RETICULATION OF GELATINE
By S. E. Sbeppard and F. A. Elliott
Received July 23, 1918
The reticulation of the surface of negatives is often
a source of trouble to photographic workers. This
trouble is most likely to occur in hot weather and is
generally produced after fixation, either during or
just subsequent to washing. The wet gelatine layer
becomes more or less finely wrinkled or corrugated, the
network of puckers forming a pattern, generally ex-
tending over the whole of the negative, but sometimes
only over part of it.
As will be seen from the illustrations (Figs. I, II,
III) the "grain" of the network may vary consider-
ably from very coarse dimensions down to very fine
and even microscopic dimensions. This reticula-
facts on the normal swelling and shrinkage of photo-
graphic gelatine film which takes place in this treat-
ment and use.
There are two aspects to this : in one we have only
to consider change of mass or bulk; in the other, change
of shape. As to the first, any piece of gelatine placed
in water within a temperature range of roughly o°
to 200 C. swells, at first rapidly, then more slowly,
and finally reaches a limit. Fig. IV shows the curve
of this swelling plotted against the time.
The limit attained not only depends upon the tem-
perature, but also upon the character of the gelatine,
and, to a very marked extent, upon the presence of
foreign substances, especially electrolytes, in the
water. Acid and alkali in particular have a very
great influence upon the swelling, as will be seen from
tion persists with only slight modification after dry-
ing. At the same time, as will be seen from the fig-
ures, if it occurs on a developed plate, the silver de-
posit undergoes a redistribution along with the reticula-
tion of the gelatine, accumulating in the raised por-
tions and diminishing or vanishing in the valleys or
troughs between.
This reticulation has been utilized in some photo-
mechanical processes; thus it is by the reticulation of
gelatine that the "grain" of a collotype is produced.
It has been employed in the production of irregularly
grained "half tone" screens, in which the reticulation
pattern takes the place of the cross line rulings of the
regular screens.
An understanding of the conditions affecting and
determining reticulation will not only be of practical
use but will tend to throw light upon the physico-
chemical nature of gelatine, and perhaps help toward
the scientific specification of gelatines for photographic
use.
SWELLING OF GELATINE IN WATER AND ITS SHRINKAGE
ON DRYING
The immediate cause and mechanism of reticula-
tion will be best understood if we first consider a few
the curve (Fig. V), which shows results actually ob-
tained with a sample of gelatine.
In this curve the ordinates give the amount of
water absorbed by i g. air-dry gelatine on final swell-
ing (about 48 hrs.) while the abscissae give concentra-
tions of acid and alkali in normality. As is evident,
the swelling or absorption of water is extremely sen-
sitive to both acid and alkali or, in terms of the ionic
theory, to hydrogen and hydroxyl ions. In fact, the
actual sensibility is of the same order as that of the
dyes used as analytical indicators. The minimum ab-
7-'
THE JOURR I/. OF INDUSTRIAL AND ENGINEERING ( HEMISTRY Vol. io, No.
m
130
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Fig. IV
sorption probably lies in reality at a point represented
by the dissociation of pure water, according to the
equilibrium,
H+ + OH" ^± H20,
but this is masked usually by residual acidity or
alkalinity of the gelatine. The precise determina-
tion of this point for a given gelatine will probably
prove of some importance in the specification of photo-
graphic gelatines. It is of great interest since in pass-
ing from an alkaline to an acid state the swelling goes
through a very pronounced minimum.
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The influence of neutral salts in solution upon swell-
ing is too complex to be discussed fully. It will be
sufficient to note that some, such as iodides, act in
the .lire, lion of increasing the swelling (hydration);
others, as sulfates, in the direction of diminishing it . So
long as only salts of the alkali metals and ammonia
are considered, it is the acid part or anion which is
of chief importance, and these salts have been ar-
ranged in a series, indicating their effect upon swelling.
The effect of a given salt depends much upon its con-
centration and above all on the acidity or alkalinity
of the solution.
Now, turning to the influence of shape upon swell-
ing (and conversely) we find that a dominant factor
here is that of the condition in which the gelatine
first swelled or was cast and dried. Gelatine, in the
abstract, as a homogeneous material alike in all direc-
tions, should, theoretically, tend to swell or shrink
uniformly without change of shape, only altering its
mass or bulk. If gelatine could be dried very slowly
so that the loss of moisture proceeded at the same rate
in all parts of the mass then it would shrink without
change of shape, but such a condition cannot be real-
ized in practice and gelatine dries more rapidly on
the surface than in the interior, thus producing stresses
and distortion. In the case particularly important
to us, the gelatine is coated on glass or film support
and firmly attached to it, so that one side is eliminated
as regards drying, etc. The gelatine cannot spread
off the plate, so that its
swelling and shrinkage are
limited to one direction,
viz., that perpendicular to
the plane of the support
(Fig. VI). This state of
affairs is determined in ad-
vance by the first drying
down of the jelly (or
, . , , MO. VI
emulsion) on the support; it
is not peculiar to the photographic film, since ordinary
sheet or leaf gelatine which had been dried on nets
shows the same tendency to have its principal expan-
sion perpendicular to the face of the sheet.
PRODUCTION OF RETICULATION"
A gelatine film, under normal conditions, can be
repeatedly swollen and dried without losing its capacity
to swell and shrink normally to the plate. It is evi-
dent that a certain strain must be imposed upon the
gelatine in drying, which is removed by swelling. If
we consider an ideal unit cube of the swelling gela-
tine, supposed free from all constraint, it would tend
to expand uniformly in all direction^. This ideal uni-
form expansion corresponds to a uniform swelling
pressure, i. c, a pressure the same in all directions.
We can consider this resolved into forces perpendicular
to the surface, and forces parallel to the surface.
Actually, the gelatine layer in sheets or on plates
does not swell uniformly. The forces parallel to the
surfaces which would, of course, tend to remove the
film from the glass or support, must be compensated.
This compensation is in a measure external or initially
external, being due to the adhesion of the gelatine
to a rigid support, but it is chiefly internal, arising
from a uniform strain or tension impressed by the
mode of drying.
Now suppose the gelatine layer be subjected to
^ ' :
Sept., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
drastic internal action, excessive swelling and excessive
dehydration, either successively, or, in a measure,
simultaneously, then gelatine jelly will be strained
beyond its elastic limit, showing either a total or a
partial reaction.
Total reaction would imply the detachment of the
layer from its support, a result which is seen in frill-
ing and floating off, as a result of excessive lateral
expansion.
If, however, the adhesion to the support is main-
tained, but the newly disengaged tangential or lateral
forces are not entirely compensated, then the strain
distribution in the gelatine layer ceases to be uniform
and we get a local puckering or folding, similar in
character to that produced in the earth's surface by
tangential forces acting on restricted areas of semi-
liquid igneous rocks.
Thus the immediate mechanism of reticulation is the
production of restricted tangential dilation, which is
partially arrested.
This, however, leaves unsettled the inner physical
chemistry of the process, that is, the origin of an ex-
cess swelling pressure (the super-pressure) and of a
partial or localized arrest Of this. This can be dis-
cussed best in dealing with specific cases of the pro-
duction of reticulation.
susceptible Of control, although it must be emphasized
that in any case the balance between hardening and
softening agents must be delicately adjusted, and
that the measure of control is limited. Further,
the occurrence or production of reticulation is in a
very large degree dependent upon the nature of the
gelatine. The so-called "hard" gelatines tend readily
to reticulation, while the "soft" ones only give transient
signs of it.
An experiment on this point gave the following re-
sults:
Gelatine
A- Hard...
B-Hard...
C-Soft...
D-Soft....
E-Soft
Reticulation in Potassiun
Mercuric Iodide
Strong, permanent
Strong
Very faint, transient
Very faint, transient
Very faint, transient
The following results were obtained with combina-
tions of softening and hardening agents 3 and 4.
chromic acid and hot water — Chromic acid is,
of course, a well-known hardening agent for biological
tissues. Working with 8 per cent hard gelatine,
machine-coated on glass, a 10 per cent solution of
chromic acid at 200 to 22° C, followed by washing
with water at 56 ° C, was found to afford the best con-
ditions.
EXPERIMENTAL PRODUCTION OF RETICULATION
A typical case, which has the advantage of following
ordinary photographic procedure, is as follows: A
Seed 23 plate is "flashed," developed in a standard
pyrosoda developer for 4 min. at 8o° F., then rinsed,
and fixed in a standard hypo-bisulfite fixing bath at
8o° F. Reticulation was then found to depend upon
the temperature of the wash water as follows:
Temperature Reticulation
70° F. None
80° F. None
90° F. Faint
100° F. Strong
Instead of water, stronger and more definite results
were obtained by an after-treatment with the follow-
ing solution:
50 cc. 95 per cent Ethyl Alcohol
40 cc. ."> per cent Formaldehyde
1 10 cc. Water
In this case the following factors may have played
a part:
1 — Prehardened gelatine in the emulsion.
2 — Tanning agents produced in development.
3 — Excess swelling pressure in hot developer, etc.,
and particularly in washing.
That reticulation can be produced by the combined
action of both a swelling or softening agent and a
hardening or anti-swelling agent to restrain this is
shown hy the production of reticulation by the follow-
ing combination:
Hardening Agent
. . Tannic Acid
. Quinone
Softening Agent
Acetic Acid
Acetic Acid
Hot Water
Potassium Iodide
All of these combinations produce reticulation,
but 1 and 2 have only a theoretical interest, as they
are difficult to control. The other two pairs are more
' - --:._... •* "
Fig. VII
potassium mercuric iodide — The solution of mer-
curic iodide in potassium iodide known as Brucke's
reagent was found to be a convenient strength for use.
According to the formula for this, 120 g. of mercuric
iodide are to be dissolved in a solution of 50 g. potas-
sium iodide in 500 cc. water, and the whole diluted
to 1000 cc. We found, however, that under these
circumstances only about 72.6 g. of mercuric iodide
could be dissolved at room temperature; nor was this
result much affected by heating to 500 C. It should
be noticed that these quantities are near to those
necessary for the double salt, 2KIHgI2 or K?HgI4.
In this combination, the softening agent is the iodide,
or more specifically the iodion, I-, while the hardening
73°
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol.
Xo.
or coagulating agent is the mercuric salt, or, again, the
mercuric ion Hg++. Attempts made to increase the
proportion of mercury were without success. A
saturated solution of potassium iodide at i8° to 200 C.
was made, containing 128 g. potassium iodide to 100
cc. of water, or 56.2
g. in 100 g. solution,
which agrees fairly
with the value 50 per
cent at 200 C. given
as the solubility in
Landolt - Bornstein.
This solution was sat-
urated at 20° C. with
mercuric iodide, tak-
ing up 64 g. In this the ratio of 2KI to Hgla is 0.69,
whereas the actual double salt would call for o. 73.
This solution was used as a saturated stock solution
and Brucke's reagent is equivalent to 10 parts stock
saturated plus 90 parts water.
Working with the 10 per cent saturated (Brucke's
reagent) and hard gelatine, 8 per cent machine-coated,
the following results were obtained:
V////////////////A
Fig. VIII
Effect
Small pock marks about 1 mm. apart pro-
duced in 40 sec. followed by reticulation
which was much lessened in drying
As before, but reticulation somewhat more
persistent on drying
As before, but with continued treatment
reticulation became fainter and vanished
on drying
As before, but the whole surface finally soft-
ened and could not be dried, softening and
2Vi.
3Vt.
After treatment, this was chilled 15 min. on
ice, then immersed for 2 min. in 3 per cent
formaldehyde. This conserved the re-
ticulation
The formaldehyde after-treatment seems generally
necessary with this agent to "fix" the reticulation.
Using soft gelatine, 6 per cent solution machine-
coated, and a wide range of concentration of the potas-
sium mercuric iodide solutions, only slight and transi-
tory reticulations were observed in the higher concen-
trations, giving way, however, to a general softening
and liquefaction. Attempts to overcome this by pre-
liminary hardening with formaldehyde were not suc-
cessful. Prehardening with chrome alum showed
better results. In the case of the mercury -potassium
iodide combination, while it is not possible to increase
Fig. IX
the mercuric iodide ratio above a certain limit, other
permanent or temporary hardeners may be added. In
particular it was found that Brucke's reagent with
the addition of 6 per cent of saturated Na2SO< solu-
tion gave very fine, uniform reticulation.
Sodium sulfate used in the reticulation process
makes the "grain" finer, while after-treatment with
formaldehyde increases or conserves the depth of the
wrinkles.
An important conclusion from these experiments
is that apparently reticulation may start in more than
one way. Thus with the Brucke reagent, and with
chromic acid followed by hot water, reticulation
proper was generally preceded by the appearance of
small pock-like markings of about 0.2 to 0.3 mm.
diameter. These would sometimes align themselves
in "streaks," and in any case seemed the foci of the
subsequent reticulation. These markings are shown
in Fig. VII. On the other hand, in the reticulation
produced by the use of hot water after development
and fixation, these initial markings did not appear.
EFFECT OX THE SILVER IMAGE
It is noteworthy that when the reticulating film
contains developed silver particles — as in negatives
. • .''■.'-■■•■■ '■ ' L- . '. v > :% ■'<■''■ .'♦:."-.
.j~. •*••■: V •■ / • . -'-v- • • . •
".-'■ *tC:*r\ '
.-'.-*C :"'~ '
-. - :r-- •.:/•• ■ • •■••-. ."-£•' ;•;»"-
after fixation — there is an apparent migration of the
silver particles, the ridges being denser, the valleys
much less dense or even quite clear.
The question arises, whether reticulation is simply
a puckering of a sheet grown larger by lateral dila-
tion, larger than the support boundaries, but retained
on this by local adhesion, particularly at the edges, as
is indicated in Fig. VIII, or is a mosaic-like alteration
of hardening and softening effects, the ridges being
more swollen, the valleys more tanned, as suggested
by Fig. IX.
It is evident that in the first case the excess in the
ridges is simply due to the total thinning (by the
lateral dilation) plus local thickening due to folding
of the increasing sheet. In the other case, the greater
density in the ridges would be due to an actual migra-
tion of silver due to tension, similar to that occurring
on the drying of moisture spots, when the tension in
drying softens the gelatine and forces the particles
into the periphery of the spot. This effect is shown
in Fig. X, a drawing made by Mr. M. B. Hodgson
Sept., 101S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
73 i
from microscopical observations. In the latter case
we should have in reticulation a great and increasing
number of microscopic replicas of such "moisture
spots," tending to run into each other and form one
system, like cracks in a drying mass.
The theory of alternate softening and hardening, or
of differential swelling, couples up readily with the
fact already noticed that in many cases reticulation
starts from a number of isolated points. When
softening and tanning agents are present together in
a gelatine gel, a certain amount of selective adsorption
and differential diffusion will occur. A molecule or
ion having a tanning action will tend to be adsorbed
or fixed in situ, and its own specific diffusion will be
hindered. Molecules or ions having a softening
action may modify the action on tanning agents,
but their own diffusion will be facilitated by their
hydrating and softening action on the gelatine.
It is easy to see that we should have then a condi-
tion of rhythmic coagulation of the gelatine very
similar to that shown in the well-known Liesegang
rings. In this latter case, when two salts which re-
act to form a precipitate are allowed to diffuse to-
gether through a gelatine gel, the precipitate, such as
silver chromate or silver halide, is not deposited uni-
formly, but rhythmically, in alternate rings or
layers.
Actually it is observed that reticulation generally
starts in one or more regions and fills up by the spread
of these; in some cases from isolated foci. It seems
then that reticulation in its earliest stage involves
something like the nucleation of a crystallizing solu-
tion. In such a solution, crystallization may start
either at nuclei already present in the solution or by
the formation of new ones, but in the latter case
there is required a higher degree of supersaturation
for crystallization to start. At what points in such
solution or melt the first nuclei appear is a matter
of pure chance and it is apparently much the same
with the start of reticulation.
THE CONNECTION BETWEEN RETICULATION AND THE
"GRAININESS" OF NEGATIVES
In one important case where it is very probable
that incipient reticulation is at work, foreign nuclei
are available. This is in the case of the ordinary
development of a photographic emulsion.
It is known that, apart from differences in emul-
sion, different developing agents and treatments af-
fect the "graininess" of the developed image. By
this is not to be understood the elementary plate
grain, but such clumping in second order aggregates
as is liable to be objectionable in projection. This
granulation depends upon development, and in the
same way, resolving power depends upon development
and the developer.1 It is hardly to be doubted that
we have in this case a selective adsorption and differ-
ential diffusion of developers, producing what
amounts to incipient reticulation, nuclei being formed
by the developed silver particles, with their tendency
to adsorb the colloidal reaction products of develop-
ment, which have tanning or coagulating properties.
Consideration of the great change in the swelling
equilibrium shown on passing from an alkaline to an
acid condition (Fig. V) shows also that the opera-
1 K. Huse, "Photographic Resolving Power," J. Am. Optical Soc,
1 (1918), 119.
73*
THE JOURNAL OF INDUSTRIAL AND ENGINEERING ( HEMISTRY Vol. 10. No. 9
tions subsequent to development are very liable to
develop still further any sub-microscopic reticula-
tion, and again to coarsen the "grain'' of the image.
It is hoped to follow this up experimentally when
time permits, instruments having been devised for
measuring both granularity and minute swellings.
In Fig. XI are given photomicrographs of some of
the reticulated preparations described, taken with
vertical illumination at 100 diameters.
Research Laboratory
Eastman Kodak Company
Rochester, N. Y.
LABORATORY AND PLANT
METHODS OF ANALYSIS USED IN THE COAL-TAR
INDUSTRY. I— CRUDE TARS
By J. M. WBISS
Received July 20, 1918
INTRODUCTION
In April 191 1, S. R. Church1 published a paper
which described in some detail the analytical methods
as used by The Barrett Company at that time. This
was supplemented by a later paper in 1913,2 giving
certain revisions and additions which had been made
up to that time. These methods, with others, have
been in use in the laboratories of The Barrett Com-
pany and many other companies for an extended
period and have been given the test of continued use.
Some of the methods have been the subject of exhaus-
tive investigations to determine the variants which
limit the accuracy of the tests. For instance, J. M.
Weiss presented a paper3 dealing with the "free car-
bon" tests on tars and pitches and the factors influ-
encing the results, together with some theoretical con-
sideration of the material known as "free carbon."
There have also been numerous publications on the
testing of tar products, emanating from various
sources, such as the Office of Public Roads, the U. S.
Department of Agriculture, the American Society for
Testing Materials, the American Gas Institute, etc., and
"also from many individuals, but we do not intend to pre-
sent here a bibliography of the literature on coal-tar
product methods of analysis, but merely to indicate
under a few of the tests published the main sources
from which we have drawn.
About a year and a half ago, we realized that the
directions of our testing methods were more or less
incomplete in detail and that in many cases important
points were left unemphasized. Accordingly, a chem-
ists' committee was formed, consisting of S. R. Church,
F. J. Gerty, J. B. Hill, K. B. Howell, H. E. Lloyd,
J. G. Miller, M. R. Walczak, and the writer, whose
purpose it was to revise and standardize the existing
tests. A description of each test was prepared by
one or another of the committee and sent for comment
to each member of the committee, a majority of whom
were actual laboratory workers of long experience.
The comments were compiled and, where necessary,
experimental work was instituted to settle points
which were in dispute. The methods were not put
into final form until the committee was substantially
unanimous regarding all the details of the methods.
We are presenting in this paper a selected list of
methods which we believe are of very general interest
1 This Joi-rnai.. 3 (19111, 227.
1 Ibid., 5 (191.li. 195,
' Ibid., 6 (1914), 279.
to all engaged in the manufacture or use of coal-tar
products. This paper will be followed by three others,
one dealing with the methods of test for refined tars
and pitches, another with methods of test for creosote
oils and carbolic oils, and the last, benzols and light
oils.
Many of the tests are widely used throughout the
country and have been adopted by a majority of the
producers and consumers of tar products. A number
of these tests are the standard methods of such asso-
ciations as the American Railway Engineering Asso-
ciation, American Society for Testing Materials, etc.
We are presenting them in the belief that it will be
helpful to those engaged in the testing of tar products
to have these standard methods collected together in
compact form convenient for reference. The illus-
trations are mainly assembly drawings, but the special
apparatus can now be obtained through almost any
apparatus house. We have furnished detailed plans
and specifications of all our special laboratory appara-
tus to every chemical glassware manufacturer and lab-
oratory supply house of whom we were cognizant.
For each test on which we have carried out sufficient
exhaustive research, to enable us to do so, we have
made a statement as to its accuracy.
SAMPLING
Before considering the tests in detail a few words on
sampling would not be out of place.
The sole practical purpose of laboratory testing or
analysis is to obtain information as to the composi-
tion, quality, and properties of a given material.
Usually, this material is in large bulk. To make the
desired test on the entire bulk of material would ob-
viously be impracticable as well as necessitating fre-
quently the destruction of the material. It therefore
becomes necessary to select from the bulk of a ma-
terial, a portion or sample of same, which shall be
representative of the entire bulk and which can be
tested and its properties determined. Obviously, the
interest and commercial values attach to the proper-
ties and qualities of the bulk of material and only to
the properties and qualities of the sample as far as the
sample is representative of the bulk. It is therefore
necessary to take every possible precaution to see
that the sample is in every case representative. The
laboratory methods, apparatus, and technique may
be perfect and the results recorded may be accurate
as to the quality of the sample tested. If. however.
that sample is not representative of the bulk, the
value of the test is commercially nil. The entire
theory of sampling is therefore based on the principle
Sept., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
733
of obtaining a sample which shall be and remain repre-
sentative.
Materials may be grouped as homogeneous and
heterogeneous. A homogeneous material is a material
which is uniform in quality and composition through-
out. A heterogeneous material is one which varies
in quality or composition throughout. There is, of
course, no such thing as a perfectly homogeneous ma-
terial, except in the cases of pure chemical compounds.
true solutions, and mixtures of perfect gases. Ob-
viously, a sample taken from any part of a homo-
geneous material will be representative of the entire
bulk. Sampling of homogeneous materials therefore
becomes a relatively simple matter.
liquids — The sampling of liquids presents a some-
what more difficult problem. Where the liquid is
thin, non-viscous, and does not contain immiscible
constituents, a homogeneous condition usually ex-
ists, and a sample from any part of the bulk is usually
representative of the whole. Where, however, viscous
or immiscible materials are present, the constitution
is usually heterogeneous.
Most of the liquids handled by the coal-tar chemist
fall into this latter class. In such cases, great care
must be taken to obtain thoroughly representative
samples. While it is impossible to set absolute stand-
ards as to the methods of sampling these materials,
the following mehods represent good practice.
method I — A \ 2 in. sampling pipe shall be inserted
in the line through which the oil is being pumped,
on the discharge side of the pump, preferably in a
rising section of the pipe line. This sampling pipe
shall extend half way to the center of the main pipe
and with the inner open end of the sampling pipe
turned at an angle of oo° and facing the flow of the
liquid. This pipe shall be provided with a plug cock
and shall discharge into a receiver of 50 to 100 gal.
capacity. The plug cock shall be so adjusted that,
with a steady continuous flow of the oil, the receiver
shall be filled in the time required to pump the entire
shipment. The receiver shall be provided with a
steam coil sufficient to keep the contents at a tempera-
ture not exceeding 120° F. Immediately upon com-
pletion of the pumping, the contents of the receiver
shall be very thoroughly agitated and a duplicate 1 qt.
sample taken immediately for the test. The amount
of the drip sample collected shall be not less than 1
gal. for each 1000 gal. of oil handled, except in the
case of large boat shipments, where a maximum of
100 gal. is sufficient. Care must be taken that the
bleed cock does not shut off partially or entirely dur-
ing the pumping. It is necessary to insure a uniform
flow of material throughout.
method II — Where the material to be sampled is
handled by gravity flow, Method I can frequently be
employed by inserting a drip sampler into the end of
the discharge nipple. Where this is for any reason
impracticable, an alternate method, II, consists in
taking dipperful samples at, frequent and regular inter-
vals, from the open stream. These dipperful sam-
ples should be combined in a covered receiver. The
combined gross sample should be not less than o. 1
per cent of the whole material of which the sample
is representative. The combined gross sample should
be placed in a receiver, in which the material can be
kept fluid, and stirred thoroughly to homogeneous con-
sistency. Small samples may then be taken for
analysis.
While it is preferable to take a sample of material
during passage through a pipe or in gravity flow, it
is also necessary to take samples of materials while at
rest, as in storage tanks, mixing tanks, etc. In such
cases, Method III or IV shall be employed.
method III — Small bottles weighted with metal
should be fitted with tight stoppers to which strings
are attached. The bottle shall be lowered to a fixed
depth into the liquid, whereupon the cork shall be
pulled from the bottle by the string and the bottle al-
lowed to fill with material. After sufficient time for
the filling of the bottle, it is pulled up. A cut of a
suitable arrangement in use at several of our plants
is shown in Fig. I.
Dctai I
of
Bottle Sampler
Note
A Tolerance of 10% is
Allowable in Dimensions
Elevation
Fig. I
Bottled samples should be taken from a sufficient
number of differenl depths in the liquid to insure
obtaining a combined sample which is representative
of the whole. The combined sample should then be
agitated and a similar sample taken from it for analy-
sis. In case the cross-sectional area of the container
734
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No.
varies throughout the vertical depth of the liquid, a
number of samples should be taken at different levels,
the number at each level being proportional to the
cross-sectional areas at such levels.
In tank cars for all ordinary cases we recommend
that samples be taken from three zones, viz., the top
foot section of the car, the middle foot section, and
the bottom foot section. These should be combined
in various proportions depending on the diameter
of the car. We recommend that composite samples
be made up as shown in the following table:
jam. of car
Feet
Zone
Proportionate weight
to be given sample
6
(Top
■, Middle
\ Bottom
25
11
7
, Middle
■ Bottom
I Bottom
1
2
1
8
Top
• Middle
I Bottom
1
3
1
Of course, if free water is present in large amount,
this should be noted separately and care be taken not
to include it in the samples taken.
method IV — Many storage tanks, particularly large
ones, are equipped with sample cocks along the side
of the tank and arranged at one-foot intervals. After
taking samples by this method an equal amount is
drawn from each cock and the samples thoroughly
mixed before the final laboratory sample is taken.
(This, of course, assumes that the tank is one of uni-
form cross section.) In taking a sample by this
means, the nipple from each cock shall extend at
least 6 in. inside from the shell of the tank and the
operator shall allow sufficient material to flow through
the cock to clear the line before taking his final sam-
ple. We would caution the operator, however, that
samples from the side of the tank should not be taken
too close to the bottom of the tank. This will avoid
inclusion of the sediment normally present in the bot-
tom of the tank.
solids — Solids are almost always heterogeneous in
constitution. It is impossible to advise definite and
arbitrary methods for obtaining samples. Each case
must be worked out for itself, bearing in mind the
particular conditions in the case. It is usually pref-
erable to take samples during the unloading of cars
or the transit of the material in conveyors. In such
cases, a number of small samples should be taken at
frequent and regular intervals from the material in
transit and these samples combined to form a repre-
sentative combined sample.
Occasionally, solids are tested as received, in bags or
barrels. In such cases, it is desirable to take a small
sample from every »th bag or barrel combining same
to obtain the representative combined sample.
Generally, samples taken from the bulk, in piles or
cars, are unreliable and not representative. Where
it is necessary to take such samples before the un-
loading of the car, small samples should preferably
be taken from at least twelve spots throughout the
bulk and these small samples collected to form the
representative combined sample.
In taking such small samples, it is desirable to take
8 samples from the corners of the car, 4 near the bot-
tom, and 4 near the top of the material. To these
should be added 4 samples from the center of the car.
2 from the top, and 2 from the bottom of the material.
The combined representative sample taken by any
of the above methods should be in amount at least
0.1 per cent of the total bulk of material sampled.
These combined samples should be carefully mixed
and reduced in size to a convenient laboratory sam-
ple, by the standard method of quartering. In carry-
ing out this quartering, a hard clean surface should be
selected, free from cracks and protected from rain,
snow, wind, and beating sun. Do not let cinders,
sand, chips from floor, or any other material get into
the sample. Protect the sample from loss or gain in
moisture. The combined sample should be care-
fully mixed, spread out on this surface into a circular
layer and divided into four equal quadrants. Two
opposite quadrants should be combined to form the
representative reduced sample. If this sample is
still too large for laboratory purposes, the quartering
operation shall be repeated. In this manner, the
sample shall finally be reduced to a size suitable of
handling by the laboratory.
general PRECAUTIONS — Scarcely second in im-
portance to the necessity of obtaining a representa-
tive sample, is the necessity of preventing the composi-
tion or property of the sample from changing during
handling or storage prior to laboratory analysis. Some
materials are very hygroscopic and must be kept in
tightly stoppered bottles to prevent absorption of
moisture. This is particularly true of dry felt, lime,
and finely divided mineral materials. Other materials
are volatile and must be kept in tightly closed cans or
bottles to prevent loss of their lighter constituents.
A great many samples are taken of hot materials
in process of distillation where the high temperature
has produced a high vapor pressure which will cause
considerable loss of the more volatile constituents
when exposed to the atmosphere. Usually in the case
of these materials, the volatilization of oil is apparent
by the vapor rising from the liquid and becoming con-
densed in the cold atmosphere to a cloud. In the
case of some of the lower-boiling materials, however,
a high vapor pressure is produced at moderately low
temperatures and a volatilization of the sample is
continually going on, although this may not be so
apparent by reason of the fact that the vapors from
this material are not readily condensed in the atmos-
phere.
It is, therefore, particularly desirable to watch the
sampling of such materials carefully and make sure
that the sample is kept in a tightly covered container
until it has cooled to a point where it exhibits an
inappreciable vapor pressure.
CRUDE TAE TESTS
TKST B2 WATER
apparatus — Copper still, 6 in. by 5! 2 in. Ring
burner to fit still. Connecting tube. Condenser
Sept., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
trough. Condenser tube. Separatory funnel. Ther-
mometer, o°— 250° C. See Fig. II.
V- n"Z'
H\
method- — Fifty cc. of coal-tar naphtha or light oil
shall be measured in a 250 cc. graduated cylinder.
200 cc. of the tar to be tested shall be added. The
contents shall be transferred to the copper still, the
cylinder shall be washed with 100-150 cc. more of
naphtha, and the washings added to the contents of
the still. The lid and clamp shall be attached, using
a paper gasket, and the apparatus set up as shown in
Fig. II. The condenser trough shall be filled with
water. Heat shall be applied by means of the ring
burner, and distillation continued until the vapor
temperature has reached 205 ° C. (401 ° F.). The
distillate shall be collected in the separatory funnel,
in which 15 to 20 cc. of benzol have been previously
placed. This effects a clean separation of the water
and oil. The reading shall be made after twirling the
funnel and allowing to settle for a few minutes. The
percentage shall be figured by volume.
precautions — When fresh supplies of naphtha or
light oil are obtained, they shall be tested to deter-
mine freedom from water.
accuracy — One-tenth of 1 per cent.
note — For works-contro'l an iron still of the same
size and shape as the copper still specified above may
be used. Some laboratories omit the use of the ther-
mometer and judge when the water is off by the ap-
pearance of the distillate . These variations must
never be applied where check test is required or in
case of dispute.
TEST B3 DEHYDRATION (PREPARATION OF DRY TAR)
apparatus — Same as Test B2.
method — About 300 to 400 cc. of tar shall be placed
in the copper still without the addition of naphtha.
The apparatus shall be set up as in Fig. II, except that
an ungraduated separatory funnel may replace the
special graduated one. The distillation shall be car-
ried on cautiously at first to prevent foaming and con-
tinued until the vapor temperature reaches 1700 C.
(3380 F.). Any oil which has distilled over shall be
separated from the water (warming sufficiently, if
crystals are present, to insure their solution). This
separated oil shall be thoroughly mixed back into the
residual tar in the still, after the latter has cooled to a
moderate temperature. The dehydrated tar shall be
then transferred to a suitable container.
note — A temperature of 1700 is used because this
is sufficiently high to expel all water from the still.
In Test B2 a higher temperature is used to insure flush-
ing out the condenser tube.
TEST B4 SPECIFIC GRAVITY (SPINDLE)
apparatus — Hydrometer: special, calibrated against
water at 15.5° C. (6o° F.), of suitable scale range.
Cylinder: see Fig. II.
method — It is not usually possible to make the test
by this method at 15. 5° C. (6o° F.) as ordinary tars are
not sufficiently liquid at this temperature. The
cylinder shall be filled with the dry tar (see B3), the
latter thoroughly stirred, and the temperature noted.
The hydrometer shall be inserted and the reading
taken. Care shall be taken that the hydrometer does
not touch the sides or bottom of the cylinder and that
the surfaces of the tar are free from froth and air bub-
bles. For every degree centigrade above 15.5° C, at
which the test is made, add 0.000685 t0 the observed
reading. (This is equivalent to 0.00038 for every
degree Fahrenheit above 6o° F.) Unless instructed
to the contrary, report results at 15.5° C. (60 ° F.).
accuracy — This method is not recommended as an
accurate method. If accuracy is desired, use Test
B5 or B6. It is sufficiently accurate for ordinary
testing of incoming tar shipments.
note — The hydrometer used, when first obtained,
should be standardized.
test B5 — specific gravity (pycnometer)
apparatus — Modified Hubbard Bottle (Fig. III).
Wafer Inlet/'
Wire support lor.
Filter Cup
No 4
Condenser Alo 2
Copal filftreaperarAluralymlttrt
FitlrCvp (2 "so Whatman's Ibpaj
No. 3
Flask No 1
Ettracior For Free Cart/on
Fig. Ill
No5
Specific Gravity Bottle
No. 6
PlatinfrnSpecifiC OrjrituPon
standardization of bottle — The bottle shall be
weighed empty, filled with water, and held in a bath at
15. 50 C. (6o° F.) until the volume becomes constant.
The water shall then be adjusted to the mark, the
bottle dried superficially, and weighed. Each bottle
used in the laboratory should be numbered and a
736
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 9
record kept of its weights — empty, and filled to the
mark with water at 15.5° C. (60 ° F.).
METHOD — Tar, dehydrated as under B3, shall be
used. Introduce 10 g. of dry tar into the bottle at
40°to 50° C; allow to cool and weigh. Freshly boiled
distilled water shall then be added and the bottle
kept in a bath at 15.5° C. (60° F.) until no further
volume change takes place. (This usually takes
about 30 min.) The water shall then be adjusted to
the mark, the bottle dried superficially, and weighed.
Let A = weight of bottle
B = weight of bottle + water at 15.50 C.
C = weight of bottle + tar
D = weight of bottle -j- tar ■+- water at 15.5 ° C.
Then: Sp. gr. at 15.5 ' C. = {B_^Z^_C)
precautions — The use of freshly boiled distilled
water is essential to accurate results.
accuracy — Within 0.003.
note — In exceptional cases tar is very liquid, and,
upon the addition of water, partially floats through the
water, giving an oily film on the surface. In such
cases, do not add water, but fill the bottle with tar,
hold at 15.5° C. (6o° F.) until the volume becomes
constant, adjust to the mark and weigh. The weight
of the tar divided by the weight of water necessary
to fill the bottle to the mark at 15.5° C. (6o° F.)
gives the specific gravity.
TEST B6 SPECIFIC GRAVITY (PLATINUM PAN)
apparatus — Special platinum pan (Fig. III).
standardization of pan — The clean pan shall be
ignited, cooled, and suspended by a waxed thread on
the left-hand arm of an accurate chemical balance. Its
weight in air and its weight in freshly boiled, distilled
water at 1 5 . 5 ° C shall then be noted in the usual way.
method — The clean pan shall be filled with tar and
suspended from the balance by the same thread as
was used in the standardization. The weight of the
pan plus tar should be noted, first in air and second
in freshly boiled, distilled water at 15 . 5 ° C.
Let A = weight of pan in air
B = weight of pan in water at 15.50 C.
C = weight of pan and tar in air
D = weight of pan and tar in water at 15.5° C.
(2 a
Then: Sp. gr. at 15.5° C. =
0 (C — A) — (D — B)
precaution — Allow the pan and tar to remain in
water at 15. 5 ° C. for 10 min. before taking the water
reading.
accuracy — Within 0.003.
TEST B7 INSOLUBLE IN BENZOL (FREE CARBON)
apparatus Extraction flask. Condenser and cover,
wire support. See Fig. III. Extraction thimble (pre-
pared by operator1). Cap of filter paper or alundum.
1 These shall be made of Whatman No. 50 filter paper. To make a
cup, two 15 cm. circles shall he taken and one cut down to a diameter of
14 cm. A round stick about 1 in. in diameter shall be used as a form.
The stick shall be placed in the center of the circles of filter paper, the
smaller inside, and the papers folded symmetrically around the stick to
form a cup about 2]/i in. lone.. A little practice enables the operator to
make these evenly and quickly. After being made they shall be soaked
in benzol to remove grease due to handling, drained, dried in a steam oven
at 97" to 100° C. cooled in ■ desiccator and kept there until used.
The latter are 30 mm. inside diameter by 14 mm.
high. Balance: an ordinary analytical balance ac-
curate to 0.0005 g- Steam bath, water bath, or elec-
tric hot plate. Beakers, 100 cc. Carbon filter tubes,
37 mm. size. Weighing bottle, 32 mm. by 70 mm.
Camel's hair brush, 14 mm.
method — Tar dried as under B3 shall be used.
After drying, it shall be passed hot through a 30-mesh
sieve to remove foreign substances. The amount of
tar to be taken for test depends on the content of in-
soluble material and shall be:
Less than 5 per cent. 10 g.
5 per cent to 20 per cent, 5 g.
Above 20 per cent, 3 g.
If the content of insoluble material cannot be ap-
proximated, the larger amount shall be taken. The
amount shall be weighed into a 100 cc. beaker and
digested with pure toluol at oo° to ioo° C. for a
period of not over thirty minutes. The solution shall
be stirred to insure complete digestion. A filter cup
prepared as described shall be weighed in a weighing
bottle and placed in a filter tube supported over a
beaker or flask. The thimble shall be wet with toluol
and the toluol-tar mixture decanted through the fil-
ter. The beaker shall be washed with toluol until
clean, using the camel's hair brush as a policeman to
detach solid particles adhering to the beaker. All
washings shall be passed through the filter cup. The
filter cup shall then be given a washing with pure
benzol and allowed to drain. The cap shall then be
placed on the cup and the whole placed in the extrac-
tion apparatus and extracted with pure benzol until
the descending benzol is completely colorless. The
cup shall then be removed, the cap taken off, and the
cup dried at 97 ° to 100° C. After drying, it shall be
allowed to cool in a desiccator and weighed in the
weighing bottle. The increase in weight represents
matter insoluble in benzol.
precautions — If the first filtrate shows evidence of
insoluble matter, it should be refiltered. The 30-min.
period allowed for digestion must not be exceeded.
accuracy — s per cent of insoluble matter present.
In other words, with 20 per cent of "free carbon"
present, a 1 per cent accuracy may be expected.
note — Where only approximate results are desired,
tars containing not over 5 per cent of water may be
tested without dehydration and the results calculated
back to a dry tar basis.
TEST B8 FIXED CARBON1
apparatus — Platinum, Rhotanium, or Palau cruci-
ble, 20 cc, standard shape, provided with a tightly
fitting cover.
method — Dry tar (see B3) shall be used. One
gram of tar shall be placed in the crucible, the cover
applied, and the crucible placed on a platinum, ni-
chrome, or fireclay triangle over a Bunsen burner,
with the bottom of the crucible 6 to S cm. from the
top of the burner. The burner flame shall be regula-
ted to a height of 20 cm. when burning free. The tar
' Based on report of Committee on Coal Analysis. J. Am. Chtm. So*..
SI (1899), 1116. el stq.
Sept., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
737
shall be heated gently until the tendency to foam has
passed and shall then be exposed to the 20 cm. flame
of the burner for 7 min. At the end of this period the
flame shall be removed, the crucible transferred to a
desiccator, and allowed to cool. The residue in the
crucible, less ash, is "fixed carbon."
precautions — The test shall be carried out in a part
of the laboratory free from draughts. The upper sur-
face of the crucible cover should be free from carbon at
the end of the ignition period.
accuracy — 1 per cent.
note — The loss on ignition in the above test is
called "volatile combustible matter" and may be re-
ported if desired.
TEST B9 ASH
apparatus — Open platinum, porcelain, or silica
crucible.
method — Tar dried as under B3 shall be used.
Weigh 10 g. of tar into the crucible and incinerate to
constant weight. The residue in the crucible is ash.
precaution — The heating shall be conducted so as
to avoid foaming at the start or carrying away of ash
during the ignition. It should be carried out in a part
of the laboratory away from currents of air.
test bio — viscosity (engler)
apparatus — Engler viscosimeter: A. H. T. 41352;
E. & A. 4790, or improved model A. H. T. 41360;
E. & A. 4792. The latter type differs from the former
in that the inner container is totally immersed in the
outer bath and the top of the inner container is double-
walled. The outer bath is also larger and provided
with a stirrer. It is easier to maintain a uniform tem-
perature with the latter instrument, but with careful
temperature regulation identical results are obtained
with both instruments. Sugar flasks, 100 cc. Stop-
watch.
method — Tar dried as under B3 shall be used. Be-
fore use it shall be screened through a 20-mesh wire
gauze to remove extraneous matter. The tar shall
be heated on a steam bath to approximately the cor-
rect temperature before introduction into the vis-
cosimeter. The outer bath shall be kept at a tem-
perature of from 1° to 3° C. above the inner tempera-
ture desired. The tar shall be filled in up to the top
of the fixed points in the viscosimeter. (This requires
approximately 250 cc. of tar.) The tar shall be kept
at the proper temperature for 3 min., the plug released,
and the time of flow (in seconds) of 100 cc. noted.
precautions — In allowing the material to run from
the viscosimeter, it is better to let it impinge on one
side of the measuring flask, as this avoids the forma-
tion of bubbles and consequent obscurity of the read-
ing. After each test the aperture should be examined
to make sure that it is free from obstruction.
The aperture should be cleaned with a soft piece of
tissue paper and not with rough twine or any other
material which may scratch or damage the aperture.
Up to 8o° C, water may be used as the bath in
the outside jacket; above this, it is better to use a
heavy lubricating oil.
notes — The temperature differential to be main-
tained between the inner and outer baths varies with
the temperature of test and the room temperature.
The temperature of the inner bath usually drops after
the material has flowed out to a point sufficient to
uncover the thermometer bulb (more particularly
with the old type of Engler viscosimeter), but if the
outer bath remains constant, this apparent drop does
not affect the results.
Some specifications require the use of 200 cc. In
this case use 200 cc. sugar flasks and note the time of
flow of 200 cc, otherwise the procedure is the same.
Specific viscosity is sometimes required. This is a
ratio and is obtained by dividing the time of flow of
the material by the time of flow of an equal volume of
water at the same temperature. Unless otherwise
stated, the volumes compared should be 200 cc.
TEST B1I SULFUR
apparatus — Crucible 50 cc. platinum, nickel, or
silica. Usual inorganic, gravimetric, analytical ap-
paratus.
method — One gram of material shall be weighed
into the crucible and 1.5 g. of Eschka mixture added.
(Eschka mixture consists of 2 parts of pure magnesium
oxide and 1 part of pure anhydrous sodium carbonate.
The mixture should be light and fluffy.) The tar and
Eschka mixture shall be intimately mixed and the
crucible placed over a very low Bunsen flame. The
crucible shall be set in a round hole in a 6 in. sq.
asbestos board so that the flame impinges only on
the bottom of the crucible and the products of com-
bustion from the burner are deflected from the open
top of the crucible.
The heating of the crucible shall be conducted
very slowly until no more fumes are given off. This
requires 5 to 6 hrs. The heat shall then be gradually
increased and the mixture stirred with a platinum rod
or wire until all the carbon particles are burnt off
and the mass is white. At the close of the ignition
the bottom only of the crucible shall not be more than
at a dull red heat. The white residue shall be washed
into a beaker with 200 cc. of water, 20 cc. of pure
bromine water added, boiled for 5 min., and filtered.
The precipitate on the filter shall be washed with
boiling water until the filtrate gives no test for bro-
mides with nitric acid, and silver nitrate solution. The
filtrate and washings shall be combined, acidified
with 5 cc. of pure concentrated hydrochloric acid,
and the excess of bromine removed by boiling. 10 cc.
of 10 per cent pure barium chloride solution shall
then be added drop by drop to the boiling solution
and the precipitated barium sulfate allowed to col-
lect and agglomerate by standing in a warm place
over night. The barium sulfate shall be filtered out
in a Gooch crucible, using suction, washed with hot
water until free of chlorides (test with nitric acid and
silver nitrate), ignited, cooled in a desiccator, and
weighed. From the weight of barium sulfate, deduct
the weight obtained in a blank test (see Notes below)
and multiply by 0.13734 to obtain the weight of
sulfur.
73«
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, Xo. o
notes — A blank test shall be made heating the same
length of time under the same conditions as in the
regular determination, and using the same amount
of all reagents in each step of the test.
The asbestos mat on the Gooch crucible used in filter-
ing the barium sulfate should be prepared as follows:
Finely cut Tremolite (Italian) asbestos is shaken up
with water and an asbestos mat deposited under suc-
tion on the Gooch. The mat is washed with dilute acid,
dilute alkali, and distilled water, and the crucible
ignited. The washing and ignition are repeated to
constant weight. A Gooch prepared in this way is
quick and accurate, quick because of speed of wash-
ing and the fact that there is no paper to burn off,
and accurate because there is no chance of reduction
of barium sulfate by the carbon of filter paper.
Thb Barrett Company
17 Battery Place. New York City
SYNTHETIC PHENOL1
By Albert G. Peterkin. Jr.
Received July 20. 1918
It is difficult to estimate the quantity of any of the
products from coal tar which is available, because, on
the one hand, the production of tar is changing from
day to day, due to the continued increase in the num-
ber of coke ovens, and on the other hand, its consump-
tion for fuel purposes is affected by greater or less
difficulty in obtaining supplies of coal. It is safe to
say, however, that it would not be practical or even
possible to-day to make more than five to six million
pounds of phenol per year available from this source.
The United States used before the war some 5,000,-
000 lbs. of phenol per year, the consumption being
divided among pharmaceuticals, resins of the Bakelite
type, dyestuff intermediates, and the explosive, picric
acid. At the beginning of the war, the demand im-
mediately increased, due to. the increased manufac-
ture of picric acid. The French Government, par-
ticularly, became a large customer of manufacturing
concerns in this country, both for phenol and picric
acid. The production at the time just before the
entrance of this country into the war had jumped
to something like 72,000,000 lbs. of phenol per year.
It is likely that 1919 will see a very great increase
in the production of phenol in this country. Coal
tar as a direct source of phenol is therefore a negligi-
ble factor in view of the present demand.
' ever the merits of picric acid as an explosive,
a real objection to its manufacture in such times as
these lies in the relatively enormous amount of raw
materials involved, and the necessity for the corre-
spondingly great consumption of our valuable trans-
portation facilities. For example, to make 100,000,-
000 lbs. of synthetic phenol requires in round numbers:
Pounds
Benrol 115.000.000
Fuming sulfuric acid (9'/i per cent) 280,000,000
Caustic soda 1 80 000 000
Lime 42.000.000
Limestone 1 90 000 000
Coke 35.000.000
Niter cake 42 000 000
or nearly nine times that of the finished product,
using the generally adopted process and working with
fair economy. To say that it is an extravagant
process is to put it mildly, but it has maintained
itself with considerable obstinacy in the face of many
attempts to improve and shorten it.
Fig. I shows the old process diagrammatically. It
RatvMaffak Charges
Products
Bu- Products
Total 884 .000 . 000
1 Read before the American Institute of Chemical Engineers, at Berlin.
N. H., June 21, 1918.
Fio. I — Chart Suowino thb Old Synthetic Phbnol Process
Sept., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
739
413
'Wafer So,
of S A to
Neutrahzer
Fro. II — Dbnnis-Bull Procbss
has been described many times and a bare outline will
suffice now. Benzol is sulfonated at temperatures vary-
ing from 50 ° to 70 °. The strongest acid that may be
used with economical results, in the writer's opinion, is
fuming sulfuric acid containing 9V2 per cent of free
■SO3,' the limitation being enforced by the necessity
of avoiding the formation of diphenylsulfone. Since
the composition of the spent acid from the sulfona-
tion is a constant, the amount of sulfonic acid neces-
sary for the completion of the reaction is increased
very largely as the concentration of the initial acid is
decreased. It has not been considered economical,
therefore, to use acid weaker than one containing
08 per cent H2SO4. The figures given above are for
the higher concentration. The result of the sulfona-
tion is a solution of sulfonic acid, sulfuric acid, and
water. The sulfuric acid and water together make a
spent acid of approximately 80 per cent H2SO4 and 20
per cent H20. The solution then contains, in round
numbers, 60 per cent sulfonic acid and 40 per cent
spent sulfuric acid. The sulfonic acid is required in
the form of sodium salt. The procedure in all plants
is essentially the same, although many minor varia-
tions have been adopted. Slaked lime is placed in the
agitators and the mixture of sulfonic and sulfuric acid
slowly added during agitation. The sodium salt may
be formed by addition of sodium sulfite obtained from
the fusions later in the process. When this procedure
is adopted, the mixture in the agitators consists of a
water solution of sodium benzosulfonate and a mix-
ture of solid calcium sulfite and calcium sulfate. The
whole is heated to 115° in order to obtain the sulfate
in proper crystalline form for filtering, and is passed
through the filter presses. The resulting solution of
sodium benzene sulfonate contains approximately 1 2
per cent of the salt and small quantities of calcium
sulfate, due to the slight solubility of this material.
It is important to remove all calcium salts, both for
the sake of- the tubes in the evaporators and because
of the havoc they cause in the fusion operation. This
is accomplished by the addition of the necessary small
FlC. Ill — SuLPONATORS. TOP Vl8W
Fig. IV — Sulponators. Side View
amount of sodium carbonate and refiltration. Some
factories make the soda salt in two steps, adding sodium
carbonate to the filtered solution of calcium benzosul-
fonate; others add only the amount of lime necessary to
react with the sulfuric acid, in making the soda salt in
one step, which makes the use of the by-product sul-
fite difficult, due to the liberation of SO2. The 10
per cent solution is evaporated down to the saturation
point, and the salt obtained from the syrup by means
of drum dryers. The salt, preferably retaining about
10 per cent of water, is fed into melted caustic soda
in the fusion kettles, there being about one mole of
soda in excess. The temperature during the fusion
is maintained between 320° and 350°, the salt being
fed in slowly during the operation.
3 200 C. appears to be the critical temperature of
the reaction. As the result of the fusion, a light brown
74©
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. o
Ms*
m.A .a
i^t --— -
^^
C3I"*1
Fig. V — Agitators
liquid mass with 'the appearance of melted chocolate
is obtained, which is poured hot into such an amount
of water as will dissolve the phenolate and leave the
sodium sulfite in solid form. This is done in vessels
marked "dissolvers," which are provided with stir-
rers. Only about 10 per cent of the sulfite formed
remains in the solution and this amount can undoubt-
edly be decreased. The phenolate liquor is filtered
from the sulfite on open sand filters. The sulfite is
agitated with water, separated by means of filter
presses, washed free of phenol, and marketed as an
impure sodium sulfite. A typical analysis of this
material is:
Per cent
Moisture 24.20
Na,SO. 7.12
NaiSOj 62.30
Insol. in hot HiO 0.46
C»HiONa 0.60
The wash water is used in the dissolvers so that its
sulfite is deposited again on the filter beds.
The phenolate liquor is carefully diluted to a gravity
corresponding to a phenol content of about 16 per
cent. This diluted solution is placed in a series of
tanks. Thirty per cent carbon dioxide gas generated
from a mixture of coke and limestone is passed through
it. These so-called "blowers" are arranged so that
the gas may pass from one to another in any direc-
tion desired. The strong gas goes first through the
neutralized phenolate and leaves from a strongly
alkaline solution, thus avoiding any possibility of loss due
apor pressure of phenol at the temperature of the
spent gases involved, which is about 50° C. It is not
possible to entirely neutralize the phenolate solution by
means of carbon dioxide in one operation unless such
a large excess of C02 is introduced as to transform all
the carbonate to bicarbonate, which is undesirable.
When the passage of the gas is discontinued, the
phenol layer contains in solution about 10 per cent
phenol as sodium phenolate, while the carbonate
layer is free from phenolate but contains approxi-
mately 2 per cent of phenol. The carbonate is com-
pletely freed from phenol by means of a steam dis-
tillation; a 4 per cent solution of phenol is obtained
in this way. The crude phenol, containing 10 per
cenl of phenolate, may be completely acidified with
CO2, by replacing the carbonate solution with water.
Niter cake, however, used as an acidifying agent, has
the advantage of simultaneously removing a large
percentage of the water present. The dehydration
reduces the water content of the crude phenol from
30 per cent to less than 14 per cent, and relieves the
refining stills of a great burden. The crude acid is
placed in a simple still from which is obtained a first
fraction of water and phenol, a middle fraction of
pure phenol, and a residue of the more complex phe-
nolic bodies formed in the fusion. The synthetic
phenol produced is exceedingly pure; it is compara-
tively easy to obtain material melting at 400. Re-
distillation gives a product melting at 40. 6° C. The
true melting point of pure phenol is in our opinion
40. 8° C.
The great economies possible in the process are
obviously to be made in the cutting down of the 100
per cent excess of sulfuric acid, the reclaiming of the
caustic soda, and the marketing of the sodium sulfite
in a useful and valuable form. The maximum yield
Pro VI -Evaporators DlSSOLVKKS
Sept., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
74i
Fig. VII — Recording Gaogb, Automatic Temperature Control
which has been claimed for the process is about 80
per cent. Our work has shown that the fusion opera-
tion alone will not yield more than 90 to 92 per cent
of the theoretical, and in practice it is difficult to
maintain this high standard. Under present condi-
tions, the average American practice probably re-
sults in a total over-all yield of between 60 per cent
and 75 per cent. As chemical processes go, the
process requires an inordinate amount of labor and the
repeated handling of the material gives ample oppor-
tunity for mechanical losses, particularly in view of
the restlessness of workmen under present condi-
tions.
Two methods have been suggested to reduce or
conserve the excess of sulfuric acid used. Daniel
Tyrer of England (U. S. Patent No. 1,210,725) passes
Fig. VIII — Drum Dryers
ing between 100° and 1850 C. That part of the
benzol vapor not reacted upon carries with it to a
condenser the water of reaction, and so gives a constant
concentration to the sulfuric acid, keeping it active.
Tyrer claims in this way to get about 80 per cent of
the amount of sulfonic acid theoretically obtainable
from the sulfuric acid used. This method has not yet
.been tried on a large scale in this country.
The second method is that of Dennis and Bull.
Some two years ago, Professor L. M. Dennis,1 of Cornell
University, discovered that although the solubility of
pure sulfonic acid in benzol was negligible, benzol
would take up from the mixture of sulfuric and sul-
fonic acids between 2 and 3 per cent of its own vol-
ume of the sulfonic acid. In working out this idea, it
occurred to Mr. Hans Bull,2 of The Barrett Company,
benzol vapor through sulfuric acid of as low concen
tration as 00 per cent H2S04, at temperatures vary
11. S. Patents 1,212,612,' 1,211,923, 1,227.894, 1,228.414. 1,229.393.
U.S. Patents 1.247,499, l,260.832.'_208,632.
74-'
I III: JOCKS A L OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 9
! [rM^1
W>/ fifli^^^s
i_
Fig. XI — Washers
that the sulfonation could be made simultaneously
with the extraction. These ideas have been utilized
in the evolution of an extremely simple process which
not only saves 90 per cent of the excess sulfuric acid
as a spent acid containing 70 to 77 per cent H2SO4,
but eliminates a good percentage of labor, all the
lime, and substantially reduces the deplorable cost of
repairs, due to the many moving parts of the old in-
stallation.
The process will be easily understood from Fig.
II. The vessels 1, 2, 3 and 4, so-called "ex-
tractors," each contain at rest a layer of a solution of
sulfonic and sulfuric acids of varying proportions.
The benzol passes continually upward through this
series of extractors, the vessels being under a pressure
equivalent to the head of benzol. The distribution of
the liquid in fine bubbles is effected by means of per-
forated branch pipes. After the passage of the
benzol for a certain length of time, the solution in
No. 1 is free from sulfonic acid and consists of 77 per
Fig. XII — Pumps and Only Working Pakts
cent H2S04. When this has been accomplished the
so-called "spent acid" is withdrawn. The solution
in No. 2, which probably contains 10 per cent of sul-
fonic acid, is dropped into No. 1. The solution in
No. 3, which contains probably 25 per cent sulfonic
acid, is dropped into No. 2, and the solution in Xo. 4,
which contains probably 40 per cent sulfonic acid, is
dropped into No. 3. Into No. 4 is then slowly intro-
duced a charge of 98 per cent sulfuric acid. The flow
of benzol is not interrupted at any time. Sulfona-
tion takes place almost immediately and the volume
of the benzol flowing through, approximately 200 gal.
per min., is so great as to effect almost instantaneous
removal of the heat of reaction. The benzol is main-
tained throughout at a temperature of 60° C. This
is accomplished by heaters at the bottom of the sys-
tem and coolers at the top. After passing through
the coolers, the benzol, which will contain approx-
imately 2 per cent sulfonic acid, passes successively
through the washers 5, 6, and 7, containing water.
^^H
rx^jjJr
mm
■ - ii a<
1
"" lk '^^
«u-
feL >
* "**~ >y Hj^ \m?
1 .JpW*"
^v -
P10. XIII — Extractor
Fig. XIV — Final Wash Tank and Receiver for Water Solution of
Benzene Sulfonic Acid
Sept., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
743
Fig. XV — Coolbrs
The benzol falls from one vessel to another by gravity,
there being no pressure on this part of the system.
The sulfonic acid remains in the water and the benzol
leaves the last washer entirely relieved of its burden.
It is passed to large settling tanks where the rate of
flow is slowed down to such an extent as to allow the
sulfonic acid solution, carried in suspension, to set-
tle, and from these tanks flows to the pump and is
forced through the heaters to the extracting system
once more. When such an amount of sulfonic acid
has been deposited in washer 5 as to bring it to
the strength desired, it is removed to an evaporator
and the solution from washer 6 pumped to No. 5,
and that from No. 7 to No. 6. Fresh water is put into
No. 7. A water solution of sulfonic acid can be ob-
tained containing 60 per cent or even more sulfonic
acid and contains also about 2 per cent by volume
of benzol in solution. The benzol is removed by
evaporating a small percentage of the water. The
solution of sulfonic acid is then neutralized, either by
the carbonate solution from the phenol blowers or
with the solid sulfite of soda. The sodium benzo-
sulfonate obtained contains some 5 or 6 per cent of
sodium sulfate, due to the solubility of sulfuric acid
in the benzol solution of sulfonic acid (one part sul-
furic to twenty parts sulfonic). The advantages
of the process are obvious. The initial cost of the
plant is about 50 per cent of the old style plant, which
it displaces, it runs practically without attention,
and requires from one-third to one-fourth the
number of laborers. Taking for granted complete
extraction of the sulfonic acid, which proves quite
possible, and a removal of the benzol from the water
solution of sulfonic acid, the losses possible are con-
fined to mechanical causes, that is, either leaks or
evaporation. The yield under the old process, from
benzol to sodium benzosulfonate, is about 90 per cent.
The new process makes easily possible a yield of 98 per
cent, leaving the mechanical losses out of considera-
tion. The formation of disulfonic acid and of sul-
fone is negligible. The spent acid is concentrated
to 93 per cent and used repeatedly. The operations
(1) discontinuous sulfonation, (2) liming, (3) filtering,
and (4) evaporating, involving complex machinery
and many moving parts, have all been displaced
with the one simple and continuous operation, ex-
traction and sulfonation going on simultaneously,
the only moving parts being two small pumps. The
enormous simplification of the process achieved will
be made more evident by photographs than by any
description.
• Another improvement in the process, very generally
adopted, has been the so-called "liquid fusion," by
means of which the drum dryer, with its dust and
spatter, has been eliminated. "Liquid fusion" consists
in the introduction of a saturated solution of sodium
benzosulfonate directly into liquid caustic soda at a
point above the reaction temperature. The reac-
tion, when the temperature is properly controlled,
goes even more smoothly than with the solid, since
there is no tendency to dust and float, and the rapid
evolution of the steam gives better agitation. The
fusion is a great source of loss in yield. Well-conducted
fusions, where the temperature has been kept down
and which for that reason show no evidence of oxida-
tion, give between S6 and 90 per cent yield. Our ex-
perience shows that using the liquid fusion method
a high yield is more easily obtained than with the dry
salt.
So much for innovation. Another important econ-
omy to be achieved in this process, and one even
F10. XVI — Sbttuno Tanks
744
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 9
more important than that of sulfuric acid, is that of
caustic soda. Neutralizing the phenolate with sulfuric
acid, as is often done, is a gross and inexcusable waste.
Providing that the lime can be utilized, the differ-
ence in cost between the neutralization with CO:, as
generated from limestone and with sulfuric acid, is im-
rably in favor of the former and the operation
is exceedingly simple, once the necessity for clear
solutions is understood and the fact of the solubility
of phenolate in phenol. If any salts are precipitated
by the carbonation of the phenolate, an emulsion is
obtained from which the phenol will settle only with
great difficulty. The avoidance of this emulsifying
is merely a question of dilution, however, and no
real obstacle is involved. The soda, not only of the
phenolate, but the excess soda, is obtained in the form
of a weak solution of sodium carbonate, which can be
readily causticized and made available at the plant
for the fusion operation.
The fusion reaction is:
C6H6S03Na + 2NaOH = C6H5ONa + Na2S03 + H;0
If half of the sulfite is used for the formation of the
soda salt, only one molecule of soda is consumed and
this goes out of the plant in the form of sodium sul-
fite, a useful and marketable product. Since in the
Dennis- Bull process, SOj is evolved from the neutraliza-
tion of the sulfonic acid when sulfite is used, it is
possible also to produce bisulfite of soda.
The large amount of limestone needed is not a rela-
tively important objection from the point of view of
cost, but it presents a transportation problem of con-
siderable magnitude. The disposition of the calcium
carbonate sludge from the causticization may involve
considerable expense. From the transportation point
of view alone, the calcination of the carbonate sludges,
in rotary kilns, as a source of C02 and of lime, is justified.
This has been successfully tried in connection with
other operations and has been found economical in
districts somewhat remote from the limestone fields.
Were the various economies indicated taken advan-
tage of there would result a startling decrease of raw
materials
Sulfuric Acid 40
Caustic Soda 60
Lime 90
Limestone 1 00
and a corresponding decrease of tonnage to be trans-
ported from a total of 884.000,000 to 397,214,400 per
million pounds of phenol, or about 50 per cent.
The Barrett Company
17 Battery Place, New York City
CURRENT INDUSTRIAL NLW5
By A. McMillan, 24 Westend Park St., Glasgow, Scotland
FAN DYNAMOMETER BRAKE
In the fan dynamometer of W. G. Walker and Co., Emery-
hill St., London, intended for measuring the brake horse-
power of aero and other engines, the power is absorbed by re-
volving the instrument in air. The device consists of a pair
of jaws or arms, made of well-seasoned asb, adapted to grip at
their central part or propeller hub. The blades, of aluminum
or steel, can be moved radially to any suitable position. Given
the revolutions of the engine, the horse-power can be im-
mediately read off from the curves supplied with the instru-
ments. A correction is given for variation in atmospheric
conditions. The instruments are made in four sizes, covering
between them a range from 300 to 500 h. p.
SOAP AND GLYCERIN MANUFACTURE IN INDIA
It is understood that the Madras government contemplates
shortly opening a soap factory at Hyderabad and that a recent
visit of the Director of Industries and Commerce of Hyderabad
to Malabar was for the purpose of collecting information and
cupving the government soapery in Malabar as regards plant,
etc. It is believed that the Bombay government will soon
establish a soapery and indeed it is evident that the several
provinces are inquiring into the possibilities of the soap business
which Sir F. A. Nicholson has so successfully established and
proved to be a sound commercial proposition. More than all
this, it is quite probable that the Munitions Board before very
long will be running large factories at various centers in India
l"i the manufacture of glycerin. A glycerin industry is well
calculated to bring in its wake factories for the manufacture of
soaps and candles and altogether the outlook for the oil trade is
cei tainly promising. The west coast, it may be mentioned, is
eminently suited for the manufacture of glycerin, since oils of
all descriptions are very largely available.
NEW VOLTAIC CELL
La Nature for April 6, 1918, describes a new form of voltaic
cell, with electrodes of zinc and carbon in a solution of sal-
ammoniac, which is due to Mr. Fery.and has been in use for some
time on the French railways. The negative electrode is a plate
of zinc which rests on the bottom of the glass containing jar,
the copper wire connected to it being insulated up to a point
well above the level of the solution in the jar. The positive
electrode is a carbon tube of diameter about half that of the jar,
pierced with holes, which rests on the zinc plate, being insulated
from it by an ebonite cross. The evaporation of the sal-ammo-
niac solution is prevented by the wooden cover. During the
action of the cell, the lower part of the solution becomes acid,
owing to the descent of the dense zinc chloride, while the upper
part becomes alkaline, owing to the ammonia produced. The
depolarization of the cell is effected by the air alone. The
electromotive force of the cell is 1.18 volts, and a cell giving 90
amp. hrs. weighs only 2.1 kg.
OILSEED INDUSTRY OF RHODESIA
In view of the fact that even before the war it was becoming
difficult to cope with the world's demand for oils and fats for the
manufacture of margarine and that this difficulty has been in-
creased during the war, it is interesting to note that the cultiva-
tion of oilseeds promises to become an important industry in
Rhodesia. At present, ground nuts and sunflower seeds are the
only oilseeds produced commercially, but experiments con-
ducted with other oilseeds show that these may be successfully
grown Castor seed, sunflower seed, sesame seed, and linseed
grown in Rhodesia have been tested at the Imperial Institute.
London, and have given entirely satisfactory results. Before
the war sesame seed was chiefly crushed on the continent but this
is now being done in the United Kingdom.
Sept., 191S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
745
CANE BY-PRODUCTS IN NATAL
A comparatively new South African enterprise is represented
in the manufacture of rectified alcohol, methylated spirit ether,
and cane-wax by a cane by-products company at Merebank
in Natal. The original venture was the extraction of wax from
the refuse of the sugar mills This product is termed mila
and in appearance is like rubble. Mila is dried on the sugar
estates and then sent to Merebank where it is put in an extrac-
tor which is constructed in two sections, the upper part of which
has a false perforated bottom. At the top is a con-
denser and a benzene tank combined, and, after being sub-
jected to a certain process, the wax and benzene pass through
a side-glass into the bottom chamber. Here the benzene is
driven from the wax and the latter put into moulds. The com-
pany lately, according to the Board of Trade Journal, has under-
taken to manufacture "natalite" (or motor spirit) which it is
claimed will in time displace petrol for driving machinery and
particularly motors. The source of natalite is molasses from
the sugar estates, which is brought to Merebank and drained
into 250,000 gal. tanks. The molasses is then run into large
vats and fermented. Next it is pumped up into a receiver and
the wash run into a still. The spirit is separated by a heater
from the wash which is used for fertilizing purposes. The
vapor of the spirit passes through two columns and a still in
which the good spirit is separated from the best of 70 overproof.
The best is used for the preparation of natalite, the weaker for
making methylated spirit.
THE SYNTHETIC MARKET
Owing to the continued scarcity of cloves and clove oil, says the
Oil and Color Trade Journal, 53 (1918), 1483, the price of eugenol
has risen still further, and vanillin is a very firm market at Si 7 to
Si 7.50 with an upward tendency. There has been no further
advance in artificial rose products, and phenylethyl alcohol is
still obtainable at $31.25 to $35, according to quality, but phenyl-
ethyl aldehyde is dearer and up to $45 has been paid for small
quantities. Coumarin is scarce at $43.75, and heliotropine is
in fair demand at about $8.75. All kinds of synthetic musk
are scarce and the cheapest, pure, is xylene musk at $20.75.
Cheaper varieties, diluted usually with acetanilide which was,
of course, the diluent used in original musk-Baur, are offered
at about $7.50 to $8. Safrol is dearer at Si. 25 and bromo-
stysol can only be obtained in small quantities at $24 to $24.50
per lb. Terpineol is worth nearly, if not quite, $i-8o per lb.,
for best qualities free from water.
SULFATE OF AMMONIA
Recently published statistics show that the production of
700,000 tons of sulfate of ammonia was expected in Germany
for 1917, while, according to recent available data, the quantity
for 1915 was.549,000 tons. For 1917, the American production
is estimated at 400,000 tons and the capacity for production for
1918 may reach 50o;ooo tons. The Japanese output is continually
increasing. In 1914, it scarcely exceeded 16,000 tons, in 1915
the figure had risen to 31,824 tons, while in 1916 the total be-
came 38,203 tons. For 1917 the estimated output was 50,800
tons.
EXPLOSIVE CHEMICALS
M. Stettbackcr discussed this question before the Swiss
Chemical Society recently. Nitroglycerin develops 1,580
calories; oxylignite (explosive with liquid-air base), 2,200
calories; ethylene ozonide and benzene triozonide give similar
figures but are more disruptive. More powerful explosives arc
conceivable; trichloratc of glycerin can develop 3,000 calories
and, if a mixture of liquid hydrogen and liquid ozone were
feasible, the calorific value would be 4,500.
DETERMINATION OF OXYGEN IN IRON
The' method for the quantitative determination of oxygen in
iron was proposed by Ledebur in 1882. He heated the iron
in a current of hydrogen and absorbed the water formed by the
combination of part of the hydrogen with the oxygen in the iron
by the aid of phosphorus pentoxide. This and similar methods
have found little application, however, because the analysis
takes too long a time, 4 to 5 hours, and Ledebur was doubtful
as to its reliability. The oxygen may be present in the
iron as such or it may be combined with the iron and with
various other elements in the iron and these compounds are not
reducible with the same ease. It is assumed that manganous
oxide and silicates, likely to be present as slag enclosures, are
not reduced by hydrogen at temperatures of 9000 or i,oooc C.
which are generally the prescribed limits of such analyses, when
ferrous iron is reduced. At the same time, says Engineering,
it would be highly desirable to follow the advancing deoxidation
of metallurgical processes by analytical means and to have some
method of determining the occluded oxygen in iron to which
some metallurgists attribute considerable importance. It is
interesting to note that P. Oberhoffer, of Breslau, claims to have
simplified the Lederbur method so that a complete analysis can
be made within an hour and that metallurgical processes can be
followed. The apparatus (Stahl und Eisen, Feb. 7, 1918) con-
sists of a hydrogen generator apparatus for purifying that
gas, a mercury air pump of the Bentell type, a combustion
tube of silica-glass, and a tubular electric furnace. The iron
specimen, turnings as a rule, is heated in a tube by means of
burners to facilitate the complete evacuation of the tube, the
hydrogen is then admitted and the furnace slipped over the tube
which is raised to a temperature of 950 ° C.
ITALIAN DYE AND CHEMICAL INDUSTRY
An Italian contemporary, says the Chemical Trade Journal,
62 (1918), 398, commenting on the status of the aniline dye
industry in Italy, states that the necessities of the war have
obliged producers of coal gas in that country to make benzol
and toluol for the manufacture of explosives but that, after the
war, these products will serve for the manufacture of aniline
dyes. It is calculated that the plants now in Italy can already
supply the following quantities of materials annually: pure
benzol, 12,000 tons; toluol, 2000 tons; naphthalene, 3000 tons;
phenol, 500 tons; and anthracene, 560 tons. These quantities,
it is said, are more than sufficient to meet any demands from
future aniline factories in Italy. As regards chemicals, it is
said that large quantities of such chemicals as sulfuric acid,
oleum, nitric acid, ammonia, chlorine, soda, etc., are being
manufactured in Italy and that that country will in future
not be so dependent upon foreign sources of supply as she has
been in the past.
SKODA WORKS PEACE PREPARATIONS
Die Zeit quotes from an article in the Pravo Lidu on the
measures taken in the Skoda Works in preparation for peace.
A special department of engineers and commercial directors
has been formed to work out a detailed plan for converting the
works from an undertaking for the production of war material
into one for the manufacture of peace products. A great de-
partment is being set up for the manufacture of machinery.
especially agricultural machinery for export trade, with the ob-
ject of secur'ng the Balkan market iv the first place. The
Skoda factories have large sto'eks of machines which will be
thrown on the Rumanian market. It is expected that a great
impetus to shipping will be witnessed in the Da-danelles and
part of the works will be devoted to the manufacture of motor
boats for export to Turkey and Bulgaria Ships (for Adriatic
ports), motors, and living machines are also to be built.
746
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 9
MACHINERY IN SOUTH AMERICA
Imports of machinery to South America must always "be of
paramount importance since none of the states are at present
self-supporting in this direction. How considerable is the
demand may be judged from the fact that just before war broke
out there were in active operation in the Argentine no fewer
than 29,690 industrial establishments showing an increase of
65 per cent since 1904. The capital invested in these establish-
ments represented a sum of $330,000,000, the percentage of
native-owned factories being 14.67. Over 118,000 employees
are constantly at work producing goods — all more or less in
competition with foreign importation — worth $982,000,000.
Naturally, the greater number of these factories are to be found
in the cities — Buenos Aires, Rosario, Santa Fe, Mendoza, etc.,
where there are plants and equipment equal to any in Europe,
if foundries and machine shops are excepted. Other markets
for engineering ware, such goods as iron and steel plates and
sheets, tubes, pipes, iron and steel fittings, electrical appliances
and apparatus are available. The German concern which
supplied Buenos Aires with electric light and made all its pur-
chases direct from Berlin has offered to hand over everything
to the Buenos Aires municipality. Fully one-half of the total
imports into Argentina of electrical appliances formerly came
through this company. Now this source is cut off and the sale
of small motors, insulators, cables, dynamos and accessories
might be greatly augmented by having agents for these goods
in the port towns.
CEMENT MORTARS AND MAGNESIUM CHLORIDE
Some experiments, according to Engineering, 105 (1918), 636,
on the influence of magnesium chloride on cements to be used in
frosty weather, were made last winter, by the Verein Deutsche
Portland Zement Fabrikanten. Pure specimens were mixed
with standard sand in the proportion 1 : 3 and with ordinary
water or with an aqueous solution of magnesium chloride. The
specimens were exposed to a temperature of — 70 C. (200 F.),
and the ordinary specimens took three days to set sufficiently
for removing the mould casing, while the specimen made with the
magnesium chloride set within one day. On the other hand the
strength tests performed after one week and four weeks were in
favor of the cement made with water only; the values were
185 kg., 205 kg., 295 kg., and 344 kg. per sq. cm., respectively.
Thus, the addition of magnesium chloride lowers the strength
of the cement somewhat, not sufficiently, however, to exclude the
use of the reagent when cement has to be laid down in cold
weather.
BLAST FURNACE PRACTICE
Several communications made at the annual meeting of the
Iron and Steel Institute related to practice with blast furnaces.
The report of the committee on this subject summarizes the
replies to a series of inquiries addressed to all owners of blast
. furnaces in this country. Mr. T. C. Hutchinson describes some
modifications in practice and design that led to considerable
fuel economies, in one case a reduction of coke consumption by
2 cwt. per ton, and increased the output of iron by 33.7 per
cent. The saving of fuel was attributed entirely to the better
distribution in the furnace by the increased size of the bell and
the life of the furnace lining was also considerably improved.
A paper by Dr. J. E. Stead on "Blast Furnace Bears," makes
interesting reading. "Bears," it should be explained, are the
masses of metal which are found below the hearth level of a
blast furnace after the furnace has been blown out. A number
of bears were analyzed with somewhat curious results. Quite a
variety of compounds and crystalline formations were found to
occur. Among the substances noted were nitrocyanidc of
titanium, large idiomorphic crystals of double carbide of man-
ganese and iron, and carbonless iron masses rich in phosphorus.
CHROME TANNING
At a recent lecture before the Royal Society of Arts, London,
on "Recent Developments of Leather Chemistry," Dr. H. R.
Procter suggested an alternative method of chrome tanning
which would overcome the difficulties arising out of the shortage
of glucose and sugar. He did not claim the method to be the
result of some great discovery but thought that it might be of
value to the trade. The process depends on the use of sodium
dichromate, which is preferable to the potassium salt besides
being more soluble in water. Four pounds of sodium dichromate
can be dissolved in a gallon of water without giving a thick
solution. Into this is passed a current of liquid sulfur dioxide
or the fumes from sulfur burning in a furnace are passed through
the solution, this latter method being both cheap and effective.
In this way is obtained a chrome extract containing i8'/j per
cent of chrome oxide to the gallon, richer than any on the market
and requiring only dilution with water. Professor Procter
admitted that he had not experimented long with this solution,
but in the experiments which he had carried out he found that
in 24 hrs. the skins were apparently thoroughly tanned and
rather thicker than when they went into the solution. As a
sole leather tannage, he considered this solution to be very
promising.
ELECTRICAL MACHINERY
A pamphlet issued by Messrs. Vickers, Glasgow, contains
about 60 excellent reproductions of photographs illustrating the
electrical machinery made by the firm. Some views of the shops
in which the machines are manufactured are followed by a section
dealing with generating plant of all kinds for both direct and
alternating current. Another section is devoted to rotary
converters and motor generators and a third to both direct and
alternating current motors of numerous types and sizes. The
last section illustrates the application of electric motors to the
driving of machinery, such as lathes, small rolls, winches, mine
hoists and particularly planers fitted with the firm's patent
automatic "reversing drive. The brief descriptions under each
photograph are printed in English, Spanish, Fr ench, and Italian
ELECTROLYTIC PROCESS
By a new electrolytic process, aluminum can be coated with
nickel, silver, copper, or other metal. The process can be
applied to sheets, rods, wire, tubing, etc., and to aluminum
alloys in castings or worked products. With nickel plating a
hard, beautiful finish, taking a fine non-tarnishing polish, is
given while the aluminum is much strengthened with no great
addition to its weight.
RECOVERY OF TIN
Chemical Trade Journal quoting from a contemporary gives a
review of the methods which have been proposed for the recovery
of tin from waste tinplate. One depends on the use of acids to
dissolve the tin from the steel but here there is the difficulty in
preventing the steel from being dissolved at the same time.
Another in which caustic alkali is the solvent employed has been
used to dissolve the tin and obtain clean steel. In a third the scrap
tin is treated with dry chlorine gas, the product being stannic
chloride. According to a process suggested by Bergser, an
aqueous solution of tin tetrachloride is used as a solvent. The
product obtained is stannous chloride which can be electrolyzed
into tin and chlorine. The latter can in turn be used for making
tin tetrachloride from stannous chloride. By electrolysis also
the metal can be recovered from the solution formed with the
aid of acids or alkalies. Solder can be extracted in a desoldering
furnace provided with a means for obtaining a neutral atmos-
phere to prevent excessive oxidation and when a clean steel is
obtained, hydraulic or mechanical presses are used for pressing
it into blocks weighing about 1 cwt.
Sept., 1918 TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
747
ANALYSIS OF ALUMINUM ALLOYS
Rapid methods of analysis of aluminum alloys, says Engi-
neering, 105 (1918), 587, are now in demand. Messrs. B. Collitt
and W. Regan in a recent paper express their agreement with the
recommendations previously made by Mr. J. H. Stansbie, viz.,
(1) to open out the alloys with a solution of caustic soda, (2)
that in this way practically all the zinc and aluminum would be
in the filtrate, while copper, iron, nickel or magnesium and all
the manganese (except a trace) would remain on the filter,
(3) that a small amount of aluminum would also remain on the
filter so that the iron could not be precipitated by ammonium.
They distinguish for analytical purposes alloys containing 10
per cent and 20 per cent of zinc, up to 5 per cent of copper, and
small amounts of one or more other metals (Fe, Ni, Mn, Mg);
alloys with up to 5 per cent copper and amounts up to 2.5 per
cent of other metals including zinc; lead and tin were absent
in the alloys they had dealt with. They did not make use of
gravimetric (density determination), magnetic, and electrolytic
methods (though the latter would be convenient for zinc).
Manganese they estimate volumetrically with the aid of stan-
nous chloride; silica was always tested for but a convenient
method for determining aluminum does not exist as yet.
CATALYST FROM METALLIC SALTS
According to a new German patent, the mass obtained by
precipitating the metallic salts on an inorganic carrier is dried
and mixed with the material to be treated, or is triturated with
an inert solvent and is then treated to expel the water and
volatile acid of the salt which would otherwise act adversely
on the reduction process. If the catalyzer is intended for
reducing fats and oils, Kieselguhr, asbestos, etc., are saturated
with nickel acetate, the dried mass being ground extremely fine
with a little oil and then heated to 1500 or 2000 C. in a closed
apparatus filled with stirrers and connected to a vacuum pipe.
When the water and volatile acid have been drawn off, the
catalyst is rendered more active by a current of hydrogen.
The product is claimed to be stable and to stand carriage.
NEW MINING EXPLOSIVE
The Board of Trade Journal says that a new explosive is now
being used in South African mines and is resulting in a great
saving of nitroglycerin. The shortage of the latter owing to
its use for ammunition was, indeed, leading to difficulties in
the industry. Hitherto, the standard explosive used has been
gelignite, which contains 57 per cent of glycerin. It is now al-
most replaced by sengite, which is a gun-cotton explosive specially
prepared and put into cartridges for the mines. The ingre-
dients of sengite are more readily obtainable than nitroglycerin
and they are added to gun-cotton. "Sengite is not altogether
a new explosive, but it is new to mining practice.
NEW SOURCES OF OIL SUPPLY IN GERMANY
The straits to which Germany has been reduced by the cut-
ting off of oil supplies from outside has led to some remarkable
discoveries or at least communications of discoveries. Prof.
R. France, of Munich, claims to have discovered a new source
of oil in certain cryptogrammic plants growing in Bavaria to
which he has given the name "Esaphone." He calculates that
by adding thereto certain other parasitic plants growing in
Germany some 1,200,000 kilos of oil of excellent quality can
be obtained per annum. As it does not congeal except at
about 40 ° below zero, he suggests that it would be highly use-
ful for aeroplanes and the engines of vessels going to arctic
regions. Prof. France also states that by collecting the drops
of resin which collect in spring upon felled pine and fir trees
about 60 liters of oil could be secured from every cord of wood.
ULTRA-FILTER
In many analyses, especially in acid determination by the
inversion of sugar, rapid filtration of turbid liquids is necessary.
Such liquids are apt to pass turbid through ordinary filter
paper. In the Chemiker Zeitung, Dr. Wolfgang Ostwald de-
scribes how an ultra-filter may be made from an ordinary fil-
ter with the aid of some 4 per cent collodion solution. The
filter is placed in a funnel and wetted with water so as to lie
well against the glass; the collodion is then poured into the
filter; as the collodion is insoluble in water, it turns into an
emulsion which soaks into the paper. The collodion solution
is filtered and the paper allowed to dry. After 5 min. the process
is repeated. The filter is now stiff; it is taken out of the fun-
nel, placed in distilled water to coagulate the collodion, and is '
afterwards ready for use. As a rule, only the small filter cone
which is fitted into the lower part of the funnel need be treated
in this way.
LUBRICATING MATERIAL
Owing to the scarcity of grease in Germany, engineers in
that country are paying much attention to other forms of lubri-
cating material. Der Papier Fabrikant says that from 40 to
60 per cent of tallow mixed with mineral oil is effective and
economical and that high grade graphite may be substituted
for the tallow. Artificial graphite is manufactured in Ger-
many, both by intensive chemical treatment and by subjecting
carbonaceous material to the heat of an electric arc in a space
from which air has been excluded.
INDIAN RESIN
The Indian Munitions Board Handbook, recently issued,
states that the Indian pure resin industry has made rapid strides
within recent years and shows promise for the future. At
present, resin tapping is carried out only in the United Prov-
inces and the Punjab and- is confined to one species of pine,
namely, the chir of the Himalayas, which covers some 1,500
sq. mi. in the Government forests and another 1,800 sq. mi.
in the native states. Even if it is assumed that only a portion
of the total area will lend itself to remunerative tapping, an
extension of operations is possible on a larger scale in the case
of this pine alone, while it is possible that systematic tapping
on an appreciable scale may be introduced later in the case of
the blue pine of the Himalayas and the pines of Assam and
Burma. Tapping and distillation are in the hands of the Forest
Department which, at present, manages two distilleries, one at
Bhowali, in the United Provinces, and the other at Jallo, in the
Punjab. Statistics still show that there is room for a large ex-
pansion in the Indian output for the supply of India's require-
ments alone, apart from stimulating trade with China, Java
and other foreign countries. At present, the Indian resin in-
dustry is in the position of having to retard or accelerate its
expansion with reference to the speed with which the remain-
ing Indian markets can be secured and foreign markets de-
veloped.
BRITISH BOARD OF TRADE
During the month of June inquiries have been made by firms
at home and abroad regarding sources of supply of the follow-
ing articles. Firms able to supply information regarding these
things are requested to communicate with the Board of Trade,
73 Basinghall St., London, E- C:
Acetylene gas burners Serrated edge on grass hooks
Agate in the rough for mortars and Spouts of galvanized iron for use
pestles, 4 in. to 5 in. in diameter in tapping rubher trees
Bootlace tags Straw tubes, for iced drinks, etc.
Earrings, cheap Tenter hooks, tinned
Machinery pok Making: Wood travelling trunks, cheap,
Roofing papers covered in leather, cloth or
Buffalo hide pickers (as used in canvas
looms)
748
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 9
SCIENTIFIC SOCILTIL5
CLEVELAND MEETING, AMERICAN CHEMICAL SOCIETY
The 56th General Meeting of the American Chemical Society
will be held at the Hotel Statlcr, Euclid Avenue and East 12th
Street, Cleveland, Ohio, September 10 to 13, 1918.
Registration and all meetings, except as specially announced,
will be held at the Hotel. Registration will begin at 3 p.m.,
September 9. Information regarding other hotels may be
obtained from the chairman of the committee on hotels.
CHAIRMEN OF LOCAL COMMITTEES
Executive: A. W. Smith, Case School of Applied Science,
Cleveland, Ohio. Hippolyte Gruener, Adelbert College, Cleve-
land, Ohio.
Finance: W. A. Harshaw, 720 Electric Bldg., Cleveland,
Ohio.
Entertainment: Hippolyte Gruener, Adelbert College, Cleve-
land, Ohio.
Hotels: H. H. Gronemeyer, 1887 East 93d St., Cleveland,
Ohio.
Entertainment of Ladies: Miss Josephine Grasselli.
Cou
GENERAL PROGRAM
Monday, Sbptbmber 9
■il Meeting. University Club.
to the Council at University Club (tendered by the
Cleveland Section).
Tuesday, September 10
General Addresses.
Address. Assistant Secretary of War, Benedict Crowell
Chemists' Place in Warfare." Charles L.
Morning:
Afternoon
Evening:
"The Work of the. Chemical Section of the War Industries
Board." Charles H. MaeDowell.
"War Disturbances and Peace Readjustments." Grinnell
"The Place of the University in Chemical War Work."
Edward W. Washburn
"The Work of the Government Research." Lieut Col.
Wilder D. Bancroft.
General Symposium on the "Chemistry of Dyestuffs."
Banquet and Smoker at Hotel Statler.
Wednesday, September 1 1
Divisional Meetings, Hotel Statler.
Excursions [see This Journal. 10 (1918), 653].
President's Address: "A Retrospect and an Application."
Thursday, September 12
Morning: Divisional Meetings.
Afternoon: Divisional Meetings. Outing to one of the country clubs,
followed by reception at Cleveland Museum of Art.
DIVISIONAL PROGRAMS
The usual meetings, including the annual election of officers,
will be held by all the Divisions, and by the Rubber Chemistry
Section, with the following special program :
Tin; division of biological chemistry is planning a sym-
posium on plant chemistry.
THE division of industrial chemists and chemical engi-
neers, besides continuing the symposium on the chemistry
of dyestuffs, is planning a symposium on potash and a continua-
tion of the very successful symposium on metallurgical sub-
jects started at the Boston meeting.
PAPERS for Tin; MEETING
Tin: division of industrial chemists and chemical engi-
neers have voted that the titles of a!! papers shall be sent to
the Secretary of the Division, which title should be accom-
panied by ; i ii abstract; that any title scut without an abstract
shall not be printed in the program, ami that the time limit
for the p hall be 5 minutes, unless special arrange-
iii' made «itli the Secretary of the Division.
By vote of the Council no papers may be presented at the meet-
ing, titles for which art- not printed on the final program.
"By Title" should be placed on the announcement of any
paper where the author is to be absent, so that members may
Understand in advance that the paper will not be read.
ADDRESSES OP DIVISIONAL SECRETARIES
Agricultural and Food Chemistry: Fred. F. Flanders, 88 Corey Road,
Brookline, Mass.
Biological Chemistry: I. K. Phelps, Bureau of Chemistry, Washing-
ton, D. C.
Fertilizer Chemistry: F. B. Carpenter, Virginia-Carolina Chemical Co.,
Richmond, Va.
Industrial Chemists and Chemical Engineers: S. H. Salisbury. Jr.,
Northampton, Pa.
Organic Chemistry: H. L. Fisher. Columbia University, New York City.
Pharmaceutical Chemistry: George D. Beal, Chemistry Building, Uni-
versity of Illinois, Urbana, 111.
Physical and Inorganic Chemistry: W. E. Henderson, Ohio State Uni-
versitv, Columbus. Ohio.
Water, Sewage and Sanitation: W. W. Skinner, Bureau of Chemistry,
Washington. I) C
Rubber Section: J. B. Tuttle, Firestone Tire & Rubber Co., Akron,
Ohio.
ABSTRACTS OF PAPERS
In order that the meeting may receive due and correct notice
in the public press, every member presenting a paper is re-
quested to send an abstract to Dr. Chas. H. Herty, 35 East 41st
St., New York City, Acting Chairman of the Society's
Publicity Committee. The amount of publicity given to the
meeting and to the individual papers will entirely depend upon
the degree to which members cooperate in observing this re-
quest. A copy of the abstract should be retained by the mem-
ber and handed to the secretary of the special division before
which the paper is to be presented in Cleveland. Short ab-
stracts will be printed in Science.
FINAL PROGRAM
The final program will be sent to all members signifying their
intention of attending the meeting, to the secretaries of sec-
tions, to the Council, and to all members making special re-
quest therefor to the Secretary's office.
THE CHEMICAL SOCIETIES IN NEW YORK CITY
1918-1919 SEASON— RUMFORD BALL, THE CHEMISTS' CLUB
October 1 1 — American Chemical Society.
October 25 — -Society of Chemical Industry.
November 8 — American Chemical Society.
November 22 — Society of Chemical Industry.
December 6 — American Chemical Society. Joint Meeting with
Society of Chemical Industry and American
Electrochemical Society.
January 17 — Society of Chemical Industry. Perkin Medal
Award.
February 7 — American Electrochemical Society. Joint Meeting
with Society of Chemical Industry and American
Chemical Society.
March 7— American Chemical Society. Nichols Medal Award.
March 21 — Society of Chemical Industry.
April n — Society of Chemical Industry. Joint Meeting with
American Chemical Society and Society of Chem-
ical Industry-
May 9 — American Chemical Society.
May 23 — Society of Chemical Industry.
June 6 — American Chemical Society.
CALENDAR OF MEETINGS
American Institute of Mining Engineers — Annual Meeting,
Denver, Colorado, September 2 to 7, 191S.
American Chemical Society — Fifty-sixth (Annual) Meeting.
Cleveland, Ohio, September 10 to 13, 1918.
National Exposition of Chemical Industry (Fourth)— Grand
Central Palace, New York City, September 23 to 2S, 1918.
American Electrochemical Society — Autumn Meeting, Prince-
ton. X. J., September 30 to October 2, 191S.
Sept., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
749
FOURTH NATIONAL EXPOSITION OF CHEMICAL INDUS-
TRIES, GRAND CENTRAL PALACE, NEW YORK,
WEEK OF SEPTEMBER 23 TO 28, 1918
PROGRAM OF ADDRESSES AND MOTION PICTURES
Monday, September 23
Evening: Opening Addresses:
Dr. C. H. Herty, Chairman Exposition Advisory Committee.
Dr. Wm H. Nichols. President American Chemical Society.
Mr. F. J. Tone. President American Electrochemical Society.
Dr. G. W. Thompson, President American Institute of Chemical
Engineers.
Tuesday, September 24
Afternoon: Symposium on Acids and Chemical Engineering:
A. Hough, "Chemical Engineering in Explosives; T. N. T.,
T. N. A., Picric Acid, Nitrobenzol."
E. J. Pranke, "Development of Nitric Acid Manufacture."
Evening: Motion Pictures.
Wednesday, September 25
Afternoon: Symposium on Potash:
C. A. Higgins, "Recovery of Potash from Kelp."
Linn Bradley, "Recovery of Potash from Iron Blast Furnaces
and Cement Kilns."
John W. Hornsey, "Potash from Desert Lakes and Alunite."
H. W. Morse, "Potash from Searles Lake."
Evening: Motion Pictures:
Alkali Industries:
1. Electrical Precipitation of Potash from Cement Dust.1
(Research Corporation.)
2. Colloid Chemistry.
Thursday, September 26
Afternoon: Symposium on Ceramics — Meeting of the American Ceramics
Society :
L. E. Barringer, "Manufacture of Electrical Porcelain." (Illus-
trated.)
A. V. Bleininger, "Recent Development in the Ceramic In-
dustries."
H. Ries, "American Clays."
F. A. Whitaker, "Manufacture of Stoneware." (Illustrated )
J. B. Shaw, "Fuel Conservation."
S. C. Linberger, "Carborundum Refractories."
Evening: Motion Pictures:
Glass Making1 (Corning Glass Works).
The Making of Cut Glass2 (Ford).
Manufacture of Electrical Porcelain1 (General Electric Com-
pany).
The Making of Pottery1 (Ford).
1 1 reel. 2 2 reels.
Friday, September 27
Afternoon: Symposium on Metal, Industries:
Leonard Waldo, "Development of Magnesium Industry."
Alcan Hirsch. "Ferrocerium Pyrophoric Alloys."
Theodore Swann, "Ferromanganese."
Joss ph W. Richards, "Ferro-AIloys of Silicon .Tungsten, Uranium
Vanadium, Molybdenum and Titanium."
Evening: Motion Pictures.
Saturday, September 28
Afternoon: Symposium on Industrial Organic Chemistry:
S. P. Sadtler, "Industrial Organic Chemistry and Its Progress."
C. A. Higgins, "Kelp as a Source of Organic Solvents."
G. H. Tomlinson, "Wood Waste as a Source of Ethyl Alcohol."
Evening: Motion Pictures.
Among other films that will be shown each evening of the
week are the following:
On. Industries
The Spirit of the Flowers — Essential Perfume Oils.
The Story of a Cake of Soap.
Light from the Rocks— Natural Gas.
Lake Asphalt Industry (Barber Asphalt Paving Co.).
Asphalt Roofing Industry (Barber Asphalt Paving Co.).
Asphalt Colloids (Barber Asphalt Paving Co.).
Water Power; Its Development and Use
Niagara Falls.
Power Transmission.
Power of Wealth — Hydraulic Development.
Canadian Shawinigan Falls Power Development and Its Surrounding
Chemical Industries3 (Shawinigan Water & Power Co.).
Fixation of Atmospheric Nitrogen at Niagara Falls and Feeding the
Soil with It2 (American Cyanamid Co.).
Carelessness; the Destruction of Life, Wealth and Resources
Careless America (Firestone — Universal).
The Crime of Carelessness.
The Workman's Lesson.
Vaccines for Prevention of Disease.
Keep your Business Going3 (General Fire Extinguisher Co.).
Miscellaneous Chemical Industries
Manufacture of Zinc Oxide (New Jersey Zinc Co.).
Manufacture of Genuine Wrought Iron Pipe3 (A. M. Byers Co.).
From Log to Lumber* (Southern Pine Association).
Moving a Forest to France4 (Southern Pine Association).
The Wonderland of the Appalachians3 (Clinchfield Railway).
The Operation of a By-Product Coke Plant3 (H. Koppers Co.).
3 3 reels. * 4 reels.
LIST OF EXHIBITORS AT THE FOURTH NATIONAL EXPOSITION OF CHEMICAL INDUSTRIES
Complete as Furnished by the Managers of the Exposition on August 14, 1918
Abbe" Engineering Company
Abbe\ Paul O.
Ainsworth & Sons, Wm.
Air Reduction Company
Alberene Stone Company
iline Products Company, Inc.
lugas Corporation
American Ceramic Society
American Chemical Manufacturing Company
American Chemical Society
i Cyanamid Company
DyestufT Reporter
Electrochemical Society
. Institute of Chemical Engineers
American Kron Scale Company
American La France Fire Engine Company, In<
American Leadburning Company
American Metal Company, Ltd.
Meter Company
i Pipe Bending Machinery Company
i Scientific Instrument Company
1 Steel Package Company
ansformer Company
American Water Softener Company
Anaconda Copper Mining Company
Angel, H. Reeve & Company, Inc.
Aniline Dyes & Chemicals Company
Anti-Hydro Waterproofing Company
Apex Chemical Company
Arnold, Hoffman & Company, Inc.
Arkell Safety Bag Company
Bachmeier & Company
Baker. J. T., Chemical Company
Baltimore Cooperage Company
Barber Asphait Paving Company
Bario Metal Corporation
Barrett Company
Bary de, Albert. Jr.
Bausch & Lonib Optical Company
Bayonne Casting Company
Beach-Russ Company
Becker, Christian. Inc.
Bcckley Perforating Company
Bethelebm Foundry & Machine Company
Bound Brook Chemical Company
Boyer Oil Company, Inc.
Boyer Oil Manufacturing Company
Bristol Company, The
Brown Instrument Company
Buffalo Foundry & Machine Company
Butterworth-Judson Corporation
Byers, A. M., Company
Calco Chemical Company
Campbell, John, & Company
Canada Carbide Company
Canadian Chemical Journal
Canadian Electro Products Company
Canadian Electrode Company
Carborundum Company
Carrier Engineering Corporation
Celite Products Company
Celluloid Zapon Company
Central Dyestuff & Color Company
Central Scientific Company
Ceylon Company, The
Chemical Catalog Company. Inc.
Chemical Color & Oil Daily
Chemical Company of Amer ca
Chemical Construction Company
Chemical Engineer, The
Chemical & Metallurgical Engineering
Chemical Pump & Valve Company
Chemical Warfare Service
Chile Copper Company
Chile Exploration Company
Chromos Chemical Company, Inc.
Clinchfield Products Corporation
Color Trade Journal
Consolidated Color & Chemical Company
Consumers Dyewood Products Company
Contact Process Company
Corning Glass Works
Crandall, Pettee Company
Crane Company
Crane Packing Company
Crescent Color & Chemical Company
Crescent Ink & Color Company
Day, J. H , Company
De Laval Separator Company
Denver Fire Clay Company
Department of Agriculture — Bureau of Chemistry
Detroit Rang) BoUei I <unpany
Dcvine, J. P., Company
Diamond State Fibre Company
Dorr Company, The
Dow Chemical Company
Drackett, P. W., & Sons
Du Pont Chemical Works
Du Pont, E. I., de Nemo
mington
Du Pont, E- I., de
Arlington Works
Du Pont Fabrikoid Company
Duriron Castings Company
Dye Products & Chemical Co
Edison International Corporation
Electro Bleaching Gas Company
Electrolytic Engineering Corporation
Electrolytic Zinc Company
Electron Chemical Company
& Company — Wil-
Company —
Elr,
. G. H.
ueled Products Company
Empire Chemical Company
Empire Laboratory Supply Company
Everlasting Valve Company
Fleisher, W. L., & Company, Inc.
Foote Mineral Company
Foxboro Company, Inc., The
Fuller Lehigh Company
Garrigues, Chas. F., Company
General Bakelite Company
General Bauxite Corporation
General Ceramics Company
General Chemical Company
General Electric Company
General Filtration Company
General Fire Extinguisher Company
Georgia Chamber of Commerce
Georgia Mineral Products Company
Georgia Potash & Chemical Company
Glens Falls Machine W< iks
Gordon Enwineerint,' Company
Greincr, lCinil. Company
Groch CentrifiiRal Flotation Company
Guernsey Earthenware Company
Hanovia Chemical & Manufacturing Company
Hardinge Conical Mill Company
Harrison Works
llaustr-StaiidcT Tank Company
Haynes Stellitc Company
Wayward, S I' '.. ( ompanv
Heald, John II . Company, tni
Hemingway, Frank. Inc.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 9
Hepworth, S. S., Company
Hellenic Chemical & Color Company
Hercules Engineering Company
Hercules Powder Company — Chemical Sales
Department
lU-rold China & Tottery Company
Hodges Water Still Company, Inc.
Holly Pneumatic Systems
Hood, B. Mifflin, Brick Company
Hooker Electrochemical Company
Hoskins Manufacturing Company
Huff Electrostatic Separator Company
HuntCf I>ry Kiln Company
Huyck, F. C, & Sons
Imperial Color Works
Imperial Dyewood Company, Inc.
Independent Chemical Company
Industrial Filtration Corporation
Innis, Speiden & Company
Irving National Bank
Isco Bantz Company
Isco Chemical Company
Jacques Wolf & Company
Janney, Steinmetz & Company
Jewell Polar Company
Journal of Industrial & Engineering Chemistry
KalbBeisch Corporation
Kalbperry Corporation
Kewaunee Manufacturing Company
Kcstone Minerals Company
King Chemical Company
Klipstein, A., & Company
Knight, Maurice A.
Know-ilk- Board of Commerce
Koppers, H., Company
Leeds & Northrup Company
Life Savings Devices Company
Little, Arthur D., Inc.
Lummus, Walter E., Company, The
Lungwitz, Emil
Luzerne Rubber Company
Macbeth-Evans Glass Company
Machinery Utilities Company
Manufacturers Record
Marden, Orth & Hastings Company, Inc.
Mathieson Alkali Works, Inc. — Niagara Branch
Mathieson Alkali Works. Inc.
Maynard, T. Poole, Ph.D.
Maywatd, Frederick, F. C. S.
Meek Oven Manufacturing Company
Mendlcson Corporation
Merck 8c Company
Metals Disintegrating Company, Inc.
Metz, H. A.
Mine & Smelter Supply Company
Miner-Edgar Company
Monarch Manufacturing Works, Inc.
Monongehela Valley Traction Company
Mott, J. L., Iron Works
AMERICAN ELECTROCHEMICAL SOCIETY FALL MEET-
ING AT PRINCETON
The August bulletin of the Society contained the following
notice :
The officials of Princeton, and our local members, headed by
Professor Northrup, have given us a most cordial invitation and
we are assured of a warm welcome. There are fine physical and
chemical laboratories to be seen, and fine fellows to get better
acquainted with, and a real, rich scientific program. The date
is September 30 to October 2, 1918, immediately following the
Chemical Exposition in New York. Programs will go out with
the September bulletin. If you have never visited Princeton,
now is your best chance; if you have, you do not have to be
urged to go again.
AMERICAN ELECTROCHEMICAL SOCIETY
The American Electrochemical Society has passed the follow-
ing resolutions concerning alien enemy members:
Whkreas, A communication has been submitted to the Board
of Directors bearing the signature of sixteen members, in accord-
ance with Paragraph 5, Article III of the Constitution, request-
ing "that all members of the Society who are subjects of Germany
or Austria be dismissed, on the ground that they are opposed
to the United States of America in its war for the preservation
of civilization, and are consequently enemies of the majority
of the members of our Society, " therefore be it
Resolved, That it is the sense of this Board that all members
of the Society who are enemy aliens and who are in sympathy
with the enemies of the United States of America in the present
war should be dismissed from membership on the grounds above
set forth, and
Resolved, That the Secretary be instructed to send a copy of
this Resolution to all such members requesting that they either
Moulton Engineering Corporation
Multi Metal Separating Screen Company
Nash Engineering Company
Nassau Valve & Pump Corporation
National Aniline & Chemical Company
National Color & Chemical Company
National Glue & Gelatine Company
National Gum & Mica Company
New Jersey Zinc Company
Newport Chemical Works, Inc.
New York Commercial
New York Revolving Portable Elevator Com-
pany
Niagara Alkali Company
Niagara Electro Chemical Company
Nichols Copper Company
Nitrogen Products Company
Norton Company
Obex Company
Oil, Paint & Drug Reporter
1 tliver Continuous Filter Company
Ontario Bureau of Mines
Organic Salt & Acid Company
Page Steel & Wire Company
Palo Company
Parks, G. M., Company
Peerless Color Company
Penn. Salt Manufacturing Company
Pfaudler Company
Philadelphia Quartz Company
Philadelphia Textile Machinery Company
Pneumercator Company. Inc.
Powdered Coal Engineering & Equipment Com-
pany
Pratt Engineering & Machinery Company
Precision Instrument Company
Precision Thermometer & Instrument Company
Process Engineers. Ltd.
Product Sales Company
Provost Engineering Company
Quigley Furnace Specialties Comp any
Raritan Copper Works
Raymond Bros. Impact Pulverizer Company
Rector Chemical Company
Republic Chemical Company
Research Corporation
Roessler & Hasslacher Chemical Company
Rolling Chemical Company
Rossendale-Reddaway Beltin : & Hose Company
Ruggles-Coles Engineering Company
R. U. V. Company, Inc.. The
Schaeffer & Budenberg Manufacturing Company
Schaum & Uhlinger. Inc.
Schutte & Koerting Company
Schwartz Sectional System
Scientific Equipment Company
Scott, Ernest, & Company
Semet-Solvay Company
Seydel Manufacturing Company
Sharpies Specialty Company
Shawinigan Electro Metal Company
Shawiuigan Water & Power Company
Shriver, T., & Company
Sidio Company of America, Inc.
Simmons. John, Company
Solvay Process Company
Southern Pine Association
Southern Ball Clay Company
Sowers Manufacturing Company
Sparks, John C.
Stamford Extract Manufacturing Company
Standard Emarex Company
Stevens-Aylsworth Company
Stauffer Chemical Company
Stein, Hall & Company
Sterling Color Company
Stokes, F. J., Machine Company
Stresen-Reuter & Hancock Company
Stuart & Peterson Company
Sturtevant Mill Company
Evaporator Company
Tagliabue, C. J., Manufacturing Company
Takamine Laboratory. Inc.
Tank Equipment Company
Taylor Instrument Companies
Textile Colorist
Textileather Company
Textile World Journal
Thermal Syndicate. Ltd.
Thermo Electric Instrument Company
Thwing Instrument Company
Tolhurst Machine Works
Trades Reporting Bureau, Inc.
Uehling Instrument Company
United Lead Company
U. S. Cast Iron Pipe & Foundry Company
U. S. Industrial Alcohol Company
U. S. Industrial Chemical Company
Universal Oil Company
Valley Iron Works
Van Dyk & Company
Van Emden, H., & Company
Wallace & Tiernan Company, Inc.
Warner Chemical Company, Inc.
Warner Klipstein Chemical Company
Werner & Pfleiderer Company
Westinghouse Electric & Manufacturing Com-
pany
Whitall Tatum Company
Williamsburg Chemical Company
Zapon Leather Cloth Company
Zaremba Company,
Zavon, Inc.
appear in person at the meeting of the Board of Directors to be
held at the Niagara Club, Niagara Falls, N. Y., Saturday,
August 24, 1918, at 11.00 a.m., or file answer by letter stating
whether or not they support the aims and ideals of the United
States of America in the present conflict.
GENERAL SYMPOSIUM ON THE CHEMISTRY OF
DYESTTJFFS
At the Cleveland Meeting of the American Chemical Society
there will be held in connection with the Division of Industrial
Chemists and Chemical Engineers a symposium on the
chemistry of dyestuffs, in all its phases, including the use, ap-
plication, and manufacture. This symposium will be held on
Tuesday, September 10, at 2 p.m., and will be continued to
Wednesday morning.
Successful establishment of a complete dyestuff industry in
America together with its continuous development is so funda-
mentally related to the chemistry of the subject that all interested
in this industry must try to develop to the fullest possible extent
every phase of the chemistry of dyestuffs.
The plan is that out of this symposium will grow regular
sectional meetings on dyestuffs and we bespeak the cooperation
of everyone interested in dyestuffs.
While every chemist in this industry has been busy with de-
velopment and problems occasioned by the abnormal conditions
of the war, yet we feel sure that now is the time to start laying
emphasis on the chemistry of dyestuffs, the very backbone of the
industry. We ask all interested to cooperate by attending this
symposium.
Thb Calco Chemical Company R. NORRIS SHREVB
Bound Brook, N. J.
Sept., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
75i
NOTE5 AND CORRESPONDENCE
ASSOCIATION OF BRITISH CHEMICAL MANUFACTURERS
The Second Annual General Meeting of the Association was
held at the Chemical Society's Rooms, Burlington House,
Piccadilly, London, on Thursday, July 11, 1918, for the pur-
pose of appointing scrutineers to examine the ballot papers,
for the reception and adoption of the report and accounts, the
election of auditors, and the reception of the report of the scruti-
neers. Dr. Charles Carpenter, D.Sc, M.I.CE-, occupied the
chair.
After the notice convening the meeting had been read by the
Secretary, Captain G. Mount, D.S.O., and the scrutineers to
examine the ballot papers had been appointed, the Chairman
moved the adoption of the report of the Council of the Associa-
tion.
Dr. Carpenter in the course of his speech said that the Asso-
ciation had made satisfactory progress and that one indication
of that progress was the increase in membership and the corre-
sponding increase in capital.
During the year the Association suffered loss in the death
of Mr. R. D. Pullar, who had been a loyal and conscientious
member of the Council, and of Mr. Thomas Tyrer, well known
in the chemical trade for many years.
In dealing with the item in the report referring to the Direc-
tory, the Chairman said that it was now well in hand, the bulk
of it being in the printers' hands. A good part of the work of
translation had been done, that which was not complete being
the translation of the Russian and Japanese sections. This
portion had been delayed by reason of the great demand for
translators of these languages. The Directory will be printed
in English, French, Italian, Spanish, Portugese, Russian, and
Japanese, and will thus provide for a very comprehensive cir-
culation throughout the markets of the world of information
relating to British manufacture in connection with chemical
products.
In the paragraph dealing with foreign trade there was de-
scribed a very useful system which has been put into operation
for placing at the disposal of members of the Association in-
formation available at the Department of Overseas Trade and
the Foreign Office. Some fifty members had taken advantage
of this machinery and expressed appreciation of it.
In the matter of reconstruction, it was reported, the Council
had done very useful work. The Chairman outlined what
had been done from the setting up of the Committee appointed
by Dr. Addison to advise as to the procedure which should be
adopted for dealing with the chemical trade down to the pres-
ent negotiations with reference to the establishment of joint
industrial councils. He thought the Meeting would agree with
him that in dealing with the question of industrial alcohol the
Association had also been very helpful. When it was remem-
bered how long it had taken to educate the Government on the
technical questions connected with the use of alcohol in chem-
ical manufacture, he felt that a great advance had been made
in the acceptance of the recommendations of the Alcohol Com-
mittee of the Association. In this connection he thought they
owed something to the foundation laid by their late lamented
friend, Mr. Thomas Tyrer.
The Information and Statistical Bureau has been established
with the view of avoiding overlapping and waste of time and
energy in research and manufacture. The scheme for the forma-
tion of the Bureau has met with a large amount of approval
and has given proof that the Council is at any rate making an
endeavor to do something substantial in dealing with what is
one of the difficult problems facing chemical industry at the
present time.
The Council has supported the efforts of the Chemical Society
in establishing a comprehensive library of chemical technology.
The desire is not only to extend the library, but to extend the
hours during which the library is available, and in financially
supporting this scheme the Association is contributing to the
future welfare of chemical work in the country.
With regard to the difficult problem of the dye industry the
speaker thought that the course followed in 1915 in developing
the explosive manufactures of the country, viz., to use all and
everybody, great and small, in order to get all working in the
direction of making up the terrible shortage, was the right one,
and the concentration of the work in the hands of only a few
firms, as appears to be the present policy in dealing with the
dye situation, would not produce such a measure of national
success as if all the resources of the country were utilized.
In conclusion, the Chairman referred to the appointment of
Mr. W. J. U. Woolcock as General Manager of the Association,
and to that of Captain G. Mount as Secretary. The appoint-
ment of suitable persons for these positions had been no easy
matter, but he could assure the Meeting that in these two officials
they had two men admirably suited in every way to carry out
the particular duties required of them.
The motion for the adoption of the report was seconded by
the Vice Chairman, Mr. R. G. Perry, and after discussion was
carried unanimously.
Messrs. Feasey and Company were elected auditors for the ensu-
ing year, and after the scrutineers had reported the result of the
ballot the Chairman announced the constitution of the new
Council and group committees and moved a vote of thanks
to the Chemical Society for the use of their rooms. This was
seconded by the Rt. Hon. J. W. Wilson, M.P., and carried
enthusiastically.
The Vice Chairman, in moving a vote of thanks to Dr. Car-
penter, stated that for two years Dr. Carpenter had been the
mainstay of the Association. He had done more work than any-
body else in connection with its formation and he had done the
lion's share of it since. The vote of thanks was seconded by
Mr. Roscoe Brunner, who remarked that it might quite rightly
and justly be stated that Dr. Carpenter had led the Council*
in all its work. The vote of thanks having been most heartily
accorded, and Dr. Carpenter having replied, the proceedings
then terminated.
THE SULFURIC ACID INDUSTRY1
By C. J. Goodwin
The report recently published by the Departmental Com-
mittee on Sulfuric Acid and Fertilizer Trades is already bear-
ing fruit in steps taken to form a National Association of Sul-
furic Acid Makers, and it is to be hoped that the other recom-
mendations made by the Committee will also lead to a more
complete examination of manufacturing details. War condi-
tions did much to arouse inefficient manufacturers from their
former lethargy, and led to the gradual introduction of more
efficient plant and methods by means of individual trial and
error, but the Committee's conclusion that in the majority of
cases' scientific cost-keeping is usually conspicuous by its ab-
sence, is well founded. The strict control of output and prices,
and especially profits, has since caused a partial return to this
lethargic attitude, but the probability that only the more effi-
cient works will be permitted to survive on account of reduced
post-war requirements should now result in well-directed cf-
' Reprinted from the Chemical Trade Journal and Chemical Engineer,
April 20, 1918.
752
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 9
forts in regard to scientific management and the elimination of
waste.
While the Committee recommend that the information re-
garding cost-keeping, etc., collected at Government establish-
ments, should be placed at the disposal of private manufac-
turers after the war, it would seem a more obvious and satisfac-
tory course to do so now in order that manufacturers may put
their houses in order forthwith. This also applies to the cost
data upon which the Committee base their conclusions in re-
gard to the relative advantages of the available systems for the
manufacture of different strengths and grades of acid. By thus
fostering not only scientific cost-keeping and management, but
also the spirit of competition, the process of ultimately elimina-
ting inefficient works will be facilitated, as the necessary data
will be available over a sufficient period of time.
It is clear that 'pre-war data of manufacturing costs are no
longer applicable, and, indeed, very little has been published in
this country regarding them since Guttman's paper.1 The posi-
t;on is further complicated, not only by the arguments adduced
by the Committee, but by many other considerations. Among
these may be mentioned: (1) That it is now possible to install
and operate contact plant either without the payment of royal-
ties or, at any rate, with reduced royalties; (2) the present and
future increased freight charges and other dues on imported
pyrites and sulfur; (3) the crude sulfur position; and (4) the
cost and de-arsenication of acid from the lead-chamber process.
Taking these in order, the conclusion of the Committee that
the Grillo process, or a modified form of the Grillo process,
is the most likely competitor of the chamber or tower systems
will find general acceptance. In comparing the value of Grillo
acid with chamber acid, allowance must be made for the fact
that it is free from arsenic, iron, and other impurities.
The Committee also make no mention of the possibilities of
a "mixed" system of contact and chamber plant such as has
been introduced in America. As regards pyrites and crude
and recovered sulfur, the cost of, these will be interdependent,
and the post-war situation will naturally depend largely on
available tonnage, freight rates, the attitude of the sulfur-pro-
ducing countries and companies, and the position of the metal
market. The dominating factor will be the cost per unit of
available sulfur after making allowance for residual ore values,
arsenic content, and extra cost of additional fuel for ores of
low sulfur content, and as crude sulfur only requires about one-
half as much tonnage as pyrites, and a still smaller proportion
as compared with zinc or the like concentrates, the question of
freight rates, available tonnage, etc., will be important fac-
tors, and give rise to continual controversy. At present, mainly
owing to difficulties in importation, sulfur is increasingly dis-
placing pyrites in America and elsewhere, and as a result great
improvements have been effected in the design of rotary and
other types of sulfur burners. Apart from the prime cost per
unit of available sulfur, such plant leads to more intensive
working as a richer gas results. Economies also result in labor
and running expenses, and in the cost of purifying plant for the
burner gases. When all these factors have been taken into
account, it is not improbable that the use of crude and recovered
sulfur will be introduced in this country to a greater extent
than at present, especially it freight rates remain high.
As regards de-arsenication, it seems desirable to place com-
parative costs also at the disposal of manufacturers, both as
regards plant in which the arsenic is removed prior to entering
the Glover tower by methods similar to those obtaining in
contact 1 in which weak acid is treated
by sulfuretted hydrogen and the like prior to concentration or
sale. Naturally, the whole output of a given works do< not,
as a rule, require de arsenication, and in cases where the output
' J. Soc. Chem. Ind., 22 (1903), 1331.
is intended solely for superphosphate and certain other processes,
de-arsenication is unnecessary. For such plants it is unlikely
that the chamber or tower processes will be superseded, and
the aim of the largest works will be to cater for all branches
of the trade, and to install and operate the various types of sul-
furic acid plant in such proportions that the output of each
grade of acid can be regulated to correspond with current sales.
If the Xational Association of Sulfuric Acid Makers is to
justify its title, the component parts of that body will, it is
hoped, sink all trade differences and jealousies, and pool informa-
tion, trade, and results in the fullest sense of the word. In
addition, a Central Information or Intelligence Department,
combined with a properly conducted Industrial Experiment
Station attached to one of the larger and more efficient works
should be organized and supported by all the individual mem-
bers of the Association, who would draw upon it, not only for
cost and experimental data, but for all information regarding
the future development of the industry. Such a Central In-
telligence Department would, without interfering with indi-
vidual enterprise, try out and report on improved plant an
processes; it should be a self-supporting institution earning
dividends by results, but would require a guaranteed minimum
income in the first instance.
These notes are not intended as a detailed criticism of the
Committee's Report, but are written to stimulate investigation,
discussion, and correspondence, through the medium of this
Journal and otherwise. Much could be written regarding manu-
facturing methods, details of plant, and new processes, but
this would be outside the scope of the present article. Among
such topics may be mentioned the pre-drying of air supply to
burners, etc.;1 the cost of storage of acid for contact and tower
systems; the relative advantages of the different kinds of filling
material for towers; pyrites and fuel storage; drying and con-
veying plant; concentration plants; with special reference to
packed concentration towers; electrical fume and dust precipi-
tation; burners for spent oxide and low-grade ores;' use of am-
monia and Ostwald process instead of nitrate of soda; leadless
Glover ana Gay-Lussac towers, in .acid-proof masonry; and,
last, but not least, the scientific control of the chamber process.
The latter point was not dealt with by the Committee, and the
proposals of investigators like Fairlie3 merit further attention.
It is to be hoped that the authorities will give further material
and individual support to these problems.
CHEMISTRY FOR THE PUBLIC
Editor of the Journal of Industrial and Engineering Cliemistry:
I have arranged with a local paper to contribute a weekly
article on various phases of industrial chemistry' in relation
to the war. I have undertaken this because I am anxious to do
what I can in litis community to advertise chemistry and give
the layman a more intelligent conception of what industrial
chemistry is. The paper, which is the largest in the district
has taken very kindly to the idea and has given me a column on
the editorial page.
I would be glad to have any suggestions for material which the
Publicity Committee might be able to give, and your permission
to make occasional use of ideas or phrases from your editorials.
I believe that if someone could be found in each community
who is willing to do something of this kind, a great deal of good
could be accomplished.
Turks Haots, [no. Raymond D. Cooke
July 8
i British Patent No. 16,981, 1915.
'Ibid., No. 108,986, August. 1917.
' Tram. Am. fiuf. Cktm. En£.. p 319, rl stq.
Sept., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
753
CIVIL SERVICE RULES WAIVED FOR WAR GAS
INVESTIGATORS
EXECUTIVE ORDER
The Secretary of War is hereby authorized to employ, with-
out reference to the requirements of the civil service act, such
persons in the Research Division, Chemical Warfare Service,
at the American University, as may be needed in conducting
certain investigations and construction work relating to gases
and chemicals used in war, it being understood that all possible
use will be made of the registers of eligibles of the Civil Service
Commission. This authority shall continue only during the
present war.
The Commission concurs with the War Department in recom-
mending this order because of the urgent and highly confidential
character of the work involved and the fact that it must be organ-
ized and prosecuted with the greatest dispatch and be safe-
guarded most effectively.
The White House Woodrow Wilson
July 19, 1918
RESEARCH FELLOWSHIP
STATE COLLEGE OF WASHINGTON
The Department of Chemistry of the State College of Wash-
ington, Pullman, Washington, announces the establishment
of a fellowship, to be devoted to research on the extension of the
chemical uses of magnesite, paying $600 a year. Applications
are invited from young men having the Bachelor's degree in
chemistry from a college giving a four-year course. The appointee
will give twelve hours a week to instructional work in elementary
chemistry, the remainder of his time being given to research
and study in advanced courses leading to the M.S. degree.
Interested parties should send photograph with their applica-
tion, together with letters of recommendation and statement
of special qualifications.
CHEMICAL ENGINEERING IN OUR UNIVERSITIES
Editor of the Journal of Industrial and Engineering Chemistry:
In the list of institutions given on p. 645 of the August number
of the Journal, I notice that we are reported as possessing no
course in Chemical Engineering. I cannot understand how the
writer of the paper arrived at such a notion.
As a matter of fact we had one of the first complete courses
given although we do not claim to have really started before
1 91 2. You may be very sure that we have a course now and
have had one since that date, a comprehensive and difficult
course.
By this mail I am sending you our latest catalog on page 94
of which you will find the course in Chemical Engineering set
forth and I beg of you to note that there is no camouflage in it
nor any so-called paper courses.
We are situated near "large manufacturing enterprises in-
volving chemical control and chemical processes." Our students
are not given "an opportunity" to visit such plants but are
compelled to do so, and are conditioned if they fail to make a
proper report.
Department of Chemistry W. P. MASON
Rensselaer Polytechnic Institute
Troy, N. Y., August 13, 1918
WASHINGTON LETTER
By Paul Wooton, Union Trust Building, Washington, D. C.
Two pieces of legislation which are of direct importance to
chemical industries are on the point of taking final form at this
writing. They are the Revenue Bill and the War Minerals
Bill.
Regardless of the levies on war profits and excess profits,
which may be contained in the bill which the Committee on
Ways and Means will report to the House, it is practically certain
that the legislation will go on the statute books with an 80
per cent, or greater, tax on war profits and with nothing more
than the perfecting of the existing graduating tax on excess
profits. The Senate does not hold the present Committee on
Ways and Means in high esteem in regard to its ability to draft
revenue legislation. Extensive changes are certain to be made
in the Upper House. The temper of the House of Representa-
tives apparently is unusually critical of the work being done
by the Ways and Means Committee. The bill is certain to
receive a very general overhauling in the House itself. It is
very certain, however, that the bill will be out of the hands of
Congress prior to the launching of the fourth Liberty Loan cam-
paign on September 28. The Ways and Means Committee ex-
presses its opinion in the platinum controversy by applying the
luxury tax of 10 per cent on platinum jewelry and by singling
platinum jewelry out for an additional tax of 10 per cent.
The War Minerals Bill, which is of vital interest, not only to
the mining and metallurgical industries, but to all users of
mineral materials, which heretofore have been largely imported,
is in process of being rewritten by the Senate Committee. The
bill which will lie introduced is likely to be a compromise be-
tween proposed measures submitted by Senator Henderson,
of the War Industries Board, and the Interior Department.
From information reaching Washington, it would seem that the
chemical industries are well divided as to whether control of
these minerals is necessary or whether the placing of broad
powers in the hands of a government agency would not produce
me ire harm than good.
istenf demand for a bonus on gold production is coming
from the West. Economists in the government 1
giving the matter studious attention. They apparent!
convinced thai a bonus will do more than double Chi
The matter has come prominently to the attention of the Com-
mittees on Mines and Mining of the'Senate and of the House.
Attention by Congress to the problems involved is assured.
Those best informed are of the opinion that no more can be done
than to remove the petty annoyances that are hampering gold
mining. They take little stock in the various proposals whereby
the industry would be cleared of its difficulties by a single radical
step. That encouraging things are being done already is shown
by the action of the Priorities Board in announcing that it will
give preferential treatment to tools, machinery, and equipment,
and will use its influence in securing ample fuel and labor supplies
and the maximum of transportation service. Decided aid also
was given the gold mining industry by the stabilization of the
price of silver, which now is enjoying what is tantamount to a
fixed price in excess of $1.00 an ounce.
More should be done to utilize potash-bearing materials,
in the opinion of one of the best known authorities on this subject
in the country. With the reluctance so characteristic of
scientists, he declines to allow his name to be attached to an
informal statement but his thought on the subject is as follows:
According to the 6gures given out by the U. S. Geological Survey,
the production of potash for the first half of this year was between
20,000 and 25,000 tons of K:0. and it is estimated that the total for the
year will reach 00,000 tons. This is abouc 25 per cent of our pie-war im-
portations, and if this country is to become independent of Germany,
immediate steps should be taken to develop further our own sources of
supply.
I ' ment works and blast furnaces alone should be able to supply
our total requirements, but so far these industries have done very little.
By the end of 1918 about a dozen cement eompauies will be recovering
potash as B uod incidentally abating the dust nuisance. The
blast furnaces are doing practically nothing, although ii is generally
recognized that they would benefit considerably i*\ obtaining (leaner gas
foi 'I" stovi "m I gas engini H nufacturers can hardl] be blamed
foi nol putl Hi' necessary additions to their plants under
ii uncertainty "t the win,], potash 'i1" tion. Although the
in i ii i in high, no one knows how long they will last, and under
the proposed revenue bill, mosl oi 'In profits would lie taken by the Govern-
I ii' Phi '" tnufai turers would nol object to this if they were
7 54
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 9
allowed to amortize the cost of plant before being subject to any profits
tax. The producers of potash should also be given definite assurance by
the Government that there will be no "dumping" of German potash after the
war.
A source which it seems to me should be thoroughly investigated is
the potash -bearing silicate rocks. There are large deposits of these running
fairly high in potash, notably the greensands of New Jersey, the leucite
deposits of Wyoming, and the sericites and potash bearing slates of Georgia.
Although no commercially successful method of extracting potash from
silicate in general has developed as yet, this problem should not be beyond
the skill of American chemists and metallurgists.
Congress granted an appropriation of $175,000 in 1916 to the Depart-
ment of Agriculture for an experimental plant for treating kelp, and it
seems to me that the silicates offer an even more promising source of potash.
I think it would be a very good idea if a similar appropriation were made
to the Bureau of Mines for carrying out experiments on these silicates,
as, if a successful process for extracting the potash can be developed, the
supply of raw material is practically unlimited.
As a result of successful experimentation, pyrite cinder from
the South is about to enter quite generally into use as iron ore.
Due to the fact that this cinder is low in phosphorus and contains
50 per cent of iron, it can be used to advantage in blast furnaces.
An amplification has been made of the commodity list of
articles which may be exported to Holland and Denmark. The
new list contains dyes and dyestuffs and the following drugs:
Acetylsalicylic acid
Aconite, pure
Agaricin
Althaeae root
Amidol and substitutes
Argentamine
Arsenobilin
Arsenous acid
Camomile Metol
Chromic acid Nitrate of silver
Diethyl barb it uric acid Opium alkaloids
Digitalis Paraldehyde
Eucaine Phenacetine
Ferric compounds Salicylic acid
Fruit of fennel Sodium arsenate
Hydrobromic acid Sodium bromide
sulfate, pure Ichthyol Sodium cacodylate
for X-ray Inula root Sodium nitroprusside
Beta-naphthol Iron, reduced Sodium salicylate
Bromine Kharsevan Sulfuric acid
Butylchloralhydrate Leaves of hyoscyamus Veronal
An announcement made August 11 by the Department of
Labor reads as follows:
Tentative findings of the preliminary survey of the chemical industries
at Niagara Falls, New York, made by representatives of various federal
departments acting under the direction of the Women in Industry Service
of the Department of Labor were announced to-day.
The committee assembled by the Women in Industry Service went to
Niagara Falls in response to an invitation from the Employers' Association.
The manufacturers working on war contracts wished to introduce women in
greater numbers into employment into which they have not previously
entered. The committee included in its membership public health experts
and consulting engineers.
It was found that the matter of approving the employment of women in
the chemical industry was only a part of the entire problem of the labor
supply for that region. Looking ahead, it is plain that a greater and greater
demand for women workers will be experienced. Accordingly the technical
experts on the committee made a quick survey of the processes in order to
discover how, if possible, the industry might be made suitable for the
employment of women.
The committee expects to make a continuous observation of conditions
in this industry. It will assist the individual manufacturers in so arranging
their processes that conditions of employment of women— and of men as
well — will be improved. The Women in Industry Service is thus planning
to operate as a consultant organization rather than as a bureau of research.
Methods being tried out at Niagara will, if successful, be applied to other
fields where the demand for women is great.
An announcement from the War Department, August 12, fol-
lows in its entirety:
Chemically treated cotton cloth, as a substitute for silk, is being tested
out by the Ordnance Department.
If found practicable for ordnance uses, the discovery will effect the
double result of meeting a serious shortage in silk, and of bringing about a
money saving in the ordnance program estimated at between $25,000,000
and $35,000,000.
Preliminary tests already made at the Aberdeen Proving Grounds have
encouraged the Department to proceed further with its experiments; and
for this purpose an order for 5,000 yards of the new material has been
placed with the concern responsible for developing the process of treating
the cotton cloth.
At present, millions of yards of silk are required in making the bags
which contain the large powder charges used in the firing of heavy artillery.
These bags arc inserted in the gun immediately behind the projectile, and
the firing of them gives the propelling force that hurls llie projectile at the
target. This propelling charge is, of course, entirely distinct from the
charge within the projectile that explodes the missile after it reaches the
target.
Heretofore, silk has been depended upon for these bags for the reason
that no other cloth material has been found that would meet the peculiar
conditions required. It is essential that not a particle of the bag container
shall remain after the gun is fired. Otherwise a smoldering piece of the
fabric might cause a premature explosion when a new charge was inserted.
Owing to the great scarcity of silk, however, the cost of this material
has increased enormously. This shortage is felt by all the warring powers,
including Germany. Early in the war Germany is understood to have used
a chemically treated cotton as a substitute for silk, but has since been
compelled by the diminishing cotton supply to resort to other substitutes.
It is estimated that the chemically treated cotton cloth now being
tried out by the Ordnance Department, if entirely suitable, could be pur-
chased in almost unlimited quantities and at a cost far below that of the
silk fabric now used.
Chemicals to the value of $14,953,083 were exported in June
of 1918, according to returns to the Department of Commerce.
This compares with exports to the value of $19,104,020 in June
of 1917. Imports of chemicals in June 1918, amounted to
$i3»5i3. 552, as compared with $16,441,353 in June of 1917-
One of the striking features of the export figures is that for-
wardings of sulfuric acid to foreign countries increased from
4»535,68i pounds in June of 1917 to 10,053,178 pounds in June
of 1918. The exports of sulfate of copper fell off more than
two-thirds. In June of this year, exports were 1,195,306 pounds,
as compared with 3,607,804 in June of 1917.
An agreement has been effected by the Food Administration
whereby the prices of dynamite glycerin have been stabilized.
Allied requirements, estimated at 7,000 long tons, will be
furnished at 60 cents a pound in August and September; 58
cents in October and November; and 56 cents in December,
f. o. b. production points in drums — drums included in price —
deliveries to be divided into quotas of approximately one-third
for each of the three periods. Sales to domestic consumers
will be made on the same basis, and it is suggested that they
accept the same deliveries, as nearly as possible.
It is assumed that the price of crude glycerin and chemically
pure glycerin will be stabilized by market conditions to a basis
conforming to the prices cpecified for dynamite glycerin.
The price agreement was entered into for the manufacturers
by a Soap and Candle War Committee which held its first
meeting at the Food Administration, June 3. This committee
was appointed by the trade, and its personnel is as follows:
Sidnev M. Colgate, of Colgate & Co., New York, chairman;
SamuelS. Fels, of Fels & Co., Philadelphia; W. E. McCaw, of
Procter & Gamble, Cincinnati; W. O. Thompson, of N. K.
Fairbanks Co., Chicago; L. H. Waltke, of William Waltke &
Co., St. Louis; N. N. Dalton, of Peet Brothers Manufacturing
Co., Kansas City; Sidney Kirkman, of Kirkman & Son, Brook-
lyn, N. Y.;and George B. Wilson, of the Globe Soap Co., Cin-
cinnati, ex-ofricio chairman.
The Committee and Food Administration recommend that all
soap makers who manufacture soap containing more than 1
per cent of glycerin take steps at once to reduce it to that per-
centage. Glycerin is especially in demand at present in Great
Britain and Italy, where it is used to make cordite, a smokeless
powder, and in Canada for explosives.
The United States War Industries Board and the United
States War Trade Board jointly announce the following rules
and regulations with respect to the sale for export, and the
exportation of caustic soda:
On and after August 1, 1918, manufacturers of caustic soda in the
Unittfti States will not enter into any contract lor the sale of caustic soda
with any person in the United States for the purpose of exporting the
same, unless and until advised by the prospective purchaser that a United
States export license covering such caustic soda has been duly obtained
and the tin rut at thereof is furnished.
Manufacturers will not sell on and after the above named date, caustic
soda .for domestic consumption unless the purchaser agrees not to export
same nor to sell same for export, and if it is resold in the domestic market,
to exact or cause to be exacted a similar agreement from each and every
subsequent purchasei
On and after August I 1918. the United States War Trade Board will
not license for exportation caustic soda to any destination until the appli-
cant has filed a statement showing either:
0) That on August 1, 1918. the applicant did not own or have any
interest in any contracts for the sale of caustic soda to be exported from.
the United States; or
Sept., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
755
(2) A list of all contracts with purchasers abroad existing on August 1 ,
1918, for the exportation of caustic soda which had not been exported on
that date, showing, (a) the names of the purchasers abroad, or consignees;
(6) the dates of the contracts; (c) the quantities; id) the price paid or con-
tracted to be paid therefore; and (e) if the applicant on August I, 1918,
owned or had any interest in the title to the caustic soda to be exported
the place or places of storage on or about that date, or if in transit on
August 1, 1918, from an inland point within the United States, the date of
shipment from such point and port of exit in the United States to which
such shipment was destined.
On and after August 1, 1918, applicants for licenses to export caustic
soda will also be required to state on their applications whether or not
they have acquired any title or interest in the caustic soda which it is pro-
posed to be exported, and if the caustic soda is in existence, the place of
storage in the United States, and to agree that in the event an export
license is granted, not to ship or permit to be shipped under such license
any other caustic soda than that specified in the application.
The foregoing requirements are supplemental to the regula-
tions contained in circular letters issued by the United States
War Trade Board under date of March 30 and May 21, 1918.
For the convenience of exporters the regulations with respect
to caustic soda have been consolidated and revised into one
ruling (W. T. B. R. 175, issued July 26, 1918). Copies thereof
may be obtained upon application to any branch office of the
War Trade Board on and after July 27, 1918.
During the absence of L. L. Summers, head of the Chemical
Section of the War Industries Board, A. W. Chase is acting as
chief of the Section.
PERSONAL NOTES
Lieutenant Andrew P. Peterson, a member of the Chicago
Section of the American Chemical Society, who had been in
military service in France since September 191 7, was reported
in the June casualty list as having been severely wounded. In-
formation was received indirectly a few days later that he was
recovering from his wounds, but on July 15 the casualty list
announced Lieutenant Peterson's death as the result of wounds
received at the front.
Lieutenant Peterson was a resident of Lamberton, Minne-
sota. He attended the University of Minnesota, receiving the
degree of Bachelor of Science in chemical engineering in 1910
and Master of Science in 191 1. He entered the service of the
Western Electric Company at its Hawthorne plant in the Sum-
mer of 191 1, and remained in that service until the time of his
enlistment at the First Officers' Training Camp at Fort Sheri-
dan, in May 191 7.
Lieutenant Peterson was a chemical engineer of unusual
ability and attainment. In the service of the Western Electric
Company he specialized upon the technology of the fabrica-
tion of rubber. He conducted some important industrial re-
searches, and soon distinguished himself by the ability to put
to practical use his scholarly attainment. He was not only
well balanced intellectually, being quite as proficient in math-
ematics as in the physical sciences and philosophy, but he was
unusually well developed physically, having several times carried
off honors as a wrestler.
Shortly before his enlistment he had been promoted to Chief
of the Research Department of the Chemical Engineering Divi-
sion at the Hawthorne Works, and had been strongly urged
to use his scientific training and experience in engineering ser-
vice for the Government. While he admitted that he un-
doubtedly could be more useful in that service, he felt that be-
cause he was physically able, he ought to go into active military
service. After debating for several weeks as to what was
his duty in the matter, his powerful sense of the justice ot the
Allied cause and his duty as an American citizen forced him to
enlist for direct military service. He obtained his commis-
sion at the close of the First Officers' Training Camp at Fort
Sheridan, and was sent immediately to England, whence, after
several weeks' training, he was sent to a point near the front
line trenches for intensive training with certain British units.
He was among the first Americans to take part in the opera-
tions on the Western front during the past Spring. — F. W.
WnxARD, Chicago Section.
Mr. Charles V. Bacon was commissioned a captain in the
Engineer Reserve Corp on July 2 and is now stationed at the
General Engineer Depot, Washington, D. C, in the Division of
Investigation Research and Development, being a member
of the executive committee. Capt. Bacon was formerly asso-
ciated with the American University Experiment Station as
Chief of Section on Flaming Liquids, and later as Chief of
Section on Oil Research. Mr. Bacon's laboratory in New York
City is being conducted in his absence by Mr. Ernest Molnar.
Mr. C. H. Crawford, formerly of the Nashville, Chattanooga
& St. Louis Railroad, and prominently associated with the
exhibit of that railway at the Third National Exposition has been
appointed Lieutenant Colonel, U. S. A., and is stationed at the
General Engineer Depot, Washington, D. C.
Dr. Ira E. Lee has resigned from the University of Rochester,
Rochester, N. Y., where he acted as instructor of chemistry, to
accept employment as research chemist with E. I. du Pont
de Nemours & Co., Wilmington, Del.
Mr. John M. Sanderson, for the past several years chief
chemist of the Ohio Varnish Company, lias recently entered the
employ of the Larkin Co., Buffalo, N. Y., as superintendent
of their paint and varnish department.
Miss Jessie Y. Cann, formerly head of the chemistry depart-
ment at Rockford College, Rockford, 111., has just accepted an
assistant professorship in analytical chemistry at Smith College,
Northampton, Mass.
Mr. Albert J. Kraemer, formerly employed by the Union Oil
Co., California, as chief chemist of the Avila Refinery, is now
engaged in the Chemical Warfare Service, Research Division,
in the small scale production of gas chemicals.
Professor George Borrowman has resigned his professorship
at the University of Nebraska to take up research work for the
Niagara Alkali Company, under the direction of Dr. John E.
Teeple, in the Chemists' Building, 50 East 41st Street, New York
City.
Mr. H. E. Shiver, assistant chemist, South Carolina Experi-
ment Station, Clemson College, S. C, has accepted a position
as chemical engineer with the Air Nitrates Corporation at their
electrochemical plant at Muscle Shoals, Ala. He will be in a
supervisory position in Unit 5 of the plant.
Mr. Cyril B. Clark, employed for the past few years in the
Research Department of the General Chemical Company, 25
Broad St., New York City, has been detailed to some special
work at the Bay Point Works near San Francisco. To com-
plete this special work will take about four months, after which
Mr. Clark will return to New York.
Dr. R. P. Calvert has been transferred from the position of
Head of the General Chemical Division of the Experimental
Station, Wilmington, Del., to that of Director of Delta Labora-
tory, Arlington, New Jersey. Both laboratories are under the
direction of the chemical department of E. I. du Pont de Nemours
& Company.
Mr. Joseph Prescott, formerly assistant superintendent in
the tinning department of the De Laval Separator Company
at Poughkeepsie, N. Y., is now assistant metallurgical chemist
in the Ordnance Department. His work consists in super-
vising the heat treatment of steel, physical properties, etc.
Mr. O. L. Thomas has been transferred from the Experimental
Station of E. I. du Pont de Nemours and Co., Wilmington, Del.,
where he acted as research chemist, to the U. S. Government
Powder Plant at Jacksonville, Tenn., where he will be chief
supervisor of caustic soda manufacture and soda ash recovery.
Dr. J. H. Ransom, after eighteen years in Purdue University,
has been elected professor of chemistry and director of the
chemical laboratories in Vanderbilt University, Nashville,
Tenn.
Mr. John A. Coye has resigned his position as chief chemist
with the Engineering Experiment Station of thy Iowa State
College, Ames, Iowa, to accept the position of assistant chemist
with the General Chemical Company at their Laurel Hill
Works.
Mr. J. Raymond Hess, until recently head chemist for the
Ismert-Hinckc Milling Co., Topeka, Kansas, is now with the
Omaha Flour Mills Co., Omaha, Nebraska, acting as chief
chemist.
Mr. J. Thaddeus Batson has been transferred to the Gas
Defense and is now stationed at the Edgewood Arsenal, Edge-
wood, Maryland.
Dr. Raymond I'reas has resigned as adjunct professor of
chemistry in the University of Virginia to accept a commission
as First Lieutenant in the Sanitary Corps.
7 5°
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 9
Mr. D. L. Williams, formerly of the chemistry department
of the College of the City of New York, is now in the Research
Division of the Chemical Warfare Service at American Uni-
versity, Washington, D. C.
Mr. James B. Pratt, formerly chemist of the Southern Cotton
Oil Co., Charlotte, N. C, has been commissioned captain in the
Chemical Warfare Service and is stationed at Niagara Falls.
Sir Alexander Pedler, F. R. S., known for his research work in
chemistry, for many years professor of chemistry in the Presi-
dency College, at Calcutta, later vice-chancellor of the Calcutta
University and minister of public instruction in Bengal, died on
May 13, at the age of sixty-eight years.
Mr. M. W. Hcnsel, an expert in the sugar-beet industry, is
now in the mountain zone of Avery, Ashe, Buncombe, Burke,
McDowell, Mitchell, Watauga, and Yancey counties, North
Carolina, having been specially detailed to look after the yield
of the excellent syrup obtained from the sugar beet.
Mr. Jean Piccard has been promoted to associate professor
of chemistry at the University of Chicago.
Mr. L. J. Plctcher, who was formerly assistant professor of
chemistry at Southern Methodist University, Dallas, Texas, has
withdrawn from teaching and is now associated with the Texas
Refinery, Port Arthur, Texas, as research chemist.
Dr. E. C. Shorey, in charge of the Division of Chemical In-
vestigation in the Bureau of Soils, U. S. Department of Agri-
culture, has resigned to accept a position with the National
Aniline and Chemical Co., Inc., at Marcus Hook, Pa.
Mr. Harry C. Brill, who has acted as chief of Division of
Organic Chemistry, Bureau of Science, Manila, P. I., for the past
five years, resigned last February to accept the position of
acting professor of chemistry at Miami University, Oxford, O.
In June of this year Mr. Brill was appointed professor of chem-
istry and head of the department of chemistry at Miami Uni-
versity.
Mr. Harvey H. Wilson has been transferred from the Jersey
City plant of Marden, Orth and Hastings Corporation, where
he was acting as chief chemist, to the Jones Point plant of the
American Potash Corporation to act as the former's special
representative, and also to do consulting work on potash for the
American Potash Corporation.
Mr. Charles S. Rewe, chemist of the United States Office of
Public Roads and Rural Engineering for several years past, has
resigned his position to enter the Research Department of the
Barrett Company, 17 Battery Place, New York City.
Mr. Vilhelm Gruner has severed his connections with E.I.
du Pont de Nemours and Company, Wilmington, Del., to take
up work at the plant of the Monmouth Chemical Co., Keyport,
N. J.
Mr. Samuel Wierman, formerly chief chemist and process
manager of the citrus by-products factory of the California
Fruit Exchange, at Corona, California, is now with the Societe
Financiere des Caoutchoucs of Antwerp, Belgium, and London.
England, as chemist in charge of their Chemical and Agricultural
Department, Federated Malay States.
Mr Sterling Temple, associate professor of industrial chem-
istry at tin- University of Minnesota until January 1918, and
since then Captain, Ordnance R. C, has been stationed at
Edgewood Arsenal since April 4 of this year.
Mr. Ralph A. Holbrook, chemical engineer, has recently
located his headquarters at Rutland, Mass.
Mr. G. A. Armstrong, formerly employed by E. J. Loomis
vS: Co., Philadelphia, Pa., as chemical engineer 111 charge of their
tungstic acid and tungsten metal department, has severed his
connection with this company to accept a position as chemical
engineer in charge of intermediates with the Central Dyestuff
and Chemical Co., Newark, N. J.
Dr. Harrison Hale, fur a number of years professor of chemi-
isiiv at I >i in v College, has resigned his position their to become
head ol the department ol chemistry at the I uiversity of
Arkansas. Associated with him will be Mr. < >. B. R
uieilv assistant professor in the loua State Teachers College,
and Mi. II M. Trimble, of the University of Michigan.
Mi Stiles Kennedy, who has been connected with the Northern
Sugai Corporation in the 1 apacitj of chiel chemist, is now acting
oi Henn M Winslow, Harriman, Tenn.
I >i Allien \Y ituens, who has been working for the degree
ol I'h .D. at the University of Illinois, is now connected with the
Division of Chemical Metallurgy of the Bureau of Standards.
Washington, D. C.
Mr. Joseph B. Nichols, previous to his enlistment in the
Ordnance Department, was engaged in graduate research work
in organic chemistry at the University of California, Berkeley,
Cal. Since his enlistment Mr. Nichols has been stationed at
Edgewood Arsenal, Edgewood, Md., and assigned to organic
research work.
Mr E. P. Fager, formerly employed as chemist by the Ameri-
can W iter Works and Electric Company at Birmingham, is now
serving as a chemist in the Ordnance Department at the Edge-
wood Arsenal, Edgewood, Md.
Dr. K.'Iv Nelson has resigned his instructorship in chemistry
at Purdue University to accept an appointment as assistant gas
chemist in the Research Division, Chemical Warfare Service,
American University Experiment Station, Washington, D. C.
Mr. F. A. McDermott, who has been doing industrial re-
search work at the Mellon Institute, University of Pittsburgh,
Pittsburgh, Pa., and has been research chemist with the Corby
Co., Washington, D. C, has taken a position with E. I. du Pont
de Nemours & Company at their Experimental Station, Henry
Clay, Del.
Prof. Miles S. Sherrill, of the department of chemistry, Mass.
Institute of Technology, has been granted a leave of absence
from the Institute and has commenced work on explosives for
the Ordnance Department.
Mr. G. A. Menge, formerly connected with the Dairy Division,
Bureau of Animal Industry, U. S. Department of Agriculture,
as a chemist in charge of condensed milk laboratory, has been
transferred to New York, assigned to control of quality, both of
raw material and of finished product, in the production of
evaporated milk and of sweetened condensed milk.
Mr. Chas. N. Jordan, formerly instructor in chemistry,
Marvin College, Fredericktown, Mo., is now engaged in chemical
and metallurgical work for the Ordnance Department.
Mr. John O'Connor, Jr., one of the assistant directors of the
Mellon Institute of Industrial Research of the University of
Pittsburgh, has gone to Washington to assume the duties of a
civilian appointment in the Plan and Scope Division of the
Quartermaster General's office. Mr. O'Connor has been a
prominent figure in scientific and especially in chemical circles
both in Pittsburgh and elsewhere. He has been one of the
leaders of the movement to eliminate smoke. In 191 2 he be-
came economist on smoke investigation in the University's
department of industrial research, which later became the
Mellon Institute. The following year he was appointed senior
fellow on smoke investigation and in 1914 was made one of the
assistant directors of the Institute. Mr. O'Connor has been
secretary of the Dust and Smoke Abatement League since its
organization in 191 2. He is a member of the Civic Club of
Allegheny County and of its Smoke Abatement Commi.tee.
He was editor of The Crucible, the monthly bulletin of the Pitts-
burgh Sec ion of the A. C. S , and was secretary of ihe Society's
publicity commit:ee.
Dr. Thomas L. Watson, professor of geology in the Uni-
versity of Virginia and state geologist of Virginia, has been
engaged for some months in cooperative state and federal work
on war minerals and materials in Virginia. He is a member
of the subcommittee of the National Research Council on ma-
terials for rapid highway and railroad construction behind the
front, and an associate member of the War Minerals Committee.
Prof. Gerald L. Wendt has been promoted to assistant pro-
fessor of chemistry .it the University of Chicago.
Mr. A. Douglas Macallum, research chemist, Toronto, has
been granted exemption from military service on the ground
of being engaged in the manufacture of diarsenol.
Professor E. P. Schoch has been promoted to the head of the
school of chemistry and chemical engineering of the University
of Texas.
Mr. C. A. Nash has resigned as associate in chemistry at the
University of Chicago and has accepted the position of research
chemist for the Cutler- Hammer Manufacturing Company, of
Milwaukee.
Mr. Donald E. Cable, a recent graduate of the department of
chemical engineering, Armour Institute of Technology, is now
employed as assistant chemist in the department of derived
products. Forest Products Laboratory. Madison. Wisconsin.
Mr. L. Duane Simpkins, who for some time held the position
Uurgist and chemist for the American Smelting and
Refining Company's Lead Plant, located at Murray. I'tah.
and who for a few mouths was a chemist in the Civil Service,
is now chief metallurgical chemist and .metallographer for the
Peteis Cartridge Co., Kings Mills, Ohio.
Sept., 1018
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
757
INDUSTRIAL NOILS
List of Applications Made to the Federal Trade Cc
Year Pat. No.
1905 782,739
1902
1905
711,377
795,755
1906 837,017
1910 976,760
1903 718,340
1913 1,078,125
Patentee
Emil Fischer, Berlin, Ger-
Carl Auer von Welsbach,
Vienna, Austria-Hungary
Otto J. Graul, Ludwigshafe
on-the-Rhine, Germany
mmission for licenses under
the Enemy Act"
Assignee
E. Merck, Darmstadt, Ger-
Badiscbe Anilin & Soda
Fabri k, Ludwigshafen,
Germany
Badische Anilin & Soda Fab-
rik, Ludwigshafen-on-the
Rhine, Germany '
Treibacher Chemische Werke
Gesellschaft, M. B. H.
Enemy Controlled Patents Pursuant to the "Trading '
Patent
C.C- Dialkylbarbituric
and process of
Applicants
acid Victor Halper, 562 West 148th
iking St., New York City
Solid alkaline hydrosulfites Merrimac Chemical Company,
and process of making same 148 State St., Boston, Mass.
Process of making stable dry Merrimac Chemical Company,
148 State St., Boston, Mass.
hydrosulfites
Pyrophoric alloy
Pyrophoric mass
Badische Anilin & Soda
Fabrik. Ludwigshafen-on-
the-Rhine, Germany
American Pyrophor Company,
317 East 34th St., New York
City
American Pvrophor Company,
317 East 34th St.. New York
City
E. I. du Pont de Nemours &
Co., Wilmington, Del.
Cellular drying apparatus
The General Pharmacal Co. has been incorporated under the
laws of Delaware with a capital of $100,000. Incorporators are
H. B. Thompson, Coatesville, Pa.; J. Pratt, Philadelphia, Pa.;
and James A. Dugan, Wilmington, Del.
Clay deposits, said to be as fine as any in the country, have
been found by Dr. Heinrich Ries of Cornell University in
Tallahatchie County, Mississippi. The clay is useful for a
multitude of war purposes, and it is expected that the extensive
fields will be developed as soon as the report of the expert is
made public from Washington. Clay of the sort located by Dr.
Ries was formerly imported from Germany in large quantities,
and there has been a shortage in the material since the war
began.
On July 2, 50 persons were reported killed and 60 injured in
a series of terrific explosions at the huge plant of the Semet-
Solvay Company, located at Split Rock, a suburb of Syracuse,
N. Y. Three T. N. T. plants, one nitric acid plant, the large
laboratory, and a boiler house were destroyed by the explosion
and the fire following, resulting in a loss estimated at $750,000
to $1,000,000.
The firm of Geisenheimer & Company has been dissolved; Mr.
Geisenheimer has retired from business. The property and
assets of this firm have been acquired by the Aniline Dyes and
Chemicals, Incorporated. The officers of the new corporation
are: President and Treasurer, Alfred F. Lichtenstein ; First Vice
President, W. H. Van Winckel, formerly sales manager of the
Dow Chemical Co., Midland, Mich.; Second Vice President,
Robert Hilton, Vice President of the Ault & Wiborg Co., Cin-
cinnati, Ohio; and Secretary, Henry A. Dalter. The corporation
will have its principal office at Cedar and Washington Streets,
New York City, with branch offices in Boston, Philadelphia, and
Columbus, Ga.
Within two months the Standard Sulfur Corporation of
Detroit, Mich., expects to begin the production of sulfur at its
plant near Orla, Texas. The daily output will be from 100 to
150 tons of refined sulfur. The officers of the company are:
President, Alfred F. Pudrith, of Detroit; Vice President, Alfred
Tinally, of Pecos; Engineer, Paola Fisher, of Chicago.
Fire which started from a motor in the duplex heater house
of the Aetna Chemical Company at Mount Union, Pa., on July
2, destroyed four buildings comprising the recovery and purifica-
tion- departments and the main portion of the plant. About
450,000 pounds of guncotton and much valuable machinery was
consumed. The loss is estimated at $900,000. There was no
loss of life, but several employees were severely burned. The
company announced that it would require four or five months to
rebuild and that the fire would delay its plans for moving its
plant at Oakdale, near Pittsburgh, to Mount Union. An ex-
plosion at the Oakdale plant recently resulted in the loss of
more than 100 lives.
$5,000,000 will be required for the by-product coke plant
which the Sloss-Sheffield Steel and Iron Company will build
near Birmingham, Ala. 120 Semet-Solvay ovens will be in-
stalled for the manufacture of toluol, benzol, sulfate of ammonia,
and other chemicals for the Government.
Am explosion of T. N. T. in the plant of the Hercules Powder
Co., Kenvil, near Dover, X. J., on July 5, result
of three men and property damage estimated at $25,000.
Steams-Roger Manufacturing
Company, 1718-1720 Cali-
fornia Street, Denver. Col.
On June 29, the Badische Anilin and Soda Fabrik Works, of
Mannheim, Germany, were ignited by bombs from Allied air-
planes. The plant burned for many hours.
A substitute for absorbent cotton made from ground wood
is likely to prove of inestimable advantage to the Government in
the present emergency of absorbent cotton shortage. The
Kimberley and Clark Paper Mill, Neenah, Wis., is making the
product at the rate of 3 or 4 tons per day.
The War Trade Board has introduced restrictions upon the
importation of chrome ore and chromite from overseas. The
home supply is believed capable to meet the demand when its
numerous sources are developed. Imports from Cuba, Guate-
mala, Newfoundland, and Brazil will be permitted to provide
for the interim demands.
A new woodpulp substitute for absorbent cotton, a cellulose
wadding known as Cellulosavadd, is being manufactured in
Sweden. The cost of the batting in large quantities is somewhat
less than $0.18 per lb., f. o. b., Swedish ports.
On July 29, A. Mitchell Palmer, Alien Property Custodian,
took over the Heyden Chemical Works with its large plant at
Garfield, N. J., on evidence showing that the concern, the second
largest of its kind in this country, was of German ownership.
The real owner of the company was Fabrik von Heyden, of
RadebeuL Germany, one of the largest chemical concerns in the
world. The Heyden Chemical Works has the exclusive use in
this country of many valuable patents, processes, and formulas
for the making of many by-products of carbolic acid. These
will now become Americanized. Mr. Palmer has appointed
the following directors and officers pf the company: President,
Leroy Baldwin, President of Empire Trust Co., 120 Broadway,
New York City; Vice President, James A. Branegan, Chemist,
1421 Chestnut Street, Philadelphia; Secretary, F. N. B. Close,
Bankers Trust Co., 16 Wall Street, New York City; Counsel,
J. Harry Covington, former Chief Justice of the Supreme Court,
District of Columbia, and Royal H. Weller, Ex-Assistant District
Attorney, 31 Nassau Street, New York City.
At the present time, as the result of cooperation between the
manufacturers and scientists, large quantities of optical glass
of the kinds needed for military fire-control instruments are
being produced of a quality equal in practically every respect
to the best European glass.
The first unit of a plant for making toluol by a new process is
now being installed at the works of Hiram Walker & Sons,
Limited, distillers, Walkerville, Ont., and if the success of the
process is demonstrated other units will probably be added.
France is experimenting with benefing, an oleaginous plant
well known in French West Africa, which, it is expected, will
produce an excellent substitute for linseed oil. The seed of this
plant produces 37.32 per cent oil when treated with carbon
disulfide, 'flu: resultant oil has an ambej yellow color, is of
average fluidity, and its smell resembles that of linseed oil. The
oil cake made from the seed husks after extraction of oil is
sufficiently rich in nitrogenous compounds to be useful for agri-
cultural purposi
The British Board of Trade is taking steps approved by the
Government to protect the British dye industry against German
competition after the war. The principal measure proposed
is that the importation of all foreign dyestuffs shall be controlled
758
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. Xo. 9
by a system of licenses for a period of not less than ten years
after the war.
The plant for the fixation of atmospheric nitrogen, to be used
in the manufacture of explosives for the Navy, provided for in
a Senate amendment to the naval appropriation bill, is to be
located at Indian Head, Md., where the Navy has its great
powder plant. Unlike the plants for the fixation of atmospheric
nitrogen, which are to make nitrates to be used in explosives
for the Army and for the manufacture of fertilizers, which have
been located on water-power sites in Alabama and Tennessee,
the Navy plant will not be a water-power plant. The Haber
method for the fixation of atmospheric nitrogen, which has heen
used successfully in Germany for some time, will be adopted at
the Indian Head plant. Coal is used instead of water power.
The proponents of the plan claim that nitrogen can be extracted
from the air by this method at a much less cost and outlay of
money than in the case of water-power plants. The pro-
posed plant for the fixation of atmospheric nitrogen for the
Navy is expected to turn out sufficient nitrate of soda to fill all
the requirements of the huge powder plant at Indian Head,
which has been greatly increased in size since the war began.
In the Senate amendment to the naval appropriation, the sum of
$9,150,000 is provided for the establishment of the Indian Head
plant and for its operation during the coming fiscal year.
The Hardaway Construction Company which is building the
supplementary power dam at the American Aluminum Com-
pany's plant at Badin, N. C, suffered a loss of two months'
time by a fire, due to lightning and poor fire protection, which
burned its concrete-mixing plant, which had a daily capacity of
1500 cu. yds. The loss was total, with no insurance. This
dam will cost about $1,500,000 and will develop 32,500 h. p.
It is not built for pondage, but to use the water from the gigantic
dam 180 feet high, 2 miles above, taking this water under a
head of 50 feet.
The Consumers Dyewood Products Co., Mobile, Ala., has
been capitalized at $300,000, and will locate at Choctaw Point
for the manufacture of dyes.
The Steel Cities Chemical Company is planning to rebuild
its sulfuric acid plant at Ensley, Ala., which was recently burned
at a loss of $300,000.
The department for the manufacture of dyestuffs at the
United Piece Dye Works has been transferred to E. I. du
Pont de Nemours & Co., Wilmington, Del. The United Piece
Dye Works, represented by the Messrs. Albert and Henry Blum,
were among the first to undertake the manufacture of certain
difficult fines of dyestuffs, and deserve much credit for the work
they accomplished.
The French Minister of Commerce has decided to concentrate
all importations into the hands of consortiums. The General
Syndicate of Chemical Products will be the authority to form
these bodies with reference to the chemical industry, and will
supervise the appointment of three consortiums: (1) for heavy
chemicals and fertilizers, (2) for diverse chemical products,
and (3) for tannins and dyestuffs.
Women chemists are needed by the Government and also to
stabilize the industries by replacing men chemists who have
been called into service, according to Major F. E. Breithut, of
the Chemical Warfare Service, U. S. A. This call is so urgent
that he has asked the Women's Committee of the Council of
National Defense to cooperate with the Army Medical Depart-
ment in making a census of all the available women chemists
in the country.
A report on the tannin-bearing plants and trees of Latin
America issued by the Bureau of Foreign and Domestic Com-
merce is ready for distribution. It is the work of Dr. Thomas H.
Norton. The purpose of the study is to enumerate and describe
as completely as possible the known occurrence of sources of
tannin in the countries in question and to show the extent to
which they are already utilized, or are susceptible of easy exploi-
tation. The sources of tanning of industrial importance to be
found in Latin American countries are summarized by Dr. Norton
as follows: Woods, 12; barks, 102; leaves, 9; roots, 3; fruits
and seeds, 17.
GOVERNMENT PUBLICATIONS
By R. S. McBrtdb, Bureaii of Standards, Washington
NOTICE — Publications for which price is indicated can be
purchased from the Superintendent of Documents, Government
Printing Office, Washington, D. C. Other publications can
usually be supplied from the Bureau or Department from which
they originate. Commerce Reports are received by all large
libraries and may be consulted there, or single numbers can be
secured by application to the Bureau of Foreign and Domestic
Commerce, Department of Commerce, Washington. The regu-
lar subscription rate for these Commerce Reports mailed daily is
$2.50 per year, payable in advance, to the Superintendent o€
Documents.
PUBLIC HEALTH SERVICE
Some Qualitative and Quantitative Tests for Arsphenamine
(3,3'-Diamino-4,4'-Dioxy-Arsenobenzene Dihydrochloride) and
Neo-Arsphenamine (Sodium-3,3' - Diamino - 4,4' - Dihydroxy-
Arsenobenzene-Methanan-Sulfoxalate). C. N. Myers and
A. G. DuMez. Public Health Reports 33, 1003- 1016. Issued
June 21.
Previous to the year 1914, all of the arsphenamine (salvarsan)
and neo-arsphenamine (neosalvarsan) on the market was manu-
factured by a single German firm under the supervision of Paul
Ehrlich, one of the patentees. Naturally the products were
fairly uniform in their composition and properties.
Examinations made by the authors, as well_as evidence pre-
sented by clinicians (Martin and others, 1916), have revealed
the fact that the products of different manufacturers appearing
on the market in this country are not all uniform with respect
to either their chemical or their physiological properties. Even
the last of the German supplies received are stated to be more
toxic than the products obtained before the beginning of
hostilities in Europe (Ormsby and Mitchell, 1916).
Tentative standards for these preparations (arsphenamine
and neo-arsphenamine) have been adopted by the Federal
Trade Commission on the recommendation of the United States
Public Health Service, but these do not appear to meet all
exigencies. It is for this reason and for the purpose of better
defining the properties of good preparations that the following
qualitative and quantitative tests have been worked out and
compiled.
Dried Milk Powder. Anonymous. Public Health Reports
33i 1052-5- Issued June 28. This is a review of "Food Report
No. 24" issued by the Local Government Board of Great Britain.
It discusses the important conclusions on preparation, com-
position, and nutritive values of dried milk powder with special
reference to their use in infant feeding.
The Growth-Promoting Properties of Foods Derived from
Corn and Wheat. C. Voegtlin and C. N. Myers. Public
HealthjReports 33, 843-868. Issued May 31.
The purpose of the present investigation was to answer the
question as to whether the corn and wheat products used in
human nutrition exhibit similar dietary deficiencies as those
of the whole grains. The bulk of the corn and wheat foods of
the American dietary are derived from the wheat and com kernel
by means of a process of milling (roller mills) which is known
to eliminate most of the germ and superficial layers of the grain.
It, therefore, seemed to us a question of practical importance
to determine whether the milling process improves, or causes
a decrease in, the dietary value of the milled product. More-
over, it was desirable to decide whether or not the food addi-
tions made to flour (yeast, salt, milk) in the preparation of bread
improve the nutritive value of this food.
Establishments Licensed for the Propagation and Sale of
Viruses, Serums, Toxins, and Analogous Products. Anony-
mous. Public Health Reports 33, 869-872. Issued May 31-
Sept., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
7 59
Color Blindness. G. L. Collins. Public Health Bulletin
92. This discusses means for detecting various degrees of color
blindness and summarizes a considerable number of observa-
tions on various phases of this general question.
Phosphorus as an Indicator of the "Vitamine" Content of
Corn and Wheat Products. C. Voegtlin and C. N. Myers.
Public Health Reports 33, 911-917. Issued June 7. The
phosphoric anhydride determination of wheat and corn products
yields fairly satisfactory information as to the content of these
products in accessory foods. A low phosphoric anhydride con-
tent indicates that the product is poor in vitamines.
GEOLOGICAL SURVEY
Copper in 1916. General Report. B. S. Butler. Separate
from Mineral Resources of the United States, 1916, Part I.
55 pp. Published April 22.
The copper-producing plants of the country were operating
at capacity at the beginning of 1916, and under the spur of
active demand and unusually high prices a general enlargement
took place. There was comparatively little interruption from
labor troubles or other causes, and the combined result was
by far the largest output in the history of the domestic copper
industry.
The average cost per pound of copper showed a decrease in
191 5 from 1914, owing both to the plants being worked more
nearly at capacity and to the relatively slight increase in cost
of labor and material. In 1916 the cost of both labor and ma-
terial had advanced and this advance was reflected in the in-
creased cost of copper. In 191 5 the average cost of copper
per pound, as given in the annual reports of the companies
giving this item, was about 8 cents; in 191 6 the average was
1 1.3 cents. The figures for both years are below the actual
average cost of all copper produced, but the increase in 1916
doubtless represents approximately the increase in average cost.
The average price receiyed for copper in 1916 as reported by
the selling agencies was 24.58 cents per lb., as compared with
about 17.5 cents in 1915 — an increase in 1916 of about 7 cents
per lb. The profit per pound of copper was probably at. least
3.5 cents greater than in 1915, and this was reflected in the large
earnings of the principal copper companies.
The effect of the remodeling of plants to improve metallurgic
practices, which has been in progress for the last few years,
was shown in the recoveries in 1916. For several years prior
to 1915 the quantity of copper recovered per ton of ore showed
a steady decrease. This was caused by the treating of constantly
increasing quantities of low-grade concentrating ore. In 191 5
and 1 9 16, in spite of large increase in the concentrating ore
treated, there was an increase in the average quantity of copper
recovered per ton of ore, and this in spite of the fact that some
plants were operated beyond their capacity for greatest metal-
lurgic efficiency.
Summary of Statistics of thb Copper Industry in the United States
1915 1916
Production of copper
Smelter output, lbs 1,388,009,527 1,927,850,548
Mine production, lbs 1,488,071,528 2,005,875,312
ReBnery production of new copper
Electrolytic, lbs 1,114,345,342 1,579,620,513
Lake. lbs 236,757,062 269,794,531
Casting and pig. lbs 36,603,119 39,337,155
Total domestic, lbs 1,387,705,523 1,888,752,199
Total domestic and foreign. lb=.... 1.634.204.448 2,259,387.315
Total new and old copper, lbs 2,026,000,000 2,922,000,000
Total ore produced, short tons 43,415,133 57,953,357
Copper ore produced, short tons 43,404,182 57,863,365
Average yield of copper, per cent 1 .66 1 , 70
Average price per pound, cents 17.5 24 . 6
Imports, lbs 315,698,449 462,335,980
Eiports. lbs 681,917,955 784,006,486
Consumption
Total new copper, lbs 1,043,497,328 1,429,755,266
Total new and old copper, lbs 1,435,000,000 2,024,000,000
World's production, lbs 2,346,300,299 3,106,995,660
Value of production in the United'Statcs. $242,902,000 $474,288,000
Exports of metallic copper were larger than in 1915, but were
still below those of 1914 and 1913. Domestic consumption,
however, showed a large increase and, as in 1915, much of this
was exported in manufactured form. As the capacity of British
and French munitions plants increased, more raw materials
and less manufactured products were exported.
At the end of 1916 the capacity for producing copper in the
United States was larger than it has ever been and was increasing.
No systematic attempt has been made to ascertain the pro-
portion of the copper output of 191 6 used in different industries,
such as electric transmission, brass manufacture, and casting,
but some idea of the quantities entering the different indus-
tries can be gained from the forms in which the output of the
refineries was cast. The following table shows the approximate
quantity of copper cast in the different forms during 1916 as
reported by the refining companies. It will be noted that the
total is not the same as the refinery output for 1916.
Copper Cast in Different Forms in 1916
Form Quantity, Lbs. Percentage
Wire bars 853,028,629 37
Ingots and ingot bars 873,281,265 38
Cakes 298,399,153 13
Cathodes 192,109,762 8
Other forms 92,676,974 4
It may be assumed that a large portion of the 37 per cent cast
as wire bars was used in the electric industry and that much
of the 13 per cent cast as cakes was used for rolling. The other
forms are less easily classified. The 8 per cent cast as cathodes,
together with a considerable portion of the ingots, and prob-
ably some of the cakes, entered the brass industry, and a large
quantity of copper ingots was used in casting. The refinery
output for 19 15 was cast as follows: Wire bars, 37 per cent;
ingots, 45 per cent; cakes, 9 per cent; cathodes, 6 per cent;
other forms, 3 per cent. The most notable change was the
relative decrease in ingots and increase in cakes.
Clay-Working Industries and Building Operations in the
Larger Cities in 1916. J. MtodlETon. Separate from Mineral
Resources of the United States, 1916, Part II. 72 PP- Issued
April 13.
This report deals with the products of the clay-working in-
dustries as well as with clay mining, and the tables are made up
to show the output of manufactured clay products as best ex-
pressing the production of clay.
The year 1916 m the clay-working industries was one of general
progress. In spite of strikes, scarcity of labor, increased cost of
materials, and congestion in transportation, the output of 1916
was much larger than in any preceding year. In some sections
of the country the business in brick and tile lagged during the
earlier part of the year, but later was unusually active, reflecting
the general prosperity of the country. The total value of all clay
products marketed was $207,260,091, an increase of $44,139,859.
or 27 per cent. This is the greatest value recorded in these
industries and is nearly $26,000,000 more than the highest
previous record.
The refractories branch of the industries, the products of
which are so essential, both to modern civilization and to military
operations, showed the largest increase, and was followed next
in order by the great structural material, common brick. Only
fancy brick and enameled brick, both minor items in the total
output, decreased in value, and the decrease in these was very
small.
The value of all domestic pottery marketed in 1916 was
$48,217,242, an increase of $10,891,854. or nearly 30 per cent,
over 1915, and of $10,224,867, or 27 per cent, over 1913, the pre-
vious year of highest value. The pottery imports decreased
$1,027,501, or 16 per cent, and the ratio of production to con-
sumption, 92 per cent, was the highest recorded.
The total value of imports of all clay products decreased
$1 034,222, or 15 per cent, in 1916; in 1915. there was a decrease
760
Till- JOlk.XM. OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 9
of $1,806,350, or nearly 21 per cent. The total value of imports
for 1 9 16 was the lowest in 30 years, except in 1890, and was less
than that of 1907, the year of maximum value, by $8,045,267,
or 58 per cent. Of the imports for 1916, about 97 per cent was
pottery and about 3 per cent was brick and tile.
The value of exports of domestic clay products in 19 16 in-
creased $2,150,290, or 79 per cent, over 1915. In 1915 there
was a decrease of $872,765, or 24 per cent, from 1914. Of
the exports in 1916, 62 per cent was brick and tile, 22 per cent
pottery, and 16 per cent unclassified.
The clay sold as such in 1916 amounted to 2,932,590 short tons,
an increase of 569,636 tons, or 24 per cent. This clay was valued
at $5,751,774, or $1.96 per ton, an increase of $1,779,833, or
45 per cent, and of 28 cents in the average price. Every variety
of clay except brick clay increased in quantity and value, and
paper clay, ball clay, and fire clay reached their maximum
quantity and value in 19 16. Fire clay made the largest gain
in production, 487,333 tons, or 31 per cent; paper clay increased
40,401 tons; kaolin, 19,692 tons; ball clay, 14,413 tons. Slip
clay, which has been declining in production since 1912, made
a large increase in output, 6,418 tons, or 84 per cent, in 1916,
compared with 19 15. Fire clay showed the largest increase in
value, $1,346,527, or 57 per cent; paper clay increased $229,289,
or 42 per cent; slip clay, $29,165, or 155 per cent; kaolin, $65,299,
or 27 per cent; and ball clay, $89,242, or 30 per cent. Brick
clay decreased 4,804 tons and $17,009. Fire clay is the chief
kind, judged by production, and constituted 70 per cent of the
quantity and 64 per cent of the value of the clay marketed in
1916. Paper clay ranked second in value of output, and ball
clay third. The average price per ton varied but little in 1916,
compared with 19 15.
The Salt Creek Oil Field, Wyoming. C. H. Wegmann.
Bulletin 670 45 pp Paper, 15 cents. "The Salt Creek
oil 'field, which produces daily 10,000 barre s of high-grade
paraffin oil, is at present the largest proved field in the State of
Wyoming. A number of fields more recently developed — such
as Grass Creek, Big Muddy, and Elk Basin — are attract ng
much attention, but so far none of these promises to include an
area so large or wells so productive."
Bauxite and Aluminum in 1917. J. M. Hill. Separate
from Mineral Resources of the United States, 1917, Part I.
9 pp. Published June 21.
The quantity of bauxite marketed in the United States in
1917 was 568,690 long tons, which had a value at the mines of
$3,119,058, an increase over the production of 1916 of about
34 per cent in quantity and about 36 per cent in value. The
production from the Georgia, Alabama, and Tennessee field in
191 7 was 62,134 l°ng tons, an increase of about 26 per cent,
and the Arkansas production of 506,556 long tons showed an
increase of approximately 35 per cent.
Apparently the producers of aluminum consumed about
375,000 tons, the makers of chemicals about 82,000 tons, makers
of abrasives about 110,000 tons, and the makers of refractories
about 2,400 tons of bauxite in 1917.
The prices received for bauxite in 1917, as reported by pro-
ducers, ranged from $4.75 to $10.50 a long ton; the average price
paid for the whole of the domestic bauxite sold in the country
was $5.48 a long ton at the shipping point.
The value of primary aluminum produced in the United
States in 1917 was $45,882,000, an increase of 35 per cent over
the value of the output in 1916. This increase is due in part
to the increased price and in part to the greater output of
primary aluminum in 1917. No estimate can be made at this
time (March, 191 8) of the recoveries of secondary aluminum
during 1917, but the data at hand, though incomplete, indicate
that the recoveries will not be smaller than in 1916. Information
concerning this phase of the aluminum industry will be found
in the chapter of Mineral Resources on secondary metals in
19 1 7, which is now in preparation.
In the United States the quoted prices for primary or "virgin"
aluminum ranged from 62 cents per lb., \n January, to 37 cents
per lb., in October, a price which was maintained to the end
of the year. The average for the year was 51.59 cents per lb.,
as compared with 60.71 cents in 1916. These prices are for
small lots and immediate delivery, offered in the open market,
and do not represent the price received by the single producer
of primary aluminum in this country.
The principal aluminum salts made in the United States are
alumina, alums, usually ammonium and sodium alums, aluminum
sulfate, and aluminum chloride. Alumina is largely consumed
in the manufacture of aluminum and no figures of domestic
production are available for publication.
Alums of various qualities are produced at 9 plants in the
eastern United States, the total production of alum in 191 7
being 19,714 short tons, valued at $1,017,083, a decrease of
approximately 28 per cent in quantity and of 14 per cent in
value from the production in 1916. The average price reported
by makers of alums was $51.60 a short ton. The wholesale
market quotations ranged from 4 to $l/t cents per lb., or $80
to $102 a short ton. The quotations on lump alum were fairly
constant at 4 to 4V4 cents up to May, when an increase to 4V1
to 5 cents was made. This price remained steady till November,
when it dropped to 4 to 4V2 cents. Ground alum at the first
of the year was quoted at 4'/s to 43/s cents, but prices rose to
46/8 to 5 '/a cents about the middle of May and remained
stationary until the last of September, when they began to drop,
and reached 4V10 to 5 cents at the end of 19 17.
Aluminum sulfate is made at 24 plants, 7 of which are at
municipal or industrial waterworks, which consume their entire
output. The total quantity of aluminum sulfate produced in
the United States in 191 7 was 178,738 short tons, of which
4,947 short tons did not enter the market but was used for water
purification at the place of manufacture. The quantity of
domestic aluminum sulfate which entered the market, 173,791
short tons, was greater than the quantity in 1916 by approxi-
mately 18 per cent, and the total domestic product'on increased
about 16 per cent. The price reported by makers of aluminum
sulfate for the 1917 output averaged $32.15 a short ton. Market
quotations for low-grade aluminum sulfate ranged from a low
of 2 cents to a high of 4 cents per lb., or $40 to $80 a short ton.
Low-grade aluminum sulfate was quoted at 2 to 2'/j cents per
lb. until October, when quotations rose to 2 to 31/* cents, but
fell to 2 to 3 cents during the second week of November, and
closed at ia/< to 2 '/« cents per lb. at the end of the year.
Aluminum chloride is used for various purposes, among which
may be mentioned the refining of mineral oils. This salt was
produced at 3 plants in 1917, and the total output reported to
the Geological Survey was 4.702 short tons, valued at $311,900,
or approximately $66 a short ton. Market quotations on
aluminum chloride remained stationary throughout the year at
4 to 4V10 cents per lb. 01 $80 to $82 a short ton.
Bauxite abrasives sold under various trade names, such as
alundum, aloxite, exolon, and lionite, are made by fusing bauxite
in an electric furnace. These products are sold in the form of
powders, cloth, grinding stones, and wheels of various shapes
for a multitude of uses.
The total marketed production of artificial abrasives made
from domestic bauxite in 191 7 was 48,460 short tons, valued at
approximately $6,970,000, or about $144 a short ton. This is an
increase over the production in 1916 of 58 per cent in quantity
and of 200 per cent in value. The average value is deceptive,
however, in that the prices received for the product depend on
many factors, among which hardness, size of grain, degree of
finishing, and many others may be mentioned.
There are two classes of high-alumina refractories now on the
Sept., 1918
THE JOURNAL OF INDUSTRIAL- AND ENGINEERING CHEMISTRY
761
market. What are commonly called bauxite brick are made by
mixing various proportions of calcined bauxite or high-alumina
clay with a binding material such as fire clay, sodium silicate, or
lime. The other class of high-alumina refractories consists of
those made by the electric fusing of bauxite. These are manu-
factured by the companies that make artificial abrasives.
The use of high-alumina refractories seems to be expanding,
particularly in the construction of copper, iron, and lead furnaces
and of cement kilns. No figures are now (March, 1918) available
to show the production of high-alumina refractories, though it is
known that at least 2,313 long tons of bauxite were consumed in
making refractories.
Strontium in 1017. J. M. Hcu,. Separate from Mineral
Resources of the United States, 1917, Part II. 2 pp. Pub-
lished June 19. "Domestic strontium ores were used by makers
of strontium chemicals to a considerable extent during 191 7.
Prior to 19 16 most of the salts made in this country were prod-
ucts of imported celestite. In 1917, however, the domestic
deposits supplied over 70 per cent of the domestic require-
ments."
From the best information available to the United States
Geological Survey it would seem that approximately 4,035 short
tons of strontium ore, valued at about $87,700, of which about
10 per cent was strontianite (strontium carbonate) and the re-
mainder celestite (strontium sulfate), was mined in the United
States during 191 7. This ore was mined in California, Texas,
and Washington. By far the greatest production was made
from California deposits.
Approximately 1,700 tons of English celestite was imported
in 191 7 for use in this country.
Prices reported by sellers of celestite ranged from $20 to $22
a short ton, but for strontianite ores prices from $35 to $90 a
short ton were reported. The Foote Mineral Co. on July 14,
19 1 7, was selling ground celestite (90 per cent SrSO<) at 2 cents
per lb. ($40 a ton) and ground strontianite (83 per cent SrCO»)
at 7 cents per lb. ($140 a ton).
Four companies in the United States reported sales of strontium
carbonate and strontium nitrate in 191 7, aggregating about
3,000,000 pounds or 1,500 short tons. The principal salt sold
was the nitrate. A few thousand pounds of strontium bromide
was sold, and several thousand pounds of sulfide, which was
presumably used for making other salts.
The demand for strontium salts comes principally from
makers of fireworks and night signals. Quotations on strontium
carbonate have been steady throughout the year at 40 to 45
cents per lb. for technical carbonate and 55 to 60 cents per lb.
for pure carbonate. Strontium nitrate was quoted at 42 to 52
cents per lb. at the beginning of 1917 but declined to 25 to 30
cents per lb. in June and remained at that figure till the end
of the year.
Arsenic in 1917. J. P. UmplEby. Separate from Mineral
Resources of the United States, 191 7. Part I. 5 PP- Pub-
lished June 19.
The production of arsenic or arsenious oxide in the United
States in 19 17 amounted to 6,151 short tons, valued at $1,118,313,
an increase over 1916 of less than 3 per cent in quantity and of
more than 101 per cent in value. The value of the output is
somewhat uncertain, however, as in some returns it represents
the value f. o. b. destination in carlopd lots and in others the
value at the reduction plant. Throughout, however, the value
reported by the producers is much lower than that quoted in
the trade journals.
Nearly all the output in 1916 was recovered as a smelter
by-product. One plant only, at Brinton, Va., began late in the
year to mine and treat ore primarily for its content of arsenic.
The unusual demand for insecticides incident to increased
gardening led the Government to place the industry under
license late in the year. Early in 1918 the Food Administration,
after exhaustive investigation during the later part of 191 7.
fixed a maximum price of 9 cents per lb. to be charged by pro-
ducers for white arsenic in carload lots delivered in the United
States. Half a cent per lb. additional is permitted for ship-
ments in less than carload lots.
The refined arsenic produced is reported to be above 99.5
per cent As2Os.
The small increase in the domestic production of arsenic and
the great increase in its value in 191 7 are noteworthy features.
The imports of white arsenic and arsenic sulfide, or orpiment,
increased from 2,163 short tons in 1916 to 3,955 short tons in
1917, or nearly 83 per cent. This increase should be compared
with a decrease of 32 per cent in 19 16 and is due to the re-
sumption of production in Mexico as well as to increased imports
from Canada. The Canadian output is derived as a by-product
in the smelting of ores from Cobalt and adjacent silver deposits
in northern Ontario.
The present demand for arsenic consumes about 12,000 short
tons a year, whereas the available supply in 191 7 from both
domestic production and imports was only about 10,000 short
tons. The supply in 191 7, however, was much larger than in
previous years. The average yearly supply from all sources
for the period from 191 1 to 1916, inclusive, was a little less
than 8,150 tons During 1918 the domestic production may be
expected to increase and unless the output from Mexico and
Canada finds another market the imports will also increase.
On the other hand, the demand for arsenic will almost certainly
increase and probably at a more rapid rate than production.
It seems likely that a scarcity of arsenic will persist throughout
1918 and that the price will hold close to the maximum fixed
by the Food Administration.
The deficiency in arsenic is not confined to the United States.
In England and France prices even higher than those in the
United States clearly reflect a shortage in the supply of arsenic,
although both these countries are large producers of arsenic,
England from the Cornwall deposits and France principally
from the auriferous arsenopyrite deposits in the Department of
Maine-et-Loire.
Antimony in 1916. E. S. Bastin. Separate from Mineral
Resources of the United States, 1916, Part I. 7 PP- Pub-
lished June 14.
The production of antimony ores in the United States in
1916 according to the best information available was about
4.500 short tons, valued at $40,580. The metallic antimony
content of this material was about 1,770 short tons. The
average tenor of the ore in metallic antimony was therefore
about 40 per cent.
In contrast to the small domestic production of antimony
ore— about 4,500 short tons— the total imports in 1916 amounted
to 7,764 short tons of antimony ore and 9,875 short tons of
metallic antimony. In the customs classification for monthly
import returns antimony matte, which is liquated sulfide, and
antimony regulus, which is metallic antimony, are grouped
in one class, but the quarterly returns of imports for consumption
differentiate between these materials and record no imports
of the matte or liquated sulfide during 1916.
In 1914 normal prices were maintained until the outbreak of
the war, when the price rose from an average of 7.2 cents in July
to 17.2 in August.
The price at the beginning of 1916 was about 42 cents per lb.,
from which it rose to 46 cents in March and then declined
steadily to about 1 1 cents early in October. Later there was a
slight recovery to about 15 cents at the close of the year. The
decline was the result of overproduction in China, which flooded
the American market with the Chinese products. With these
762
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No.
the American antimony miners soon found themselves unable to
compete, and the latter part of the year witnessed a great decline
in antimony mining in this country.
BUREAU OF STANDARDS
Resonance and Ionization Potentials for Electrons in Cad-
mium Vapor. J. T. Tate and P. D. Foote. Scientific Paper
317. 8 pp.
Application of Dicyanin to the Photography of Stellar Spectra.
P. W. Merrill. Scientific Paper 318. 19 pp.
Thermal Expansion of Alpha and of Beta Brass Between
o° and 600 ° C. in Relation to the Mechanical Properties of
Heterogeneous Brasses of the Muntz Metal Type. P. D.
Merica and L. W. Schad. Scientific Paper 321. 20 pp.
Paper, 10 cents. The difference in the thermal expansion of
alpha and of beta brass of compositions which normally are in
equilibrium in such alloys as Muntz metal, naval brass, etc.,
has clearly been shown by the measurements made. Funda-
mental variations in behavior as regards thermal expansion at
temperatures up to 600° C. were noted, due to the occurrence
of a transformation in the beta constituent.
The effect of the local or, as they might be called, "grain"
stresses, on the physical properties and service behavior has
been only incompletely indicated. Tests showed that stresses
of this sort produced by quenching commercial drawn 60 : 40
brass i-in. diameter rod did not cause cracking in mercurous
nitrate. On the other hand, a lowering of the proportional
limit of the alloy amounting to about 2000 lbs. per sq. in. re-
sulted from this treatment.
It would appear to the authors that further investigation into
this general question of the expansion behavior of different con-
stituents of other alloys might reveal causes of mysterious failures
and weakness now considered quite obscure. Such materials
as hypereutectoid steels, cast iron, type metal, and bearing
metals contain two constituents. In many cases one of these
constituents is brittle, a fact which would accentuate the effect
of local contraction stresses. The authors hope to be able to
present some data later along these lines, indicating also more
definitely the physical effect of such stresses.
Effect of the Size of Grog in Fire-Clay Bodies. F. A. Ktrk-
patrick. Technologic Pap'er 104. 37 pp. The results throw
some light upon the question of the bonding power of plastic
clays. The strength of clay-grog bodies in the raw state is a
measure of bonding power. Since size of grog has great effect
upon strength, size of grain of the clay must exert considerable
influence upon this property. The size of grain of bond clays
cannot at present be measured accurately. Any means for
determination or indirect estimation of this property, such as
viscosity of the clay slip, would be of great help in working out
this problem.
Comparative Tests of Chemical Glassware. P. H. Walker
and F. W. Smitiier. Technologic Paper 107. 21 pp.
Legal Weights (in pounds) per Bushel of Various Commodities.
Circular io, 3rd Edition. 17 pp.
Standard Specifications for Incandescent Electric Lamps,
Tungsten (or Mazda) and Carbon. Circular 13, 8th Edition.
9 PP.
Radio Instruments and Measurements. Circular 74. 320
pp. Paper, 60 cents. This circular presents information re-
garding the more important instruments and measurements
actually used in radio work. It is hoped that the treatment will
bo of interest and value to Government officers, radio engineers,
and others, notwithstanding the subject is not completely
covered. Many of the matters dealt with are or have been
under investigation in the laboratories of this Bureau and are
not treated in previously existing publications. Xo attempt is
made in this circular to deal with the operation of apparatus in
sending and receiving. It is hoped to deal with such apparatus
in a future circular. The present circular will be revised from
time to time, in order to supplement the information given and
to keep pace with progress. The Bureau will greatly appreciate
suggestions from those who use the publication for improvements
or changes which would make it more useful in military or other
service.
The methods, formulas, and data used in radio work cannot
be properly understood or effectively used without a knowledge
of the principles on which they are based. The first part of this
circular, therefore, attempts to give a summary of these princi-
ples in a form that is as simple as is consistent with accuracy.
A large proportion of this publication is devoted to the treat-
ment of fundamental principles for the reasons, first, that how-
ever much the methods and technique of radio measurement
may change the same principles continue to apply, and second,
that this will make the present circular serve better as an intro"
duction to other circulars on radio subjects which may be issued.
A familiarity with elementary electrical theory and practice
is assumed.
Instruments and Methods Used in Radiometry. ILL The
Photoelectric Cell and Other Selective Radiometers. W. W.
Coblentz. Scientific Paper No. 319. 30 pp. Paper, 10
cents. Issued June 17, 191 8.
Photoelectric Sensitivity of Bismuthinite and Various Other
Substances. W. W. Coblentz. Scientific Paper 322. 14 pp.
Paper, 5 cents. Issued June 14. The present paper sum-
marizes the results of an examination of various substances,
to determine their electrical sensitivity to light, and describes
the results of a more detailed examination of the photoelectric
sensitivity of bismuthinite, Bi^Ss, and molybdenite, MoSj.
Some Characteristics of the Marvin Pyrheliometer. P. D.
Foote. Scientific Paper 323. 30 pp. Paper, 10 cents.
Issued June 28.
Standardization of the Saybolt Universal Viscosimeter.
W. H. Herschbl. Technologic Paper 112. 23 pp. Paper,
10 cents. Issued June 27. It has previously been impossible
to determine whether a Saybolt Universal viscosimeter gave
normal readings, as neither the dimensions nor normal times of
flow for any given liquids were known. Now that these data
have been determined, limit gauges have been prepared, and the
Bureau of Standards is now in a position to certify whether or
not a given instrument is of standard dimensions.
Determination of Permeability of Balloon Fabrics. J. D.
Edwards. Technologic Paper 113. 29 pp. Paper, 10 cents.
Issued July 2. "One of the most essential characteristics of a
balloon envelope is that it shall be gas tight, or nearly so. There-
fore the determination of the permeability of balloon fabrics to
hydrogen, which is the gas used in the modern dirigible and kite
balloons, is of first importance in determining their suitability
for balloon construction. In connection with a study of the
permeability of balloon fabrics it has been necessary to in-
vestigate different forms of apparatus and the influence of
experimental conditions in order to interpret test results in-
telligently. The results of the Bureau's investigation of methods
of determining permeability are presented in this paper. The
effect of composition, method of construction, etc., upon the
permeability are not discussed in the present paper, which
deals only with testing methods."
Copper. Circular 73. 100 pp. Paper, 20 cents. Issued
June 25. "This circular is the first one issued on the metals;
copper has been chosen for the reason that much of the accurate
Sept., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
763
information regarding copper has been obtained at this Bureau,
and that, in general, our knowledge of the properties of this
metal is more complete than of any other. Furthermore, com-
mercial copper has a very high degree of purity. The data and
information have been put in the form of tables and curves, the
curves have been reproduced in such dimensions that accurate
interpolation of values on them is possible by the use of a rule
graduated in decimal parts of a centimeter. The probable
degree of accuracy of data is indicated, or implied, by the number
of significant figures in the values given.
"The Bureau plans to issue from time to time circulars on
individual metals or alloys., with the idea of grouping in these
circulars all of the best information which the Bureau has as a
result of its tests and investigations together with that available
in all records of published tests and investigations of such ma-
terials.
"The circulars deal primarily with the physical properties
of the metal or alloy; all other factors, except a few statistics of
production, such as methods of manufacture, presence of im-
purities, etc., are discussed only in their relation to these physical
properties; it must be realized that the physical properties of
metals and alloys are often in great degree dependent upon such
factors, so that the statement of values for such properties
should include an accompanying statement regarding those
factors by which the properties are affected.
"The endeavor in the circulars, therefore, is to reproduce only
such data • as have passed critical scrutiny, and to suitably
qualify in the sense outlined above all statements, numerical or
otherwise, made relative to the characteristics of the metal."
DEPARTMENT OF AGRICULTURE
Fertilizers from Industrial Wastes. W. H. Ross. Yearbook
Separate 728. 13 pp. Paper, 5 cents. Contribution from the
Bureau of Soils.
Varieties of Cheese. C. F. Doane and H. W. Lawson.
Department Bulletin 608. 80 pp. Paper, 5 cents. This
bulletin includes descriptions and analyses, with sources of data
indicated in detail.
Effect of Varying Certain Cooking Conditions in Production
of Sulfite Pulp from Spruce. S. E. Lunak. Department
Bulletin 620. 24pp. and 12 plates. Issued March 14. Paper,
15 cents.
Conservation of Fertilizer Materials from Minor Sources.
C. C. Fletcher. Yearbook Separate 733. 8 pp. Paper,
5 cents. Contribution from the Bureau of Soils.
Sources of Our Nitrogenous Fertilizers. F. W. Brown.
Yearbook Separate 729. 10 pp. ( Paper, 5 cents. Contribu-
tion from the Bureau of Soils.
Principles of Liming of Soils. E. C. Shorey. Farmers'
Bulletin 921. 30 pp. Paper, 5 cents. Issued March 1918.
Popular treatment for general use; a contribution from the
Bureau of Soils. '
Phosphate Rock, our Greatest Fertilizer Asset. W. H-
Waggaman. Yearbook Separate 730. 9 pp. Paper, 5 cents.
Contribution from the Bureau of Soils.
Butter Fat and Income. J. C. McDowell. Yearbook
Separate 743. 9 pp. Paper, 5 cents. Popular style for general
use; a contribution from the Bureau of Animal Industry.
Manufacture of Casein from Buttermilk or Skim Milk. A. O.
Dahlberg. Department Bulletin 661. 32 pp. Paper, 5
cents. Issued April 9. Contribution from the Bureau of
Animal Industry.
Some Common Disinfectants. M. Dorset,. Farmers'
Bulletin 926. 12 pp. Paper, 5 cents. A revision of Farmers'
Bulletin 345; popular treatment; a contribution from the Bureau
of Animal Industry.
Cottonseed Meal for Feeding Beef Cattle. W. F. Ward
Farmers' Bulletin 655. 8 pp. Paper, 5 cents. Issued April 10.
Non-technical; a contribution from the Bureau of Animal In-
dustry.
Commercial Freezing and Storing of Fish. E. D. Clark and
L,. H. Almy. Department Bulletin 635. 10 pp. Paper, 5
cents. Issued March 9. Contribution from the Bureau of
Chemistry.
Commercial Stocks of Fertilizers and Fertilizer Materials in
United States as Reported for October 1, 1917. Anon. De-
partment Circular 104. 12 pp. Paper, 5 cents. Issued
February 28. Published by the Bureau of Markets.
Production of Drug Plant Crops in United States. W. W.
Stockberger. Yearbook Separate 734. 10 pp. Paper, 5
cents. Contribution from the Bureau of Plant Industry.
Influence on Linseed Oil of Geographical Source and Variety
of Flax. F. Rabak. Department Bulletin 655. 16 pp. Paper,
5 cents. Issued April 20. Contribution from the Bureau of
Plant Industry.
Experiments on Digestibility of Fish. A. D. Holmes. De-
partment Bulletin 649. 15 pp. Paper, 5 cents. Issued April
13. A contribution from the States Relations Service.
Studies on Digestibility of Some Nut Oils. A. D. Holmes.
Department Bulletin 630. 19 pp. Paper, 5 cents. Issued
April 16. A contribution from the States Relations Service.
Relative Resistance of Various Hardwoods to Injection with
Creosote. C. H. TeesdalE and J. D. Maclean. Bulletin
606. 36 pp. Paper, 15 cents. Published April 15, 191 8. A
technical description of results of experiments in injecting
creosotes in various species of hardwoods.
A Physical and Chemical Study of the Kafir Kernel. G. L.
Bidwell. Bulletin 634. 6 pp. Paper, 5 cents. Published
April 4, 1918. A study showing that, if properly handled,'
kafir products might be substituted for corresponding corn
products.
Articles from the Journal of Agricultural Research
Influence of Carbonates of Magnesium and Calcium on
Bacteria of Certain Wisconsin Soils. H. L. Fulmer. 12,
463-505 (Feb. 25).
Humus in Mulched Basins, Relations of Humus Content to
Orange Production, and Effect of Mulches on Orange Pro-
duction. C. A. Jensen. 12, 505-18 (Feb. 25).
Digestion of Starch by the Young Calf. R. H. Shaw, T. E.
Woodward and R. P. Norton. 12, 575-8 (March 4).
Toxicity of Volatile Organic Compounds to Insect Eggs. W.
Moore and S. A. Graham. 12, 579-88 (March 4).
Effect of Nitrifying Bacteria on the Solubility of Tricalcium
Phosphate. W. P. Kelly. 12, 671-83 (March n).
Respiration of Stored Wheat. C. H. Bailey and A. M.
Gurjar. 12, 685-714 (March 18).
Determination of Fatty Acids in Butter Fat. E. B. Holland
and J. P. Buckley, Jr. 12, 719-32 (March 18).
Studies on Capacities of Soils for Irrigation Water, and on a
New Method for Determining Volume Weight. O. W. Israel-
sun. 13, 1-36 (April 1).
Soil Acidity as Influenced by Green Manures. J. W. White.
13, 171-98 (April 15).
Relation between Biological Activities in the Presence of
Various Salts and the Concentration of Soil Solution in Different
Classes of Soils. C. E. Millar. 13, 213-24 (April 22).
A Study of the Streptococci Concerned in Cheese Ripening.
A. C. Evans. 13, 235-52 (April 22).
764
THE JOURNAL OF INDUSTRIAL AXh ENGINEERING CHEMISTRY Vol. 10, No. g
The Calcium Arsenates. R. H. Robinson 13, 281-94
(April 29).
Chemistry of the Cotton Plant, with Special Reference to
Upland Cotton. A VlERHOEVBR, L. II. Chernoff and C. 0.
Johns. 13, 345-52 (May 13).
Stability of Olive Oil. E. B. Holland, J. C. Reed and J. P.
Buckley, Jr. 13, 353-66 (May 13).
Hydration Capacity of Gluten from "Strong" and "Weak"
Flours. R. A. Gortner and E. H. Doherty. 13, 389-417
(May 20).
Boron: Its Effect on Crops and Its Distribution in Plants
and Soil in Different Parts of the United States. F. C. Cook
and J. B. Wilson. 13, 451-470 (May 27).
Destruction of Tetanus Antitoxin by Chemical Agents. W.
N. Berg and R. A. Kelser. 13, 471-494 (June 3).
Relation of the Density of Cell Sap to Winter Hardiness in
Small Grains. S. C. Salmon and F. L. Fleming. 13, 497-506
(June 3).
Physical Properties Governing the Efficacy of Contact In-
secticides. W. Moore and S. A. Graham. 13, 523-536
(June 10).
Comparative Transpiration of Corn and the Sorghums. E. C.
Miller and W. B. Coffman. 13, 579-581 (June 10).
Inorganic Composition of a Peat and of the Plant from which
it was Formed. C P. Miller. 13, 605-609 (June 17).
Digestibility of Corn Silage, Velvet-Bean Meal, and Alfalfa
Hay when Fed Singly and in Combinations. P. V. Ewtng
and F. H. Smith. 13, 611-618 (June 17).
Effects of Various Salts, Acids, Germicides, Etc., Upon the
Infectivity of the Virus Causing the Mosaic Disease of Tobacco.
H. A. Allard. 13, 619-637 (June 17).
A Study of the Physical Changes in Feed Residues which
Takes Place in Cattle During Digestion. P. V. Ewtng and
L. H. Wright. 13, 639-646 (June 17).
SMITHSONIAN INSTITUTION
Atmospheric Scattering of Light. F. E. Fowle. Publica-
tion 2495. 12 pp.
Smithsonian Physical Tables. T. Gray. 3rd reprint of 6th
revised edition, prepared by F. E. Fowle.
BUREAU OF FOREIGN AND DOMESTIC COMMERCE
Foreign Markets for Cotton Linters, Batting, and Waste.
Special Consular Reports No. 80. 84 pp. Paper, 10 cents.
Compilation of reports prepared by American consuls in various
trading centers throughout the world and transmitted to Bureau
of Foreign and Domestic Commerce during 1915 and 1916.-
COMMERCE REPORTS. JUNE, I918
A fcreat increase in the use of cement and concrete in England
after the war is predicted, including house construction, roads,
railway sleepers, etc. (P. 840)
Three new plants for the manufacture of bichromate for
tanning, have been erected in Denmark, to use Norwegian
chrome ore. (P. 843)
Importation of vegetable ivory into the United States is per-
mitted only on condition that all waste produced from it is de-
livered to the Gas Defense Service. (P. 851)
Electrical manufacturers are urging conservation of tin by
reducing the amounts used in Babbitt metal, alloys, and solder.
(P. 868)
Hull, England, is the largest vegetable-oil center in Europe.
This industry has increased, due to demands for glycerin for
explosives, castor oil for airplanes, oils for margarine, and oil
cake for cattle food. The products include the following oils:
Cotton, coconut, olive, palm, palm kernel, castor, linseed, rape,
and soy bean. (Pp. 919-927)
The cultivation of the Buchu plant in South Africa is in-
creasing. (P. 970)
Rich deposits of bauxite are reported from Dalmatia, of in-
terest to Germany, which is now using inferior Austrian bauxite.
(P. 1025)
Efforts are being made to develop the cultivation of castor
beans in Malaysia. (P. 1061)
Arrangements have been made for the British Government
to obtain annually from Australia 250,000 tons of zinc con-
centrates during the war, and 300,000 tons for a period of nine
years after the war. The annual production is about 400,000
tons, the balance being smelted in Australia or Japan. (P.
1068)
Saccharine is now being manufactured in Great Britain in
amounts sufficient to meet domestic demands. (P. 1109)
In outlining the dyestuff situation in England before the
House of Commons, Sir Arthur Stanley, President of the Govern-
ment Board of Trade, announced that loans and grants for re-
search work would be granted especially to those desirint, to
manufacture special dyes, of which not many are now being
made. Plans are being considered for the amalgamation of the
two largest manufacturers, viz., British Dyes, Ltd., and Messrs.
Levinstein, to be permanently under Government control.
It is expected that importation of foreign dyestuffs will be con-
trolled by rigid licenses for a period of ten years after the war.
(P. 1 148)
While the castor bean is not native to Japan, it is raised there
to a certain extent and could be produced in large quantities if in
sufficient demand. (P. 1158)
A long and detailed description is given of the history and
development of the guayule rubber industry of Mexico and
Texas. The rubber is found, not in a latex, but in the cell
structure of the epidermis of the wild shrub. Experiments on
cultivation of the shrub are promising. The rubber may be
extracted by a number of processes, some mechanical and others
chemical, as, e. g., by heating under pressure with caustic solu-
tion, whereby the wood 'fiber is destroyed. The product ob-
tained contains about 20 per cent of resin, removal of part of
which improves the quality of the rubber. Exports of guayule
rubber from Mexico in 1914-15 were nearly 6,000,000 lbs. (P.
1172)
Experiments in Scotland have shown that it is possible to
produce satisfactory news print paper by using 35 per cent
of sawdust pulp, 30 per cent of waste paper, and 35 per cent im-
ported wood pulp. (P. 1229)
Special
Supplements
France— 56
China — 52b, c, d
Switzerland — 17a
Japan — 55a
Argentina — 3S6
New Zealand — 61a
Aden — i9a
Pbilippine Islands — 80d
Exports to
THf
U
'jitbd States
France — Sup. 5b
Argentine — Sup. 38fc
Camphor
Cement
Bones
Drugs
Quebracho extract
Bono fertilizers
Casein
Optical glass
Glue
Guano
Hides
Hides
Lead
Rubber
Colza oil
Filter paper
Switzerland — Sup. 1*
Flint pebbles
Aluminum
Potassium cyanide
Asphalt
Rubber
Art i!u-i.il silk
Chemicals
Paper pulp
Aniline colors
New Zealand — Sup
61a
Artificial indigo
Copra
Hides
Electric light carbons
Glue
Tallow
Artificial silk
Sept., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
76s
NEW PUBLICATIONS
By Ibbnb DeMatty. Librarian. Mellon Institute of Industrial Research. Pittsburgh
Analysis: Laboratory Manual of Elemental Qualitative Chemical Analysis.
A. R. Buss. Jr. 2nd Ed. 8vo. 194 pp. Price, $2.25. W. B. Saun-
ders Co., Philadelphia.
Carbon and Alloy Tool Steels. Ludlum Steel Co. 12mo. 155 pp.
Price. $1. 00. The Author, Watsrvliet, N. Y.
Case-Hardening; A Bibliography. Carnegie Library. 10 pp. Carnegie
Library, Pittsburgh.
Chemistry: Cours de chimie. R. de Forcrand. 8vo. 438 pp. Price,
14 f. Gauthier-Villars et Cie, Paris.
Chemistry: A History of Chemistry. F J. Moore. 12 mo. 292 pp.
Price, $2.50. McGraw-Hill Co., New York.
Concrete Engineers' Handbook. G. A. Hool and Others. 8vo. 885
pp. Price, $5.00. McGraw-Hill Co;, New York.
Engineers' Handbook. W. H. Thorn* and Son. 2 vol. 8vo. 758 pp.
Price, 21s. T. Reed & Co., London.
Engines and Boilers: How to Run Engines and Boilers; with a New
Section on Water Tube Boilers. E. P. Watson. 12mo. 165 pp.
Price, $1.00. Spon & Chamberlain, New York.
Glass and Glass Manufacture. (Amer. Ed.) Percival Marson. 12mo.
127 pp. Price, $0.85. Sir Isaac Pitman & Sons, New York.
' Gums and Resins. E. J. Parry. 12mo. 106 pp. Price, $0.85. Sir
Isaac Pitman & Sons, New York.
Heating and Ventilation. J. R. Allen and J. H. Walker. 8vo. 305 pp.
Price, $3.00. McGraw-Hill Co., New York.
Market Prices Appearing Currently in Technical and Trade Journals. 8vo.
6 pp. Carnegie Library, Pittsburgh.
Metals: Les Metaux et leurs conditions d'emploi dans l'industrie moderne.
J. Oertle. 8vo. 271 pp. Price, lOf. Protat freres, Paris.
Mineral Enterprise in China. W. F. Collins. 8vo. 307 pp. Price, 21s.
William Heinemann. London.
Sand, Its Occurrence, Properties and Uses; A Bibliography. 8vo. 72 pp.
Carnegie Library, Pittsburgh.
Sewerage; the Designing, Construction and Maintenance of Sewerage
Systems. A. P. Folwell. 8th Ed. 8vo. 43 pp. Price, $3.00.
John Wiley & Sons, Inc., New York.
Sulfuric Acid Handbook. T. J. Sullivan. 18mo. 239 pp. Price, $2.50.
The McGraw-Hill Co., New York.
RECENT JOURNAL ARTICLES
Acid: The Two Systems of Acid Making. H. R. Heuer. Paper, Vol. 22
(1918). No. 18, pp. 33-34.
Alunite: Recently Recognized Alunite Deposits at Sulphur, Nevada. I. C.
Clark. Engineering and Mining Journal, Vol. 106 (1918), No. 4, pp.
159-162.
Aniline Dyes: The Importance of Aniline Dyes in Microscopical Work. A.
O'Callaghan. Color Trade Journal, Vol. 3(1918), No. 2, pp. 272-274.
Artificial Color in Food Products. Albert Burger. Color Trade Journal,
Vol. 3 (1918). No. 2, pp. 282-285.
Belts: How Far Does a Belt Slip? W. F. Schaphorst. Paper, Vol. 22
(1918), No. 21, pp. 13-14.
Bleaching Powder: The Efficient Use of Bleaching Powder. E R. Darl
inc. Textile World Journal. Vol. 54 (1918), No. 4, pp. 35-37.
Brick: Testing and Inspection of Refractory Brick. C. E. Nesbitt and
M. L. Bell. The Blast Furnace and Steel Plant, Vol. 6 (1918), No. 8, pp.
341-345.
By-Product Coke Ovens: Methods for More Efficiently Utilizing Our Fuel
Resources. F„ B. ELLIOTT. General Electric Review, Vol. 21 (1918),
No. 7, pp. 467-480
By-Product Coke Oven Pressure Regulation. C. H. Smoot. The Blast
Furnace and Steel Plant. Vol. 6 (1918), No. 8, pp. 331-335.
Cascade Method of Froth Flotation. W. A. Fahrenwald. Mining and
Scientific Press, Vol 117 (1918). No. 3, pp. 87-88.
Copper: The Maintenance of High Ampere Efficiency in Electrolytic Copper
Refining. M. H. Msrriss and M. A. Mosher. Engineering and Mining
Journal, Vol 106 (1918), No. 3, pp. 95-99.
Copper Tuyeres for Blast Furnaces. A. K. Rbese. The Blast Furnace
and Steel Plant, Vol. 6 (1918). No. 8, pp. 329-330.
Dehydrogenation of Petroleum Oils and Other Hydrocarbons. A. S
Ramac.e. The Canadian Chemical Journal, Vol. 2 (1918), No. 8. pp.
192-195.
Deresination of Rubber. A. H. King. Chemical and Metallurgical Engi-
neering, Vol. 19 (1918). No. 3, pp. 141-145.
Destructive Distillation of Oil Shales. J. C Morrell and G. Eolopp.
Chemical and Metallurgical Engineering, Vol. 19(1918). No. 2, pp. 90-96
Dyeing of Cotton Khaki with Special Reference to the Iron and Chrome
Process. L. J. Matos. Textile World Journal, Vol. 54 (1918), No. 4.
p. 39.
Dyestuffs: The Fastness of Dyestuffs to Light and Ultraviolet Exposure.
E. W. Pierce. Color Trade Journal, Vol. 3 (1918), No. 2, pp. 267-268.
Electric Furnace for Heat Treating. T. F. Baxly. The American Drop
Forger, Vol. 4 (1918), No. 7, pp. 257-260.
Electrochemistry: Elements of Electrochemistry. Joseph Haas, Jr.
The Metal Industry, Vol. 16 (1918), No. 7, pp. 315-316.
Engineering Profession Fifty Years Hence. J. A L. Waddell. The
' Scientific Monthly. Vol. 7 (1918), No. 2, pp. 130-148.
Flax: Influence on Linseed Oil of the Source and Variety of Flax. Frank
Rabak. Paint and Varnish Record, Vol. IS (1918), No. 1, pp. 18-19.
Flotation Apparatus, Their Design and Operation. A. W. Fahrenwald.
Chemical and Metallurgical Engineering, Vol. 19 (1918), No. 3, pp. 129-
134.
Drop
Fuel Analysis of a Drop Forge Plant. B. K. Read. The Ar
Forger, Vol. 4 (1918), No. 7, pp. 268-270.
Gold: The Importance of Gold Production. Lionel Phillips. Mining
and Scientific Press, Vol. 117 (1918), No 5, pp. 158-160.
Groch Flotation Machine. F. O Groch and W. E. Simpson. Mining
and Scientific Press, Vol. 117 (1918), No. 2, pp. 53-54.
Gypsum: Influence of Gypsum upon the Solubility of Potash in Soils. P.
R. McMeller. Journal of Agricultural Research, Vol. 14 (1918), No. 1,
pp. 61-66.
Illumination: Fundamental of Illumination Design. Ward Harrison.
General Electric Review, Vol. 21 (1918), No. 8, pp. 535-541.
Limonite Deposits in Porto Rico. C. R. Fettke and B. Hubbard. The
Iron and Trade Review, Vol. 63 (1918), No. 4. pp. 210-211.
Macquiston Tube Flotation Machine. C. T. Rice. Engineering and
Mining Journal, Vol. 106 (1918), No. 4, p. 163.
Margarine: Modern Methods of Crystallizing Margarine Emulsion. Alan
P. LEE. The American Food Journal, Vol. 13 (1918), No. 7, pp. 382-
385.
Materials: Requirements in Treating of Materials. J. F. Bealb. The
American Drop Forger, Vol. 4 (1918), No. 7, p. 283.
Melting Points and How to Take Them. Louis Boritz. Color Trade
Journal, Vol. 3 (1918), No. 2, pp. 271-272.
Metallography and Heat Treatment of Metals Used in Aeroplane Con-
struction. F. Grotts. Chemical and Metallurgical Engineering, Vol.
19 (1918), No. 3, pp. 12L-128.
Metallurgy: Notes on Recent Metallurgical Progress. E. P Mathew-
son. Engineering and Mining Journal, Vol. 106 (1918), No. 3, pp.
138-145.
Mining on the Rand. H. F. Marriott. Mining and Scientific Press,
Vol. 117 (1918), No. 3, pp. 77-86.
Paper: The Yellowing of Paper. A. B. Hitchins. Paper, Vol. 22 (1918),
No. 20, pp. 11-15.
Para-Amidophenol. Samuel Wein. Color Trade Journal, Vol. 3 (1918.1,
No. 2, pp. 287-289.
Paraffins: Boiling Points of the Paraffins. G. LeBas. The Chemical
News. Vol. 117 (1918), No. 3052, pp. 241-242.
Potash: The Estimation of Potash. Bertram Blount. The Chemical
News, Vol 117 (1918). No. 3052, pp. 242-244.
Pottery: Status of American Pottery Industry. A. V. Bleininger. Brick
and Clay Record, Vol. 53 (1918). No. 2, pp. 125-128.
Refractory Materials in Canada. N. B. Davis. The Canadian Chemical
Journal, Vol. 2 (1918), No. 7, pp.- 176-177.
Research and the Industries. P. G. Nutting. The Scientific Monthly,
Vol. 7 (1918), No. 2, pp. 149-157.
Ruth Flotation Machine. A. J. Hoskin. Mining and Scientific Press,
Vol. 117 (1918), No. 4. pp. 119-121.
Silicon Carbide Useful as a Resistor. W. S Scott. The Iron Trade Review.
Vol 63 (1918). No. 4, p. 209.
Silver-Lead Smelter: Ideal Layout for Silver-Lead Smeltery. G. C. Rid-
dell. Engineering and Mining Journal, Vol. 106 (1918), No. 3, pp. 115-
122.
Spelter Statistics for 1917. W. R. Ingalls. Engineering and Mining
Journal, Vol. 106 (1918), No. 4, pp. 176-481.
Sulfite Coal. R. W. STRBHlENBRT. Pulp and Taper Magazine. Vol. 16
(1918), No. 30, pp. 671-672.
Wood: The Use of Wood in Chemical Apparatus. A. W. Scborobr.
Metallurgical and Chemical Engineering, Vol. 18 (1918), No. 10, pp.
528-531.
Zinc: Research Preparedness in the Zinc Industry. P. C. Choatb.
Chemical and Metallurgical Engineering. Vol. 19 (1918), No. 1. pp. 20-22.
MARKET REPORT— AUGUST, 1918
WHOLESALE PRICES PREVAILING IN THE NEW YORK MARKET ON AUGUST 17, 1918
INORGANIC CHEMICALS
Acetate of Lime 100 Lbs.
Alum, ammonia, lump 100 Lbs.
Aluminum Sulfate, (iron free) Lb.
Ammonium Carbonate, domestic Lb.
Ammonium Chloride, white Lb.
Aqua Ammonia, 26°, drums Lb.
Arsenic, white Lb.
Barium Chloride Ton
Barium Nitrate Lb.
Barytes, prime white, foreign Ton
Bleaching Powder, 35 per cent Lb.
Blue Vitriol Lb.
Borax, crystals, in bags Lb.
Boric Acid, powdered crystals Lb.
Brimstone, crude, domestic Long Ton
Bromine, technical, bulk Lb.
Calcium Chloride, lump, 70 to 75% fused Ton
Caustic Soda, 76 per cent 100 Lbs.
Chalk, light precipitated Lb.
China Clay, imported Ton
Feldspar Ton
Fuller's Earth, foreign, powdered Ton
Fuller's Earth, domestic Ton
Glauber's Salt, in bbls 100 Lbs.
Green Vitriol, bulk 100 Lbs.
Hydrochloric Acid, commercial Lb.
Iodine, resublimed Lb.
Lead Acetate, white crystals Lb.
Lead Nitrate Lb.
Litharge, American Lb.
Lithium Carbonate Lb.
Magnesium Carbonate, U. S. P Lb.
Magnesite, "Calcined" Ton
Nitric Acid, 40* Lb.
Nitric Acid, 42* Lb.
Phosphoric Add, 48/50% Lb.
Phosphorus, yellow Lb.
Plaster of Paris Bbl.
Potassium Bichromate Lb.
Potassium Bromide, granular Lb.
Potassium Carbonate, calcined. 80 & 85%.. .Lb.
Potassium Chlorate, crystals, spot Lb.
Potassium Cyanide, bulk, 98-99 per cent Lb.
Potassium Hydroxide, 88 @ 92% '. ... Lb.
Potassium Iodide, bulk Lb.
Potassium Nitrate Lb,
Potassium Permanganate, bulk.U. S. P Lb.
Quicksilver, flask 75 Lbs.
Red Lead, American, dry 100 Lbs.
Salt Cake, glass makers' Ton
Silver Nitrate Ox.
Soapstone, in bags Ton
Soda Ash, 58%, in bags .100 Lbs.
Sodium Acetate Lb.
Sodium Bicarbonate, domestic 100 Lbs.
l Bichromate Lb.
1 Chlorate Lb.
1 Cyanide Lb.
1 Fluoride, commercial Lb.
1 Hyposulfite 100 Lbs.
1 Nitrate, 95 per cent, spot 100 Lbs.
1 Silicate, liquid, 40° Be
Sodium Sulfide, 60%. fused in bbls Lb.
Sodium Bisulfite, powdered
Strontium Nitrate Lb.
Sulfur 100 Lbs.
Sulfuric Acid, chamber 66° Be Ton
Sulfuric Acid, oleum (fuming) Ton
Talc, American white Ton
Terra Alba, American, No. 1 100 Lbs.
Tin Bichloride, 50" Lb.'
Tin Oxide Lb.
White Lead, American, dry Lb.
Zinc Carbonate .' Lb.
Zinc Chloride, commercial Lb.
ORGANIC CHEMICALS
Acetanilld. C. P., in bbls Lb.
Acetic Acid, 56 per cent, In bbls Lb.
Acetic Acid, glacial, 99>/i% Lb.
Acetone, drums. Lb.
Alcohol, denatured, 1 80 proof Gal.
Sodiun
Sodiun
Sodiun
Sodiun
Sodiun
Sodiun
Sodiun
nominal
4</4 @
5'/
3«A @
4
nominal
20 @
22
nominal
9'/« @
17
65.00 @
70.00
12 @
14
30.00 @
35.00
2 @
3V<
9'A @
9»/i
7>A @
lO'/i
7'/. @
8»/4
nominal
75 @
22.00 @
24.00
4.15 @
4'A @
5
20.00 @
30.00
8.00 @
15.00
nominal
20.00 @
30.00
2.00 @
3.00
1.15 @
1.25
C. P. nominal
4.25 ®
4.30
nominal
C. P. 85
8 @
8'A
60.00 @ 65.00
7»A
8V1
35
1.20
2.00
40
1.25
2.50
46Vl
1.36
41
1.50
0
2.00
25.00
a
130.00
10.79
@
12.75
25.00
0
30.00
62'A
0
65
10.00
®
12.50
2V
0
30
2.35
3'/«
0
3>/i
24»/l
®
25'/t
25
0
25'A
40
@
42
17
0
18
2.60
@
3.60
4.12'A
©
5.00
18.00
32.00
10.76
19.50
lO'/i
20
15 '/»
10.77
19.70
Alcohol, sugar cane, 1 88 proof Gal.
Alcohol, wood, 95 per cent, refined Gal.
Amyl Acetate Gal.
Aniline Oil, drums extra Lb.
Benzoic Acid, ez-toluol Lb.
Benzol, pure Gal.
Camphor, refined in bulk, bbls Lb.
Carbolic Acid, U. S. P., crystals, drums Lb.
Carbon Bisulfide Lb.
Carbon Tetrachloride, drums, 100 gals Lb.
Chloroform Lb.
Citric Acid, domestic, crystals Lb.
Creosote, beechwood Lb.
Cresol, U. S. P Lb.
Dextrine, corn (carloads, bags) Lb.
Dextrine, imported potato Lb.
Ether, U. S. P. 1900 Lb.
Formaldehyde, 40 per cent Lb.
Glycerine, dynamite, drums extra Lb.
Oxalic Acid, in casks Lb.
Pyrogallic Acid, resublimed, bulk Lb.
Salicylic Acid, U. S. P Lb.
Starch, cassava Lb.
Starch , corn (carloads, bags) pearl 1 00 Lbs.
Starch, potato, Japanese Lb.
Starch, rice Lb.
Starch, sago flour Lb.
Starch, wheat Lb.
Tannic Acid, commercial Lb.
Tartaric Acid, crystals Lb.
OILS, WAXES, ETC.
Beeswax, pure, white Lb.
Black Mineral Oil, 29 gravity Gal.
Castor Oil, No. 3 Lb.
Ceresin, yellow Lb.
Corn Oil, crude 100 Lbs.
Cottonseed Oil, crude, f . o. b. mill Lb.
Cottonseed Oil, p. s. y 100 Lbs.
Menhaden Oil, crude (southern) Gal.
Neafs-foot Oil, 20° Gal.
Paralfin, crude, 118 to 120 m. p Lb.
Paraffin Oil, high viscosity Gal.
Rosin. "F" Grade, 280 lbs Bbl.
Rosin Oil. first run Gal.
Shellac, T. N Lb.
Spermaceti, cake Lb.
Sperm Oil, bleached winter, 38* Gal.
Spindle Oil, No. 200 Gal.
Stearic Acid, double- pressed Lb.
Tallow, acidless Gal.
Tar Oil, distilled. .. .^ Gal.
Turpentine, spirits of Gal.
METALS
Aluminum, No. 1, ingots Lb.
Antimony, ordinary Lb.
Bismuth, N. Y Lb.
Copper, electrolytic Lb.
Copper, lake Lb.
Lead, N. Y Lb.
Nickel, electrolytic Lb.
Platinum, refined, soft Oz.
Silver Oz.
Tin, Straits Lb.
Tungsten (WO») Per Unit
Zinc, N. Y
FERTILIZER MATERIALS
Ammonium Sulfate 100 Lbs.
Blood, dried, f. o. b. Chicago Unit
Bone, 3 and 50, ground, raw Ton
Calcium Cyanamide Unit of Ammonia
Calcium Nitrate, Norwegian 100 Lbs.
Castor Meal Unit
Fish Scrap, domestic, dried, f. o. b. works... .Unit
Phosphate, acid, 16 per cent Ton
Phosphate rock, f. o. b. mine: Ton
Florida land pebble, 68 per cent Ton
Tennessee. 78-80 per cent Ton
Potassium "muriate." basis 80 per cent Ton
Pyrites, furnace size, imported Unit
Tankage, high-grade, f. o. b. Chicago Unit
4.90
<*
91'
s
5.30
g
28'/»
0
2.65
a
23
•
43
0
9
o
31
0
70
0
82
14
2.00
0
24
0
8
<*
27
0
16 '/«
'4
62
0
41
0
6.50 @
7.00
13'/* @
13'A
12'/i 0
13
9 'A @
10'A
nominal
17.50
0
17.75
17 "A
0
—
20.50
0
21 .50
1.00
«
1.10
3.45
(A
3.55
9«A
0
10
40
0
41
10.95
0
11.00
60
0
65
65
0
67
32
0
34
2.23
@
2.25
38
0
40
24
0
25
1.58
&
1.60
13
0
13',
3.50
@
3.65
26
0
26
0
8.05
55
0
nominal
95'/.
nominal
56
20.00
0
24.00
8.70
0
8.90
7
75
0
B
.00
6
70
0
6
7 5
37
00
0
40.00
nominal
7
30
and
10c
16
00
@ .
nominal
17
lX>
3
50
0
3
75
5
50
0
nominal
nominal
6
00
6
65
0
6
-o
The Journal of Industrial
and Engineering Ghemistry
Published by THE AMERICAN CHEMICAL SOCIETY
AT KA3TON. PA.
Volume X
OCTOBER 1, 1918
No. 10
Editor: CHARLES H. HERTY
Assistant Editor: Grace MacLeod
Advertising Manager: G. W. Nott
ADVISORY BOARD
H. E. Barnard H.K.Benson F.K.Cameron B.C.Hesse A. D. Little A. V. H. Mory
Published monthly. Subscription price to non-memben of the American Chemical Society, $6.00 yearly; tingle copy, 60 cents
Price per single copy to American Chemical Society members, 50 cents. Foreign postage, seventy-five cents, Canada, Cuba and Mexico excepted
Entered as Second-class Matter December 19, 1908, at the Post-Office at Easton, Pa., under the Act of March 3, 1879
Acceptance for mailing at special rate of postage provided for in Section 1103. Act of October 3, 1917. authorised July 13. 1918.
All communications should be sent to The Journal of Industrial and Engineering Chemistry.
Telephone: Vanderbilt 1930 35 East 41st Street, New York City
Subscriptions and claims lor lost copies should be referred to Charles L. Parsons, Box 505, Washington, D. C.
ESCHBNBACH PRINTING COMPANY, EasTON, Pa.
TABLE OF CONTENTS
Annual Meeting American Chemical Society :
President's Address — -A Retrospect and an Application.
William H. Nichols 768
Council Meeting 772
General Meeting 774
Chemists in Warfare:
The American Chemist in Warfare. Charles L. Parsons 776
The Work of the Chemical Section of the War Industries
Board. Charles H. MacDowell 780
War Disturbances and Peace Readjustments in the
Chemical Industries. Grinnell Jones 783
Chemical Warfare Research. Wilder D. Bancroft 785
The Place of the University in Chemical War Work. E.
W. Washburn 786
Symposium on Chemistry of Dyestuffs:
Introductory Remarks. R. Norris Shreve 789
America's Progress in Dyestuffs Manufacturing. Louis
Joseph Matos 790
The Development of the Dyestuff Industry since 1914.
J. F. Schoellkopf, Jr . 792
Application of Dyestuffs in Cotton Dyeing. J. Merritt
Matthews 794
Natural Dyestuffs — an Important Factor in the Dye-
stuff Situation. Edward S. Chapin 795
The Manufacture, Use, and Newer Developments of the
Natural Dyestuffs. C. R. Delaney 798
Photographic Sensitizing Dyes: Their Synthesis and
Absorption Spectra. Louis E. Wise and Elliot Q.
Adams 801
The Color Laboratory of the Bureau of Chemistry. H.
D. Gibbs 802
Problems in Testing Dyes and Intermediates. E. W.
Pierce 803
On the Quantitative Analysis of Dyestuffs. Alfred H.
Halland 804
Chemical Markets of South America:
Chemical Trade of Chile, Peru, and Bolivia. O. P.
Hopkins 805
Original Papers:
Valuation of Raw Sugars. W. D. Home 809
On the Preparation of an Active Decolorizing Carbon
from Kelp. F. W. Zerban and E. C. Freeland 812
The Rdle of Oxidases and of Iron in the Color Changes-
of Sugar Cane Juice. F. W. Zerban 814
Laboratory and Plant:
Methods of Analysis Used in the Coal-Tar Industry.
II— Distilled Tars and Pitches. J. M. Weiss. ..... 817
A Convenient Electric Heater for Use in the Analytical
Distillation of Gasoline. E. W. Dean 823
Fourth National Exposition of Chemical Engineers:
Permanent Chemical Independence. Charles H. Herty. 826
The Exposition in War and in Peace. F. J. Tone 828
The Importance of Practical Chemistry. G. W.
Thompson 829
Development in Nitric Acid Manufacture in the United
States since 1914. E. J. Pranke 830
Recovery of Potash from Kelp. C. A. Higgins 832
Recovery of Potash from Iron Blast Furnaces and
Cement Kilns by Electrical Precipitation. Linn
Bradley 834
Potash from Desert Lakes and Alunite. J. W. Hornsey. 838
Potash from Searles Lake. Alfred de Ropp, Jr 839
Recent Developments in Ceramics. A. V. Bleininger. . 844
Carborundum Refractories. S. C. Linbarger 847
'The Pyrophoric Alloy Industry. Alcan Hirsch 849
The Ferro-Alloys. J. W. Richards 851
Advances in Industrial Organic Chemistry since the
Beginning of the War. Samuel P. Sadtler 854
Solvents from Kelp. C. A. Higgins 858
Wood Waste as a Source of Ethyl Alcohol. G. H. Tom-
linson 859
Current Industrial News:
Iron and Steel Industry in Japan; Goods in Demand in
Australia; Jute Production in China; Cranes and
Transporters; Natural Indigo Industry; Refractory
Material from Bauxite; Substitute for Shellac;
Electricity in Silk Industry; Vegetable Oils in Japan;
Aluminum; A New Heat Insulator 861
Scientific Societies:
Fifty-Sixth Meeting, American Chemical Society, Cleve-
land, September 9 to 13, 1918; Communication from
United States Shipping Board ; Committee on Organic
Accelerators, Rubber Section, American Chemical
Society; Division of Industrial Chemists and
Chemical Engineers; Fall Meeting, American Electro-
chemical Society, September 30-October 2, 1918. . . . 863
Notes and Correspondence :
Platinum Regulations; Platinum Wanted by the Govern-
iihtU; Two Letters on Reproducing Beilstein's
Handbuch der Organischen Chemie; Library for
Edgewood Arsenal Laboratory; Ordnance Depart-
ment, School of Explosives Manufacture, Columbia
I Diversity'; Chemistry for Soldiers in Training (.imp
The Emblem of the American Chemical Society .... 866
Washington Letter 870
Personal Notes 871
Industrial Notes 872
Government Publications 873
New Publications 875
Market Report 876
768
THE JOURN I/. 01 INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
ANNUAL MLLTING AMERICAN CHEMICAL 50CILTY
PRESIDENT'S ADDRESS
A EETEOSPECT AND AN APPLICATION
By William il XkiiuLS
I happen to be one of the few men now living who
can look back to the very beginning of the American
Chemical Society, a little more than forty-two years
ago. On an occasion like this, it is unavoidable that
my thoughts should travel backward to those earlier
and simpler days when it was a great question as to
whether such a society could be formed and, if formed,
whether it could be supported and produce results
which would be worth while. As you know so well, it
was the outcome of a suggestion of a lady who, with
ether chemists, had gathered at the grave of Priest-
ley to bear silent witness to their appreciation of what
that early spirit had contributed to the cause of chem-
istry.
The first meeting for organization was held on the
evening of April 6, 1876. at the rooms of the New York
College of Pharmacy in New York University build-
ing, Washington Square, since demolished and rebuilt.
There were present thirty-five gentlemen, and letters
of regret were received from four who approved of the
object of the gathering. As might have been expected,
Professor Chandler was elected Chairman of the meet-
ing, and that brilliant man, Dr. Walz, long since passed
away, recorded. In the report which he presented
he said :
"A list of chemists in this city and vicinity was first made out,
and though it was by no means complete, we found to our
astonishment that there were nearly, if not quite, 100 chemists
in this neighborhood who might properly be admitted as mem-
bers of this Society."
Compare that with the present membership of the
New York Section alone!
At this meeting every one was invited to speak
frankly and freely, and several of our most distin-
guished chemists expressed the view that it was not
opportune to found a chemical society at that time,
although they all agreed that at some future time it
would be desirable to do so. The Chairman remarked
that it would almost seem as though we had met for
the purpose of deciding not to organize a chemical
society, and asked for further expression of opinion.
The result you all know, and the American Chemical
Society was launched on that evening, a constitution
and by-laws adopted, and a committee appointed to
nominate officers for the society. The committee re-
ported the same evening, nominating my old preceptor,
Dr. John W. Draper, that great chemist with so many
attainments besides chemistry, for president, and a
splendid list of vice presidents and other officers was
provided. Fortunately, Dr. Draper accepted the nom-
ination and thus became the first president of what
was to become the greatest chemical society of the
world. Before this result was reached, there was no
division of opinion as to the wisdom of commencing
at that time, and those whose objection had been
most strenuous became ardent supporters and so re-
mained.
Dr. Draper's inaugural address, which was delivered
on November 16. 1876. in Chickering Hall, with a
large public attendance, was a very noteworthy paper.
After a few congratulatory remarks he said:
"Let us consider some of the reasons which would lead us
to expect success, not only for our own, but also for other kindred
societies The field of nature is ever widening before us: the
harvest is becoming more abundant and tempting, the reapers
are more numerous Each year the produce that is garnered
exceeds that of the preceding. Perhaps then, you will listen
without impatience for a few minutes this evening to one of the
laborers who has taken part in the toil of the generation now
finishing its work, who looks back not without a sentiment of
pride on what that generation has done, who points out to you
the duties and rewards that are awaiting you, and welcomes
you to your task."
Certainly an exordium full of wisdom and prophetic
vision !
The first meeting for which papers were announced
was held on May 4. 1876. The first paper was by Dr.
H. Endemann on "The Determination of the Relative
Effectiveness of Disinfectants." It is interesting to
read that
"The discussion closed at a late hour on which account the
papers of Mr. P. Casamajor and I. Walz were laid over till the
next meeting."
Imagine what would happen at a Section meeting to-
day if every paper should receive similar consideration.
These early meetings of the Society were simple and,
of course, there was only one Section. Intermediate
meetings, or conversaziones, as we called them, of a less
formal character were held at which various matters
of interest were discussed in conjunction with beer and
sandwiches and much good feeling and mutual respect
engendered. I do not believe that one of the chemists
who attended these early meetings had the faintest
conception of what would be the outcome of the enter-
prise. Chemistry in those days was not considered a
vital matter, as it is to-day, and the chemist himself
was usually a somewhat humble member of some
manufacturing staff, when he was not a professor in
a college. To-day we have a membership of 12.000,
still growing rapidly, and the profession is recognized
as being of such great importance that it is secondary
to none, and in the minds of many it assumes the first
place. I believe that in the future it will be generally
conceded that the chemist represents the most im-
portant of all the sciences, and that on him will depend
to an increasing extent not only the welfare of the
world but possibly the very lives of its inhabitants.
Looking back into that past, which is after all not
so far away, we note that many things were unknown
which, during the interval, have become so well known
that many of my younger hearers would suppose that
they have always been part of human knowledge.
Take, for instance, the transportation of sulfuric acid
in bulk: I can remember well when the only means of
transportation of this vital material was in carboys
with occasional use of drums, which were always a
source of trouble. I remember the discussion with Dr.
Herreshoff as to why it should be practicable to store
and ship this material in bulk; and when the decision
Oct., iqiS
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
769
was finally reached to make the attempt, the first con-
tainer was an iron cylinder made to stand pressure and
placed upon a barge, and which would hold about 50
tons of product. With great difficulty, one small oil
refiner was induced to provide a storage tank of steel
and receive the acid in this way, but for one whole
year it was impossible to secure a second customer
because of the belief that the acid would not only
destroy the container but would itself become weak
and unfit for oil refining. In these days when the,
greater part of sulfuric acid is transported in this way,
by boat and car, not only for moderate distances but
across the continent, it is hard for any of us to believe
that so short a time ago its possibility was unknown.
I do not need to enlarge upon the effects of this sim-
ple invention to show what an effect it has had upon
the industries of the world.
I can also remember when, with the exception of
one or two attempts, which were not successful, pyrite
was not used in this country. To-day, while the sub-
ject of pyrites is so prominently before the minds of
everybody from the President down, it seems hard to
believe that so few years ago, comparatively, its suc-
cessful use was unknown here. It had been used
abroad, and it was from England that we obtained the
first men to operate the first kilns that were erected
here, for the reason that no one of our small staff knew
how to burn it or to teach others. We all know now
that millions of tons per annum are burned in this
country in the production of sulfuric acid, not includ-
ing zinc and copper ores in the treatment of which
sulfur is a by-product.
I also remember when lead burning was such a
secret that its modus operandi was known to a very
limited circle. The first set of lead chambers I ever
constructed were according to the design of a French
engineer who, in addition to performing his supervising
duties, undertook to teach me lead burning. I am
happy to say I proved a moderately good pupil and
found that of all the trades probably none was more
easily learned or offered better pay. I think it is safe
to say that in a very few months any man with a
mechanical turn of mind can master all the intricacies
of the trade, and I have always wondered why more
young men did not take it up. It is vital in all chem-
ical engineering, and offers an occupation which is far
more interesting in itself, on account of its variety,
than almost any other trade.
Forty years ago the copper industry in this country
was a comparatively small affair. If we except the
production of the Lake companies, whose ore had been
refined by nature to a considerable degree of purity,
the output was small, and owing to impurities, of not
much value except for certain casting purposes. Must
of it found its way to Wales, where it. was refined after
a fashion, the precious metals remaining as impurities.
No accurate and reliable method of analysis was in
use, and differences in results led t<> considerable <-<>n
fusion. A correct analytical method was demanded by
the producers in the West, who lirsl saw its absolute
necessity as a foundation of a large industry. The
electrolytic method of assaying, while practiced spo-
radically in certain laboratories, had made no head-
way as a basic method which could be absolutely
relied on. I was present when this was worked out
and given to the copper industries as a solution to the
difficulties of their business. It did not occur to the
chemist who worked it to completion that if one could
deposit a gram of copper by electric current, he couid
just as well deposit a ton or a thousand tons. It was
this last application of the discovery which evolved
into the great electrolytic copper industry, which not
only provides the purest copper that the world has
seen, but also makes available all the precious metals
which up to its introduction had been wasted, and
which since have amounted to hundreds of millions of
dollars. It is fortunate for the world that this analy-
tical method was worked out, for in addition to many
other uses it made possible the great electric industry,
and who can say what that has meant in the devel-
opment of the arts of peace and war?
Of course, there are many instances of facts which
to-day are known to everyone, which forty years ago
were entirely unknown, but I will not tire you by add-
ing to the list. Forty years is not a long time in the
history of the world, but it has been an age in the
development of chemistry. As knowledge begets
knowledge unfailingly, it is bewildering to contemplate
what the next forty years will add to the knowledge
of the chemists, who will be filling our places, applying
what has been learned and searching out into the lim-
itless expanse of the still unknown. Every step up the
hill the view expands, but the horizon ever retreats.
Much has been written, particularly of late, on the
progress of chemistry, and I am rather of the opinion
that instead of searching for subjects where so many
able men have preceded him, the President of this
Society in his annual address should be required to
give a resume' of the work and accomplishments of the
past year. In the absence of this rule, however, I have
been warned to keep away from that subject on the
ground that it has already been sufficiently covered. Be
that as it may, so much has come under my observation
during the past few years, of accomplishments made
absolutely necessary by 'new conditions, that I stand
in wonder as I see how fully and admirably the Amer-
ican chemist has grasped the problems as they were
presented, and promptly solved them, in many cases
better than they have ever been solved before. It
seems to have been the fashion to belittle the work
we have done in the past and to apologize for it. It is
great pleasure for me to say here that apologies are un-
called for and explanations can be seen in the results,
which are more conclusive than arguments. For
example, a great dye industry has been brought up
from the foundation and is serving our textile trade
with efficiency in spite of the slimy propaganda which
tries to implant the impression that what has been
done here may answer for a temporary affair, but that
by and by we will get. back tin ■ i old German dyes
on which we can rely. This propaganda is treason-
able. All that the dye industry needs is intelligent
legislation and a sympathetic public. The brains and
77©
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. 10
the materials are here in abundance. We may not
have had time to work out all of the delicate shades
which the ladies in peace times admire for their eve-
ning toilettes, but we have got all the fundamentals
that are necessary for a self-respecting nation and the
frills will come later. This has been a great triumph
and I take off my hat to the American chemists, and
there are many of them, who have made it possible,
through the faith and courage of American capital.
The idea that they cannot go farther and do better
than has ever been done before is unworthy, and
everything that can be done to encourage the chem-
ist in his work in this great field should be done. A
little praise is a great stimulant. The American chem-
ist has had altogether too little of it.
Another great work will soon be accomplished by
the fixation of atmospheric nitrogen. What has been
done on this side of the ocean is not in imitation of
what has been done abroad. It has been worked out
from the foundation, and I believe it shows a great
advance. It involves not only chemistry, but also
engineering of the highest type, and no one has ever
yet accused the American chemical engineer of being
inferior to those of any other country. From a some-
what intimate knowledge of this branch of the field, I
say with confidence that in chemical engineering this
country stands comparison with any other in the
world, and I can do so without fear.
I have alluded to only two great steps which have
been taken, but of course there are hundreds of others,
possibly not as startling, but still of the utmost
moment and importance. In the quiet of his labora-
tory, the chemist has not been found wanting, although
denied the stimulus of notoriety to spur him on.
Since the early days of the Society, to which I have
thought it worth while to allude, its progress has been
steady and even phenomenal. Naturally, this has been
largely due to the great increase in the number of men
who have entered the chemical profession, but for its
success we are under everlasting obligations to the
great men, early and late, who have done so much in
its upbuilding. The Society started with the earnest
and enthusiastic support of the best men of that day,
and since that time it has been fortunate in keeping
that class of men active in its councils; but even with
these two advantages success could not have been
attained if there had been serious disagreements or
jealousies among those in charge of its affairs. During
all these years we have been singularly free from that
element of weakness, and it is by the intelligent coop-
eration of all these men that we find ourselves to-day
in the enviable position we occupy. It is a brilliant
example of unselfish cooperation, and I shall use that
fact as my text in discussing briefly the importance
of cooperation in other fields, with the full belief that
by it alone can the tremendous world problems of the
future be successfully met and overcome.
When considering the subject of cooperation, I think
we must always have in mind the object which is sought
to be attained. It is said that there are two kinds of
microbes — friendly and unfriendly. In the same way
there are at least two purposes of cooperation — one
injurious, the other beneficial. There have always
been a great many instances of the former variety; in
fact, they probably largely outnumber the instances
of the latter.
If the world is to progress and its people are to reach
that stage which all well-wishers desire, these propor-
tions must change and instances of cooperation for
beneficial purposes must largely outnumber the other
variety, when it will naturally follow that those exam-
ples which lead to injury will gradually become less
effective and finally tend to disappear altogether.
Unless properly attended to, the weeds in the garden
become the most successful plants in it. So it is with
the forces of evil in a community.
Any cooperative activity whose object is purely self-
ish must belong to the objectionable class. It may
have many good points, but the object sought to be
attained qualifies them all. You will readily recognize
the existence to-day of many cooperative efforts, the
object of which is to attain something for some man
or set of men without regard to the general good.
There are rings and pools and associations of one kind
and another in which exceedingly intelligent work is
being done, but which are all working against the
general good. The law of cooperation applies here as
elsewhere, but this is not the true cooperation which
I am advocating. I simply allude to it so that it may
not be left out of consideration.
I have in mind that class of cooperation which looks
toward the general good, not only of a community,
but of the nation and the world. It has made more
headway within the last three or four years than In
the century which preceded. It seems as if the ter-
rible war forced upon the world by the house of Hoh-
enzollern and its satellites was necessary to awaken
the conscience of all civilized peoples. There can be
no question that in general we in this country had been
following after Mammon. We might just as well
admit it without argument. Anyone who will take the
trouble to read the history of this country in the last
century cannot fail to note the tremendous energy
necessary to make first the footing and afterwards the
development of the unlimited resources which lay
around us everywhere. A long series of battles with
nature was followed by such great success that it
was comparatively easy for a man of large intellect to
grasp, with or without pure motives, a way to acquire
a large share of the wealth produced. Where the
motives were not the best I fear it frequently hap-
pened that large fortunes were built up at the expense
of others. Whether that be true or not, it naturally
resulted in what is known as the capitalist class, as
differentiated from the others, workers with hands or
brains, or ordinary consumers. This made it easy to
implant in the minds of wage earners the idea that
they must organize in order to secure their share of
the results, and more if possible. Like nearly all such
movements, the selfish idea was apt to predominate on
both sides and the result has been a species of warfare
between capital and labor, which is not only unwise,
but unnecessary and enormously expensive. It must
be clear to everyone that without a leader an army is
Oct., 1918
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
77i
lost. It is equally clear that the best leader without
an army is of not much value. Cooperation, there-
fore, between the leaders and the army is absolutely
essential before we can consider ourselves on the high
road to that success which our abundant resources
make possible.
At this point it would be well to look briefly at the
meaning of the word "Success." A common idea is
that it means the acquisition of money or other prop-
erty and that these are the only counters. I believe
that we will have to change our views in regard to this
matter before we can embark on that campaign of
cooperation which is so essential. If instead of the
acquisition of something tangible it is understood that
the making of all that is possible in character is our
goal, we will find that the successful man is the man
who ha; made the most of himself and that money or
title or any such thing have little real value in the case.
They are simply incidents. Some of the finest men I
have ever known are simple, honest workers, and some
of the poorest specimens I have come in contact with
are among those who consider that they have made
most of themselves because they have acquired a large
amount of property when the opportunities offered.
Now, making the most of one's self, which is the aim
in view, the matter of industrial cooperation becomes
much simplified if everyone does the best he can to
acquire character and that success which goes with it.
The capital and labor question will then solve itself.
All men are not born equal, in spite of the well-known
statement to the contrary. Some have greater natural
ability or better constitutions than others and some
have opportunities to make the most of them which
others do not possess. The rights of both are alike, of
course, and in any event, the cooperation of all,
whether highly endowed or with small opportunities,
is absolutely essential for the proper development of
the future. All this may sound Utopian and unlikely
of accomplishment, but I am of the opinion that the
best outcome for the individual, as well as for the
country, will not be reached until the large majority
are working together from the highest motives. High
aim is necessary for a long trajectory.
This is a democracy and those who rule over us are
men of our own selection. We get exactly the class
of government that we deserve, and if it does not suit
us for any reason, we have no one to blame but our-
selves. Why should it not be possible for this coop-
eration, to which I have alluded, to extend so that it
includes both the Government and the people? I do
not mean it in the way that the German Government
calls cooperation with the people, because that did not
have the right end in view. It was extremely efficient
and helped enormously in the bringing of Germany to
the front as a manufacturing nation, but the object
was selfish and nothing more nor less than was expressed
by the motto ''Deutschland uber alles." The kind
of cooperation which we should have from our Govern-
ment is assistance in every way possible in building up
the kind of success to which I have alluded. Instead
of looking on manufacturers as probable criminals,
they must be regarded as associates whose success is of
the greatest importance to the state. There are signs
that this idea is being considered in Washington and I
pray that this will result in friendly cooperation for
all rather than in an effort to discourage intelligent
initiative and to put difficulties in the way of those,
both leaders and followers, who are struggling to build
up the true greatness of our country.
The great world war, while probably not nearly
ended, will some day be concluded and the cause of
liberty and decency will surely triumph. When that
time comes and the menace which has been hanging
over the world for many years shall have finally and
completely been destroyed, what is to prevent the
widening of the scope of cooperation so that instead of
applying it to single countries it should apply to the whole
world? There is absolutely no reason whatever why
there should be any jealousy or enmity among nations, if
we once kill the greed for conquest which has been
festering so long in the German heart. Every country
has its own good qualities and every nation has certain
forms of ability different from those possessed by any
other. Why should it be beyond the range of possi-
bility that all of these various peoples should coop-
erate for the general good of the whole world with the
full knowledge and belief that what is good for the
whole world will be good for every nationality in it.
There is no necessity for attempting to make all in
one mold. This cannot be done, and it would not be
desirable if it were possible. Variety is a good thing.
Let us take the best of every one of the peoples of the
world and work with it in earnest cooperation so that
we will extract the most we can of happiness and good
out of our whole planet. The man in Kansas who was
not afraid of the anticipated bombardment of our
coast because the guns did not have long enough range
to reach him, has, I hope, long since learned that "No
man lives for himself alone" and that damage to the
coast means damage to Kansas. Why is it not equally
true, although in a somewhat different sense, that the
tragedies in Armenia and Belgium and Poland and
Russia are felt in every part of the world?
I am not endeavoring to sermonize. I began by
calling attention to the great success of our Society
due largely to cooperation of the right kind. I never
saw any instance in it of anyone trying to feather his
own nest. All the work which has come to my obser-
vation has been done from high motives and the result
is worthy of all that has been done. I have taken
the opportunity to call one force to your attention
which I consider absolutely essential to the successful
development of our civilization. There are thousands
of applications and you can make them for yourselves.
As chemists we are seekers after truth. We realize it
would be the height of folly to distort facts. We have
seen wonderful things happen in the last generation,
and those who are to follow us a generation hence will
see far greater.
Is it not probable that our first president had a vi-
sion of this universal cooperation when he concluded
his inaugural address in these words:
"Let us continue our labor unobtrusively, conscious of the
integrity of our motives, conscious of the portentous change
772
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
which is taking place in the thought of the world, conscious
of the irresistible power which is behind us' Let us not return
railing for railing, but above all, lei us deliver unflinchingly to
others the truths that Nature has delivered to us!
The book of Nature! shall not we chemists, and all our brother
students, whether they be naturalists, astronomers, mathe-
maticians, geologists, shall we not all humbly and earnestly
read it? Nature, the mother of us all, has inscribed her un-
fading, her eternal record on the canopy of the skies, she has
put it all around us on the platform of the earth! No man can
tamper with it, no man can interpolate or falsify it for his own
ends. She does not command us what to do, nor order us what
to think. She only invites us to look around. For those who
reject her she has in reserve no revenges, no social ostracism,
no index expur gator jus, no auto da fit To those who in purity
of spirit worship in her heaven-pavilioned temple, she offers her
guidance to that cloudy shrine in which Truth sits enthroned,
'dark .with the excess of light!' Thither are repairing, not
driven by tyranny, but of their own accord, increasing crowds
from all countries of the earth, conscious that whatever their
dissensions of opinion may heretofore have been, in her presence
they will find intellectual concord and unity."
COUNCIL MEETING
In spite of the manifold activities of chemists in
connection with war problems the 56th Meeting of the
American Chemical Society, held at Cleveland, Ohio,
September 9 to 13, 1018, was considered by all to have
been one of the most helpful meetings held in recent
years. Naturally, war topics were predominant.
The general meetings and the meetings of divisions
were held in the Hotel Statler, the complete registra-
tion for the sessions showing a total of 586 members
present. A unique tone was given to the meeting by
the presence of so many of the members in Army
uniform.
At the opening of the Council Meeting, held in the
rooms of the University Club on Monday afternoon,
Secretary Parsons read a letter from President William
H. Nichols, expressing his regret at being unable to
attend the meeting, because of an accident which now
confines him to his room. A message of greeting and
regret at his absence was telegraphed to Dr. Nichols.
Telegrams of greeting were forwarded, by vote of the
Council, to Dr. T. J. Parker, absent through illness, and
to former President Edward W. Morley, who was pre-
vented from attending by illness in his family.
By rising vote the Council in silence paid tribute to
the memory of the late former President, John H.
Long, and a committee was appointed to draft appro-
priate resolutions.
A communication was read from Chairman Edward
N. Hurley of the United States Shipping Board, which
was ordered printed in This Journal,1 and the President
was requested to appoint a Committee on Merchant
Marine. Dr. Nichols has named the following, the
committee to elect its own chairman:
I)k 1. It BABKBLAND, Yonlcers, New York
Mr Wm Koskins, Room 2009, 111 W Monroe SI . Chicago, 111.
Mk wm I Mathbson, 21 Burling Slip, New York
Mr C. W Merrill, 121 Second Street, s.m Francisco, California
Mr 11 s MrNSR, Welsbach Li^ht Company, Gloucester, N. J.
Mk C W Nichols, Nichols Copper Company, 25 Broad St., N V
Mi 1, D RosBngartbn, P, 0 llox, I62S, Philadelphia, Pa.
The invitation from the Philadelphia Section to hold
the annual meeting of 1919 at Philadelphia, was unan-
imously accepted. The question of holding a spring
meeting in 1919 was referred to the Directors, but the
Council recommended unanimously that no spring
1 Page 864, this issue.
meeting be held if the war is in progress at the time of
making the necessary arrangements.
The petition of the American Defense Society to
request President Wilson to suspend the publication of
German newspapers was circulated informally for in-
dividual signatures, and the response was so great that
extra sheets were needed to accommodate the names.
Miuh interest was attached to the reading, by the
Secretary, of the Report of the Committee of the Rub-
ber Section on the Poisonous Nature of Some Accel-
erators and Precautions Regarding their Use.'
All the editors and associate editors of the So-
ciety's publications were unanimously reelected. Dr.
M. C. Whitaker was unanimously reelected a mem-
ber of the Committee Advisory to the President.
The discussion of the platinum situation aroused
much interest, and upon motion the following resolu-
tions were unanimously adopted by rising vote:
WHEREAS, The Director of the U. S. Mint has, through the
press, issued an appeal to citizens to relieve the shortage of
platinum for munitions manufacture by contributions of platinum
jewelry and scraps, either through sale to the Mint at the Govern-
ment price or by gift to the Red Cross and
Whereas, The Women's National League for the Conserva-
tion of Platinum, and particularly its President, Edith Taylor
Spear, of Cambridge, Massachusetts, have through unremitting
and intelligent efforts created a strong public sentiment in favor
of the conservation of platinum for war purposes, and have by
this patriotic service greatly aided the work of chemists and
manufacturers of war munitions,
Be it Resolved, That we, the Council of the American Chemical
Society, now assembled in Cleveland, Ohio, hereby express our
deepest gratitude to the League and its President for their
educative and patriotic work;
Be it also Resolved, That copies of this Resolution be spread
upon the minutes of this meeting, be transmitted to the Women's
League for the Conservation of Platinum, and be engrossed and
presented to Mrs. Spear.
Following this action a committee consisting of
Messrs. A. V. H. Mory, R. W. Neff, and C. H. Herty,
chairman, was appointed to draft a memorandum to
local sections giving the facts regarding the platinum
question.
Upon motion it was recommended to the general
meeting of the Society that the names of Walther
Nernst, Wilhelm Ostwald, and Emil Fischer be stricken
from the list of Honorary Members of the Society, as
of date of August 1, 1914. A committee was ap-
pointed to draft a statement outlining the reasons
which led to this action, and reported resolutions as
follows:
Whereas, The behavior in war of the German people has
dishonored them among the enlightened nations of the earth
and proved them unlit to associate with civilized men and
women, and
Whereas, Walther Nernst, Wilhelm Ostwald, and Emil Fischer
have been actively associated with the German government and
its people in their conduct and offenses, now therefore be it
Resolved. Tlt.it the names of the s.tid Nernst, Ostwald. and
Fischer be dropped from the rolls as honorary members of the
American Chemical Society, and
Resolved, That this act be construed to take effect as of
August 1, 1914.
The report of the Committee on the Method of Nom-
inating the President of the Society was adopted.
Under the new procedure each local section is invited
to communicate to the Secretary not later than Octo-
ber 15 of each year a name of any member of the
1 For full report sec page 865, this issue.
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
7 73
Society for consideration by the members at large in
voting for nominations. The Secretary is directed to
ascertain whether or not each person so suggested will
accept in case of election. This list of suggestions will
then be forwarded to the membership, and is to be
considered simply in the nature of a suggestion. The
names will be arranged alphabetically, with no indica-
tion of the section which proposed them.
The report of Chairman B. C. Hesse of the commit-
tee to cooperate with the Bureau of Foreign and Do-'
mestic Commerce in obtaining statistics on foreign
commerce in chemicals was read and accepted, and a
special vote of thanks given to Dr. Hesse for his able
conduct of the work of this important committee.
The report is as follows:
As Chairman of the American Chemical Society Committee
to cooperate with the Bureau of Foreign and Domestic Commerce
in obtaining statistics on foreign commerce in chemicals for the
fiscal year 1913-14, and so to determine the extent of our chemi-
cal dependence, I beg to report that the work under Dr. E. R.
Pickrell of the U. S. Appraisers' Stores of the Port of New York
has progressed so far that the manuscript will be ready for the
printer by December 1, 1918. The Bureau of Foreign and
Domestic Commerce has now placed at Dr. Pickrell's disposal
24 persons; upwards of 20,000 invoices of imported chemicals
have been segregated from a total of more than 500,000 general
invoices from all the ports of entry (upwards of 100) in the
United States, Alaska, and Insular Possessions, and these 20,000
invoices of chemicals are now being transcribed on individual
item-cards at the rate of about 1000 invoices per day; these
item-cards will then be suitably assembled and this assembly
then transferred to manuscript form. The information thus
to be given is as follows:
1 — Name of chemical or material of or for chemical industry.
2 — Total of pounds or other quantity units.
3 — Total value.
4 — Countries of origin, arranged in the order of their participa-
tion and showing the percentage of such participation.
This manuscript, which will probably deal with upwards of
4000 entries and will amount to about 300 pages, 41, V x 71 '/' of
print, will be ready for the Government Printing Office not later
than December 1, 1918; how long it will require to print cannot
be foretold, but February 1, 191 9, seems to be a reasonable date
for its appearance; its cost to the public will probably be about
30 cents per copy.
This, therefore, concludes the work of this committee and
I therefore request that it be discharged.
In the course of these activities I have made tentative plans
for the elucidation of these statistics and for their periodical
appearance in the future, but without definite commitments
on the part of the American Chemical Society or of the various
Government agencies consulted. These plans are all based
upon preparation by the American Chemical Society of an
analysis of these 4000, or thereabout, entries, showing for tin-
manufactured and semi-manufactured articles the raw materials,
mineral, vegetable, and animal, and the approximate quantities
of each entering into their production. The Geological Survey
will then prepare a succinct statement as to the location and
production of the mineral raw materials and Dr. Carl Alsberg,
Chief of the Bureau of Chemistry of the Department of Agri-
culture, has offered to enlist that Department's cooperation
through its various bureaus for similar treatment of tin- vegetable
and animal raw materials. The Tariff Commission has been
approached for its cooperation in listing the industrial and
commercial uses of each of these 4000 entries, with prospects
not hopeless.
With such a compilation, as an appendix to the statistics
now approaching completion, it should be possible dependably
and rapidly to ascertain for any manufactured or semi-manu-
factured product the amounts imported, what raw materials
and their amounts were needed, what uses it has in the arts and
also, for any given raw material, information as to what finished
or semi-finished products made from it were imported, their
industrial uses, and the respective amounts of all and each.
Domestic production of raw materials for chemical industry,
semi-finished and finished chemical products should be greatly
stimulated and its growth intelligently directed through such a
compilation, the successful making of which is beyond the
strength of any one man or group of men as has been conclusively
demonstrated by occasional abortive efforts abroad. I have
also considered compiling information of similar scope and char-
acter for our exports and for our domestic production and have
concluded that for the present, at least, such is not only un-
necessary but without merit, for these would only confuse since
they do not show the extent of our dependence.
I have every reason to believe that if the American Chemical
Society will appoint a committee to make the analysis of this
set of statistics now nearing completion as above outlined
and this committee will cooperate in the preparation of the chap-
ters to be built up on this analysis and those statistics, the
effective and enthusiastic cooperation of the Geological Survey,
the Department of Agriculture, and the Tariff Commission
will be forthcoming.
In the course of the past 18 months I have discussed this
matter most thoroughly with many persons and I believe that
the American Chemical Society should appoint such a com-
mittee and further empower it to act as a "buffer-committee"
or "clearing house" to receive all suggestions from the chemists
of the country as to betterments or alterations for succeeding
issues, if any; to consider all such, and then, at such times as
the Bureau of Commerce may request, to transmit all such
suggestions to that Bureau together with that committee's
recommendations for appropriate incorporation into future
editions or issues, if any.
I have further reached the conclusion that this committee
should have an active, but ex officio, nucleus with power to add
to its number not only from the American Chemical Society,
but to invite cooperation of other societies. The nucleus I
have in mind is
Chairman: Editor of the Journal of Industrial and Engi-
neering Chemistry or its successor publication of the American
Chemical Society. Other members: Vice Presidents of the
American Chemical Society. This committee might be
designated "Committee on Import Statistics."
In summary, then, I suggest:
(a) that the present committee be discharged;
(i) that a new committee as above constituted and em-
powered be appointed;
(r) that corresponding action be taken by the council at
the Cleveland Meeting of the American Chemical
Society,
so that firm commitments can be entered into and discharged
at once.
Bernhard C. Hesse
August 2'), 1918 Chairman
In pursuance of the recommendations contained in
tin- above report the following motion was unanimously
pa ■
That a committee, to be known as the Committee on [mporl
statisti, I- en ited; that it shall be composed of the Vice
i ol tin- American Chemical Society and the Editor
ol 'I., Journal OF Indi'striai. and Engineering Chemistry,
thi I'M, 1 to in- Chairman of that committee; this committee <•■
have power to add to its number and also to invite cooperation
774
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
of persons not members of the American Chemical Society
and also the cooperation of societies other than the American
Chemical Society; this committee to cause to be prepared suit-
able analysis of Federal Government statistics and to cooperate
with the Bureau of Foreign and Domestic Commerce in the
editing and publishing thereof, to solicit the aid of and to co-
operate with other Governmental departments, bureaus, or
commissions in further elucidation of those statistics, as well
as the periodical or other publication of such information in
such manner as may be agreeable to the Bureau of Foreign and
Domestic Commerce or any of the Governmental branches that
are cooperating, all of which to be along the general lines set
forth in the report of the committee to cooperate with the
Bureau of Foreign and Domestic Commerce in obtaining
statistics on foreign commerce in chemicals for the fiscal year
19l3-i9>4 and dated August 29, 1918.
At a subsequent meeting of the ex- officio members
of this committee, the name of Dr. B. C. Hesse was
added to the committee.
Lieutenant James Kendall made an interesting re-
port of progress as chairman of the committee to
consider with representatives of the English chemical
societies, at their request, the question of the coop-
erative publication in the English language of compre-
hensive reference works on organic, inorganic, and
physical chemistry. As Lieut. Kendall has returned
to this country the work has been put in the hands of
Dr. H. S. Taylor, chairman, Professors J. H. Donnan
and H. B. Baker, and Dr. George Senter, members of the
American Chemical Society resident in England, who
will consult with members of the English societies and
later report.
A hearty vote of thanks was passed for courtesies
extended by the several local committees, the Univer-
sity Club, and all institutions and organizations which
contributed to the entertainment of the visiting mem-
bers.
On adjournment the Council was delightfully enter-
tained at dinner at the University Club by the Cleve-
land Section.
GENERAL MEETING
On Tuesday morning the first general meeting was
held in the ball room of the Hotel Statler. Professor
A. W. Smith, Chairman of the Local General Com-
mittee, welcomed the members of the Society to Cleve-
land, calling attention to its increase in size and indus-
trial importance since the earlier meeting of the Society
there, and to its growing importance as a chemical
center.
In the absence of President Nichols, Mr. H. S.
Miner, Chairman of the Division of Industrial Chem-
ists and Chemical Engineers and senior Vice President
of the Society, presided, and responded on behalf of
the Society as follows:
I feel that I owe the members of the American Chemical
Society assembled here an explanation and apology. Dr.
Nichols, whom you had expected to see in the chair to-day, is
unable to be present on account of a serious and painful acci-
dent, and a telegraphic word of greeting has been sent him
by the Council, with best wishes for a speedy and complete
recovery.
The senior Chairman of Divisions must, under the Con-
stitution, preside at the general meetings in the absence of the
president. So I am here through no fault of mine. About a
year ago I was elected vice chairman of a division, and through
the resignation of Dr. William H. Walker upon his entry into
the country's service, I was automatically promoted to the
chairmanship.
Conventions are important and even necessary. It had
been thought that possibly conventions should be dispensed with
during the period of the war, but upon sober second thought it
was considered that there was an even greater need for meet-
ings of this character than in peace times. Possibly they should
not be as frequent. The Spring Meeting was dispensed with,
but this Annual Meeting certainly is important, and we are
glad to see so many here at the opening session. We had feared
that there might not be this large attendance, but the need of
mutual aid and cooperation has never been as great as at the
present time. We find it necessary to know each other better
and more intimately; we find it to our advantage to know how
we can help each other. This need of cooperation therefore
seems to me to be the reason why we are gathered in such num-
bers, and I am glad to see that this spirit of cooperation is so
strongly in evidence. A recent writer, speaking of the enemy,
stated that his intelligence is highly developed along scientific
lines, but that he is utterly devoid of spiritual cooperation.
I am glad, therefore, that we are showing this spirit. The Society
has been known in the past for its cooperative work, but we
have now added to this the spirit and desire to cooperate not
only with each other, but with our Government and its Allies
for the benefit of humanity. Witness the many members of
this Society who are now directly connected with the Govern-
ment, and the many more who are indirectly, but no less effec-
tively, aiding in the present crisis. And I wish to say that I
believe that this is at a sacrifice, I nearly said a sacrifice of
personal ambition, but ambitions are being shown in an entirely
different direction. We are now anxious to know what we can
do, how we can do it, antl do it quickly and well.
We are glad to be here in this city to-day. We are glad to be
entertained in a community that is noted for its civic pride, and
especially in these days are we glad to be in a community that
is doing so much for our country, and we appreciate the privilege
of meeting these splendid men who are serving their country
here. It is not easy for a local committee to arrange for a large
gathering of this kind. We appreciate that the work has been
arduous, but the splendid program and the many items of
interest tell us how well this work has been carried out.
Secretary Parsons announced that Assistant Sec-
retary of War Benedict Crowell was unable to leave
Washington, speaking as follows:
I am sorry to have to present to you the regrets of the
Acting Secretary of War, who is unable to be here this
morning. We seem to have been entirely unfortunate, but
"C'est la guerre." Dr. Nichols is unable to be present. When
I saw Assistant Secretary Crowell he told me that Cleveland was
his home city, that he had been a member of our Society for some
years past, and that he would address us this morning. I knew
he hoped and expected to be here, but as Secretary Baker was
then on the water, he felt that he might have urgent duties there
in Washington. I will read you his wire.
"Secretary Baker is in France and certain important matters
must be acted on by War Department to-morrow. It will
therefore be impossible for me to join you in Cleveland as
planned. Very sorry.
Benedict Crowell
Acting Secretary of War"
I am sure he is not sorrier than we are that he cannot be present,
and I should like to add for the information of you all that
Secretary Crowell has been from the outset very" influential and
very sympathetic toward the work which chemists can do to
help win this war, and the organization owes a great deal to
Secretary Crowell for the sympathetic attention he has given
to the chemical needs of the War Department.
Oct., 1918
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
775
Scene in the Ballroom i
is Hotel Statler on Tuesday Night when 423 Delegates. Members
Guests Dined Together Informally
Before beginning the reading of the papers Secretary
Parsons reported the resolutions from the Council recom-
mending the striking from the list of Honorary Members
of the Society the names of Professors Walther Nernst,
Wilhelm Ostwald, and Emil Fischer. Upon motion
the recommendation of the Council was adopted by
unanimous vote.
By another unanimous vote the general session
adopted the resolutions of appreciation of the work of
the Women's National League for the Conservation of
Platinum.
Great interest was manifested in the series of general
papers bearing upon the various phases of the chem-
ist's share in the war program. These papers are
printed in full, pages 776 to 788, this issue.
At the afternoon session attention was given to
the Symposium on the Chemistry of Dyestuffs,
which had been arranged by Mr. R. Morris Shreve,
who presided at the meeting. A report of the papers
presented will be found, pages 789 to 805, this issue.
In the informal discussion which followed the comple-
ktion of the symposium the consensus of opinion seemed
to point to the need of organization of a Dyestuff Sec-
tion of the American Chemical Society, and im-
mediate steps will be taken to this end.
In the evening an informal dinner was held in the
same room in which the general meeting had been
held, 423 members and guests being present. During
the dinner a telegraphic toast was read from President
Nichols: "The American chemist, first in war, first in
peace, and first at the top and bottom of everything,"
which was received with much enthusiasm.
At the conclusion of the dinner the ladies departed
for a theatre party tendered them, while the
men remained for the complimentary smoker, which
began with the singing of patriotic songs. During the
evening addresses were made by Mr. T. S. Grasselli,
Mr. H. H. Dow, Colonel G. A. Burrell, Dr. Charles L.
Reese, Professor C. F. Mabery, Lt. Col. W. D. Ban-
croft, and Dr. Dayton C. Miller, Secretary of the
American Physical Society.
Throughout Wednesday and Thursday divisional
meetings were held, with large attendances and active
discussions. The official program of each of the Divi-
sions is printed in the Scientific Societies column of
this issue. In the afternoons the members broke up
into groups and visited the water filtration plants, the
Cleveland iron and steel industries, the laboratories of
Oberlin College, Western Reserve University, and the
Case School of Applied Science.
On Wednesday evening the President's address, in
theabsenceof President Nichols, was read by Dr. Charles
H. Herty. Following the reading of the address an
informal reception was held.
The members were delightfully entertained on Thurs-
day at dinner by the Grasselli Chemical Company, at
the Country Club on the Lake Shore, and in the eve-
ning a visit was made to the Cleveland Museum of Art,
which was courteously opened to the members of the
Society by its Director.
With the regular program completed, Friday was
devoted to excursions to Akron, Ohio, where the plants
of the Goodrich Rubber Co., the Knight Chemical
Stoneware Works, and neighboring potteries were vis-
ited. Another Friday excursion consisted of a visit to
Wadsworth, where the plants of the Ohio Brass Works,
the Ohio Salt Works, and the Ohio Match Works were
inspected, the latter company tendering a complimen-
tary luncheon to the visitors.
As we look back upon the delightful week spent in
Cleveland it seems clear that this meeting of the So-
ciety, held in the midst of such critical times, has been
well worth while. It showed a harmonious working
together of American chemists; it demonstrated the
vigorous life of the American Chemical Society; it
stimulated in all the determination to give to this
country the utmost within the power of its chemists.
776
THE JOl RNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
CHLMI5T5 IN WARFARE
Papi
.III . ti at Hi. ...Hi Ml
of the American Chemical Society. Cleveland. Scpte
THE AMERICAN CHEMIST IN WARFARE
By Chari.es L. Parsons
Chairman, Committee on War Service (or Chemists
It was the fortune of the- writer in the latter part of 1916, a
few months before the United States entered the war, to be senl
by the Ordnance Department to study in England, France,
Italy, Norway, and Sweden certain chemical processes, par-
ticularly those having to do with the fixation of nitrogen.
On this trip many chemical plants were visited. In all of them
the same story was told of depleted chemical personnel owing
to the loss of chemists in the trenches and the consequent handi-
cap under which all of these plants were laboring in their at-
tempts to furnish the armies with the sinews of war. The whole
munitions program had been retarded owing to lack of technical
men, chiefly chemists, and the statement was everywhere made
that the greatest mistake that the Entente countries had made
had been in giving too little attention to brain power and too
much to physical strength. On the other hand, it was pointed
out that Germany had carefully conserved her chemists for the
development of the new and terrible forms of warfare she was
forcing on mankind. Science was being used as it had never
been used before, to aid a relentless power, and the only means
of combating the new form of warfare was with its own weapons.
Already France, England, Italy, and Canada had withdrawn
all chemists remaining in the service for chemical duty at home,
but many had already been lost and their loss was seriously felt.
France had drawn so far as possible on the chemists and engineers
of Norway, and England drew on her colonies. Indeed, the chem-
ist who perhaps more than any other in England is responsible
for the success of England's munitions program is an American;
and several English chemists who were living in America returned
to England for chemical duty.
With this example in mind, the Director of the Bureau of
Mines and the Secretary of the American Chemical Society
called on the Director of the Council of National Defense, and
after consulting with him, at his official request, undertook to
obtain a census of American chemists for use in the war that was
already imminent. This census was started in February 1917,
and has been kept up uninterruptedly to the present time. By
July 191 7, some 15,000 chemists had sent in full data as to
their address, age, place of birth, lineage, citizenship, depend-
ents, institutions from which graduated, chemical experience.
experience in foreign countries, affiliations with technical soci-
eties, military training, publications, research work performed,
and other data of importance. The list has been contin-
ually added to, questionnaires being sent to every new name
of a chemist that could be obtained. While the list is not com-
plete, owing to the fact that some chemists, no matter how
carefully followed up, will not reply to letters, nevertheless, the
data are comprehensive and as complete as they can be made.
The cooperation between the Bureau of Mines and the AMERI-
CAN Chemical Society was perfect. The Bureau furnished its
whole statistical force ami the Society put special clerks at work.
The data obtained were indexed and cross-indexed on some
28,000 cards When America entered the war every chemist
was directed to keep the Society informed as to his military
status, and continual correspondence wa-. carried on by the
Society direct with officers and privates in order that the ehem
ists of the country might serve the country in the best possible
manner. To day the list consists of some 1 7,000 tilled out ques
tionnaires, 12,020 membership cards ol the American Chemi-
cal Society, and some 3,000 cards of bona fide chemists actually
in war sum,., most of them in uniform. A caul list is Wept of
officers and enlisted 1111 11 who are graduate chemists in the
United States Army in America; another list of those in France,
including both those in chemical service and in the Army and
Expeditionary Forces not yet transferred to chemical service,
and another list of those in the Navy. It is believed these lists
are reasonably complete and up to date.
This work has involved an expenditure of many thousands
of dollars, the writing of over 10,000 personal letters, and the
sending of over 50,000 circular communications to the chemists
of the coun try-
Already in the early part of February 19 17,1 the President of
the American Chemical Society, Dr. Julius Stieglitz, had
offered without reservation the services of the members of the
American Chemical Society to President Wilson in any emer-
gency that might arise and had received an appreciative reply.
On February 15, 191 7, a similar communication was addressed,
by direction of the President, by the Secretary of the Society to
the Secretary of War; and on April 11, 1917, at the Kansas City
meeting of the American Chemical Society, the following
resolutions were passed, which were widely circulated, and had
a profound effect on the mental attitude of American chemists:*
Resolved, That we reaffirm the tender to the President of the
United States of the services of the members of our Society in
all the fields in which we are qualified to act.
That the security and welfare of the country' demand the
organization of all the men and facilities of the United States,
so as to insure the greatest possible service and value for each.
The progress of the war thus far principally teaches us that
modern warfare makes extraordinary demands upon science,
food supply, and finance.
For the protection and success of our men under arms we
recommend the use, in their respective fields, of all trained
chemists, physicists, and medical men, including advanced
students of these subjects.
To this end, in collaboration with the United States Bureau
of Mines, we are preparing a census of chemists. With no
desire to avoid field service for men of training in the professions
named, we urge that those of special ability be held to the work
they can best perform. Thus we may avoid unnecessary loss
from lack of control of the tools and requirements of war.
We hold that the use of platinum at this time in the production
of articles of ornament is contrary to public welfare. There-
fore, we recommend that an appeal be made to the women of
the United States to discourage the use of platinum in jewelry
and that all citizens be urged to avoid its use for jewelry', for
photographic paper, and for any purpose whatever save in
scientific research and in the making of articles for industrial
need.
A committee consisting of Dr. W. H. Nichols, Dr. M. T.
Bogert, Dr. A. A. Noyes, Dr. Julius Stieglitz, and Dr. C. L.
Parsons had, in June 191 7, drawn up and presented a report on
"War Service of Chemists" and "A Plan for the Impressment
of Chemists and for the Preservation of the Supply of Chem-
ists."3 Several important editorials by Dr. Chas. H. Herty
and communications to the chemists of the country advising
them as to their procedure had appeared in This Journal. Vol.
9 (1917), pp. 332, 730, 826, 1085, and 1 128; Vol. 10 (1918),
pp. 2, 3, 95. 234, 235, 580.
That the wisdom of carefully listing the chemists of the
country more than warranted the expenditure and effort
has been apparent from the first . The war had scarcely
begun when the growth of the Ordnance and other depart-
ments developed a tremendous demand for chemists, first
to obtain chemical information from the other side, and soon
to develop information on this side. A large part of the chem-
ists now in war work were obtained and classified from this list
The offices of the Bureau of Mines and of the American Chem-
ical SOCIETY were the scene of continual conferences regarding
chemical personnel and the development of chemical warfare
1 Tins Journal, 9 (1917), ::4.
'Ibid, 444.
3 Ibid., 639.
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
777
Practically all of the chemists who early entered the Ordnance
Department in a commissioned capacity were either obtained
through the American Chemical Society or passed upon by its
officers. When the Bureau of Mines began its investigation on
gas warfare the list was invaluable, and representatives from
practically all of the bureaus and departments in Washington
consulted it from time to time as their needs increased.
When the chemists were later drafted into the Army this
census served as a basis for determining their qualifications,
which later, through the far-sighted assistance of Assistant Secr
retary Crowell, resulted in chemists being withheld for chemical
service.
From the first the chemical personnel of the Army and Navy
and the civilian bureaus was partly civilian and partly military.
As the war progressed the proportion of chemists in uniform
naturally increased as the men were taken from the Army and
assigned to chemical duty. The question is still a disputed one
—to be settled probably only when the war is over — as to whether
a chemist can serve best in a civilian or a military capacity.
Certainly in both capacities the demand for chemists has been
unprecedented and the development of chemistry in modern
warfare to those in touch with the advancement made seems
almost a fairy tale.
The first requirement for chemists in quantity in Washington
was in connection with gas work organized by Director Van.
H. Manning and carried on by the Bureau of Mines with its own
funds until July 191 7, after which, steadily increasing funds were
furnished to it by the Army and Navy. The gas research work
was located at the Bureau of Mines Experiment Station some
4 miles from the center of the city of Washington.
A branch laboratory of the Bureau of Mines was also estab-
lished at the Catholic University, Washington, and other branch
laboratories and cooperative research work carried on at such
institutions as Johns Hopkins, Harvard, Yale, Princeton, Ohio
State, Wisconsin, Washington, Kansas, Michigan, Columbia,
Cornell, California, Rice Institute, Iowa State College, Bryn
Mawr, Massachusetts Institute of Technology, Worcester Poly-
technic, etc. Also special problems were undertaken by the
National Carbon Company and the National Electric Lamp
Association, as well as by chemists and laboratories of many of
our other important chemical corporations.
One of the most interesting features of this work was the
spirit shown by American chemists and the immediate response
made by practically every chemist in America to the call to
duty. The organization was rapidly built up and contained the
names of the most prominent chemists in the country, as well as
those of hundreds of young chemists who will later become
prominent.
When this organization was taken over by the Chemical War-
fare Service in June 191 8, there were over 700 chemists at work
on problems having to do with gas warfare, the design of gas
masks, protection against toxic gases, development of new gases,
and the working out of processes for those already used, the
details of incendiary bombs, smoke funnels, smoke screens,
smoke grenades, colored rockets, gas projectors and flame
throwers, thermal methods for combating gas poison, gases for
balloons, and other materials directly or indirectly connected
with gas warfare.
This body of chemists reporting to Colonel G. A. Burrell had
nearly 11 00 helpers in the way of clerical force, electricians,
glass blowers, engineers, mechanics, photographers, and labor-
ers, so that when it became a part of the Chemical Warfare
Service some 1800 persons were transferred, of whom over 700
were chemists — among them the leaders of the profession. At
the same time the gas defense operations of the Medical Depart-
ment under Colonel Bradley Dewey, consisting chiefly of the
large scale manufacture of gas masks and gas mask chemicals,
the gas offense proving grounds under Major William S. Bacon,
and the gas defense training under Major J. H. Walton were
also transferred to the new Chemical Warfare Service. The
story has been told in detail in the September number of This
Journal and need not be repeated here.
Shortly after this work of the Bureau of Mines was begun the
development of the Ordnance and Medical Department created
an additional demand for chemists. The Chief of the Trench
Warfare Section, Lt. Col. E. J. W. Ragsdale, early called for
chemists to go to England and France in a commissioned capac-
ity to obtain necessary information. Soon other chemists were
required for the planning and building of gas plants and the
manufacture of chemicals. The Trench Warfare Section con-
tinued this work in greatly increasing personnel until the early
part of 1918, when the Chief of the newly formed Chemical
Service Section was transferred to the Ordnance Department
and given charge of the production of chemicals for gas warfare.
A new arsenal known as Edgewood Arsenal was established for
this purpose. Hundreds of chemists and engineers were em-
ployed, and the Arsenal had become almost a city in size, with
enormous plants ready for operation, when it too was transferred
from Ordnance to the newly organized Chemical Warfare Ser-
vice, in June 1918.
It was a real epoch in the history of chemistry in warfare
when, as a result of conferences held at the Bureau of Mines
with officers from the Medical Corps, War College, General
Staff, Navy, and civilian chemists, the Chemical Service Section
was established as a unit of the National Army, with Lt. Col.
Wm. H. Walker, formerly of Massachusetts Institute of Tech-
nology, as chief of the American branch reporting to Colonel
Potter of the Gas Warfare Division, and Lt. Col. R. F. Bacon
as chief of the Chemical Service Section in France reporting to
Col. A. A. Fries, head of the Gas Warfare Division overseas.
This was the first recognition of chemistry as a separate
branch of the military service in any country or any war.
Later, Col. Walker, as before stated, was transferred to the
Ordnance Department, and was replaced by Lt. Col. M. T.
Bogert. The latter was in charge of the American branch of the
Chemical Service Section at the time this Section, together with
all of the gas research laboratories and personnel of the Bureau
of Mines, and the plant and field operations of the Ordnance
and Medical Departments pertaining to gas warfare, were united
under Major General William Sibert, under the new title of
Chemical Warfare Service.
It cannot be brought out too strongly that the Chemical
Service Section of the National Army was the first organized
military body established for the sole purpose of relating chem-
istry to warfare. It took as an insignia the old alembic of
alchemy joined with the theoretical benzene ring which has so
greatly accelerated the development of modern chemistry. It
further adopted for its colors those of the American Chem-
ical Society — cobalt-blue and gold.
The Chemical Service Section was of very great service, espe-
cially in systematizing the regulations of the War Department in
regard to chemical personnel, and the status of chemists was
ably defined through its influence, in the Order of May 28, 1918.
On account of its historical importance this Order is quoted
here.1
1 — Owing to the needs of the military service for a great many
men trained in chemistry, it is considered most important that
all enlisted men who are graduate chemists should be assigned
to duty where their special knowledge and training can be fully
utilized.
2 — Enlisted chemists now in divisions serving in this country
have been ordered transferred to the nearest depot brigade.
3 — You will make careful inquiry into the number of graduate
chemists now on duty in your command and report their names
to this office. The report will include a statement as to their
special qualifications for a particular class of chemical work,
and whether they arc now employed on chemical duties.
1 This Journal, 10 ( 1918). 580.
778
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No.
4 — Enlisted graduate chemists now in depot brigades, or
hereafter received by them, will be assigned to organizations or
services by instructions issued from this office. The report
called for in paragraph 3 herein will be submitted whenever men
having' qualifications for chemical duties are received by depot
brigades, or replacement training camps, or by the training
camps organized by the various staff corps.
5 — Enlisted men who are graduate chemists will not be sent
overseas, unless they are to be employed on chemical duties.
Prior to the departure of their organization for overseas duties,
they will be transferred to the nearest detachment or organiza-
tion of their particular corps.
6 — The Chief of the Chemical Service Section will be charged
with the duty of listing all American graduate chemists, in-
cluding those in the Army and those in civil life.
7 — Whenever chemists are needed by one of the bureaus or
staff corps, request will be made on the Chief of the Chemical
Service Section for recommendation of a man having the quali-
fications necessary for the particular class of work for which he is
desired. If men having chemical qualifications are wanted for
only a short period of duty, they will be temporarily attached
to the bureau or staff corps; where the duty is of a permanent
nature, instructions covering their transfer will be issued.
Whenever the chemists, thus attached or transferred, are no
longer needed for purely chemical duties, a report will be made
to the Chief of the Chemical Service Section in order that they
may be assigned to chemical duties at other places.
By order of the Secretary of War
Roy A. Hill
Adjutant General
These regulations have since been enlarged so that at present
chemists may be furloughed back from the Army to colleges for
instruction purposes or to industrial works for essential chem-
ical production. Students may be continued in chemical courses
to meet the future need for chemists, and any chemists in the
Army may be assigned to war work wherever needed. All this
has been done not for the sake of the chemists but on account
of the scarcity of trained chemists and the great need of the
country for their services as chemists to help win the war.
Without chemistry to-day the continuation of the war would
be impossible.
A summary, necessarily brief, of the departments and bureaus
utilizing chemists may be taken up in the following order:
I— ARMY
A GENERAL STAFF
Executive Division, Chemical Warfare Service — This branch
of the service established by General Order No. 62, already
published in the chemical journals, is in command of Maj. Gen.
William Sibert of the Engineers. It has, according to the
Order above referred to, full charge of all phases of gas war-
fare, including research, manufacture, shell filling plants, and
proving grounds. It also continued the functions of the
Chemical Service Section with increased authority.
All newly drafted chemists are assigned to the Chemical War-
fan- Service to be detailed or transferred or furloughed where
needed. It is charged with the "responsibility of providing
chemists for all branches of the Government and assisting in the
procuring of chemists for industries essential to the success of
the war and Government."
It has an authorized personnel of 45,000, of which any por-
tion may be chemists if needed. At present there are approx-
imately 1400 graduate chemists in the Chemical Warfare Service.
It is unnecessary at this time to speak fully regarding the per-
sonnel or work of the Service, as this has been published in
some detail in the September issue of This Journal.
B ORDNANCE DEPARTMENT
(a) Engineering Division, Explosives Section — Under the direc-
tion of Col J 1'. Harris, this Division has 10 commissioned and
6 civilian chemists. This Section concerns itself with the solu-
tion of all engineering problems connected with propellants, the
loading of high explosives into shells, trench warfare containers,
primers, the research in high explosives, the investigation of
explosives submitted for testing, efficiency of methods of manu-
facture, and the carrying out of tests for developing substitutes.
(6) Procurement Division, Raw Materials Section — The Chemi-
cal Branch of this Division under the direction of Maj. W. H.
Gelshenen utilizes the services of 5 officers whose experience
has been chiefly on the commercial side of chemical industry.
(c) Inspection Division, Explosives Section — The chemical work
of this Division is under the direction of Maj Geo. B. Frank-
forter, who has a personnel of somewhat more than 1000 chem-
ists under his direction. Maj. Moses Gomberg is supervisor of
special process work. The chemists are divided into three grades
— "inspectors" who are responsible for all powders meeting
specifications; "analytical chemists" who analyze and test all
powders and report results to inspectors; "linemen" who are
control chemists having charge of certain steps in the process of
manufacture.
These chemists are employed throughout the United States
at explosives plants, chiefly inspecting processes of manufacture
and the finished product. The Section maintains an Officers'
Training School at Carney's Point for training for inspection,
testing, and process control of explosives. Graduates of the
school are, in a few instances, commissioned; otherwise they are
retained in a civilian capacity. There is a tendency to place
all men in uniform as rapidly as possible. There has been such
a demand for chemists that most of them have not finished the
training before being given experience in the plants, so that
they are obtaining their training and experience at the same
time, with the expectation of returning to the school for more
theoretical work before graduation.
The school at present has 150 chemists taking training with
from 6 to 10 instructors. The training consists of an extensive
review of organic and inorganic chemistry, chemical engineer-
ing, including mechanics and plant operations; also a review of
physics and a special study of the chemistry of explosives both
in the laboratory and in the plant. The school has good labor-
atory facilities and a school day of 10 hours. Civilians who are
taken into the school are paid at the rate of $1500 to $2000 from
the time they enter.
Recently a supervisory and control laboratory with 20 chem-
ists has been established in Philadelphia for the purpose of
making control analyses and investigating certain problems hav-
ing to do with the inspection of explosives.
(d) Inspection Division, Metallurgical Section — This Division
employs 79 chemists, 23 being in uniform. The work is in
charge of Major A. E. White, and laboratories are maintained
at 25 of the leading steel plants of the country, with the central
control laboratories in the buildings of the Bureau of Mines at
Pittsburgh. Also, two chemists are working in the laboratories
of the Bureau of Standards for this branch of the service. With
the exception of the central control laboratory and the work at
Standards, the work of this section consists chiefly of the anal-
yses and control of ferrous products.
(e) Production Division: (1) Explosives Section; (2) Raw Materials
5e<7ion— This work is under the direction of Major E. Moxham,
with Major C. F. Backus in charge of the Explosives Section
and Major M. S. Falk in charge of the Raw Materials Section.
The Section numbers among its personnel 18 chemists or chem-
ical engineers engaged in executive and administrative work on
the production of smokeless powder and high explosives. The
Section has no laboratory facilities, the work accomplished being
chiefly in facilitating increased production through specializing
in the various works on manufacturing problems.
The Division has been concerned with the investigation of
new processes for the production of raw materials, some of which
have been put into operation, especially the production of toluene
by the cracking of petroleum. The Raw Materials Section
arranges for the production and distribution of raw materials,
such as nitric acid, sulfuric acid, benzene, phenol, ammonia, and
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
779
sodium nitrate. Besides investigating new processes, the sec-
tion studies increased production and distribution of supplies.
For the main part the chemical personnel is on duty at various
plants investigating production and processes.
(/) Nitrate Division — Colonel J. W. Joyes is in charge of this
Division, with Lt. Col. A. H. White in charge of the Research
Technical Section. The Nitrate Division was organized shortly
after war began with the special duty of installing plants for the
fixation of air nitrogen. It now has a personnel of 130 chem-
ists and chemical engineers, enlisted and commissioned. It has
only a few civilian chemists in its employ. It has cooperated
with and received help from the laboratories of the Massachu-
setts Institute of Technology, the Geophysical Laboratory, the
University of Michigan, the Bureau of Soils (Arlington), the
Bureau of Standards and the Bureau of Mines. It has built
extensive works at Sheffield, Alabama. It has a small ex-
perimental plant at the Georgetown Gas Works, and another
at Greene, R. I. In cooperation with the Bureau of Mines, it
carried on experiments on ammonia oxidation at Syracuse, N.
Y., and at Warner's, N. J. The Division is one of the most
important from the chemical development standpoint that has
been established for war purposes. It has very large appropri-
ations at its disposal and it has two nitrate plants in Ohio in
preliminary stages of erection. It contemplates other activities
in nitrogen fixation.
The Ordnance Department also runs four arsenals — Picatinny,
Watertown, Frankford, and Rock Island — in all of which chem-
ists are regularly employed. The number of chemists in the
arsenals has been largely increased since the war began. No
figures are at the moment available.
c — quartermaster's corps
The chemical work of the Quartermaster's Corps involves the
testing and analyses of materials, foods, leather, paper, etc., the
making of specifications, and the control of materials to find if
the specifications are complied with. The Corps has few chem-
ists in uniform, as the work has been done chiefly in the labor-
atories of the Bureau of Chemistry.
The filtration plants at the various Government camps and
cantonments are also under the control and direction of the Quar-
termaster General.
D SURGEON GENERAL'S OFFICE
Food and Nutrition Division, Medical Department, Sanitary
Corps — This division has 91 food and biological chemists
who are in uniform. In each camp there is stationed one nutri-
tion officer who is preferably a food expert with as much physio-
logical, biological, and sanitary training as possible. His duty
is to inspect all food, mess halls, refrigerators, etc., with the
object of maintaining a high degree of sanitation. He has full
authority to see to it that meat, for example, is destroyed if
dropped upon the ground in hook worm territory; also any other
food that could in any way injure the health of the men. There
are 3 survey parties in the Sanitary Corps whose duties consist
in going from camp to camp getting information regarding
garbage and collecting data on nutrition problems. This is put
in the form of curves in the Washington office. The work is
part of an extensive nutritional study and is expected to give
important results for future use as well as for present Army needs.
Research, with reference to the physical properties of various
proteins, crcatin, etc., is being carried on for the Corps in the
laboratory at Cambridge under Dr. Henderson. Research rela-
tive to rope disease in bread, catalytic action in relation to yeast
activity, etc., is progressing, from which valuable results arc
already in sight. At the Harriman Research Laboratory the
special problem is meat spoilage. It is hoped it will be possil Ii
to detect incipient spoilage by chemical means. At the Bureau
of Chemistry, Department of Agriculture, members of the Sani-
tary Corps are working on garbage research and making a
survey of all food furnished to the various camps. An examina-
tion is made of all garbage cans in order to determine how much
of the food finds its way into the stomachs of the men. This
has resulted in a great saving of food material.
At the University of Rochester investigations have been made
as to the effect of temperature in desiccated vegetables, as it is
thought high temperatures used in desiccation may tend to
induce certain diseases, such as scurvy, pellagra, beri beri, etc.
A safe temperature is being studied. Independent investiga-
tions bearing upon the work of the Sanitary Corps are being
carried out in the Bureau of Chemistry.
The Sanitary Corps maintains a school for the training of
nutrition officers at Fort Oglethorpe, in connection with the
Medical Officers' Training School. Men sent to this school are
selected from the standpoint of training and experience in
food and nutrition work, together with biological training.
Frequently the men are commissioned before entering the school,
if they have had sufficient training, although in certain in-
stances privates have entered the school and been granted
commissions later.
E ArRCRAFT PRODUCTION
This Bureau now requires the services of 51 chemists in two
sections. There is the Section of Chemical Research under
Dr. H. D. Gibbs, who has 18 chemists (13 in uniform) engaged
specifically in research problems, plant operations, study of new
materials, chemical processes, methods of making new chem-
icals required in airplane construction, etc. Interesting studies
are also being conducted on certain photographic sensitizing
dyes to be used in airplane photography. This Bureau also
maintains in Pittsburgh an inspection and control laboratory
employing 33 chemists, 5 in uniform and 28 civilians. This
laboratory has 60 technical men, of whom 30 are chemists.
These chemists were afforded space in the Bureau of Standards
until April 1, when they were removed to the home of the Pitts-
burgh Testing Laboratories, Pittsburgh, Pa. The work is in
charge of Dr. H. T. Beans. The laboratory has general control
of all products purchased by the Aircraft Production Board; it
develops specifications for new materials and sends chemists into
the plants to get the grades of materials wanted.
II— NAVY
The Navy also requires chemical aid in warfare, and at the
present time has approximately 200 chemists engaged chiefly
in control work and plant operation. Each of the Navy Yards
has a control laboratory and the Ordnance Bureau has about
100 chemists, of whom approximately 20 are commissioned, 35
enlisted, and 50 civilian. These are utilized in much the same
capacity as in the Army Ordnance.
From the first the Navy has immediately transferred to Chem-
ical Service the names of all chemists enlisted in the Navy, where
the names and qualifications have been made known to them.
While of course the total number is small, the proportionate
need has apparently been greater, for there are still several
hundred graduate and experienced chemists and chemical engi-
neers, both officers and men, in the Navy, a large proportion of
whom have expressed their willingness to serve as chemists if
needed, but who are still in the fighting branch or whose duties
have no relation to chemical service.
Ill— CIVILIAN BUEEAUS
The Bureau of Chemistry, the Forest Products Laboratory
and other Bureaus of the Department of Agriculture, the
laboti " Ol thi Bureau of Mines, Bureau of Stand-
ards, and of the Treasury Department have all cooperated
with their full force in any war problems presented to them.
Many of these problems have originated and been carried to a
iul conclusion within the bureaus themselves, The ci-
vilian personnel of the bureaus has been depleted in almost every
780
Till: JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
by the war, but men have been assigned by the War
Department to assist in war problems. For example, the
Bureau of Standards at present has 70 men in uniform assigned to
it from various branches of the Government. These are for the
main part engaged on studies of new methods of analysis, re-
search on analysis of special materials, analysis of Government
supplies, and development of airplane dopes, and study of new
and improved specifications on Government supplies. The
studies of electroplating with reference to Government m
the study of the physical characters of alloys have been taken up.
The truly extensive chemical work of the civilian bureaus
and their relations to war work will be published in detail at
some future time
IV— COMMITTEE ON CHEMICALS. CHEMICAL ALLIANCE
WAR INDUSTRIES BOARD
In the very early days of the war, the Committee on Chem-
icals, headed by Dr. Win. H. Nichols, president of our Society,
and consisting of the leaders of our chemical industries, gave
unstinted and invaluable service to the Government in coordi-
nating the country's chemical manufacturing resources, in increas-
ing the output of our chemical plants, and in allocating and fix-
ing prices to the Government of the finished product.
The value of these services cannot be over-stated, although
comparatively little has been written about them.
When the various war committees of the Council of National
Defense were discontinued and their functions absorbed by the
War Industries Board, the Chemical Alliance was formed to
serve as a clearing house of the chemical manufacturers in their
dealings with the Government through the War Industries
Board. It was organized primarily at the request of the De-
partment of Commerce to assist in clearing up business questions
in connection with the importation of pyrite, but later it became
a regularly organized trade association, without any official
Government connection, to which the War Industries Board can
turn for expert advice.
Some of the directors at first were original members of the
Committee on Chemicals, with Dr. Nichols as president. Later
Dr. Nichols retired and Mr. Horace Bowker, vice president, was
made president of the Alliance.
flu War Industries Board has been active in the chemical
held since its inception. It has well-organized committees to
deal with chemical trade matters, especially with the allocating
of material, fixing of prices, study of contracts, and a clearing of
orders for both the Army and Navy.
V— NATIONAL RESEARCH COUNCIL
The National Research Council early organized a chemistry'
committee, of which Prof. M. T. Bogert was made chairman.
When later Professor Bogert was appointed Lieutenant Colo-
nel 111 tin- Chemical Service Section, Dr. John Johnston was put in
charge of this work for the National Research Council, and con-
tinues in that capacity.
A meeting of prominent chemists takes place in Washington
m the rooms of the National Research Council twice weekly,
and the conferences serve as a clearing house of research work
going on in Washington and in the country. The National
Research Council has from the first served as a valuable feeder
and intermediary on research between the universities and the
Government, The Council has suggested and cleared many
research problems both in this country and abroad.
VI GEOPHYSICAL LABORATORY
The Geophysical Laboratory', under the direction of Dr.
Arthur L. Day, has engaged in important war work since the
beginning of the war. The developments which this laboratory'
have made in optical glass are well known and have had an im-
portant bearing on the war's progress. The laboratory has been
assisting on the nitrite investigations and other problems. The
high standing of its corps of chemists is weli known to all mem-
bers of our Society.
VII— THE WAR TRADE BOARD. SHIPPING BOARD, POOD
ADMINISTRATION, TARIFF COMMISSION
These important Government departments all require chemists
and utilize chemists in a consulting and directing capacity.
The War Trade Board has as a member, Dr. Alonzo E. Tay-
lor, who is assisted in passing upon chemical matters by Dr. A.
S. Mitchell, Mr. B. M. Hendrix and Dr. R. P. Noble.
The chemical work of the Shipping Board has been under the
direction of Dr. W. B. D. Penniman, who, while shutting off the
importation of certain products, has helped produce excellent
substitutes therefor.
The Food Administration has been guided in chemical matters
chiefly by Dr. Alonzo E- Taylor and Mr. Charles W. Merrill.
The chemical work of the Tariff Commission is under the di-
rection of Dr. Grinnell Jones, who this morning gives you a full
description of the information being gathered by the Tariff
Commission on chemical matters to guide it in its recommen-
dations to Congress, both during and after the war.
Many departments of the Government have been in constant
communication with our Allies on research and industrial chem-
ical matters. Chemical liason officers have been sent from the
Army and Navy and some of the civilian bureaus to keep in
touch with foreign development and practice, and their ser-
vices have been invaluable. In this connection it should be par-
ticularly pointed out that not all of the development of chemis-
try in this country is our own accomplishment, for we have ob-
tained information of the highest importance through the efforts
of these liason officers. On the other hand, chemical informa-
tion of the highest importance has been sent from America to
Europe.
War, the destroyer, has been on the other hand the incentive
to marvelous chemical development with a speed of accomplish-
ment incomprehensible in normal tinu-s. Discoveries made in
the search for instruments of destruction are already in use for
the development of chemical industry. Many others, unpub-
lished as yet, and to remain unpublished until the war is over,
will prove of the utmost benefit to mankind. The same agencies
that add to the horror of war to-day, the same reactions which
are used in the development of explosives and poisonous gases
on the one hand, and in counteracting their effect on the other,
will find immediate and useful application in the years to come.
Tin war has been prolonged by chemistry. The German
chemist, apparently working for years with war in view, has sup-
plied the German armies with the means for their ruthless war-
fare, but the chemists of America and our Allies have met
them fully in chemical development, and when the chemical
story' of the war is written where all can read, it will be the
verdict of history that the chemists of America were not found
wanting.
The chemical program of the United States Army and Navy
has been at all times ahead of our trained man power and- the
mechanical devices necessary to apply what the chemists of
America have produced.
THE WORK OF THE CHEMICAL SECTION OF THE WAR
INDUSTRIES BOARD
By Charles H. MacDowhu
Director, Chemicals Division, War Industries Board
Mr. Hoover says that Food will win the war. Mr. Garfield
opines that Fuel will win the war Mr. Hurley knows that
Ships will win the war. Mr. Raplogle thinks that Steel will win
the war After hearing Dr. Parsons' address I am sure you all
feel that Chemicals will win the war. Of course, it is the sum
total of effort that will win the war.
Oct.. 101S
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
781
The chemical industry is a war industry; the chemist, a war
worker. Both the industry and the chemist have been con-
tributing their facilities, education, training, and ability to
defeat their enemies.
The German chemical industry has been the best advertised
industry in the world. Its personnel has been charged with
arrogating to itself the possession of most of the world's chem-
ical ability, crediting but little of the sum total of chemical
accomplishments to outsiders. This extreme claim of super-
knowledge and ability is disputed in many quarters, and it is even
intimated that their chemical success has come more from their
ability to exploit the ideas of the Anglo-Saxon and the Latin mind
than from inherent chemical imagination and creative powers, and
that much of their original work is the accomplishment of the
Jewish rather than the Teutonic mind. Be that as it may, the
Germans, through methodical work, aggressive trade exploita-
tion, careful patent manipulation, and a clear chemical vision,
have developed a war chemistry which has contributed enor-
mously, through ruthless application, to their war success as far
as they have achieved success.
Modern war calls for much that is useful in peace times.
Agricultural chemistry in its development has contributed in no
small way to the forging of the sword. Nitrogen compounds,
sulfur, sulfuric acid, phosphorus, potash — all feeders of food and
clothing crops — also feed the cannon, the trench grenade, the
gas shell.-
Germany, through developments of this industry, had it in re-
serve for use in carrying out her daring political and trade
plans. Her development of by-product coking and aggressive
maintenance of her dye monopoly covered the accumulation
and a large immediate production of war chemicals. The devel-
opment of her potash industry gave her large production of
chlorine, bromine, and alkalies, and tied in closely with her
government salt monopoly. Her work in ferro-alloys, as well
as her manufacture and sale of armament, camouflaged a large
production of special cannon, armor plate, and other steel prod-
ucts. Even in optical glass she had a substantial monopoly,
and the more or less innocent snapshotter contributed to her
war purposes. The Diesel engine, the efficient gasoline motor
developed by automobile racing and readily adapted for aero-
plane work, were both available for war use. Haber's nitrogen
fixation method was developed and working, and connected with
Ostwald's work, hastened the decision to go to it.
The Germans appreciated fully the significance of the old
negro saying, "White man's lazy." They knew that it was
easier for most folk to buy rather than to make, and they pitched
their price to the end that they would make and others would
buy. They did not, however, give full credit to the latent pow-
ers of other people and what others would do to keep from
getting licked. The Allied world has found itself chemically,
and has been happily surprised at its chemical ability. What
has been done in chemical, scientific, and mechanical accom-
plishment will be of benefit long after the war is over.
When our country entered the fight, we were confronted with
the necessity of starting a big business at the top — always a
difficult task. We were credited with rather an unusual ability
for organization, standardization, and "get together," and we
had to draw heavily on this credit. War material is a sub-
stance and not a theory. Ore had to be dug and shipped. Ma-
chinery had to be built. Articles had to be made. Vision had
to be enlarged. We were asking much of our peace-time war
organization. Our immediate political accomplishments were
remarkable as evidenced by the draft law, the marshalling of
our man power. The American mind is a direct mind. It is
too near pioneer days to be otherwise. It has, however, a pecul-
iar conceit somewhat akin to that possessed by the young man
who wants to find out for himself rather than follow his father's
counsel. In some directions we were unwilling to accept Brit-
ish and French practices as a foundation and improve by expe-
rience. We thought we could do better than they to begin with,
and lost valuable time in consequence. In organization we have
had to get the round pegs into the round holes, and this has
taken time. On the whole, our progress has been remarkable.
Our public has naturally been impatient, not always fully appre-
ciating the enormity of the task, and this impatience has at
times tended to force premature action. On the whole, con-
structive criticism has been very beneficial. The public have
responded promptly to all calls made on them for financial help,
both for direct and indirect war purposes. The discipline of the
country has been splendid and the people have responded will-
ingly to every request calling for self-denial. The various
scientific associations have answered quickly all calls, and their
members have contributed largely, both in a military and civil-
ian capacity, to the results which have been obtained.
It was the task of the Council of National Defense, and later
of the War Industries Board, to marshal the industrial forces of
the country and the raw materials of the world that we might
assemble, manufacture, and distribute what was needed. At
the start the call for raw materials was relatively small, as manu-
facturing facilities were not sufficient to make for large produc-
tion; but as the months have gone by production has increased
and with it the need for greater supplies. This demand, coupled
with the growth of our military forces, has borne down hard on
many industries which normally have their right to full pro-
duction but which must now be more or less dislocated and
reduced in output or converted to direct war manufacture. The
War Industries Board is endeavoring to handle these questions
with as little injury as possible to the industries. Sacrifice is
called for on the part of industries as well as individuals. It has
been a source of great satisfaction to the Board to note not only
the willingness but the desire of the industries to assist in carry-
ing out its work even though great sacrifice were entailed. All
they needed was to have the problem clearly stated and to have
an understanding of the necessities.
Before the formation of the War Industries Board, the Chem-
icals Committee of the Advisory Commission of the Council of
National Defense, under the chairmanship of your president,
Dr. Nichols, laid the foundation for much that has been accom-
plished. The chemical needs of the country were foreseen,
and plans were laid for supplying them. When the Chemicals
Committee was dissolved, along with other committees, the
Chemicals and Explosives Division of the War Industries Board
assumed in part the duties of the Chemicals Committee, the
Chemical Alliance, Inc., as a war service committee representing
in large part the chemical industry.
Mr. L. L. Summers, who had been acting in a technical advis-
ory capacity for Messrs. Morgan and Company, of New York, on
Allied buying, had come to Washington at the beginning of the
war and was associated in a similar capacity with Mr. B. M.
Baruch, now Chairman of the War Industries Board, Mr. Baruch
at that time handling raw materials. Later Mr. M. F. Chase
joined the ranks working on the explosives program. Your
1 r was commandeered about the first of November, taking
charge of nitrates and general chemicals.
At this time plans were arranged for the building of smokeless
powder plants, nitrogen fixation plants, new by-product coke
plants, gas-Stripping plants, chlorine, and other needed facilities.
Mr. Chase joined with Mr. D. C. Jackling, who acted as special
agent in arranging for the erection of the smokeless powder
plants. All of this work was done in cooperation with the War
Department and the Navy. Dr. Marston T. Bogert joined the
staff in November as its technical chemical adviser. In those
days the organization was far from complete and every one
acted as his own office boy; the hours wen- long and the work
782
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
Owing to the need of wood distillation products for aeroplanes,
propellants, etc., the production of wood distillation plants
throughout the United States was taken over and the product
distributed. Platinum was also taken in hand. Arrangements
were made for the international control of nitrate of soda and for
its importation and distribution.
This is in part the early history of the Chemicals Division of
the War Industries Board.
Mr. Baruch has been charged by President Wilson with the
securing of new facilities for making war, with the conversion of
existing facilities to war work, with the exercise of priorities, and
has been termed the "official eye" of the Government to view
the entire field of war needs and arrange for procurement. In
carrying out this work as Chairman of the War Industries Board,
which is no longer directly connected with the Council of De-
fense, he has continued as far as possible the organization exist-
ing at the time he took hold. The Board is composed of mem-
bers, directors of divisions, chiefs of commodity sections, a
Priorities Division, a Price Fixing Committee, a Conservation
Division, and a Requirements Committee.
This latter committee meets each morning, its membership
consisting of representatives of the Army, Navy, War Industries
Board, Allied Buying Commission, Emergency Fleet, Fuel and
Food Administrations, Department of Commerce, etc.
Present and future requirements for the different commodities
handled by the War Industries Board are submitted from time
to time and distributed to the various divisions and commodity
sections handling the different commodities. In this way a
reasonably correct idea of the present and future requirements
is obtained. These are studied and from this suggestions are
made as to the best method of procurement. If new facilities
are required, the best way of obtaining them is studied and
recommendations are made.
While the Price Fixing Committee of the War Industries
Board fixes maximum prices on many products, the actual buy-
ing of material needed for war purposes is carried out by the
various procurement divisions of the Army, Navy, Emergency
Fleet, and so on.
The Conservation Division of the Board studies the possibilities
of economies in industries, the substitution of more available
materials for scarcer ones, the standardization of products as to
packing, sizes, varieties of output, etc. It has frequent consulta-
tions with the industries before asking that their manufacturing
procedure be modified in any way.
The Priorities Division studies the subject of preference in
raw materials, supplies, machinery, finished articles, etc., issuing
to manufacturers priority orders of different grades in accord-
ance witli the need for the article desired. The Priorities Com-
mittee has recently issued a list of certain industries entitled to
priority in accordance with their importance to the war program;
industries in this list carry an automatic priority according to
their classification. Certain industries not listed in this general
classification have priority as to specific plants. This classifica-
tion will be changed from time to time as necessity dictates.
There has recently been organized a new Facilities Division,
which passes on all new facilities from the standpoint of building
materials, fuel, power, transportation, etc., after consultation
witli tin' different sections interested in these particular subjects
The Board has what is known as a "Clearance List." Where
articles are in short supply or where special reasons exist for
keeping a close control, clearance for purchase is secured by the
various Go\ ei ami nt departments before finally closing contracts.
Before the Allied governments can negotiate for business,
either for war purposes or for the use of their nations, clear-
ance must be secured.
The line-up of the different divisions and sections follows gen-
erally the organization of the Chemicals Division, which I will
describe briefly.
This Division at present has twenty commodity sections, each
headed by a commodity chief. Your speaker is Director of the
Division. Mr. Marsh P. Chase, after finishing his work with Mr.
Jackling, returned to the Board and has become Director of
Explosives. The following is a list of the Sections and com-
modity chiefs:
Alkalies and Chlorine Products Mr. H. G. Carrell
Tanning Materials Mr. K. J. Haley
Inedible Fats, Oils, and Waxes Mr. Prosscr, Associate
Paints and Pigments Mr. R. S. Hubbard
Mr. Atwood, Associate
Acids and Heavy Chemicals Mr. Albert Brunker
Sulfur, Pyrites, and Alcohol Mr. Wm. Woolfolk
Coal-Gas Distillation Products Mr. J. M. Moorehead
Creosote Mr. Ira C. Darling
Artificial and Natural Dyes Mr. J. F. Schoellkopf, Jr.
Fine Chemicals Mr. A. G. Rosengarten
Refractories and Clays Mr. Catlett
Ferro-Alloys Mr. Hugh Sanford
Electrodes and Abrasives Capt. DuBois
Chemical Glass and Stoneware Mr. R. M. Torrence
Asbestos and Magnesia Mr. R. M. Torrence
Wood Distillation Products Mr. C. H. Conner
Platinum Mr. C. H. Conner
Mica Dr. Leith
Nitrates Mr. C. H. MacDoweU
Technical
These sections work with the chairman and heads of the dif-
ferent sub-divisions of the Chemical Alliance, Inc. Officers of
the Army and Navy, and representatives of the Emergency
Fleet, Fuel, Food, and other administrative bodies, have been
assigned to membership in these commodity sections. This per-
sonnel constitutes the section.
The technical staff of the Chemicals Division consists of Dr.
E. R. Weidlein, Dr. H. R. Moody, Dr. Thomas P. McCutcheon,
and Dr. Staley. These men keep in touch with the research
facilities of the country and are in constant contact with manu-
facturers. The facilities of the Mellon Institute of Industrial
Research are at the disposal of the Chemicals Division, and inter-
esting work is being carried on at that Institute. Of necessity
the work is of a secret nature, and cannot be discussed at this
time.
A number of commodities handled by the commodity sections
qf the Chemicals Division are allocated by the chiefs of the
sections, notably chlorine and its products, alkalies, sulfur and
pyrite, wood chemicals, toluol, platinum, nitrates; and a control
is exercised over the distribution of acids, electrodes, tanning
material, and other commodities. The task is to secure in time
the materials needed by the Government, by our Allies, and by
our people.
Mr. Baruch has asked me to assure you that the War Indus-
tries Board appreciates fully the splendid cooperation which has
been extended by the chemical industry and by the chemists to
the solving of the problems of the Board and of the Government
as a whole.
As we approach higher efficiency in the manufacture of war
materials it will be necessary to restrict the production of many
articles normally required by our people. There is not sufficient
raw material, steel, power, labor, or transportation to take care
of all industries.
In following out this maximum production program it may be
necessary to ask the chemical industry to forego in part or in
whole the manufacture of many less essential articles. The
cause is worth the sacrifice, and Mr. Baruch feels sure that as an
industry and as a personnel you all will understand the real
reason for such curtailment, and that it will only be asked after
careful study and with every' desire to cripple industry as little
as possible.
There is an old saying that "A little knowledge is a dangerous
thing." The Germans, through their knowledge and through
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
783
their instinctive desire to make use of this knowledge to carry-
out an ambitious and brutal war program, have built a
Frankenstein monster which bids fair to destroy them.
WAR DISTURBANCES AND PEACE READJUSTMENTS IN
THE CHEMICAL INDUSTRIES
By Grinnell Jones
Chemist on the staff of United States Tariff Commission
When peace is restored the competitive strength of the nations
in all industries will have been profoundly altered. Chemistry
and machinery have played a larger part in this war than in any
previous war, and therefore the greatest changes may be ex-
pected in the metal working and in the chemical industries.
Moreover, our new American cargo ships will make us more
than ever interested in foreign trade. The Tariff Commission
is actively studying these war disturbances in order to assist
in the readjustment and reconstruction that must follow when
peace comes.
Among the chemical industries, the first to feel the stimulus
of war was the explosives industry. The expansion of American
smokeless powder plants was sufficient to prevent a German
victory in France and Russia in 1915. It is not revealing
military secrets to say that there has been some growth since
19 1 5. We all hope that the peace terms will be so satisfactory
that the military explosives plants themselves will no longer be
needed. Nevertheless, there will be a permanent increase
in the competitive strength of the American chemical industries
through the growth of the subsidiary industries which now
supply the raw materials to the explosives industry.
Our production of sulfuric acid is at least twice what it was
before the war. The growth has been largely in contact acid,
and therefore when the demand for explosives disappears, the
American chemical industries will have available large supplies
of pure and concentrated sulfuric acid. Moreover, the growth
of the acid industry has been made possible by a great increase
in the production of American sulfur and by a smaller, although
significant, increase in the mining of pyrites.
The nitric acid industry has grown relatively more than the
sulfuric acid industry. The output of nitric acid from Chilean
niter is now more than ten times as great as it was before the
war.
The significance of this growth of the sulfuric and the nitric
acid industries to our dynamite, dyestuffs, and pyroxylin plastic
industries need not be emphasized here.
Of greater significance than this stimulus to industries already
well established has been the birth of new industries. We have
a new synthetic ammonia and nitric acid industry. Plants have
been built and, during the war at least, will be operated by the
Government. When the full story of these plants can be told,
it will reveal that American chemists have, under the pressure
of war needs, been able to devise substantial improvements
upon the Haber and Ostwald processes developed by the Ger-
mans before the war. These processes were the result of nearly two
decades of work on these problems as a part of their military
preparedness. It is not improbable that after the war nitric
acid made from synthetic ammonia may prove to be cheaper
than nitric acid made from Chilean niter. In any case, American
agriculture will assuredly have a new large source of nitrogenous
fertilizer materials.
In 1 914 our production of crude light oil would have been
sufficient for the production of only about 4,500,000 gallons of
benzol and of about 1,500,000 gallons of toluol, and only a p:irt
of this was distilled. As is shown in our forthcoming report
on the production of American dyes and coal-tar chemicals, in
191 7 our output of benzol was 40,200,000 gallons, of toluol,
10,200,000 gallons. In 1918 further substantial growth is to
be expected through the installation of stripping plants at
city gas works. The toluol is now going almost entirely into
explosives as is also a considerable fraction of the benzol. When
the demand for explosives disappears, it is to be expected that
the prices of benzol and toluol will drop to the point where it
will be profitable to add them to gasoline for motor fuel. A
similar condition will probably exist abroad and, since America
has the greatest known natural resources for the production of
gasoline, benzol and toluol should be as cheap or cheaper here
than abroad. Therefore the industries consuming benzol and
toluol may be assured of ample supplies of these materials at
favorable prices.
Before the war we had no synthetic phenol industry, whereas
in 1917, as is shown in our forthcoming report, 15 plants pro-
duced 64,146,499 lbs. of phenol valued at $23,715,805, most of
which was used in making picric acid. If this new industry is
to survive, there must be a greater consumption of phenol in the
industries for peaceful purposes. Fortunately, phenol is used
as an intermediate in the manufacture of some representatives
of every class of finished coal-tar chemical products, including
dyes and lakes, photographic developers, medicinals, flavors,
perfume materials, synthetic resins, synthetic tanning ma-
terials, and explosives. Leaders in the chemical industries are
already making plans for the industrial development of the uses
of phenol when the phenol is no longer needed for explosives.
Another war-baby is monochlorbenzol, which was made
during 191 7 by eight American firms, with an output of
24,624,099 lbs., valued at a little less than $5,000,000. The dye
industry will use a part of this productive capacity permanently,
but new discoveries by American chemists will probably be
needed to utilize the total productive capacity. Incidentally,
this product furnishes a new outlet for chlorine, a new by-product
source of muriatic acid, and raises a new problem in the utiliza-
tion of dichlorbenzol, an unavoidable by-product.
Before the war there was but one producer of aniline oil in the
United States. In 191 7 there were twenty-three producers
with an output of 28,806,524 lbs., valued at $6,758,535. As
only a relatively small proportion of this substance goes into
explosives, the peace readjustments will not be complicated by a
collapse of a military demand, but will depend primarily on the
competitive strength of the American industry.
The war has also stimulated the production of mercury for
the manufacture of fulminates. The American production has
been about doubled since the beginning of the war. Formerly
we had a balance of imports — now we have a larger balance of
exports.
Poison gas warfare is also destined to have a permanent in-
fluence on the chemical industries. Although there is no reason
to expect that uses will be found for phosgene and mustard gas
on a scale approaching the present and prospective military use,
the plants erected for their manufacture need not prove a total
loss when the military demand ceases. Nearly all of the noxious
substances used in poison gas warfare require chlorine for their
manufacture, and an increase in the production of chlorine in the
United States is therefore certain. There is much hope that
some of the substances produced as intermediate steps in the
manufacture of the poison gases may be utilized for purposes
other than warfare, but these are matters not yet to be discussed.
Phosgene, except for the dangers attending its use, is an excellent
reagent for many processes involving chlorination or dehydra-
tion and for making Michler's ketone. Fortunately, the risk
in using phosgene is greatly minimized by the development of
the new gas mask. The intensive work which hundreds of
American chemists have been and are doing to improve the design
of the gas mask will undoubtedly prove a blessing to workmen
exposed to noxious fumes in chemical factories throughout the
world when peace is restored.
Still another industry which has been stimulated by a direct
w:.i demand is the manufacture of acetone, which is used as a
784
J HE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
gelatinizing agent in the manufacture of the explosive, cordite;
as a solvent for airplane dopes; and in the manufacture of poison
gases. Before the war, acetone was obtained entirely as one
of the products of the wood distillation industry, but there are
now at least four new processes in commercial operation in the
United States or Canada for the manufacture of acetone.
It has been found that glucose can be fermented by a suitable
organism to give acetone directly. Butyl alcohol is a byproduct
of this fermentation and becomes commercially available in
appreciable amounts. The development of uses for butyl
alcohol is an attractive problem.
The other processes for making acetone produce acetic acid
or an acetate as an intermediate step, and may therefore per-
manently affect the acetic acid industry. The most obvious
and perhaps the simplest of these processes depends on fer-
menting molasses to alcohol, which is then converted into acetic
acid by the rapid vinegar process. The conversion of acetic
acid into acetone is an old and well-known process but the
details have been improved.
Another process depends on making acetylene from calcium
carbide. By the aid of a suitable catalyst, the acetylene is
made to combine with water yielding acetaldehyde which may
be readily oxidized to acetic acid. Still another process depends
on fermenting kelp under such conditions that sodium acetate
and potassium salts are secured.
The war has stimulated the production of many other products,
a few of which may be briefly mentioned : castor oil for lubrica-
ting airplane motors; phosphorus for incendiary bombs and
smoke screens; barium and strontium nitrates for signal rockets.
The output of soda ash has increased by 68 per cent since 1914,
and the output of caustic soda has more than doubled.
New conditions in the chemical industries have also been
created by the curtailment of imports. As a direct consequence
of this stoppage of imports from Germany, a new American dye
industry has been established. It is true that some dyes were
being made in the United States before the war, but the makers
relied on Germany for the necessary intermediates, with the
exception of a small amount of aniline made here by a single
producer. During 1917, 134 different intermediates were made
by :i8 firms. One firm made 53 different intermediates. Dyes
were made by 81 firms. The total production of dyes in the
United States during 191 7 was approximately equal in gross
weight to the annual importations before the war. The exports
of American dyes exceeded in value, although not in quantity
or variety, our imports before the war. The dye industry is not
dependent on any imported raw material except sodium nitrate
from Chile. Many important dyes are still lacking, but indigo
and alizarin are now on the market in significant amounts, and
the vat dyes for cotton derived from anthracene are com-
ing.
A ih w potash industry has also arisen, but its future does not
seem so promising as the future of the new dye industry. Here
Germany has an inherent geological and geographical advantage.
Although shipments from Germany ceased early in 1915 and
although prices have advanced to about ten times the pre-war
prices, the American production during 191 7 was only about 13
per cent of our pre-war consumption. This relatively small
production was obtained from many sources and by many
processes. There is an excellent prospect that the recovery of
potash as a by-product of cement will survive German com-
petition and ultimately supply about one-third of our needs.
In addition, significant amounts will probably be secured as a
by-product of the pig iron blast furnace. That the other
of the potash industry can survive German competition
is open to serious question,
Within a few months after tin outbreak of the war, imports
to the United States from Germany and her Allies came to an
end. As the months went by. it became increasingly difficult
to obtain cargo space for imports from any part of the world.
Xow the limiting factor in the American participation in the
war is shipping for our troops and their supplies, and therefore
ships are no longer free to seek the most profitable cargo and
route, but are being assigned to routes and cargoes by the Ship-
ping Board on the basis of military needs rather than profits.
The Shipping Board has organized a Division of Planning and
Statistics, which is making a study of world commerce and the
military and civil requirements, for the purpose of utilizing
available shipping in a way that will contribute most to the
winning of the war. Military requirements make it essential
that an abnormally large proportion of the world's shipping
shall be used in the N'ortli Atlantic. This has made it necessary
to curtail imports from other parts of the world to essential
requirements.
The chemist on the staff of the Shipping Board is W. B. D.
Penniman, of Baltimore. He must decide what chemicals need
not be imported at all, and the amounts of others which must
be imported to supply essential needs. The importance of this
work can perhaps best be made clear by an example. The
Shipping Board, after consultation with the Food Administra-
tion, decided that ships could not be spared for the importation
of tapioca from Java and the Straits Settlements. The War
Trade Board accordingly announced that licenses for the im-
portation of tapioca would not be granted. Efforts were im-
mediately made to secure a modification of this order on behalf
of one of the manufacturers of nitro-stareh for the Army and on
behalf of manufacturers of mucilage for the Post- Office Depart-
ment. Nitro-starch has been improved until it is now one of the
safest of all explosives to handle and finds important military
uses. Until a few months ago it was being made from tapioca.
Penniman, however, succeeded in convincing the officers of the
War Department and the manufacturers that a satisfactory pro-
duct could be made from cornstarch. The details of the manufac-
ture have been worked out cooperatively by the starch producers,
the manufacturers of nitro-starch, and the experts of the War De-
partment with such success that nitro-starch from corn is not
only better but more economically produced than nitro-starch
from tapioca. The Post-Office Department also readily agreed
to use some locally available material instead of tapioca for
mucilage on stamps. The shipping saved on this one item of
tapioca for nitro-stareh is sufficient to transport and sustain
in France more than twenty-five thousand fighting men. Mr.
Penniman's services to the nation on questions of this character
deserve to be better known and appreciated. Imported ma-
terials for the time being should be used with the utmost economy
and only for essential needs. American chemists can render
valuable public service by finding substitutes for materials which
must be imported from overseas.
It seems probable that many of the discoveries in regard to the
use of substitutes for imported materials made under this pres-
sure of war needs will prove of permanent value and have a
permanent influence on international trade.
A third source of war disturbances in the chemical industry
has been due to the diversion of materials from their customary
use to war uses. The fertilizer industry has probably made the
greatest sacrifices of this sort. Sodium nitrate and ammonia
are required for the manufacture of explosives in such large
quantities that the amounts left for use in fertilizers has been
and will be much reduced. Raw phosphate rock has of course
been plentiful but the acid used in the manufacture of acid
phosphate has been largely diverted to making explosives.
The relatively small supplies of potash have been very high in
price and normal amounts have not been available at any price.
The peace readjustments may, however, be expected to bring
compensation to the fertilizer industry. Large new supplies
of nitrogenous fertilizer materials will be available from the new
nitrogen fixation plants. The new and enlarged sulfuric acid
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
785
plants must again find the chief outlet for their product in the
making of fertilizers. Finally, the German monopoly of the
potash market is likely to be broken through the French control
of Alsace and the new developments in America and Spain.
It is therefore reasonable to expect a large increase in the manu-
facture and use of fertilizers with a resulting benefit to all pro-
ducers and consumers of food.
Chlorine also is likely to be diverted from its normal uses
to the manufacture of poisonous gases to a considerable extent.
In spite of the erection of new plants we may all be asked to use
paper lacking in the whiteness to which we have been accus-
tomed. Chemists in industries using chlorine should prepare
to facilitate this diversion now, and plan to use more chlorine
later when the military demand ceases.
It is evident that the status quo ante cannot be reestablished
in the chemical industries any more than it can be reestablished
in international relations. Peace will bring new conditions of
international competition and radical readjustments in industry
from a war basis to a peace basis.
The Tariff Commission is endeavoring to secure and have ready
for immediate use all information likely to be helpful to Congress
in determining the part which the tariff is to play in these read-
justments. We desire information in regard to the industrial
development and technical progress of industries throughout
the world ; in regard to the sources of their raw materials and the
uses of their products; and in regard to any changes in conditions
likely to have a permanent influence on costs of production or
the competitive strength of industries here and abroad. The
assistance and cooperation of manufacturers, importers, and
consumers in the collection and interpretation of this information
is desired.
CHEMICAL WARFARE RESEARCH
By Wilder D. Ba
Lieutenant Colonel, Chemical Warfare Service, U. S. A.
As Dr. Parsons has told you, the Bureau of Mines started a
research laboratory in gas warfare about a year and a half ago.
On July first that was taken over by the War Department, but
the organization as it stands at present is practically the same
as that developed by the Bureau of Mines. The outward signs
of the change are that Major General Sibert is the official head
instead of Mr. Manning, and that Mr. G. A. Burrell is now
Colonel Burrell. On the other hand, Dr. E. P. Kohler, who
had charge of all the offense problems, holds the same position
in the new organization without having put on a uniform.
Instead of running over the various sections and outlining
their duties, it seems to me that it would be a good deal more
interesting, though perhaps less thorough, if I described the
procedure in regard to any given war gas.
The term "war gas" is a flexible one. The substance may be
a liquid, a solid, a vapor, or a true gas. However, it must have
some pretty striking characteristics : it must be poisonous; or pro-
duce tears (lachrymatory); or must give rise to nausea, sneezing,
or blisters; have a foul smell, though otherwise harmless; or be
a smoke with obscuring powers. Of course it may have any or
all of these properties combined. Under any of these circum-
stances we call it a war gas. It must also have certain other
characteristics. It must be pretty good in its class. Nowa-
days no one would consider as a toxic substance anything which
did not kill dogs in 30 min. at a concentration of 1 mg. per
liter. It is that effective concentration which is overlooked
by people who suggest new gases or methods of using old ones.
In the case of lachrymatory substances they should be effective
at concentrations as low as 0.01 mg. per liter. The best are
much better than that.
Another determining factor in the use of any gas is the avail-
ability of raw materials. Where thousands of tons may be
needed, there is no use in considering a substance of which the
available output per year is a gram, a ton, or a hundred tons.
A good method of manufacture should be at hand. If the
substance is good enough, it will be made by any method, how-
ever wasteful; but this is not true in most cases. I could cite
an instance where a substance would be used if a good method
of manufacture were available. The present method of making
this substance is so wasteful that its good qualifications do not
counterbalance the disadvantages, and it is not used either by
our Allies or by ourselves.
A substance must be stable, or fairly stable. It must not
polymerize rapidly, hydrolyze too rapidly, be too inflammable,
or go to pieces on detonation. Our problem is different from
that of the Allies because the Allies can use their material within
2 or 3 months after loading the shells, whereas in our case shell
loading here must take place from 3 to 6 months before firing,
and consequently our limits as to stability against polymeriza-
tion must be more rigid than those of the British and French;
and as a matter of fact the French are using certain substances
which we shall not use, just because of those conditions.
How do we start with any given substance? We may take
a substance already used by the Germans or the Allies, or we
may get a suggestion from outside, or the staff may think up
something from a search of the literature, from analogy, or from
pure Inspiration. Then steps are taken to see whether it can be
considered as a toxic substance. First, the Offense Research Sec-
tion, under Dr. Lauder Jones, makes the substance. If it is a
solid, it is sent to the Dispersoid Division, Dr. R. C. Tolman in
charge, and they work out methods of disintegrating it.
When this is done, or if it is a liquid or vapor, it is sent to the
Toxicological Section, Dr. A. S. Loevenhart, and tested to de-
termine degree of toxicity, concentration producing lachryma-
tion, or any other of the delightful characteristics. If their re-
port is favorable, the substance is turned over to a number of
different sections.
The Offense Research Laboratory works to improve the
laboratory method of making. After they have worked this
out on a laboratory scale, the substance is turned over to the Chem-
ical Production Section, Mr. W. S. Rowland, and they work it
out on a larger scale, from 50 lbs. to a ton, depending entirely
on the nature of the substance. It then goes outside of the
Research Division, either to Large Scale Production (Colonel
Dorsey) for further development, or direct to Colonel Walker,
at Edgewood, for commercial production either there or to be
assigned to some manufacturer somewhere in the country.
While the Offense Research Section is working out an improved
laboratory method, the substance is sent to the Analytical
Section, under the charge of Mr. A. C. Fieldner. They de-
velop methods for determining its purity. They also analyze
mixtures in air. It is sometimes difficult to determine sub-
stances at the dilution in use. They also make tests to find
out whether the canisters will stop the substance.
It is also sent to the Pyrotechnic Section under Mr. G. A.
Richter to determine stability when fired in shells, that is, whether
it goes to pieces under the detonating charge.
At the same time the Defense Research Section, under Dr. A. B.
Lamb, is working to determine whether any change in the in-
gredients put in the canister is necessary. If the substance is
bed, some new mixture or compound must be di
which will stop it. This Section also takes up the question of
methods of detecting toxic substances in the field. That
might be considered to be a problem for the Analytical Section,
liul our whole Systl in is pretty flexible, and as a matter of fact
that work has been done by the Defl R.i earch Section, "f
course working in cooperation with the Analytical Section
786
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
The Defense Research Section also develops ointments to pro-
tect against the effect of the action of the toxic or blistering
gases of the skin.
At the same time the substance will be referred to the Me-
chanical Research Section under Mr. Fogler, because a change
in the ingredients may make it necessary to change the type of
canister. That becomes important if dealing with smokes in-
stead of vapors. The question of protective clothing may have
to be taken up.
The defensive results are then transmitted by Dr. W. K. Lewis,
in charge of all defense problems to the Gas Defense Division,
which is not a part of our Division, but is under Colonel Dewey,
and has charge of the commercial production of all defense ma-
terials.
While all this is being done, the same substance is sent to the
Pharmacological Research Section under Dr. E. K. Marshall,
and they study the question of the effect produced and the
general question of susceptibility. Certain men may be ioo
times as susceptible as are other men. It is very desirable to
make preliminary tests, and to keep out of the factory men who
are extremely susceptible, because they are sure to be casual-
ties.
The substance is also studied by the Pathological Section under
Dr. Winternitz, and they go into painful details as to the way
in which the various organs are attacked by war gases.
At the same time it is sent to the Therapeutic Section under
Dr. Underhill, of Yale, and they take up the desirable but very
difficult task of finding methods of treatment to revive men
who have been gassed more or less severely.
While all this is going on, all these various sections are mak-
ing reports twice a month on all the substances that they are
working with, so that you can see that there is an enormous
amount of pseudo-literary material piling up. All of this ma-
terial comes to the Editorial Section, of which I am in charge.
We condense it as much as possible, and get out semi-monthly
reports, which are sent to a selected list of people in this country
and abroad. These reports deal with many different topics,
and if someone wanted to look up about a certain substance
he would have a fearful task ahead of him. Consequently, as
fast as possible we are writing monographs on each particular
gas, canister ingredient, etc., which shall contain everything
that is known in the literature, everything that we have been
able to get from the Allies or from captured German reports,
and everything that has been done in this country. We hand
out the desired monograph to the inquirer, and tell him to read
it. Of course he does not do it, but the thing is indexed pretty
thoroughly, and he can look over the various sections which in-
terest him more particularly, and thereby post himself on
what is known in regard to that substance in a relatively short
time. In this way the information in our files is made fairly
accessible.
Now this whole system of handling toxic substances is a very
flexible one. Whenever necessary we increase or decrease the
number of sections. At one time Dr. J. F. Norris was in charge of
all the chemical research. That grew to be more than one man
could possibly handle. The Offense Research was left under
Dr. Norris, and the Defense Research was given to Dr. Lamb.
Since other sections were interested in the offensive work, it
necessary to tie things together again, and Kohler was
put in charge of all the problems of Offense,
We began with one Physiological Section. Now there are
Pharmacological, Pathological, and Therapeutic Sections, and
the Pharmacological Section has recently been subdivided into
testing and res
The Mechanical Work was split into two sections. When
conditions changed, this work was put back into one section.
Any section can be changed or rearranged in any way desirable
to get results, and this has worked well in practice.
THE PLACE OF THE UNIVERSITY IN CHEMICAL WAR
WORK
By E. W. Washburn
Vice Chairman, Division of Chemistry and Chemical Technology,
National Research Council
In normal peace times, so far as chemistry is concerned, the
university has two main functions, first, the training of chemists,
and second, the prosecution of research in pure and applied
chemistry. In war times these still remain the principal func-
tions of the university, but as has happened in so many other
cases, these two functions must be modified to accord with war
needs, and it is on the subject of what these modifications should
be that I wish to speak to you this morning.
THE TRAINING OF CHEMISTS
A few weeks ago the War Department's Committee on Edu-
cation and Special Training requested the National Research
Council to make an analysis of the Government's needs for
chemists, and to make recommendations covering the steps
which should be taken to provide as far as possible to supply
these needs. In order to obtain the necessary data a question-
naire was sent to all Government agencies employing chemists,
asking them to state the number of chemists, kind of training
{i. e., organic, metallurgical, etc.) desired, the increase in each
of these classes of chemists which they estimated would be
required during the coming year, and any changes in educational
methods which they thought desirable in order properly to meet
their needs.
From the answers received to this questionnaire the Research
Council was able to determine approximately what the needs
of the Government are with respect to the different kinds of
chemists required. With regard to the number of chemists
now in service in different Government departments, the data
already given you by Dr. Parsons are in accord with those ob-
tained as a result of the questionnaire referred to. and it will
therefore be unnecessary to repeat these figures. As ' > future
requirements, the data collected indicate that something over
2000 chemists will be needed by the Government during the
next year in addition to the numbers now in service. These
figures take no account of industrial requirements, but it is
safe to say that the additional chemists required for necessary
war industries will at least equal the number of those required
by the Government. We may conclude, therefore, that some-
thing over 4000 additional chemists will be needed for necessary
war work during the coming year. This number is considerably
in excess of the normal output of the colleges, and we cannot
hope to provide all of the chemists called for. The problem is,
therefore, to make provision for training, as quickly as possible,
the maximum number of chemists which the educational facili-
ties of the country can take care of.
The source of supply of the additional chemists required by
the Government and by the war industries will for the im-
mediate future be those students in the Students' Army Training
Corps who are preparing themselves for Chemical Warfare
Service. While provision can be made in training camps
for training the rank and file of certain other branches of the
Army, this is not true in the case of Chemical Warfare Service.
Most of the men in this service must be trained as chemists,
and this training can be given them only at the colleges and
universities.
The analysis of the Government requirements for chemists
indicates that, in general, the chemists needed may, for purposes
of consideration. K divided into three classes as follows:
I — Analytical chemists: that is, men who have received suffi-
cient training in chemistry to enable them to earn- out routine
analytical work under direction, W
2 — Chemists with a good general training in all of the funda-
mental branches of the subject, and with some degree of further
Oct., 19 1 8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
787
instruction in one of the following: (a) physical chemistry,
including electrochemistry and metallography; (0) organic
chemistry, including the chemistry of explosives; (c) food and
sanitary chemistry; (d) physiological chemistry; (e) chemical
engineering, including ceramic engineering, petroleum, textile,
rubber, leather, etc., technology, and metallurgy.
3 — Chemists qualified to carry on research work intelligently
in some one of the fields listed under Class 2.
Approximately one-third of the total number of chemists
required will be in Class 1, and will be employed in routine
analytical and control work.
The National Research Council, at the request of the War
Department, has drawn up a set of recommendations embody-
ing a 3 years' curriculum in chemistry and a 3 years' curriculum
in chemical engineering, each curriculum being based upon a
year composed of 4 terms of 12 weeks each. Under this scheme
the first group of chemists required can be trained in one year,
the second group in two years, and the third group in three' years.
These curricula are intended for institutions having a unit of
the Students' Army .Training Corps organized in accordance with
the following statement recently issued to the colleges of the
United States.
The man-power bill pending in Congress definitely binds the
country to the policy of consecrating its entire energy to the
winning of the war as quickly as possible. It fixes the age limits
as 18 to 45, both inclusive. It places the nation upon a war
basis. The new military program, as outlined by the Secretary
of War, calls for the increase of the Army by more than two
million men by July 1, 19 19. This will probably necessitate the
mobilization of all physically-fit registrants under 21, within ten
months from this date. With respect to students, since they
are not to be made in any sense a deferred or favored class, this
means that they will practically all be assigned to active service
in the field by June 19 19. The only exceptions will be certain
students engaged in technical studies of military value, e. g.,
medicine, engineering, and chemistry. Under these conditions
it is obvious that schools and colleges for young men within the
age limits of the new law cannot continue to operate as under
peace conditions. Fundamental changes must be made in
college and school practices in order to adapt them to effective
service in this emergency.
The following statements outline the general plan under which
the Students' Army Training Corps will operate under the
changed conditions produced by the revision of the Selective
Service Law :
1 — All young men who were planning to go to school this fall
should carry out their plans and do so. Each should go to the
college of his choice, matriculate, and enter as a regular student.
He will, of course, also register with his local board on the
registration day set by the President. As soon as possible
after registration day, probably on or about October first,
opportunity will be given for all the regularly-enrolled students
to be inducted into the Students' Army Training Corps at the
schools where they are in attendance. Thus the Corps will be
organized by voluntary induction under the Selective Service
Act, instead of by enlistment as previously contemplated.
The student, by voluntary induction, becomes a soldier in the
United States Army, uniformed, subject to military discipline,
and witli the pay of a private. They will simultaneously be
placed on full active duty, and contracts will be made as soon as
possible with the colleges for the housing, subsistence, and in-
struction of the student soldiers.
2 — Officers, uniforms, rifles, and such other equipment as
may be available will be furnished by the War Department, as
previously announced.
3 — The student-soldiers will be given military instruction
under officers of the Army and will be kept under observation
and test to determine their qualification as officer-candidates,
and technical experts such as engineers, chemists, and doctors.
After a certain period, the men will be selected according to
their performance, and assigned to military duty in one of the
following ways:
(a) He may be transferred to a central officers' training camp.
(b) He may be transferred to a non-commissioned officers'
training school.
(c) He may be assigned to the school where he is enrolled for
further intensive work in a specified line for a limited specified
time.
(d) He may be assigned to the vocational training section
of the Corps for technician training of military value.
(e) He may be transferred to a cantonment for duty with
troops as a private.
4 — Similar sorting and reassignment of the men will be made
at periodical intervals, as the requirements of the service de-
mand. It cannot now be definitely stated how long a particular
student will remain at college. This will depend on the re-
quirements of the mobilization and the age group to which he
belongs. In order to keep the unit at adequate strength, men
will be admitted from secondary schools or transferred from
Depot Brigades as the need may require.
Students will ordinarily not be permitted to remain on duty
in the college units after the majority of their fellow citizens of
like age have been called to military service at camp. Exception
to this rule will be made, as the needs of the service require it,
in the case of technical and scientific students, who will be
assigned for longer periods for intensive study in specialized
fields.
5 — No units of the Students' Army Training Corps will, for
the present, be established at secondary schools, but it is hoped
to provide at an early date for the extension of military instruc-
tion in such schools. The secondary schools are urged to in-
tensify their instruction so that young men 17 and 18 years old
may be qualified to enter college as promptly as possible.
6 — There will be both a collegiate section and vocational
section of the Students' Army Training Corps. Young men of
draft age of grammar school education will be given opportunity
to enter the vocational section of the Corps. At present about
27,5e>o men are called for this section each month. Application
for voluntary induction into the vocational section should be
made to the Local Board and an effort will be made to accom-
modate as many as possible of those who volunteer for this
training.
Men in the vocational section will be rated and tested by the
standard Army methods and those who are found to possess the
requisite qualifications may be assigned for further training in the
collegiate section.
7 — In view of the comparatively short time during which most
of the student-soldiers will remain in college and the exacting
military duties awaiting them, academic instruction must
necessarily be modified along lines of direct military value.
The War Department will prescribe or suggest such modifica-
tions. The schedule of purely military instruction will not
preclude effective academic work. It will vary to some extent
in accordance with the type of academic instruction, e. g., will
be less in a medical school than in a college of liberal arts.
8 — The primary purpose of the Students' Army Training Corps
is to utilize the executive and teaching personnel and the physical
equipment of the colleges to assist in the training of our new
armies. This imposes great responsibilities on the colleges and
at the same time creates an exceptional opportunity for service.
The colleges are asked to devote the whole energy and educa-
tional power of the institution to the phases and lines of training
desired by the Government. The problem is a new one and
calls for inventiveness and adaptability as well as that spirit of
cooperation which the colleges have already so abundantly
shown.
From this statement it will be seen that the colleges are facing
a variety of very difficult problems in making provision for the
large number of students who will enter the Students' Army
Training Corps. The president of one of the large western
ties, in starting the plans for housing and feeding 1 110
large numbers of students which they expect to take care of,
asked the supervising architect of the institution if he could
make such provision in time for the institution to open on its
regular date, which was about the middle of September. When
the architect replied that it would be impossible, the pi
expressed his disappointment and reminded him that he had
never before failed in a crisis. To this the architect 1
"Mi. President, this is not a crisis, it is a revolution; the crisis
will come on the day the university opens."
I think this statement fairly expresses the conditions which
the colleges and universities are facing. Under the new regula-
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
tions any properly equipped high school graduate may now
enter the college of his choice. He will be provided with quarters,
mess, light, heat, equipment, and free instruction, and will be
paid $30 a month. Throughout the time he is in college he will
bi under strict military discipline. At the end of every 12
weeks his record will be scrutinized and if his work is in any way
unsatisfactory, he will be immediately taken out of college and
assigned elsewhere, probably in many cases to one of the
cantonments. Former college students will find college life
an entirely new proposition. Doubtless many of you have seen
on the walls of fraternity houses such mottos as the following:
"Never permit your studies to interfere with your regular col-
lege work." The student who follows any such motto as this
under the new conditions will find himself neatly and with
great despatch removed from his academic surroundings. Such
customs as petitioning the Faculty for another trial, or for a
special examination, and all other hallowed customs of this
kind will pass out of existence. The student either makes good
or he doesn't; he either passes or he fails. The lame duck
species of college student is about to become extinct. The men
wlio remain in college after the first 3 or 4 terms will be only
those students who have displayed exceptional ability for some
special line of training.
The statements received from the various Government agen-
cies concerning desirable modifications in the training of chem-
ists may be of some interest. As might be expected, all agencies
of the Government emphasized the need of more thorough
training in the fundamental branches of the science, that is, in
inorganic, organic, and physical chemistry. In addition, certain
special subjects were mentioned by a number of different Govern-
ment agencies. For example, the various arsenals emphasized
the need of more men well trained in metallurgy and metallog-
raphy. The Navy Department pointed out that many of their
men apparently had received no definite instruction in methods
of using chemical literature or in proper methods for drawing
up specifications. As might be expected, many branches of the
Government also pointed out the need of special courses in the
chemistry of explosives. Additional numbers of (1) pharma-
ceutical chemists were called for by the Bureau of Chemistry
and by Chemical Warfare Service; (2) physiological chemists by
the Surgeon General's Office and by Chemical Warfare Service;
(3) food and sanitary chemists by the Surgeon General's Office
and by the Bureau of Chemistry; (4) ceramic chemists by the
Bureau of Standards and by the U. S. Fuel Administra-
tion.
RESEARCH ON WAR PROBLEMS
Under normal conditions every research laboratory is con-
fronted with more problems than it can take care of. Since the
war the personnel of many of the Government laboratories has
'been increased many fold, and it might be thought that with
this greatly increased personnel these laboratories would be in
a position to care for all of the problems which now exist. Such,
however, is not the case. It is true that the Government now
provides, as it must necessarily provide, for the investigation
of all the larger and more urgent problems with which it is
confronted, but nevertheless, most of the Government labora-
tories are overcrowded with work, and have trouble in securing
certain classes of equipment and the services of sufficient num-
bers of adequately trained men. It is true that more men
might be obtained if laboratory space could be provided for
them, but such additional numbers could only be secured by
further depletion of the staffs of educational institutions, and
such action would result in completely shutting off the supply
of chemists for the future.
Although the Government is providing in its own laborato-
ries and under its own direct control for the investigation of the
important research problems connected with the prosecution of
the war, there are many important problems still unsolved or
only partially solved. For example, many of the problems which
the Government has had to solve have been problems con-
nected with the production of some new material or the devel-
opment of some new process to fill an urgent need. As soon as
a material or process has been obtained which meets this need
more or less satisfactorily the laboratory in charge has then
found it necessary to transfer its attention to some other urgent
problem. As a result there are many processes and materials
which have received only that amount of study which was neces-
sary to insure their operating sufficiently well to accomplish the
desired end. In other words, output of something which would
do has been the sole purpose and result of the research work.
It thus happens that in many cases there has been no oppor-
tunity to ascertain just why certain things tried have worked,
or why certain others have failed; or just why certain conditions
seem to be more favorable than others; or just what occurs at
this or that stage of the process; or why some other method
might not give a higher yield or a better quality of material than
the one which is actually employed because it has been found to
work; or whether certain cheaper or better raw materials might
not be available; or just what is the relation between factor A
and factor B which enter into some part of the operation, etc.,
etc. There are indeed many auxiliary problems of this char-
acter which have arisen in connection with the research work,
and which are worthy of the careful scientific study which they
can receive only in some laboratory not working under the high
pressure which prevails in many of the Government laboratories.
This is where the universities may be of great service in supple-
menting and completing the research work of the Govern-
ment.
In addition to supplementary problems of the kind just
described, there are other problems, in the solution of which
the research resources of the universities can be of great
assistance. It frequently happens that a search of the liter-
ature demonstrates that the physical chemical or physiological
properties of certain important materials are very inadequately
known, the data in the literature being very fragmentary, or of
doubtful accuracy, or both. The Government laboratories have
neither the time nor, in many cases, the equipment for mak-
ing the necessary measurements to secure the desired data.
Here again many of the universities have exactly the equipment
required and can secure the data desired.
It is hoped that the investigators of the country will be willing
to lay aside for the present the lines of work in which they have
been interested in the past, and to take up some war problem
of a character which they can handle with the equipment and
assistants at their disposal The National Research Council is
undertaking to secure as many of these problems as possible
which are suitable for assignment to universities. It will also
endeavor to secure from all available sources in Washington all
of the unpublished information concerning the work which the
Government has already carried out in connection with each
problem, and to transmit such information to the investigator
to whom the problem is assigned. Where special materials or
chemicals are involved arrangements will also be made as far
as possible for supplying such materials to the investigator.
Many of these problems will be found suitable as thesis sub-
jects for graduate students or for seniors in a chemistry cur-
riculum.
If any investigator who is in a position to give a substantial
part of his own time to work of this character or who has ade-
quate assistance in the way of students or research assistants
will make known to the National Research Council the facilities
at his disposal and the nature of the problem (whether organic,
physical, physiological, or analytical, etc.) which he prefers, the
Council will endeavor as far as practicable and as soon as pos-
sible to submit to him through the authorities at his institution
a war problem for investigation.
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
789
5YMP05IUM ON CHLMI5TRY OF DYL5TUFF5
Papers presented at the 56th Meeting of the American Chemical Society, Cleveland, September 10, 19 1 E
INTRODUCTORY REMARKS
By R. Norris Shreve, of the Caleo Chemical Company
This Symposium on Dyestuff Chemistry has been arranged
with the aim in view that such discussions will contribute to
the complete establishment and full development of the dyestuff
industry in America.
During the past few years, over which time the American
chemists have become so much engaged with the problems con-
nected with the chemistry of dyestuffs, it has been a foregone
conclusion that sooner or later these chemists would naturally
gather together for the mutual discussion and elucidation of
their problems. I myself have always felt that such gatherings
ought most appropriately to come within the fold of the Amer-
ican Chemical Society, and it is hoped that out of this Sym-
posium there will arise a Section or Division of Dyestuff
Chemistry that will meet at the regular gatherings of the
American Chemical Society, and that this division or
section will be active and helpful to this industry and to
chemistry in general My own feeling is that the contemplated
Division of Dyestuff Chemistry should include not only the
coal-tar dyes but also the naturally occurring dyes.
Notwithstanding the fact that we are at war, and that conse-
quently the primary business before us all is to win the war,
yet there never has been a time more particularly opportune
for that emphasis to be placed on the chemistry of dyestuffs
in all its phases, without which the industry cannot become the
integral part of American life that lies so opportunely before it.
The war has awakened American business men and American
bankers to the importance of the entire chemical industry and
the financiers and business men in particular have given un-
grudging support to the coal-tar dyes. As a matter of fact,
some financial men have been badly bitten already by reason of
venturing into this most complex field without adequate under-
standing of its problems and ramifications. Right here seems
to me to be a field wherein the chemists can be of great service
to themselves and also to the industry by guiding the American
business men along the sound lines of investment, and also of
development, without which the integrity of the primary in-
vestment cannot be preserved.
The dyestuff industry is one that cannot stagnate and live. It
must develop or retrograde, and this development must depend
absolutely upon the original research work of the chemists. As
an editorial in the Textile Colorist (May 191 7) says, "The dye-
stuff factory cannot progress, or even exist, upon the cast-off
products of other factories. The history of the dyestuff indus-
try shows that financial success follows the research laboratory,
and the research laboratory only; the other path leads to failure
and disaster." I feel sure that these points are apparent to
any chemist who has studied this industry, but it is through the
chemists that these facts must be brought home to the business
men and the financiers who are directing our industry, and who,
in too few cases in our country, have had chemical training and
experience.
To be sure, the American business man adequately realizes
that by increasing the yield and quality of products he is now
manufacturing, he places his business in a position to earn
greater profits or to meet more rigorous competition, but the
men who are directing our industry must be brought to know
that future security will come to those factories only which main-
tain and follow the creative work of their research chemists
American directors of dyestuff enterprises must 1» brought to
•The address hy Grinm-ll Jones, not printed, was a n'sum' r,f the "Census
of Dyes and Coal-Tar Chemicals. 1917, Turin" Itiioi I
6," in press at the time of the meeting, hut "lit, imiM, no* b] applyingto
the U. S. Tariff Commission, Washington, l> I
a realization of this most important point, and to see that dol-
lars spent researching into the unknown along the lines shown
by trained experience to be most promising will reap a golden
harvest. Such has been the lesson of the past. The convincing
of the managers of the dyestuff industry of this fact is as much a
part of the work of our chemists as is the carrying out of the
laboratory or manufacturing procedure.
The relative condition of the industry in Germany in com-
parison with England and other countries just before the war
demonstrates the importance of this creative research work
absolutely and finally.
It was not the lack of chemists in England that prevented
her dyestuff industry, with its favorable start, from developing
as Germany's did, for the lack of these chemists would have been
supplied immediately had the demand for them appeared.
Englishmen directing their dyestuff industry' simply did not
recognize the paramount importance of the creative research
work for the permanence and development of the industry,
and from being initial pioneers, they became content largely
to trail behind the German effort.
Since the war England has been going ahead on a more rational
basis, and we here in America must take to heart the experience
of the past in Germany and in England and carry through into
full growth the industry of the coal-tar dyes.
I feel that by meetings of those chemists interested in dyestsuff
under the auspices of the American Chemical Society we can
go a long way toward furthering the permanent growth of coal-
tar dyes in all their complex ramifications here in America. I
do not mean to infer that the accomplishments of the American
dye manufacturers and American chemists in recent years, and
in the years since the war, have not been worthy of pride — far
from it — but I do not feel that we have been pioneers except in a
most occasional instance. To be sure, the pioneering must be
done along business as well as scientific lines. What may be good
business for one factory with certain classes of products and by-
products might be very bad business for another factory with
different products and by-products.
This development of by-products is a most important one,
and one that in the haste to turn out a given intermediate or
dye, the American manufacturer is prone to neglect. Dr.
Hesse lays great emphasis on by-products, and writes of them
as follows:1 "Broadly speaking, the entire coal-tar industry
is a complicated maze and network of interlocking and inter-
lacing products and by-products; these are great in number,
but, in most cases, small in volume individually. In numerous
instances the very existence of the by-products was the sole directing
cause for the invention of new dyes and classes of dyes."
The American manufacturer has always tended to bulk pro-
duction and this has also been true in England. This is un-
doubtedly the best policy to a certain extent, but our manufac-
turers, especially of dyestuffs, must realize that they must have
and offer a fairly complete line or else the same thing will hap-
pen in America as Dr. F. M. Perkin stated happened in Eng-
land, that is, the Germans came along with a newer, bigger, and
more complete line and took the business away from the domestic
manufacturer. Therefore, this is another way in which the
ran contribute, namely, by so designing the plant and
processes for those dyestuffs which have only a small market
dial they can lie manufactured on a relatively smaller scale
in a profitable manner. The economic laws of supply and de-
mand, coupled with that amount of reciprocity that the law
allows, will undoubtedly centralize the manufacture of those dye-
stuffs which have a limited market in tile hands of one or two
I Tims JOURNAi, 6 (1914), 1013.
790
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
manufacturers, who will, in turn, exchange or sell these products
for others of the same class manufactured in some other plant.
From time- to time, here and elsewhere, with regard to the
general policies of chemical plants, the remark is made, "What
does it matter if we are making money?" This policy is suicidal
in the long run, for continued success will only come to those
manufacturers who are always looking ahead and who view
planning for the future as an important part of the daily task.
The Germans, in the conduct of their very successful dye
plants, entrusted their direction largely, even up to the Board
of Directors, to technically trained men. England did not
pursue that policy iti the time prior to the war, although she has
changed somewhat since 1914. We must not forget the old
proverb, and neglect to learn from our enemy. In my own
opinion, this is an important reason for the German successes,
and it behooves the owners of our dye-stuff industries to call
into their councils continuously their technically trained chem-
ists and engineers, and this should be carried even up to their
Board of Directors.
In addition to the scientific work that the American Chemical
Society can do for the dyestufl industry in America, it can also
keep this industry before the public in the proper light so that
when the time comes when it is essential to establish the ade-
quate tariff or other legal protection, the American public will
be in a receptive mood to pay the necessary price, slight though
it may be, to protect the industry until it reaches the same scien-
tific and financial growth as its largest rival.
The chemists of America can show the close connection be-
tween the explosives industry and the dyestufl and pharma-
ceutical industries, and also that as a phase of national protec-
tion, it is necessary to have dyestuff plants. It has often been
remarked that dyestuff plants and personnel can, in time of
war, give great aid in manufacturing of munitions. I know of
instances in which dyestuff plants are manufacturing munitions
for the Government now that America is in the war, and I
further know that their dyestuff program has been set back by
such munition manufacture, but this is as things should be.
All in all, the work that lies before the dyestuff chemists of
America is promising as to the future, judging by accomplish-
ment of the past, and especially of the last few years. I trust
that this Symposium and its successors will contribute useful
stimulus to the continuous growth and development of the in-
dustry of dyestuffs.
AMERICA'S PROGRESS IN DYESTUFFS MANU-
FACTURING
By Louis Joshph Matos, Chemist, National Aniline & Chemical Co., Inc.
For centuries the peoples of the world have been addicted to
the use of coloring matters to produce variegated effects, not
only for raiment but for other decorative purposes. From the
earliest times there is ample evidence that the coloring matters
1 were of three chief classes, viz., animal, vegetable, and
mineral As a matter of fact, the coloring matters of animal
origin were very few in number, ami included dyes obtained
from certain varieties of shell Bsh, insects, and charred bone.
From shell lish has been obtained one of the most beautiful of
colors, namely, Tyrian purple, which, however, must not be con-
founded with another ancient and interesting color that has for
years attracted the attention of chen J pie of Cassius,
B tin gold compound Two other important dyes belonging to
the group of animal dyes are obtained from the cochineal, an
insect that thrives in the tropics. They are the scarlet made
famous by the uniforms of British soldiers in times back, and
carmine, a pigment used For ink making and in printing.
The vegetable kingdom has for centuries supplied the major
portion of the dyewares which have been handed down to us,
and which have played, even in recent times, a most important
part in the coloring of textiles. The various vegetable prod-
ucts include — first in importance, indigo, a native of the tropics;
madder, which yielded Turkey red and a small number of other
important shades; gall nuts, which the dyer of old used to pro-
duce blacks and other colors and shades; catechu or cutch, a
native of both the West and East India tropics, and which pro-
duces a shade of brown that has been duplicated with difficulty
by dyes of coal-tar origin; fustic, a tropical yellow wood of im-
portance; turmeric; quercitron bark and osage orange, the latter
two being natives of America; and logwood, probably the world's
most important source of black for wool and silk. Our list can
be augmented by the names of a number of other natural color-
ing matters that have played their part in the production of a
number of shades of lesser fastness and brilliancy, but a sufficient
number has been named to indicate the wealth of material the
dyer of the old school had to draw upon.
With a very limited number of exceptions, the great majority
of the natural dyewares have, in the course of time, been gradu-
ally displaced by products that possessed a more uniform qual-
ity, greater tinctorial strength, and vastly superior properties.
It is, however, only a question of time when these few exceptions
will be likewise displaced. In 1856 the world was startled
by the discovery of a coloring matter obtained from aniline
by a young man in England, William Henry Perkin. The
discovery which the world knew at that time as mauve or
Perkin's violet was ultimately destined to revolutionize the entire
dyeing industry and to mark the beginning of an epoch in indus-
trial chemical research and pure chemistry. The impulse given
to chemistry at that time has been constantly gaining momen-
tum as is evidenced by the great number of very far-reaching
discoveries, not only in dye chemistry, but in the chemistry of
products that have found wide use in medicine, photography,
and other branches of science. After the discovery of Perkin's
violet other chemists promptly took up the investigation of
aniline and other substances obtained from coal tar, with the
result that from 1856 upwards there was a rapid increase in
the number of dyes obtained from tar.
It is needless for me to give in detail the list of these products,
but it might be interesting to again record the most important
discoveries along this line that were made subsequent to the
discovery by Perkin: magenta, discovered in 1S5S; the produc-
tion of aniline black on the fiber by Lightfoot, an English chem-
ist, in 1862; in this same year the discovery by Nicholson of the
blues that bear his name; Poirrier's discovery of the methyl
violets in 1866; the discovery of alizarine in 186S, in which Per-
kin again played a most important part. Great credit is due to
the two chemists, Graebe and Lieberman, for the discovery of
the fact that alizarine was a derivative of anthracene and not of
naphthalene as chemists formerly believed, yet it was Perkin
who was responsible for the first successful commercial process
for producing this most valuable dyestuff, the discovery and
manufacture of which marked the downfall of the madder indus-
try. A study of the statistics of the period will show that sub-
sequent to iS6y the shipments of madder root were consequently
lessening until a time was reached when this natural product in
either the raw or ground state could be obtained only with
difficulty, in fact, the product itself had reached the position
of being but little more than a botanical curiosity. Of far-
reaching importance was the discovery by two Frenchmen in
1873 of the first sulfur color, known as Cachou de Laval,
which was the beginning of the development of an industry that
has reached very wide proportions. From time to time chem-
ists addetl to the list of sulfur colors various shades of black and
various colors, the use of which, in a number of instances, has en-
abled the dyers of cotton fabrics to inaugurate new and important
lines of goods. Methylene blue followed in 1S77. the azo scarlets
came upon the market in 1S7S, and their introduction marked the
beginning of the downfall of the cochineal industry. The discovery
Oct., 191 8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
791
of propiolic acid in 1 880 marked the beginning of what has grad-
ually developed into a most important industry, the story of which
reads like a romance. I refer to the production of synthetic
indigo. Tartrazine, the first fast acid dyeing yellow, appeared
in 1885, while two years later Professor Green in England gave to
the world the most important range of so-called ingrained colors of
which primuline was then and is now of considerable impor-
tance. This group of dyes has been from time to time gradually
increased so that at the present time a very wide variety of
shades is available to the dyer. Rhodamine, an extremely
valuable coloring matter, enabling the dyer to produce a very
wide variety of pink shades, was produced in 1893, while the
sulfur black previously alluded to was produced in 1895, being
the discovery of a French chemist. This brief outline of some
of the important dyes is given solely for the purpose of
emphasizing the important stages in the progress of this par-
ticular industry.
From the beginning of the coal-tar dye industry in 1856 until
the outbreak of the war in August 19 14 the dyers of America
were at peace with themselves and the world, there was no diffi-
culty in obtaining whatever dyewares were needed to keep their
mills going. Compound or mixed shades required by fashion
were obtained without difficulty and with the active cooperation
of chemical experts and colorists in the service of the various
dye-importing establishments of this country accurate matches
on various fabrics were promptly made and delays in the dye-
house were seldom encountered. When the war broke out, the
dyers, color makers, textile printers, mill owners, and superin-
tendents suddenly realized that the great bulk of the dyestuffs
they were then using and which they had obtained with so little
trouble came to this country from Germany, and with Germany
at war with half the world they were further brought to a real-
ization that many of the raw materials that entered into the
dyes were not likely to be obtained with any greater facility,
when the fact was considered that these same raw materials
were made use of by manufacturers of explosives. The dye-
stuff importers, confronted with these stern facts, were besieged
for information as to the probable situation. The story is
briefly told how the importers even went to the extent of charter-
ing ships for the purpose of bringing over dyes separate from
any other cargo. During the early months of the war small
supplies of dyes were landed, including some brought by sub-
marines. As the supplies of imported dyes gradually became
less, the situation became proportionately acute. Confusion
was paramount and at this time many inquiries were made by
the dye-consuming industries as to what had become of the
American dye industry, since it was believed by many that dye-
stuffs had been made somewhere in the United States. What
did become of these American manufacturers' The principal
plant in the United States at that time was located at Buffalo,
N. Y., and while it is true that many dyes had been produced at
that plant, it is likewise true that the raw materials and inter-
mediates of which those same dyes had been made had regularly
been imported from Germany. Consequently, the circumstances
were that while finished dyes had been imported from Germany,
the dyes made in America up to that time were manufactured
from German-made raw materials.
This situation put the American chemists to the test. Long
before the United States entered the conflict, the demand be-
came incessant for certain dyes that were very difficult or im-
possible to obtain, and which were sorely needed to keep a num-
ber of our textile mills in operation. This condition rapidly
aroused the interest of chemists and financiers so that eventu-
ally the two came together with the result that a number of
intermediate- and dye-manufacturing plants Sprang up through-
out the country. A number of these plants were devoted exclu-
sively to the manufacture of aniline and carbolic acid. The
aniline was used in various ways, but large quantities of it were
consumed in dye houses operating exclusively in the production
of fast black hosiery and other cotton goods. Much of the
carbolic acid found its way into picric acid plants, where it was
converted into that essential explosive. Other quantities of
carbolic acid were used in the manufacture of formaldehyde
condensation products, as well as for the manufacture of sali-
cylic acid. The dyestuff industry was compelled to get along
with few intermediates, mostly derivatives of benzol or naph-
thalene. Toluol, owing to the war necessities, was entirely lack-
ing, as every pound of that product was consumed by the manu-
facturers of explosives.
From time to time as the industry of the crudes increased in
this country, that of the intermediates likewise increased, so
that at the present time quite an imposing array of these latter
products are produced in this country. It should be kept in
mind, however, that even in the early days of the war, had there
been an abundance of some of the refined crudes, there was not
the necessary skill, either chemical or engineering, to proceed at
once with the work of turning out the much-needed raw mate-
rials for the dye maker. Many of us were familiar with the
laboratory production of a few grams of some of these highly
complex organic bodies, but when the practical application of
our laboratory knowledge was put to the test, upon even a semi-
factory scale, the results were not very promising— reactions did
not work out as the books assured us they would, yields likewise
failed to materialize, and it was only after close application and
many repetitions that a clue was obtained which gave an indica-
tion as to where the process in hand was weak. Gradually these
obstacles were overcome; while it is not intended to imply that
in every instance perfection has been achieved, yet very great
progress has been made, yields have been increased, impurities
of doubtful identity have been gradually eliminated, the finished
products have gradually increased, we see less and less of high
spots and low spots in our diagrams. On the whole, the situa-
tion is gradually clearing up and with the unselfish coop-
eration of both chemists and chemical engineers the manufac-
turing operations are becoming stabilized.
Let us not for a moment lose sight of the fact that the manu-
facture of almost each intermediate used by the dye maker
constitutes an industry in itself. For example, the manufacturer
of amidonaphtholdisulfonic acid, H-acid, is such a lengthy opera-
tion and involves sj many stages that those who are engaged in
its manufacture must give their whole time and attention to it.
The same remark applies to the manufacture of amidonaphthol-
sulfonic acid, -y-acid. I mention these two acids in par-
ticular because a large number of dyestuffs are obtained from
them in combination with other intermediates and the processes
involve almost every important operation made use of in in-
dustrial organic chemistry. In the early days of their pro-
duction in this country some phase of the work was not clearly
understood and it required prolonged experimentation to locate
the trouble, which sometimes was found either in the filtration
of certain solutions, in the melts, or in the drying.
I wish to draw your attention to the list of those products now
manufactured either by the National Aniline and Chemical
Company, Inc., directly, or in some of its affiliated plants; I am
sure you will agree with me that the list is imposing and were
you to take the time to go through the chemical and mechanical
operations involved in producing on a manufacturing scale Un-
it d you would realize that it has been no mean under
taking. The list is as follows:
Benzol
< >il «>f Murbane
I iinil inhcnzol
i Vniline
Aniline Soil
l':ir:i[thctiylcncdiamine
I 1 .1 '. ■
Metanitranilinc
Toluol
Nitrotoluol
Orthonitrotoluol
Hclanaphthol
Gamma Acid
K Salt
GSalt
Potash G Salt
Amiilo Q Sail
ff( 1 Sail
Mvtanilic Acid
Picrninic Acid
Ainido Salicylic
l,4-l)xy Acid
792
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
Paranitrotoluol
Dinitrotoluol
Metatoluylenediamine
Orthotoluidine
Paratoluidine
Mixed Toluidines
Xylidinc
Xylol
Nitroxylol
Cumidine
Diphenylamine
Naphthalene
Dinitronaphthaleue
Nitronaphthalene
Hydroquinone
Metol and Rubber Accelerator
II-Acid Dry
Distilled Benzidine
Nitrobenzol
Dinitrochlorbenzol
Paraamidoacetaniltd
Paranitraniline
Chromotropic Acid
Cleve's Acid
Koch's Acid
Naphtholic Acid
Sulfanilic Acid
Orthonitroanisidine
Dkuiisidtne
Nitro Cleve Acid
Amino Clevc Acid
Acetamino Cleve Acid
Carbazol
Crude Anthracene
Refined Anthracene
Anthraquinone
Alpha Naphthol
Dimethylaniline
Ethyl Benzylaniline
Nitroso Dimethylaniline
Diazo 1,2,4-Acid
Purified Diethylaniline
Anthraruffin
Resorcine
Phthalic Acid
Dinitrophenol
Monochlorbenzol
The basis of the dye-making industry is the foregoing, for
without the intermediates the dye maker is unable to proceed.
Fortunately at the Marcus Hook Works, Buffalo Works, and
Brooklyn Works a staff of chemists and workmen were already
in a position to undertake and carry on the dye-making opera-
tions as soon as the American factories were able to deliver the
intermediates, and this work has continued, uninterrupted,
to the present time. At the moment, owing to the war situa-
tion, certain much needed derivatives of toluol are not to be
obtained for the reason previously mentioned. Certain small
amounts of toluol, however, are permitted to be used for the
manufacture of some few dyestuffs necessary for soldiers' uni-
form material, but the general public is for the time being
debarred from using dyes in which toluol constitutes an impor-
tant ingredient.
Almost every dye chemist and colorist has been asked what
progress American chemists have made, whether we are looking
to the production of dyestuffs better than the Germans formerly
made or whether we are devoting our attention to the pro-
duction of new dyes. Answering the queries it might be well
to state at once, that we produce dyes in every respect the equal
in shade, strength, and working qualities of the pre-war type.
This the American dye manufacturer has been successful in doing.
He has not been able to produce every dye formerly imported,
but with a catalogue of about 175 dyes actually made in the
United States to-day from American raw materials and inter-
mediates, in quantity and variety sufficient for the wants of the
textile industry, one can regard the progress made as being re-
markable. Referring to the second question, the American
chemist has not had the time nor the opportunity during the
high pressure period of the war to devote his energies to discov-
ering new dyes, his whole time has been devoted to devising
successful methods for producing intermediates and dyes, the
chemistry of which required little or no further investigation.
Among the important dyestuffs that have been made in the
United States may be mentioned direct black, , a product of
great interest to cotton dyers and useful for many purposes.
This dye has been manufactured at tin- Buffalo Works of the
National Company in immense quantities, and since the war
commenced, entirely from domestic raw materials. Another
dye of great technical value is chrome blue, applicable chiefly
to wool. This dye possesses in a marked degree properties of
extreme fastness to light and weather, and therefore is almost
exclusively employed for dyeing sailors' uniform fabrics.
The dyes now being manufactured number about 175 and
include members of all the groups of colors used in American
mills prior to the outbreak of hostilities. This list 1 being
added to from time to time as progress is made in the produc-
tion of necessary intermediates
In addition to the foregoing the manufacture of synthetic
indigo is not to be omitted At one of the Works of the National
Company it is being produced and as rapidly as present condi-
tions of labor and material permit, the plant is being expanded
to a size that will deliver a quantity of indigo equal to, if not
exceeding, over half the requirement of the American market.
Another product of importance is alizarine. This is now
being produced from American anthracene at the Brooklyn
Works, in quantities equal to the total requirement of the mar-
ket, and is of a quality equal to any alizarine in paste form that
was ever imported. The manufacture of alizarine is an industry
within itself. When it was suggested that it be produced in this
country, the problem at once arose as to the source of anthracene,
since none of this raw material had ever been recovered from
domestic tars. It was known that anthracene existed in our
tars, but it was not until the necessity of supplying our dyers
with alizarine arose that steps were taken to isolate the crude
anthracene and refine it. This required a complete revision of
our usual mode of procedure, but it was successfully accom-
plished. There is no doubt but that the alizarine industry will
be permanent.
THE DEVELOPMENT OF THE DYESTUFF INDUSTRY
SINCE 1914
By J. F. Schoellkopf. Jr , of the War Industries Board
The idea of the present conference seems to me an especially
happy one, coming as it does just now when we are in the midst
of the greatest war in history and inclined to give attention to
those matters only which are directly concerned with the pro-
duction of material necessary to win the war. It is, of course, but
right and proper at this time that the production and chemistry
of war materials should have the first place in the minds of all
chemists, but it is well, at times, if conditions permit, to sit
back and think of what will, or may happen, when we are no
longer at war. I say this because I firmly believe that the prob-
lems which the American chemist will have to face in the after-
war period will be greater by far than any he has been confronted
with since 19 14, and you all know of what magnitude and com-
plexity these have been and how well they have been met. Be-
cause of these remarkable achievements of American chemists
during the past few years, I look forward to the future with
confidence and venture to prophesy that the place which Amer-
ica occupies to-day in the field of chemistry, which is at the head
of the procession, will be maintained hereafter.
The chemistry of dyestuffs which we are discussing to-day is,
it must be admitted, still in its infancy in this country and the
reasons for this will presently become clear. Germany, as is
well known, assumed the lead in this branch of chemistry some
forty years ago and has up to the present time held this, largely
due to tariffs "Made in Germany," and not as a result of superior
chemists. Why, you will ask, does this condition still exist
after we have had an almost unsurmountable tariff wall for
nearly four years? The answer is simple. For four years our
chemists and chemical engineers have been engaged in the work
of "catching up" with Germany, a task which is nearing com-
pletion, and one which has been done in a remarkably short time,
considering the difficulties encountered.
For the benefit of those who are perhaps familiar only in a gen-
era] way with conditions confronting the industry during the past
four years, it may be well to state as briefly as possible what some
of these difficulties were and how they have been effectively
overcome. It must be remembered that in 19 14 there were only
seven manufacturers of dyestuffs in the United States and
every one of these was dependent upon a foreign supply of
intermediates. The total production was less than 6,000,000
lbs., this representing approximately 10 per cent of the consump-
tion. Furthermore, due to the cut-throat competition of the Ger-
mans on those products made in this country, aided by an un-
favorable tarilT, the industry had made practically no progress
whatsoever during the preceding ten years and just before the
war came upon us its condition was going from bad to worse
When, therefore, in August 1014 the tremendous and sudden
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
793
demand for dyes came, the industry was in no shape to meet
it, especially as regards personnel, the working organizations of
the companies, as a necessary economic measure, having been
stripped to the bone. Most of us thought at that time that the
war would be a short one and hastily erected improvised build-
ings in which it was attempted to produce some of the more
important intermediates such as beta naphthol, paranitraniline,
H-acid, etc. As a result, early in November, these products
were being made in fair-sized quantities, sufficient at least to
make considerable quantities of the more staple dyes. The
situation in the fall of 1914 was not so serious, because the im-
ports from Germany had not ceased and large stocks were still
in the country, although these were largely in the hands of
speculators.
Previous to 1914 between 300 and 400 different dyes had been
imported into this country by the Germans, approximately 120
of which had been produced by American manufacturers. On
January 1, 19 15, we were only making about 16, so that you can
see what a big job was ahead of us.
In March 1915, the English blockade prevented further im-
ports from Germany and the real developments of the industry
may be said to date from that time. This brought home forcibly,
both to consumer and manufacturer, the fact that if we were ever
to become independent of Germany the opportunity was now
here. This opportunity was seized upon and immediately
the construction of new and modern plants was begun. In less
than six months these plants were producing, but it was soon
found that their capacity was entirely inadequate, although they
had served to more than double the pre-war production of the
country, and had enabled manufacturers to produce about 40
different colors by January 1, 191 6, as against 16 the year be-
fore. During the year 1916 older plants increased their facili-
ties tremendously, and the production of those who had newly
entered the field also began to be felt with the result that in the
early part of 1917 the ordinary needs for dyes were being met in
a satisfactory manner. The number of dyes produced by the
end of the year had increased to over 150, in other words, we
were producing a greater variety than was produced before the
war, and all raw materials and intermediates were of American
manufacture. According to figures prepared by the Tariff Com-
mission the production for 191 7 was nearly 46,000,000 lbs.,
approximately eight times the pre-war figure, and the value was
over S57,ooo,ooo as against $2,500,000 in 1914. Truly these
figures are remarkable and show better than words can what
has been accomplished.
Do not forget that all the men to build and operate these plants
had to be trained. It was impossible, as in the case of other
industries which have developed as a result of the war, to ob-
tain the services of experienced men by hiring them away from
competitors by inducements of a financial nature, or otherwise.
This was one of the greatest difficulties to contend with, but
was rendered comparatively easy by the remarkable adaptability
and ingenuity of the American chemist, engineer, and mechanic.
Considerable difficulty was also experienced in obtaining the
proper equipment for the plants, the design of which was in
most cases new and entirely different from anything previously
made by our foundries and machine shops. Here also, through
wholehearted and intelligent cooperation, our burdens were re-
duced to a minimum
Up to a short time ago, owing to the incessant demand for
dyes, the one idea of all manufacturers was quantity of produc-
tion, quality being more or less of secondary importance. Now
that the urgent needs of consumers are being filled, ih'1 pressure
is relaxing and it is possible to develop the various processes
in order that they may be made competitive. That is the big
problem we are facing at the moment, and one which i^ of the
utmost importance for the future of the industry. To meet
this the larger companies have established research laboratories
which will undoubtedly bring about the desired result'., and at
the same time train men for original work to be done in the
future. I do not mean to imply by this that our research labora-
tories are not doing any original work now. They are. But un-
til the processes for well-known dyes and intermediates are fully
as efficient as those of our foreign competitors, it is manifestly
more important that these be given preferential attention.
As a result of this work the quality of American dyes is con-
tinually improving, in fact, I do not believe that there are many
to-day which fall short of the former German standard. Natur-
ally, until the line of dyes made in this country is more
complete, there will always be complaints of a certain nature,
but the quality of the dyes made in this country is usually
not at fault. The cause of over 90 per cent of the complaints
which are registered is faulty application of the dyes. If the
dictators of fashions would take into account the dyes which
are available, all would be well, but they do not, for in order to
produce some of the prescribed shades, dyes not yet made in
this country should be used. The result is that unsatisfactory
substitutes must be used and complaints against the quality
of American dyes immediately arise.
As the complete and full development of the industry will,
in my opinion, require a period of at least another five years, it is
important that as much publicity as possible be given this par-
ticular phase of the situation. So much that has appeared in
the press during the past few years regarding dyes has been abso-
lutely futile and erroneous. What a pity it is this space could
not have been used to better advantage. It is interesting to
note that one of the large manufacturers is conducting an active
campaign along these lines, which is undoubtedly a step in the
right direction, counteracting as it does the insidious propaganda
against the quality of our dyes.
An important factor in the development of the industry is
the progress now being made in alizarine and vat dyes. The
most important of these, especially the latter, are covered by
German patents which have some years to run before they ex-
pire. By an Act of Congress the Federal Trade Commission has
been given the power to issue licenses under these patents to
domestic manufacturers, which fact has been taken advantage
of, with the result that this class of dyes may be expected on
the market within a short time. The importance of these dyes
cannot be over-emphasized, and only with their production in
this country will we be truly independent of Germany. It is
for this reason that it is imperative that a change be made in
our present tariff law which classes these dyes, as well as indigo,
separately, and provides no specific duty as in the case of other
dyes. It is my understanding that the Tariff Commission
which has made a study of the industry during the past two years
will report its findings to Congress in the near future. I do not
know what will be recommended, but I do know that unless
materially higher duties, than called for in the present law, are
placed on dyes, when peace does come it will place the industry
in great jeopardy. I make this statement because from ex-
perience I know how costly it is to develop new processes and
work experimentally on a large scale. Unless we can do this
regardless of expense for at least a period of years, our progress
will be slow indeed. Given, say a period of not to exceed ten
years of very high duties. I believe the industry will then have
grown and developed to such an extent that no further duties
of any kind, or at the most only very much reduced duties,
will be necessary. Why should not that be the case? We
have all the raw materials in this country and certainly our
chemists are the equal, if not the superior, of those bf any other
land. I could talk on about the tariff indefinitely, but believe
that I have covered iIm important points and have demonstrated
its importance with regard to the future of the industry.
In closing, I wish to pay special tribute to the untiring energy
and industry of those chemists and engineers who composed
the nucleus of the organizations which existed prior to the war.
It was upon them that the burden of all that has been accom-
794
THE JOURNAL OF INDUSTRIAL AND ENGIN EERINGJOHEMISTRY Vol. 10, No. 10
plished during the past four years rested most heavily and how
well they have borne it is not generally known and therefore
should be given special mention. The dean of these men is
Dr. R. C. R. Taggesell, chief chemist of the National Aniline
& Chemical Company, Inc., whom the writer has worked with
and known intimately for a long period of years. I can state
frankly that it is my opinion that without his superior knowledge
and untiring efforts the industry would not stand where it does
to-day. I am glad the opportunity has presented itself to
publicly proclaim this fact, knowing full well that the modesty
of the man would prevent it from becoming known in any other
way.
APPLICATION OF DYESTUFFS IN COTTON DYEING
By J. Merritt Matthews
Consulting Chemist, New York City
Cotton has become one of the principal textile fibers of
the world and now ranks alongside of wool and silk as the three
great sources of clothing material to meet the needs of the human
race. A great many will probably consider that cotton has al-
ways been in a very important position in this respect, but this
is not the case. It has been only during the last century that
cotton has come to the front, and this has been brought about
by the mechanical improvements in ginning, spinning, and weav-
ing, and to a great extent also by the manufacture of dyestufis
capable of readily dyeing the cotton fiber.
Before the introduction of the coal-tar dyestufis, the dyeing of
cotton, like the dyeing of wool or silk or linen, was dependent on
the use of the natural dyes and certain mineral pigments. As
most of the natural dyes require to be combined with a metallic
mordant before they yield useful and serviceable colors, and as
the cotton fiber has very little power of combination, or so-called
affinity, for metallic salts, the dyeing of cotton was attended
with many difficulties which were not present in the case of
wool, as this latter fiber readily combines with many metallic
salts that serve as useful mordants. In order to prepare the
cotton with a satisfactory mordant of metallic salt it was fre-
quently necessary to carry out very devious and complicated
operations, the very complexity of which caused the results to
be uncertain and exceedingly difficult to maintain uniform. This
is readily manifest on referring to some of the old recipes em-
ployed for the dyeing of cotton with the vegetable dyes.
With the advent of the coal-tar dyes it was soon discovered that
many of them could be applied to cotton by relatively simple
and effective methods. The basic colors which were first in-
troduced, it is true, still required a mordant in their applica-
tion to cotton, in this case the mordant consisting of tannic acid
fixed in the fiber by the use of a metallic salt, such as tartar
emetic. However, even this method of dyeing was a great
advance in simplicity and a person of average intelligence and
resourcefulness could soon master the art of dyeing by this
means. The acid colors which soon came into the market, it is
true, were only adapted to wool and silk, and found little applica-
tion to cotton, but when the benzidine or direct cotton colors
were introduced a new field in cotton dyeing was opened up and
the widespread use of dyed materials was much stimulated.
These colors, however, though varied and pleasing, were
limited in fastness, and this naturally restricted the utilization
of cotton fabrics. The introduction of aniline black as a spe-
cialized feature in cotton dyeing, however, greatly helped to ex-
tend the use of dyed cotton materials by providing an extremely
fast color.
The later introduction of various sulfur dyes also stimulated
if cotton material by providing a number of fast shades.
With the advent of the so-called vat dyes, however, permitting
of the production on cotton of a wide range of beautiful shades
of the highest possible qualities of fastness, cotton fabrics were
lifted out of their previous rather low-grade class and elevated
to the rank of fabric aristocracy. At the present time, there-
fore, it may be said that cotton materials are used for high-
grade fabrics, and in consequence demand the application of
high-grade colors.
In the application of dyestufis to cotton we must consider
several factors of prime importance. In the first place, the form
in which the cotton is dyed will have much influence in the selec-
tion of the dyestuff. Cotton may be dyed in the form of raw-
stock or loose unspun fiber, as cotton sliver; or in a partially manu-
factured condition, as yarn (either as skeins or hanks), as warps,
or as yarns on cops or tubes. Or the cotton may be dyed in
the fabric form, either as a woven piece or as a knitted fabric.
Dyestufis that are suitable for raw-stock dyeing may not be
suitable for dyeing woven cloth or knit fabrics, and vice versa.
Cotton warp dyeing requires special consideration as to dye-
stuffs. Cops and tubes are dyed in special machines and
the method of dyeing imposes certain restrictions on the kind
of dyestufis to be used. It will be seen, therefore, that the
man who contemplates manufacturing and marketing cotton
dyestufis must be more or less familiar with the processes of cot-
ton manufacture to be in a position to properly select the
products that are the more desirable.
Another consideration that is important in selecting cotton
dyes is the kind of material into which the fabric will be manu-
factured and the eventual use to which it will be put. This witt
determine the qualities of fastness of the dyestuff to be em-
ployed. Cotton goods go into all kinds of materials at the
present time; we have shirtings for men, blouse and skirt ma-
terial for women. These are more or less in fancy colors, but
as a rule the amount of color is only a small proportion of the
total fabric. These goods are subject to repeated washing;
and laundering, and they must also stand exposure to light and
perspiration, so it can readily be seen that the colors must be
fast to these agencies and a high class of dyestuff is required.
Before the war the vat dyes were being largely used for these
goods and the public was being educated to expect a color that
would last even longer than the fabric under the severe condi-
tions of laundering, especially as most modern laundries now
employ strong bleaching agents, such as hypochlorite of soda,
for the rapid whitening or bleaching of the cotton goods. Under
the present conditions there are practically none of these vat
dyes available, as they are not being manufactured in this coun-
try and it is to be presumed that all the old stocks on hand
have been used up.
We also have ginghams and fancy cotton goods which have
become quite popular as dress fabrics during the past couple of
years, replacing light weight woolens and worsteds, and even
silk to a considerable degree. The dyeing in this case is also
chiefly in fancy colors and should possess about the same de-
gree of fastness as just related, for these are all wash fabrics.
Next we have cotton denims used so extensively for overalls
and similar garments. Though this class of fabrics is perhaps
not so much before the eye of the general public as some others,
it is one of the great staples of the cotton business and very
large amounts of dyestuffs are used in them. The principal
color used is blue, the fancy shades being negligible in amount,
and the chief dyestuff used is indigo — in fact, this is where the
great bulk of indigo is used. The color has to withstand very
severe usage and repeated washings. Logwood can be used
to approximate the shade, but the fastness is very inferior.
Sulfur blues can be used with good advantage, and there are
some who may be inclined to maintain that sulfur blue is as
satisfactory for this work as indigo. Hydron blue, which may
also be classed as a sulfur dye, though in reality it is a vat dye,
is eminently satisfactory, in fact, in many respects it may be
considered as superior to indigo. But the trade has long been
accustomed to indigo and it will probably stick to it for a long
time to come.
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
795
Cotton hosiery is another form of manufactured product which
takes a large quantity of dyestuff. Of course, the chief color
here is black. Formerly most of the hosiery was dyed with
aniline black, a color developed on the fiber from aniline itself,
but now sulfur black is the principal dye used with also a goodly
quantity of direct black. There are also a number of colors
dyed on hosiery, such as tan, blue, and a relatively small line
of fancy shades. The logical and best dye to use in such
cases are the sulfur colors.
For cotton warps, used largely for cotton worsteds and for
cotton-effect threads in other lines of woolen fabrics, the sulfur
colors are also best, as they stand the cross-dyeing operation of
dyeing the wool in the woven piece. Certain of the substantive
colors may also be used.
It is not my purpose to go into all the different varieties of
cotton dyeing, as this would require too much detail, so I have
simply touched the chief points, as it were, to indicate the wide
variety of uses of dyestuffs in cotton dyeing. It will be easy
to understand why a number of different classes of dyes are
required and why a few restricted colors cannot be applied
to all forms of cotton materials. Piece goods are largely dyed
with the direct colors, and these are also used on various lines
of specialties where a great fastness to washing is not required.
The basic colors are also used to a considerable degree on cer-
tain cotton materials for bright fancy shades, and even in a
few cases some of the acid dyes are so employed for bright
shades of good fastness to light but of no required fastness to
washing.
As to the relative proportion of the different dyes used, this
is very difficult to ascertain with any degree of accuracy and
only a crude approximation can be given. As may be under-
stood from what I have already said, black is the chief dye used,
with blue in the second place. If we include the blacks dyed on
cotton with logwood and aniline black probably the following
would approximately represent a fair proportion:
Color Per cent
Blacks 60
I Sulfur Black
Direct Black
Aniline Black
Logwood
Developed Black
[ Indigo and Vat Blues
Direct Blues
I Basic Blues
Sulfur Blues
I Acid Blues
Congo Red
Benzo Purpurine
Direct Fast Reds
Alizarin Red
I'rimuline Red
Para Red
Vat Reds
A consideration of these figures will immediately show us
why our dyestuff industry has spent most of its energy so far
on the production of certain lines of dyes and why a large num-
ber of the fancy shades have not beer, touched upon as yet. Of
course, these relative proportions at the present time are con-
siderably thrown out of the normal by the tremendous demand
for Government cloth, which is chiefly in khaki, olive drab, and
navy blue. The Army requirements, of course, have sent up
the proportion of brown colors for cotton goods to an enormous
degree, and sulfur brown, for instance, which normally is not
a dye of very large tonnage, at the present time is one of those
produced in largest amount. In this connection we must also
not forget that quite a high percentage of heavy-weight cotton
goods are dyed with mineral or pigment colors to produce the
khaki brown. This color is obtained with a mixture of chrome
and iron salts by simple precipitation of the oxides in the fiber.
Sometimes manganese salts are also used, but at the present
time these are scarce and of high cost. In respect to tonnage
of cotton dyed, this mineral khaki brown forms a very important
item, as the cloth dyed in this way is mostly heavy canvas for
tent material, wagon covers, tarpaulins, etc.
In the selection of dyestuffs for cotton from the dyestuff
manufacturer's point of view, the first consideration is the quan-
tity of the dye consumed by the trade. If this is only small
and represents but an insignificant turnover during the year,
it does not appeal to the business sense as an attractive proposi-
tion. Before the war the various German dyestuff houses had on
the market quite a large number of direct cotton colors — one
would believe almost too many for profitable production. Many
of these varied very little in shade and properties, and the con-
sumption of many was relatively small. It is hardly to be pre-
sumed that our American manufacturers are going to bring
out all these various brands of dyestuffs. The most sensible
procedure would be to fix on those which offered the most advan-
tages with respect to quality of color and fastness, and if there
are several very near duplicates of one another, select for manu-
facture the one most economical to produce. We must also
bear in mind that many of the direct cotton colors have a serious
lack of fastness to washing, and while they are extremely sim-
ple and easy to apply and give good clear colors in combination,
yet fastness to washing is being more and more required for
colored cotton goods, and dyes which do not possess this fast-
ness will have a very limited use.
It is believed that in the dyeing of cotton the sulfur dyes will
have a greater development in this country than they ever had
before. It is true they are somewhat limited in range of shades,
but blacks, blues, browns, yellows, green, and orange are within
the list. They also have the limitation that they are rather dull
in tone. But their good fastness to washing is greatly in their
favor; also their fastness to acids allow of their use in cross-dye
work which much extends their field of application. A large
number of useful shades can be obtained by combinations of
the sulfur dyes, although the want of a satisfactory red and green
dye in this class seriously limits the possibilities for the produc-
tion of fancy shades.
NATURAL DYESTUFFS— AN IMPORTANT FACTOR IN
THE DYESTUFF SITUATION
By Edward S. Chapin
Consulting Chemist, Boston, Massachusetts
"Natural dyestuffs" is a term so broad and covers so many
interrelated fields of investigation and practice that it will be
possible in the brief space of this paper to treat only certain as-
pects of the subject in a fragmentary way. I shall be happy if I
can draw attention to the importance of the study of natural
dyestuffs, and if this may result in an increased interest in
and attention to these products on the part of American "science
and industry.
On the basis of the data of the past, the study of natural dye-
stuffs should lead to new and important developments in dye-
stuff chemistry and to results of high value to industry.
A little over a century ago, in 1810, M. Chevreul remarked
before the Institute of France: "When we consider the progress
that chemistry has made in recent years, we are astonished at
1! amount of exact knowledge in existence concerning the
coloring matters of the vegetables, and at the little attention
that has been paid to their study." This celebrated investiga-
tor attacked the subject with characteristic thoroughness.
A century of chemical research and development has rolled
by, and to-day there is in existence a considerable amount of
exact knowledge concerning natural dyestuffs. Among the chem-
796
THE JOURNAL OF INDUSTRIAL AND ENGINEERING < HEMISTRY Vol. 10. No. 10
ists who contributed to this development should be mentioned
Professor Graebe of Geneva, Professor Kostanecki of Berne,
Professor Herzig of Vienna, and of particular interest to dyestuff
chemists, Professor A G. Perkin, and Professor W. H. Perkin,
Jr. It is of special significance that the illustrious son of the dis-
tinguished discoverer of coal-tar dyestuffs spent over a decade,
1896-190S, in the study of brazilin and hematoxylin, the color-
ing principles of the natural dyestuffs known in the trade, re-
spectively, as hypernic and logwood.
Just prior to the present war, scientific thinkers were turning
with ever greater frequency and deepening interest to the study
of natural products; indeed some even were so bold as to state
that the trend of all the scientific development of the past half
century was to bring chemical science in humility to learn of
Mother Nature.
Witness the conclusions of Professor Ciamician as voiced at
the Eighth International Congress of Applied Chemistry, in New
York, September 1912.
"The plants are unsurpassed masters of — or marvellous
workshops for — photochemical synthesis of the fundamental
substances. They also produce the so-called secondary sub-
stances with the greatest ease. The alkaloids, glucosides,
essences, camphor, rubber, coloring substances, and others are
of high commercial value.
"The chemistry of benzene and its derivatives does not now
constitute the favorite field of research as it did during the
second half of the last century. Modern interest is concen-
trated on the study of the organic chemistry of organisms,
i. e., plants or animals. This new direction in the field of pure
science is bound to have its effect on the technical world and to
mark out new paths for the industries to follow in the future."
Witness further the conclusions of Dr. Arthur D. Little in
an address delivered in Baltimore in 1908, before the Division
of Industrial Chemists and Chemical Engineers:
"And this brings me to the main point of my thesis. A great
German chemical company tells us, in an attractive book just
issued, that it employs 218 chemists, 142 civil engineers, 918
officials, and nearly 8,000 workmen. It covers an area of 220
hectares, has 386 steam engines, 472 electric motors, and 411
telephone sub-stations. Its plant represents the highest de-
velopment which industrial chemistry has reached, but none
the less, it cannot produce an ounce of starch which a potato
growing in the ground fabricates from water and carbonic acid
gas under the influence of sunshine.
"Professor Wheeler has defined so clearly a thought which has
been in my own mind for years, that I cannot do better than
quote his words. He says:
" 'The vegetable cell is a laboratory in which are carried out a
most remarkable series of chemical reactions. As we con-
template the immense number of organic compounds of all
degrees of complexity which are formed within the wall of the
plant cell, we are convinced that this is the chemical laboratory
par excellence.. .We are led to wonder whether forces exist with
which we arc not acquainted or whether we are merely unable
to control the forces already familiar to us. It will be granted
that investigation into the activities of the cell is of profound
importance. In fact, it has been said that it is in the plant
cell where synthetical operations are predominant, that we have
to look for the foundation of the new chemistry.' "
Into- the midst of this peaceful and reasonable development
ruthlessly came the world war with its quick dislocations and
disturbances. At fust it was fondly imagined that these would
be only for a short time, and that somehow, though nobody
could till how, in a few months or at the most in a year, the war
would be over and supplies of dyestuffs would again come from
Germans as heretofore, and chemical science ami technics would
again take up their orderly development beginning at the point
at which they stood before the war. This, however, was not
to be 'flu- war continued with an ever widening grasp and
intensity, dragging ultimately our country, our industries, and
our science into the [rightful vortex.
A most significant chapter of American industrial history oc-
curred during what has been called the dyestuff (amine period
of 1915-10, before the American artificial dyestuff' manufac-
turers had reached volume production and when supplies of
synthetic dyestuffs in the country were either low or exhausted.
It was predicted freely that for lack of synthetic products the
mills of the country would be forced to shut down, industry
would stagnate, and thousands upon thousands of workers
forced into idleness. The natural dyestuffs saved the day.
Natural dyestuffs were used for all sorts of purposes. Results
were, as a mattter of course, good, bad, and indifferent.
With experience and improved methods of application, su-
perior results were secured. The prophecy, that for lack of
artificial dyestuffs the mills would be forced to shut down, has
long been discredited; but this dire catastrophe would have
occurred if it were not for the yeoman services performed for
American industry in the critical period 1915-16 by the natu-
ral dyestuffs.
It has been a matter of surprise and even of some incredulity
to many chemists that the natural dyestuffs were able to per-
form this notable service. The reasons are not far to find. So
much more work has been done on the study and the develop-
ment of synthetic products, there were so many more synthetic
products of such varying and wonderful properties, these prod-
ucts had been so widely, assiduously, and cleverly adver-
tised, and it was such a source of pride and gratification to try
to improve on Nature, that the majority of chemists confined
their attention solely to synthetical products, and knew nothing
about natural dyestuffs and the possibilities in industry from
their scientific application to fibers and materials.
As a matter of fact, even just prior to the war more than one
hundred thousand tons of dyewoods were used annually in
American industry. These products were used in spite of the un-
wearying efforts of an aggressive propagandism to displace them
with synthetical products and used because the results from the
natural dyestuffs were more economical or superior.
These unrivaled results from natural dyestuffs were due to
certain definite chemical groupings or complexes, or to certain
special methods of their application to materials and fibers.
Among the natural dyestuffs that have performed notable
special services in the past few years and that were in consid-
erable use prior to the war, may be mentioned logwood and
hematine, fustic bark or quercitron, flavine, hypernic, archil
or cudbear, sumac, catechu or cutch, and gambier. During the
war osage orange has been added to this list.
All of the above mentioned dyestuffs, except archil and sumac,
derive their chemical significance from a parent body known as
7-pyrone, C6HiOs. The -,-pyrone ring has a configuration as
follows:
/°\
HC CH
i1 II
HC CH
\C/
O
The monophenyl ortho condensation of 7-pyrone is called
chromone and has the configuration
XCH
\C/CH
O
The oxy derivative of chromone, called chromonol, is repre-
sented as follows:
XCH
-C(OH)
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
797
Phenylated chromone, called flavone, is:
li N /
O
Phenylated chromonol, called flavonol, is:
,C(OH)
The actual coloring principles of the natural dyestuffs are more
complicated in structure and in some instances controversy
concerning their exact configurations has been long continued
and voluminous.
In 1893-1894 it was decided that quercetiu. the coloring
principle of quercitron extract, is constituted as follows:
O OH
OH
\r/
C(OH)
O
The morin of fustic followed in 1896-7, represented by:
O HO
OH
,C(OH)
Brazilin, the coloring principle of hypernic, was formulated
finally in 1908 by Sir W. H. Perkin, Jr., as follows:
AK
HOf XCH.
I
xC(OH)
HO OH
Hematoxylin of logwood was represented similar to brazilin,
with one more hydroxy grouping:
HO
HO/
XCH,
/C(OH3
o
HO OH
The researches of Perkin, Htrzig, and Kostanecki on brazilin
and hematoxylin are classics of chemical investigation. The
oxidation of hematoxylin yields hematine, to which Sir W.
H. Perkin, Jr., gave the formula:
HO
HO,
CH2
I
/CtOH)
These various derivatives of the oxygen containing , pytone
ring are different in properties from their more widely known
all-carbon-ring brothers and sisters. These differences are
well summed up by Reim.1 He says that hematoxylin cannot
be nitrated. Hesse has shown that it cannot be sulfonated. It
gives no useful substitution products with chlorine or bromine.
It is attacked by phosphorus pentachloride, but it is impossible
to isolate from the result a pure compound. It does not take
up hydrogen either with sodium amalgam or zinc and sulfuric
acid. It gives no compounds with hydriodic acid or hydro-
bromic acid. With potassium chlorate and hydrochloric acid
it yields resinous non-crystallizable products. It gives with
' zinc dust crystalline bodies, but these cannot be isolated.
The question naturally arose whether this sensitive compound
could not be protected in some manner from too rapid decomposi-
tions. Before going further it will prevent confusion to state
that brazilin and hematoxylin behave similarly toward reagents
and chemical processes. Brazilin, as already noted, contains
one less hydroxy group than hematoxylin. Brazilin as being
the simpler body was first studied by investigators. The re-
actions developed were applied to hematoxylin. In the course
of an extensive series of studies, Prof. C. Schall and Chr. Dralle2
discovered methyl brazilin. Trimethyl brazilin and tetra-
methyl hematoxylin are relatively stable products, and from
these protected brazilin and hematoxylin compounds, in the
course of two decades of intensive investigation, a numerous
list of derivatives has been prepared, of which we have time* to
mention only the more noteworthy.
The methylation of hematoxylin under certain specific condi-
tions forms a tetramethyl hematoxylin. This substance oxi-
dizes to a ketone, tetramethyl hematoxylone. Tetramethyl
hematoxylone readily acetylates to acetyl anhydro tetramethyl
hematoxylone, which reduces to a-auhydro tetramethyl hema-
toxylone. a-Anhydro tetramethyl hematoxylone reacts like a
complicated (3-naphthol, and accordingly we find that it can be
combined with diazotized amines to form azo dyestuffs. A jS
series of derivatives also exists. 0-Anhydro tetramethyl hema-
toxylone reacts like a complicated a-naphthol and accordingly
can be combined with diazotized amines to form azo dyestuffs.
Acetyl anhydro tetramethyl hematoxylone nitrates to nitroacetyl
anhydro tetramethyl hematoxylone, which reduces to amido
acetyl anhydro tetramethyl hematoxylone.
Significant as these derivatives from hematoxylin may be,
it is not to them alone I would call attention. To consider
them alone would be to miss the other factors that give to log-
wood extract, to hematine crystals, and to the various forms of
natural dyestuffs their unique values for industry. "The new
direction in the field of pure science," mentioned by Prof. Ciami-
cian, and "the new chemistry" mentioned by Dr. Little and Prof.
Wheeler will undoubtedly explain these factors: at present these
remain a mystery and we are able to enumerate only the special
results from the applications of natural dyestuffs, and to try by
pure science, new chemistry methods, or what you will, to trace
our way from the results to the cause, or from the cause to the
results.
The results from natural dyestuffs that are of special value to
industry may be best illustrated by a consideration of the best
known and most prominent of the natural dyestuffs, logwood,
as it is called.
The term logwood stands loosely for a variety of products
found in trade that are derived from a tree known botanically
as Hematoxylon campechianum. The extraction of the dye-
stuff principles from the tree and the subsequent treatment of
the liquor of extraction are matters of exact technics, and con-
siderably influence the results obtained in industry. Logwood
extract, usually furnished to the trade at a consistency of 51 °
Tw.. is obtained l>v the concentration undei vacuo <>f the ex-
traction liquors; the coloring principles analyze 85 to8o pel ■ a1
1 "r, i„ , ,1 , li. m itoxylin," Btr., t (1871) 129
1 "Eta neues Brazilin Derivat," Btr., 20 (1887)
798
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
hematoxylin and 15 to 20 per cent hematine. By oxidation of the
logwood extract, the hematoxylin is changed to hematine. The
hematine pastes of the trade will run anywhere from 45 to 90
per cent of hematine, the amount of oxidation being determined
largely by the purpose for which the hematine is to be used.
Logwood extracts and hematine pastes can be brought down
to solid or crystal form, and as such are found in the trade as
solid extract of logwood, or logwood and hematine crystals.
In reality the complexes in logwood extract and hematine pastes
are more intricate than the analyses above given.
Logwood enjoys unique distinction in dyeing black on ma-
terials and fibers. It dyes wool, silk, cotton, leather, and a great
variety of fibers and materials. It is the most generally all-
round useful dyestuff for dyeing black. It is also used for the
weighting of silk.
The results with logwood on the wool and the silk fibers best
illustrate the peculiar excellences that can be secured by the use
of this natural dyestuff.
Logwood produces on wool a particularly handsome and fast
black. The logwood effects cannot be equaled with artificial
substitutes. The underhand solid blueness and the overhand
lofty bloom of logwood blacks on wool are proverbial. During
the great period of activity in the synthesis of acid and top-
chrpme blacks, the logwood black was used as a standard of com-
parison, and the usual words, reiterated almost monotonously
as each successive product was placed on the market, were these :
"Nearly equal to logwood black in rich blueness and bloom."
It has been the despair of the artificial color chemists to secure
one synthetic product combining these desirable properties.
In addition to these tinctorial superiorities on wool, logwood
possesses other properties that are noteworthy. It is a friend
to the colorist under good and adverse conditions alike. Such
cannot be said in the same measure of the artificial substitutes
for logwood. Logwood dyes uniformly, levels excellently, and
penetrates perfectly. It dyes slowly. It may be fed at a
boil. The widest blends of stock are evenly colored and pene-
trated by logwood. Defects in wet and dry finishing are most
successfully offset by its use.
Under artificial light the handsome logwood black does not
lose its beauty, but, on the contrary, retains its rich, pure tone
and, if anything, is intensified in brilliancy and richness. Arti-
ficial substitutes for logwood do not stand artificial light as well
as logwood; indeed some lose their daylight tone altogether,
becoming dull or brown. For evening clothes and for a large
variety of suiting and wearing apparel, this superiority alone,
other things being equal, establishes a preference for the use of
logwood.
If these facts are true, why, asks the intelligent inquirer, has
logwood ever been displaced at all on woolen and worsted ma-
terials? Among various reasons that may be given there is
one above all others that is peculiarly cogent to modern business
temperament. Compared with top-chrome blacks and acid
blacks, tin- dyeing with logwood takes more time. Cries effi-
ciency, we must at all hazards have the utmost of production;
quality is sacrificed to quantity. A brilliant young colorist
has remarked, "If logwood could be dyed to give the same pro-
duction as top-chrome blacks, there would not be a pound of
top-chrome black used in the country."
While this prophecy is extreme, it contains a kernel of truth,
and points to an objective for research. Top-chrome blacks
would undoubtedly be used in dyeing because of certain inherent
excellences, even if logwood blacks could be colored by one-dip
processes with equal rapidity.
Nor is the suggestion to color logwood blacks by one-dip
processes an idle fancy. Already various investigators have
obtained noteworthy results, though the processes have not
been tried out over a long period of time in industry.
The production factor on silk, strange as it may seem, is in
favor of logwood. Prior to the discovery of the value of
logwood for the weighting and dyeing of silk, processes in vogue
were most tedious. A little over a decade ago Dr. Heermann1
discovered that these processes could be greatly shortened and
improved by the use of logwood. Logwood seems to have a
biological relationship to the silk fiber. The silk fiber will ab-
sorb 200 per cent of its own weight of logwood. The volume of
the silk in the process is considerably enlarged, and the dura-
bility of the silk and its resistance to wear and tear are improved.
This important discovery has been utilized in the past years on a
large scale by the silk dyers of the world, and has created a veri-
table revolution in the silk industry.
The various synthetic top-chrome and acid blacks possess no
such biological relationship to the silk fiber, and accordingly
are utterly incapable of producing these special results so highly
prized by silk people.
An erroneous impression has prevailed in chemical and trade
circles that logwood blacks are not fast: in particular are not
fast to light. Logwood blacks properly dyed are of excellent
fastness to light, fulling, boiling in water, and the principal
mill and service requirements considered in the choice of a fast
dyestuff. Toward strong acids as hydrochloric and sulfuric
acids, and toward chlorine, logwood blacks are not fast. This
prevents their use on cotton where subsequent cross-dyeing with
strong acids or subsequent bleaching is required, but has no
effect on their use to color a vast array of materials and fibers
for numerous other purposes in the arts.
The elaboration of the use of logwood in the dyeing of leather,
the dyeing and printing of cotton, and the dyeing of hair, wood,
and various other fibers and materials would push our paper
beyond prescribed limits. So, too, with the exposition of special
results obtained by the use of the other natural dyestuffs.
The unique properties that distinguish logwood for black
dyeing find their parallel for yellow dyeing in fustic, osage
orange, and quercitron. Catechu or cutch produces on cotton
a rich reddish brown of extraordinary fastness.
It is of interest to note in passing that the yellow natural
dyestuffs and cutch are being most extensively used in the
dyeing of the olive drab shade on various of the woolen and
cotton fabrics for the Army; and that these results, when prop-
erly dyed, stand the prescribed tests of the Quartermaster's
Department satisfactorily.
We have now briefly reviewed certain fundamental facts re-
lating to natural dyestuffs. A careful consideration of these
facts will show that the study of' natural dyestuffs will con-
tribute materially to our fund of exact knowledge and conse-
quently to the further development of industry. Such study
will call for the utmost of energy and resourcefulness from the
devotees of pure science and of scientific dyeing. It is not
too much to hazard the prediction that if we will thoroughly
investigate these remarkable organic compounds and com-
plexes, formed within the chemical laboratory of nature, we
shall witness the dawning of a new era in pure and applied chem-
istry.
THE MANUFACTURE, USE, AND NEWER DEVELOP-
MENTS OF THE NATURAL DYESTUFFS
By C. R. Dklaney, of J. S. Young and Company, Hanover, Pa.
It is a cause for particular gratification to a representative
of the actual manufacturers of dyewood extracts to be asked to
address such a body as this in reference to products of which one
hears little in comparison with the newer artificial colors,
but which, nevertheless, have been and still are of inestimable
value to the various trades for which dyestuff production is the
key industry. The dyewood extract manufacturers have been
so exceedingly busy for the past four years for one reason and their
1 "The Use of Logwood in the Dyeing and Weighting of Silk," MM.
Moterialprufuntsaml, 4 (1909). 22S.
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
799
natural reluctance during the past fifty years to talk about their
own work for another, it seems that no one has felt that he had
the time to do more than roughly outline the volume and im-
portance of the natural dyewoods, while in direct opposition
to this stand, the artificial color makers, obviously taking a page
out of the book of the German manufacturers, whose products
they are imitating, have been conducting a very violent adver-
tising propaganda, all of which we, of course, have recognized,
but having been familiar with the German products of both
natures, namely, anilines and advertising, the dyewood makers
have simply exhibited a more or less mild curiosity when they
saw the German products transferred from German sources
to American ones.
We all appreciate in our work that there are very necessary
uses for the artificial colors, but unlike the unthinking, we know
that there is a very large use for our own. In fact, a chemical
analogy will indicate what might be called our state of mind.
We all appreciate the value of saccharine, the synthetic product;
we appreciate what the chemist has done in producing this ma-
terial so much more powerful than sugar, which, for certain
purposes, it can replace, but we have yet to hear that anybody
used saccharine with his buckwheat cakes, preferring the product
of Nature's own chemist, the bee. It is the same with a great
many dyers who all appreciate the strength, the ease of use, and
other salient points about the artificial colors, yet, as in the case
of saccharine, there seems to be something wanting, and recently
I read a statement made by one of the most celebrated artificial
color chemists in which he said that all artificial blacks were
judged according to their ability to compare with logwood.
It is obvious to all chemists that the explosives industry and
the artificial dyestuff industry are concomitant, but do you not
sometimes lose sight of the fact that the tanning industry and
natural dyestuff production carry the same analogy? At forty-
eight hours' notice any one of our dyewood extract plants can be
converted into the manufacture of tanning extracts, and while, of
course, the enormous profits of the explosives business, due to
its hazards, have certain attractions, nevertheless, there has been
a proverb since the time of the early Egyptians that "there is
nothing like leather." And while on this subject, it might be
well to say that to this date there has been found no substitute
for natural dyestuffs for the penetration of leather in dyeing it
black.
The prize that all of us have been striving for has been the use
of our products by the United States Government, and I
rather doubt that any of the artificial color people have any-
where near the total proportion of output in Government con-
tracts that the natural dyestuff makers enjoy. A recent ques-
tionnaire sent out to every one of the customers of our company
between the period of January 1 and June 30, 1918, discloses so
far that 72 per cent of their production of Flavine was used for
Army business, also the following percentages of their other
products: quercitron bark extract, 33 per cent; logwood extract,
80 per cent; domestic sumac extract, 42 per cent; and divi divi
extract, 50 per cent. These percentages would be much higher
were it not for the fact that another end of the industry,
namely, the wall paper trade, which has always used the natural
colors owing to their cheapness and greater efficiency for their
work, docs not come under the heading of war necessities and,
therefore, we have been compelled to deduct the very consider-
able quantity they consumed from the totals.
In addition to our own country, Canada, France, England,
Russia, Italy, Australia, India, and Japan are using larger
quantities of our products than they ever did, at least, as far
as our own exports show. It is unfortunate and thoroughly
representative of the conservatism, to give it the mildest name,
characterizing the dyewood extract manufacturers that they
have never partaken of the benefits of any propaganda that
would bring to the attention of the consumers of dyestuffs
the advantage of the natural products over the artificial, and
as a result, it seems as though the manufacturer of natural dyes
has been lost sight of by a very large number of those people
who in reality could actually use the natural dyewood extracts
for the colors that they wish to produce instead of the foreign
dyestuffs and their imitations upon which they have learned to
depend.
It is hardly necessary to inform you that the oriental rugs
of several hundred years ago still retain their beauty and bril-
liancy of color to the present day, and if anyone cares to inves-
tigate the clothing of three or four hundred years ago they would
find that at the courts of France, in particular, there were colors
of vegetable origin used in silks and satins that would rival the
most gorgeous shades of the present day. The oriental rug
will dispose permanently of the argument as to whether natural
colors are fast. Of course, if any extraordinary and ridiculous
tests are made, such as boiling in caustic or spotting with acid,
generally the natural dyestuffs, unless specially prepared, will
be found wanting; but for our part, we always have thought
that until clothes were boiled in acid in order to clean them it
was hardly necessary to employ such tests as indices of the
quality of the dye. If they will stand the exposure to the air
and rain and sun and will not run or bleed into surrounding fibers,
we believe that they have fulfilled their destiny, and it has
always been the aim of the natural dyestuff maker to produce,
shall we say, honey rather than saccharine.
Possibly you may have seen in various trade journals a rather
surprising statement to the effect that prior to the war 60
per cent of all the concentrated yellow dyestuff that we manu-
facture under the registered trade-mark name of Flavine was ex-
ported to two very large artificial dyestuff manufacturers in.
Germany and Switzerland. In fact, had it not been for the
business that we enjoyed through them it is probable that the
manufacture of Flavine would have been discontinued, owing
to the fact that we did not appeal directly in the United States
to the textile industry as it was something that no manufac-
turer then could do — compete with the German manufacturers —
and retain his self-respect at the same time. However,
our foreign business was enough to keep that section of our
plants operating and this would indicate that some of the dyes
manufactured in this country are of value to those who formerly,
we were in the habit of thinking, were the leading authorities. As
far as the manufacture of dyewood extracts is concerned, it is
exceedingly simple, and yet there are one or two things that
have to be thought of and taken into account at the same time.
Our coal-tar friends have a number of exceedingly complex reac-
tions to look after and they produce materials with unforgivable
names. They, of course, know everything about what they are
doing, but we in our business are different. We try to produce
the same kind of material to-day that was produced fifty years
ago and have a hard job keeping it precisely identical, and this
is where we need and use the best chemists that we can secure,
in spite of the fact that when we get all through our material is
known as extract and not, for instance, as monosulfonodioxy-
anthraquinone.
To cite a homely illustration of the dyewood extract maker's
art, the brewing of a pot of tea will be appropriate. The English
chemists at least know that "tea boiled is tea spoiled," and that
in the making an infusion process is used for not less than two
minutes nor more than seven, and that the water should be be-
tween 208 ° and 2120 F. in order to secure the best results, al-
lowing it to cool down slowly. It is also found that tea is made
better in earthenware vessels, which are heat retainers, than in
metallic ones, even though the metallic ones may be of such
composition that they will not easily combine with thi
present in the leaf. This is extract making on a small sc:de.
We do not confine ourselves to a narrow temperature, but ex-
tractions of the necessary raw materials are made, according
8oo
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
to experience which has stretched over many years, at tempera-
tures between 140° and 300° P.J all kinds of pressures are used
from below the amosphere to 150 lbs. to the sq. in. ; intermittent
and continuous infusion and percolation are alike used, depend-
ing upon the product to be produced, and you may be interested
in knowing that a difference of 10° in the extraction tempera-
ture of certain materials will cause a profound difference in the
quality and also in the yield or amount of extract produced.
An extract plant at best has always been an expensive proposi-
tion, and where the barks, leaves, and fruits used are of seasonal
gathering, the manufacturer is compelled to maintain an enor-
mous stock of raw material. In our own plants we have not less
than 25,000 tons of bark on hand to-day, none of which can be
used until later on this year, and there will be no more to be
had until the summer of 191 9, which in turn cannot be used again
until after October. We, therefore, have to carry stocks to
last as long as fourteen months, which makes the amount of capital
invested in these industries very great indeed.
The woods are cut in one of two manners, either by a large
revolving disc with knives placed upon the edge and to which
the logs are fed by a power feed, or else by means of the better
known wood hog, which is an exceedingly heavy piece of machinery
revolving at very high speed, and to which the wood is generally
fed by gravity. Instead of the cutting part of this apparatus
being placed on the outside of a flat disc or wheel, it is similar
to a spool or V-shaped wheel, on the inside of the V being the
chipping knives, which are generally staggered. While this
apparatus will cut wood more quickly than the disc, it does not
chip it as well; at least, this is the opinion of a number of authori-
ties, although I must say that the authorities consulted all use
the disc chipper. Some idea of the magnitude of the discs may
be had when you understand that one of these discs operating
in the United States weighs 35 tons. After the wood is chipped
it is generally run through disintegrators such as the Williams
or Jeffries mills. You probably are familiar with both of these;
but for those who may not be, these mills are simply crushing
apparatus containing several score of loose heavy hammers,
entirely free excepting at one end, near the center of the mill
and swinging from a common central disc. The edge of these
hammers moves at a speed of approximately 1V2 mi. per min.
and with about 250 h. p. behind them; any material that gets
into their grasp is generally disintegrated or else the mill gives
way. There have been times when through carelessness or
oversight a steel wedge used for splitting the larger logs or a rail-
road spike, in the case of car bark, has gone through the mill
and been hammered around inside of the cages until the edges
are worn off sufficiently for it to be thrown out white hot on the
floor or into the elevators which convey it to the rooms wherein
the ground material is generally held before extraction. This
oftentimes is the cause of the greatly dreaded dust explosions
which have wrecked several extract plants. After the material
has been properly prepared — and in passing it might be stated
that the size and cut of the preparation has a tremendous bearing
upon the time of extraction which again has bearing upon the
quality produced — it is conveyed by the necessary automatic
machinery to either autoclaves or wooden extractors. The auto-
claves are either of steel or of steel lined with tile, copper, or
bronze. We generally use the copper ones, bronze fitted.
These autoclaves take a charge of from one to three tons, accord-
ing to the size, and are fitted with lines for water, liquor, live
and exhaust steam, compressed air ami vacuum, so thai they
can be used tor any type of extract that it is desired to produce.
The open extractors are generally made of wood and hold from
6 to 12 tons at a charge, but owing to the difficulty of controlling
the oxidation, always present when liquids containing tannin are
exposed in thin solution to the atmosphere, these large tubs
have been superseded in the modern works by autoclaves,
although for certain purposes they are still largely used. After
the material is exhausted by the necessary solvents, the head
liquors are concentrated generally in vacuo although occasionally
they are partly evaporated in plenum. There are, of course,
variants of this as, for instance, in the making of powdered ex-
tract, sometimes the thin liquors are concentrated in vacuo
and then finished in the open and vice versa, depending altogether
upon the material which is to be produced. There is a multi-
plicity of apparatus for the finishing of these extracts and it
seems to me that the principal difference between them is that
one costs more than the other.
The uses of these extracts are various. Silk, wool, cotton,
leather, paper, all draw upon the natural dyewood extract
maker, but I believe that their best use is for wool, silk, leather,
and wall paper lake. They seem to be particularly fitted by
nature for these purposes and generally nature knows what she
is doing. There never has been any really satisfactory substi-
tute for the black which is produced on leather by logwood, and
the very best black silks and broadcloths are always dyed with
this particular product; and as to wall paper, even in Germany
the wall paper manufacturers used to prefer quercitron to the
color lakes that were made by the artificial color makers in
Germany. It may be that our product sold over there so well
because the artificial color makers did not use the same brand
of persuasive art upon their own people that they did upon
our dyers here before the war.
There has always been one very great advantage that the
artificial colors possessed over the natural colors and that is
their ease of application. With anilines an operator took a
certain amount of material that he wished to dye and placed it
in a vessel containing the diluted dyestuff with a little salt or
sulfuric acid, turned on the steam, and in an hour the whole
operation was finished. With the natural dyestuffs it was
different. First of all, the goods had to be soaked in some ma-
terial that had an affinity for the dyestuff, the so-called mordant,
and after this they were placed in the dyestuff and turned around
cr worked, as the expression is, until the requisite color developed.
This required two operations, first the mordanting and then the
dyeing, and twice the time; and although our business in the
United States was increasing before the war until in the early
part of 1914, we made and sold more dyewood extracts than we
ever have done for any similar period since 1869. Nevertheless,
we could not get over this seemingly insurmountable obstacle
to the general employment of our production until the fall of
1917.
It has been taken for granted by the dyewood extract chemist
that the following conditions obtain: first, that alizarine is arti-
ficial madder; that natural madder is a dyewood extract or,
if you prefer it, a vegetable product. If alizarine can be made
so that it will no longer be a mordant color, it is obvious that the
vegetable product madder can also be made so as no longer to
be a mordant color, and if the madder plant stands as a generic
type of all of the dyewoods, then by treatments similar to that
which the artificial colors receive it might be possible to produce
dyewood extracts that would no longer require mordanting in
a separate bath in order to fasten on to the fiber.
(hi November 22, 191 7, our company took out patents upon
single-bath dyewood extracts made from vegetable dyewoods
and here are some dyed swatches of wool and here one of mixed
wool and cotton dyed simply by taking a certain quantity of
the dyestuff, dissolving it in water, placing the fiber to be dyed in
the bath, and treating it exactly similar to the artificial dyestuff.
This has removed the one point of superiority possessed by so
many of the artificial colors, and we believe now that the natural
dyewood industry will develop along its just and proper lines.
Too long have we been content with producing exactly what
we produced before and too long also have we been content
to let some interested party say that ours was indeed a veritable
dying industry in the sense that it was partly moribund and that
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
801
there was no hope for us. To-day when we are operating at
what we consider normal capacity for the looms and dye houses
in this country, there are required not less than 150,000 tons
of logwood and 50,000 tons of quercitron bark to produce the
dyes that are being used for the dyeing of black, blue and yellow,
and in proportion to the number of looms engaged in 19 18 and
those engaged on similar production in 1914, there is actually a
little less proportionate use of dyewood extracts than there
was in 1914, owing to the difficulty of securing supplies from
foreign ports due to the shipping situation, and this has com-
pelled some of the dyers to cut down the quantity of logwood
and quercitron extract that they are using and substitute some
of the artificial colors instead.
Just one thing more. In the various medical journals there
have been some statements appearing recently covering the use
of Flavine in gunshot wounds. This has appeared in Chemical
Abstracts, American Medicine, and The Lancet, and inasmuch as
my company is the only manufacturer of Flavine, which is a
trade-marked, registered name for the concentrated yellow dye-
stuff made by us from the inner bark of the black oak, I have done
all in my power to bring to the attention of those interested
that Flavine has no therapeutic action whatsoever. The material
wrongfully called Flavine is one of the acridine derivatives used
for dyeing yellow, made, I believe, by the Bayer Company, and
with their usual disregard for any hampering conventions, they
have seen fit to take the name of the best yellow dyestuff they
know, namely Flavine, and label their infernal acridine deriva-
tive with it. I take this opportunity of drawing attention to
this newer use of a natural dyestuff, namely, the labeling of an
artificial color with a name that does not belong to it.
PHOTOGRAPHIC SENSITIZING DYES: THEIR SYNTHESIS
AND ABSORPTION SPECTRA
By Louis E. Wise and Elliot Q. Adams
Bureau of Chemistry, Washington, D. C.
The light sensitiveness of the silver bromide emulsion is at a
maximum at the extreme violet end of the visible spectrum, and
falls practically to zero in the green. The emulsion, however,
may be rendered sensitive to the longer wave lengths by the use
of dyes which stain silver halide. Plates with such emulsions
are known as panchromatic or orthochromatic plates.
For this purpose certain of the azo dyes, of the rosanilines, and
of the phthaleins have been used, but all of these, with the ex-
ception of erythrosine, have been superseded by dyes derived
from alkylated quinolines.
TYPES OF DYES USED
The quinolinium dyes used for photosensitization fall into four
main groups differing in methods of synthesis, in absorption
spectra, and in their sensitizing action.
(a) The isocyanines are formed by the condensation of
a-methylated quinolinium alkyl halides (quinaldine derivatives)
with themselves or with quinolinium halides. They sensitize
chiefly in the green and yellow.
(6) The cyanines are formed by the condensation of -y-methyl-
ated quinolinium alkyl halides (lepidine derivatives) with quino-
linium alkyl halides. They show marked sensitization in the
yellow, orange and red.
(c) The "pinacyanoles" are formed by the condensation with
formaldehyde of two molecules of quinolinium alkyl halide, at
least one of which must be a-methylated. They, too, sensitize
in the yellow, orange and red and have largely displaced the
cyanines.
(d) The "dicyanines" are formed from a.-y-dimethylquino-
linium alkyl halides. They sensitize in the red and infra-red.
All of these condensations take place in alkaline solution.
SYNTHETIC WORK
I INTERMEDIATES
bases — -(a) Quinoline and Bz-substituted quinolines are
prepared by the Skraup synthesis from aniline (or other pri-
mary amine), sulfuric acid, glycerin, and a suitable oxidizing
agent, preferably arsenic oxide.
(b) Quinaldine and Bz-substituted quinaldines were synthe-
sized by condensing paraldehyde with the hydrochloride of
aniline (or other primary amine), with or without an oxidizing
agent.
(c) Lepidine was formed by reduction (by dry distillation
with zinc dust) of lepidone, which had been made by condensing
aniline with acetoacetic ester.
{d) a, 1 -dimethyl quinoline and Bz-substituted derivatives
were synthesized by treating with hydrochloric acid gas, a mix-
ture of acetone and paraldehyde, and then condensing with
the hydrochloride of aniline (or other primary amine).
In general, the yields are unsatisfactory.
quaternary halides — The quaternary iodides were formed
by the addition of methyl (or ethyl) iodide to the base, with
or without a solvent. In general, the best yields were ob-
tained without solvent and with the reagents in equimolecular
proportions.
These substances are crystalline solids of a more or less pro-
nounced yellow color. They are readily purified by crystalliza-
tion from alcohol, and their iodine content is easily determined
since they yield all their iodine as iodide ion in aqueous solu-
tion.
The quaternary iodides may be quantitatively converted into
the corresponding chloride or bromide by treating their aqueous
solutions with freshly precipitated silver chloride or bromide.
11 — DYES
(a) The method of synthesis has already been given. In
the case of the isocyanines the course of the reaction is proba-
bly as indicated:
/\/%
/\
+ O(air)
N
/\
R I
%
OH
N
/\.
R I
O
A
+ HI
N
H
O H|C-
II H N
/\y\ y\ (a-Methylated quinolinium alkyl halide)
k
I
bocyanise
802
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. 10
The pairs of intermediates used in the preparation of our
isocyanines are listed in Table I as Nos. i, 2, 3, 4, 5.
Ext. W.L. Ext. Ratio
Table I
No. Pair W.L.
Isocyanines
1 Quinaldine Mel + Quinoline Mel 558
2 Toluquinaldine Mel + Tolui|iiinoline Mel 562
3 Toluquinaldine Mel + Quinoline Mel 558
4 Toluquinaldine Mel + Quinoline Btl 560
5 Quinaldine Mel + Toluquinoline Mel 558
PinacyanoUs
6 Quinaldine Mel 605
7 Toluquinaldine Mel 611
8 Quinaldine Mel + Quinoline Mel 605
9 Quinaldine Mel + Toluquinoline Mel 606
10 Toluquinaldine Mel + Quinoline Mil 611
11 Toluquinaldine Mel + Toluquinoline Mel 611
12 Quinaldine EtI + Quinoline EtI Not
Dicyanines
13 2,4-Dimethyl Quinoline Mel 653
14 2.4-Dimethvl Quinoline EtI 656
15 2,4,6-Trimethy! Quinoline Mel Not
(6) We have prepared only very small quantities of the
cyanines. The mechanism of the reaction is undoubtedly
similar to that of the isocyanines.
(c) The course of the reaction to form the pinacyanoles has
not been established but is very probably
198 563
111 0.56
290 568
135 0.55
330 562
152 0.46
218 562
102 0.47
374 568
162 0.43
288 568
138 0.48
examined
175 606
92 0.53
44 607
36 0.82
examined
CH'-\/\/
N
A
Me X Me
Pinacyanole
We have used the pairs of intermediates numbered 6, 7, 8, 9,
io, 11 and 12 in Table I in the preparation of pinacyanoles.
(d) The reaction for the formation of the dicyanines is de-
cidedly obscure.
We have made dicyanines from the intermediates numbered
13, 14 and 15 in Table I. All these products have proved to
be decidedly impure.
Determination of the iodine content of dyes of the isocyanine
and pinacyanole types has indicated in both cases that the nitro-
gen-iodine ratio is 2 : 1.
ABSORPTION SPECTRA
The spectrophotometry measurements were made with a
Konig, Martens, and Griinbaum spectrophotometer. The
dyes were studied in 95 per cent alcohol solution, in a cell 1 cm.
thick against a similar cell containing solvent alone. The
concentrations of solutions used were 0.02 g. per liter, 0.01 g.
per liter, or 0.005 E- per liter, according to the maximum ab-
sorbing power of the substance.
The results are given in Table I in terms of the specific ex-
tinction coefficient of the dye, that is, the number of liters of
solution in which 1 g. of the dye should be dissolved to give a
solution, a 1 cm. layer of which would reduce exactly tenfold
tin- intensity of a beam of light of the wave length in question.
Table I gives the intensity and location of the absorption
maxima for a number of dyes synthesized. The dyes of the
same type show very similar spectra, as can be seen from the
table.
THE COLOR LABORATORY OF THE BUREAU OF
CHEMISTRY
A BRIEF STATEMENT OF ITS OBJECTS AND PROBLEMS
By H. D. Gibhs, Chemist in Charge, Color Laboratory,
Bureau of Chemistry, Washington, D. C.
It is not my intention this morning to report on any finished
work, but merely to give you a sort of airplane view of some
of the problems that we have in hand.
About two years ago it was decided to organize the color work
of the Bureau of Chemistry. This work originated with the
investigation of the dyes employed for coloring food products,
and had been carried on in various laboratories of the Bureau
for about ten years. It included the identification, analysis,
and physiological investigations, and the entire object was the
solution of problems arising from and necessitated by the en-
forcement of the Food and Drugs Act.
The organization of the work to take up problems dealing
with the manufacture and utilization of colors is a logical step
and a natural extension of the usefulness of the organization.
The plan provided for laboratory investigation of colors, both
natural and artificial, and the substances entering into their
composition, by chemical and physical methods, and the re-
production of laboratory processes on a technical scale. The
study of the behavior of substances in large masses necessitated
the installation of manufacturing appliances. To accomplish
this a rather unique building is in course of erection and equip-
ment on the property of the Department of Agriculture on the
Potomac River directly opposite Washington.
This building is 150 ft. by 70 ft., and contains nine chemical
and physical laboratories, a library, machine shop, boiler room,
engine room, a technical floor 150 ft. by 40 ft., storage rooms,
locker rooms and showers.
The equipment will include two 100-h. p. boilers, a 10-ton
overhead crane, a 5-ton ice machine, storage battery equipment,
all varieties of electric current from a power line of 6,600 volts
down, nitrators, sulfonators, fusion kettles, evaporators, auto-
claves, dryers, stills, centrifugal machines, and many other
large pieces of apparatus in addition to a complete laboratory
equipment of chemical and physical apparatus. A railroad
siding terminates in the building. Each apparatus is equipped
with its own electric motor, where necessary to make a complete
unit permitting moving to any desired position as a whole,
just as we move the apparatus on a laboratory table. The
larger part of the apparatus will be removed from the technical
floor when not in actual operation.
The entire equipment is not ready as yet, for the reason that
the building is only about one-half completed and war emergency
work occupies the completed portion. Adjacent to the main
building is a smaller structure for use in our studies on chlorina-
tion and other noxious gases that might damage machinery
in the larger building.
LABORATORY STUDIES
The laboratory' studies naturally have predominated over the
plant studies to the present time, for the reason that the labora-
tory studies naturally come first, and that our own plant has
not been completely available for the large scale investigations,
except in the case of the chlorination reactions. However,
several large-scale operations have been attempted.
The laboratory studies have been progressing along a variety
of lines ever since the establishment of the organization. The
aim has been to study the development of processes that would
be able to withstand competition, and this goal is best reached
by the study of conditions underlying yields and costs. We
have not been interested in "war babies" that were not directly
concerned with the winning of the war. Many problems of the
latter nature have been taken up, and if any apology is to be
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
803
made for the results to date I must plead that about 80 per cent
of the staff is now engaged on war problems, and 80 per cent of
our problems are now direct war problems, and were assigned
for the reason that almost all are directly in line with our previous
experience.
So far the laboratory studies may be divided into five classes:
(1) Processes, (2) Dye Intermediates, (3) Dyes, (4) Medicinals,
(5) Analytical.
I will take these up in their order and endeavor to give a
brief outline of the different kinds of experimental work that
have been undertaken by the staff.
1. processes — Chlorination, sulfonation, oxidation, sublima-
tion. All of these investigations have been for the most part
vapor-phase problems.
Chlorination — Studies of a variety of compounds by means
of light catalysts have been carried on. Early in our chlori-
nation studies we found that it was impossible to interpret
the results because the known analytical methods were deficient.
Analytical methods for handling chlorinated toluenes have been
completed, and will be published in the next issue of the Journal
of the American Chemical Society. A technical unit for this
chlorination study has been installed.
Sulfonation — -These studies have involved the sulfonation of
naphthalene, benzene, toluene, and some other compounds
in the vapor phase by a continuous process. The analytical
methods for handling the variety of derivatives of naphthalene
have been completed and an article describing the sulfonation
and the analysis of products is practically ready for publication.
This work led to a study of methods for making H-acid, and
we hope to develop results of interest on this compound.
Oxidation — Oxidation of a variety of compounds by means
of catalysts have been carried on in the vapor phase. The
most important development of this work is an advanced study
of the manufacture of phthalic anhydride.
Sublimation — Sublimation studies have included the purifica-
tion of a variety of compounds, including phthalic anhydride
and a number of hydrocarbons. These studies have required
the construction of the vapor pressure curves of a large number
of compounds and it is hoped that these will be ready for pub-
lication shortly.
2. intermediates — An enumeration of the dye intermediates
under investigation is as follows:
Phthalic anhydride, methods of manufacture and uses.
H-acid.
A large number of sulfonic acid derivatives of naphthalene,
benzene, toluene, and cymene.
The chlorine compounds of toluene and cymene and the
study of a number of the quinolines.
3. dyes — Malachite green. A study of the Doebener process
for the manufacture of malachite green led to studies on the
production of benzotrichloride, and these have been included in
the chlorination problems. The sulfonephthaleins, cymene dyes,
dyes for sensitizing the gelatin emulsions of silver halides, and
a number of dyes useful for biological purposes have been in-
vestigated.
The manufacture of a large number of compounds from cy-
mene was made possible when the satisfactory methods for
nitrating cymene were developed. A number of cymene dyes,
homologues of aniline, and various aniline derivatives have been
made, showing the possibility of producing as many compounds
from cymene as are made from aniline.
The biological dyes have included the development of a num-
ber useful in determining the hydrogen-ion concentrations and
in blood investigations. The latter are required in considerable
quantity by the Surgeon General.
The sensitizing dyes are of great value in photography and are
especially useful in aeronautic observation.
4. medicinals — A study of the manufacture of arsphenamine
and a study of the patent literature on the subject have been
made, and it is hoped that the results will be ready for publica-
tion in the near future.
5. analytical — The prosecution of many of the investiga-
tions has been dependent upon the development of analytical
methods for handling the products. Analytical papers on chlor-
inated toluenes, oil-soluble colors for use in foods, and analysis
of anthracene have been published, and other papers are in prep-
aration. The publications that have so far appeared are as
follows :
Para Cymene. I — Nitration. By C. E. Andrews, This
Journal, 10 (1918), 453.
The Use of Thymolsulfophthalein as an Indicator in Acidi-
metric Titrations. By A. B. Clark and H. A. Lubs, /. Am.
Chem. Soc, 40 (1918), 1443.
The Benzaldehyde Sulfite Compound as a Standard in the
Quantitative Separation and Estimation of Benzaldehyde and
Benzoic Acid. By G. A. Geiger, /. Am. Chem. Soc, 40 (1918),
1453-
Crystallography. Note on the Fundamental Polyhedron of
the Diamond Lattice. By E. Q. Adams, /. of Wash. Acad, of
Sci., 8 (1918).
Detection of Added Color in Butter or Oleomargarine. By
H. A. Lubs, This Journal, 10 (1918), 436.
The Quantitative Estimation of Anthraquinone. By H. F.
Lewis, This Journal, 10 (1918), 425.
A Method for the Rapid Analysis of Mixtures of Chlorinated
Toluene. By H. A. Lubs and A. B. Clark, /. Am. Chem.
Soc, 40 (1918), 1449.
Plant Operations — -The development of a process for the manu-
facture of phthalic anhydride has been studied on a plant scale.
The work is carried on in cooperation with manufacturers, in
accordance with the announcement of the Secretary of Agricul-
ture published in June 191 7. The experimental work is still in
progress.
The chlorination of toluene on a large scale is being conducted
in the technical plant of the Color Laboratory.
Plant investigations for the manufacture of various alcohols
and acetone are in progress.
6. patents — The results of laboratory research are patented
by the inventors and dedicated to the people by the Department
of Agriculture. About twelve patents have been granted and a
large number of applications are pending.
The prosecution of a number of phases of this work has been
due to Messrs. J. A. Ambler, R. C. Young, G. S. Bohart, and
L. E. Wise, in addition to those who have already been listed as
publishing articles from this laboratory.
PROBLEMS IN TESTING DYES AND INTERMEDIATES
By E. W. Pierce, of the U. S. Conditioning and Testing Company
The purpose of this paper is not to disclose any new develop-
ments along the lines of dye testing, but rather to make a plea
for general cooperation in order to raise the subject to the level
it should occupy, now that we have the initiative.
Having been in the most intimate contact with dye testing
from an American point of view, for a period of over 20 years,
I feel that whatever criticisms I may make are at the same time
retroactive.
It cannot be denied that all the present methods of testing
dyestuffs are empiric and subject to a wide limit of error. For
commercial purposes no great objection is made if this error
is plus or minus 2 .5 per cent, that is, regarding tinctorial power
only. No attempt has been made so far in the valuation of
dyes which would take into account the presence or absence
of small quantities of by-products or impurities that, might be
less than 1 per cent and yet cause a marked loss in value of the
commercial dye. Thus some recent productions of Rhodamine
B were made almost valueless by the presence of a very small
quantity of an impurity which caused the shade to be flat and
useless for dyeing pinks. A chemical analysis of such a product
8o4
THE JOURNAL OF INDUSTRIAL [ND ENGINEERING CHEMISTRY Vol
10. Xo.
might show it to be 99 per cent pure, well within the commercial
allowance, but it is still much inferior to a lot that would analyze
90 per cent Rhodamine and 10 per cent dextrine and capable
of dyeing a bright shade.
According to the ultimate uses of the dyes, tests are made in
a manner that aims to duplicate, on a small scale, the actual
application of the color. Dyeings on wool, cotton, and silk, the
most common, are followed by paper pulp, lakes, leather, sugar,
starch, etc. Colorimetric methods are more recent, but have
many limitations.
If it were always possible to obtain identical conditions in
the comparative dye test, the only source of error would be that
of the individual's ability to read results accurately. However,
the dye test has shown that many influences, apparently insig-
nificant, are capable of causing misleading results.
The- water used in dyeing is a well-known factor, differences
of over 10 per cent being noted between filtered river water
and distilled water. Dyes that are equal when tested by one
observer may show a difference when tested by another on ac-
count of this condition. The presence of foreign material such
as salt, Glauber salt, dextrine, or soluble starch may influence
greatly the result of tests by two different laboratories. The
salts generally act as precipitants and cause both superficial
dyeing and lake formation in the dye bath, while the presence
of the organic adulterants is like that of a protective colloid
and results in slower dyeing, a less exhausted bath, and a greater
penetration of the fiber. When the dye bath is finally exhausted,
the appearance of the skein in both cases may be satisfactory
to the naked eye, but the microscope will show that the one with
the dye on the surface of the fiber has a false advantage.
The fibers themselves are not of a nature that would recom-
mend them for exact scientific work. A wool fiber invariably
dyes a very full and often bronzy shade near the tip, then be-
comes lighter toward the root, while the root end is often left
practically unstained. The carding and spinning processes so
mix the fibers that the naked eye does not notice these defects
in a skein or piece of cloth, but they exist and the final result is
modified accordingly. When the dye bath contains materials
that influence the evenness of the individual fiber the dyeing
as a whole shows the effect. These materials may be either
actual impurities or placed there intentionally.
Silks are not uniform but are classed as hard- and soft-natured
and accordingly dye superficially or uniformly.
Mordanted skeins may be the source of many differences be-
tween different observers. The tannin-antimony mordant on
cotton is at times a true colloidal adsorption between cellulose
and antimony tanuate and at others a mechanical adhesion of
the antimony compound on the surface of the fiber. The acidity
of the dye bath removes and again deposits the final combina-
tion with the dye so that the most rigid maintenance of uniform
conditions is necessary to obtain concordant results.
Lately a test of htmatines by the method of non-oxidizing
mordants was required in a hurry, and as no mordanted skeins
were on hand they were prepared as usual and the dyeings fol-
lowed at once. As the results were not satisfactory the test
was repeated on the following day with mordanted skeins from
tin same lot. The second test showed almost double the amount
of color of the first seues. and the conclusion has been forced
upon us that a chrome mordant on wool improves by ageing
for 12 hours before use Failure to observe this condition
might result in discrepancies hard to explain.
The mosl satisfactory test of dyestuff strength is by the color-
imeter, lint such methods are only dependable when the two
solutions arc identical in composition and shade. Any varia-
tion in acidity, alkalinity, or tone of the color detract from ac-
curacy. It is particularly noticeable now that the produc-
tions of different factories vary just enough to interfere with
the use of the colorimeter, although it will lie found most valua-
ble in controlling the output of any plant.
A few words may be said on the subject of intermediates. It
is vitally necessary that some authoritative body specify tests
for the proper valuation of the common intermediates. The
literature on the subjects is insufficient. Take the case of para-
phenylene diamine. We can determine ash, nitrogen, melting
and boiling point, solubility, and so on, but these are not a true
indication of its suitability for dyestuff manufacture. The
presence of isomeric bodies is the greatest fault and none of the
ordinary tests are quantitative. It cannot be hoped that we
will ever have a system of quantitative methods for aromatic
compounds but some of the gaps may be filled. At times it is
possible to convert an intermediate into a distinctive coloring
matter and make a colorimetric comparison with a sample of the
C. P. product and so far this has been the best method at hand.
Isolated cases like paranitraniline have given special methods,
such as titration in boiling solution with sodium nitrate, using
safranine as an indicator, but whenever there is a tendency to
develop a strong color this method is valueless.
If we are now to make America the center of the dye industry
it is incumbent upon us to provide the analyst with methods
and so facilitate the commercial development along proper lines
of control.
ON THE QUANTITATIVE ANALYSIS OF DYESTtJFFS
By Alfred H. Halland, of National Aniline and Chemical Company
The large majority of commercial dyestuffs contains besides
the dyestuff proper a certain amount of moisture and a great
variety of inert ingredients such as common salt, sulfate of soda,
carbonate of soda, etc. While a certain amount of these bodies
frequently are added in the process known as "Standardization,"
it is well known that it is practically impossible to isolate water-
soluble dyestuffs without a minimum amount of salt, sulfate,
and, to a lesser degree, sodium carbonate.
By the quantitative examination of a dyestuff I understand the
determination of these various ingredients as well as of the color-
ing matter proper.
Before going into details I venture to state as my personal
opinion that this line of work is being neglected in most dyestuff
factories. When a manufacturing chemist delivers a quantity
of dye to be "Standardized" he is too often satisfied if said quan-
tity yields a fair amount of "Type." Am I much mistaken
when I say that the chemist in many cases does not know what
this "Type" really consists of? A quantitative analysis of each
of his "Types" would show the chemist just what degree of
perfection his manufacturing process has reached. It would
either give him the satisfaction of knowing that his process was
good or be an incentive to him to improve it. In the case of a
great many complex dyestuffs, for example, certain polyazo
dyestuffs, the actual yield of dyestuff from given quantities
of intermediates is really quite poor. A quantitative analysis
of the finished dyestuff , as well as of the intermediate azo bodies,
should be instructive and should be carried out in all cases of
bad vulds. It would obviously only be necessary to do this
work once for each individual "Type" as all future lots could
be compared to the "Type" by the usual dyeing tests.
The quantitative determination of sulfur present as sulfonic
acid groups, or of the degree of saturation of these with soda or
potash, or of halogen, if such be present in the molecule, would
form a valuable addition to the knowledge gained by a purely
qualitative analysis of dyestuffs such as the chemist is occasion-
ally called upon to make
I now would like to review the methods which we have used
in Buffalo with a fair degree of success. While I do not claim
any scientific perfection or absolute accuracy for them, they have
not been found seriously wanting.
di;ti:rminatios of moisture
Certain water-insoluble dyestuffs such as oil-soluble azo dyes,
lake colors, bromo acid, etc., contain none, or very little moisture.
Oct., 191S
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
The great mass of water-soluble dyestuffs contain moisture,
partly loosely bound, and partly, and that I believe is the general
rule, in the form of water of crystallization. It is interesting to
observe the great tenacity with which even great quantities of
water are retained by certain dyestuffs. This explains why the
ordinary practice of drying organic compounds in a desiccator
over sulfuric acid gives altogether too low figures for moisture
when applied to dyestuffs. A sample of Wool Red 40 F, lost
in desiccator during 3 days 2 per cent in weight, while the same
sample on drying to constant weight in an air oven at 125°
C. showed a loss of 12 per cent. This could be illustrated by
a great many examples. For purposes of determining the mois-
ture content it generally suffices to place the dyestuff in an air
oven held at 125 ° C, until constant weight is observed. The
temperature of 1250 C, or even higher, is generally tolerated by
a dyestuff without any evidence of decomposition. It has been
recommended to place the dyestuff for moisture determination
in a tube through which a current of hydrogen or carbon dioxide
is conducted while the tube is maintained at a constant tempera-
ture by being surrounded by vapors of a suitable liquid, for
example, boiling toluol. These precautions are as a rule quite
unnecessary except when dealing with easily oxidized dyestuffs.
DETERMINATION OF SODIUM CHLORIDE
When the dyestuff does not contain any halogen in the molecule
or when it is not a hydrochloride, as in the case of basic colors,
the salt determination is a simple matter. The general procedure
is to mix the dyestuff intimately with from 5 to 10 times its
weight of C.P. anhydrous sodium carbonate and heat this mixture
in an iron crucible gradually to a dull red heat turning the mass
over occasionally with a steel spatula until complete charring
or partial combustion has taken place. The crucible content is,
after cooling, mixed intimately with pure potassium nitrate in
the proper ratio to insure an easy flux and the mass placed in
the crucible again, where it is cautiously heated until complete
oxidation and fusion have taken place. The crucible content is
then taken up with water, filtered, acidulated with nitric acid,
and the sodium chloride determined in the usual manner with
silver nitrate.
When halogen is present in the molecule it must be determined
separately and the sodium chloride calculated by difference.
In the case of basic dyes like Methylene Blue or Safranine, I
believe a direct titration of the dyestuff by means of a standard
solution of an acid dyestuff, for example, Naphthol Yellow
according to Knecht or by titanous chloride according to Knecht
and Hibbert would be advisable. The titanous chloride titra-
tion is altogether very satisfactory for a great many simple
dyestuffs, but fails in the case of more complex azo dyes
DETERMINATION OP SULFATE OF SODA
This is not as simple as the salt determination and calls for
greater ingenuity. Sometimes a direct precipitation in the
acidulated solution of the dyestuff gives a fairly pure barium
sulfate. As, however, a great many dyestuffs form hard soluble
barium salts, the precipitated barium sulfate is often more or
less colored. This can be corrected by washing the precipitate
with warm ammonium carbonate whereby the color lake is de-
composed into the ammonium salt of the dye which passes through
the filter and barium carbonate which can be removed by dilute
acid.
When the direct precipitation with barium chloride fails, it
sometimes is a good plan to precipitate the dyestuff from its
aqueous solution as thoroughly as possible with salt and de-
termine the sulfate in the filtrate with eventual after-treatment
with ammonium carbonate.
In some cases when the dyestuff cannot be "salted out,"
advantage can be taken of the fact that acid and basic dyestuff
mutually precipitate one another. If, for example, the problem
is to determine the amount of sulfate in Patent Blue or Acid
Green a solution of a suitable basic color free from sulfates can
be added to the solution of the acid color until a drop of the
mixture placed on filter paper shows excess of the basic color.
The condensation product is then filtered off and the barium
sulfate precipitated in the filtrate. As a suitable basic color
I prefer Chrysoidine, because it can be easily prepared free from
sulfates.
By these various methods a determination of the sulfate of
soda present in the dyestuff can be secured without a very high
degree of accuracy.
DETERMINATION OF SULFUR AND SODIUM OR POTASSIUM
When the sulfate has been determined it is often of interest
to determine the total sulfur present, including that residing
in sulfonic acid groups. The fusion of '/» g. or less of the dyestuff
with soda and niter is generally more satisfactory than the classi-
cal heating in a sealed tube with nitric acid according to Carius.
The amount of sodium or potassium present in a dyestuff
is easily found by moistening a small quantity of the sample in a
porcelain or platinum dish, driving the sulfuric acid off by heating
the crucible, and repeating this process until a perfectly white
ash remains. This is then heated to a dull red heat and weighed
as sodium sulfate.
After the chemist has made the series of quantitative deter-
minations mentioned it should be possible by piecing them to-
gether to form a correct picture of the true composition of the
dyestuff before him.
CHLMICAL MARKETS OF SOUTH AMLRICA
By O. P. Hopkins
CHEMICAL TRADE OF CHILE, PERU, AND BOLIVIA
Received August 27, 1918
The prosperity of Chile, Peru, and Bolivia depends
primarily upon the output of minerals, and in this
respect the group differs radically from Argentina,
Brazil, and Uruguay, which were examined in con-
nection with the trade in chemicals in the September
number of This Journal. Sodium nitrate, copper,
and tin are supplied by this group in enormous quanti-
ties and the value of these materials to the war in-
dustries of the belligerent countries is so great that the
exporting countries have for the past two years been
enjoying a prosperity that has transformed their whole
economic life.
Washington, D. C.
These countries are not, however, heavy importers
of industrial chemicals. The market at present is
confined largely to such articles as perfumery, medi-
cines, paper, soap, and glass, and American manu-
facturers have succeeded in increasing their sales of
these lines as the result of the shutting off of European
supplies. The opportunity of the future lies in main-
taining the advantage thus gained and developing the
trade still further.
As in the previous review, there is a table showing
the imports of each country, compiled from the original
Spanisli statistics, and more detailed tables showing
the trade with the United States, based upon statistics
published by the United States Bureau of Foreign and
Domestic Commerce.
8o6
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CUEMISTRY Vol. 10, Xo. 10
CHILE
The nitrate beds are the chief source of Chile's
prosperity, affording the country one of the most valu-
able natural monopolies in the world. Copper has also
come into its own again as a result of war demands and
is exported in great quantities. Agriculture and
stockraising are second in importance only to mining,
and in recent years manufacturing has been developed
rapidly, thanks to plentiful supplies of iron, coal, and
timber, efficient labor, and ample water power. It is
safe to assume that Chile will consume increasingly
great quantities of industrial chemicals, although it is
at present difficult to estimate what proportion will be
imported. American goods in general are highly
esteemed, but have not been pushed so energetically
as have the goods from Certain other countries.
Over $3,000,000 worth of chemicals, pharmaceutical
products, and perfumery was imported in 1913, and of
that total Germany furnished more than a third, or
more than twice the amount supplied by the United
States. Germany also had an advantage in dyes,
paints, and inks, and maintained a striking superiority
in paper and paper products. The United States
supplied the bulk of the mineral oils.
The statistics in the following table are based upon
official Chilean figures for the calendar years 1913 and
1915, the last normal and latest available war years,
and serve principally to show the extent of the market
before the war and the manner in which it was divided
among the principal competing countries. The year
191 5 shows a falling off all around from the normal
year, as the country had not recovered from the de-
pression and dislocation of trade that followed the
outbreak of hostilities. Since that time the great
demand for Chile's minerals has brought in an era of
prosperity that has never been equaled in the history
of the country.
Chilean Imports of Chemicals and Allied Products
Articles 1913 1915
Chemicals. Pharmaceutical Products, Perfumery
Chemicals $1,015,861 $ 623.200
Pharmaceutical products 1,688,444 810,782
Perfumery 336,740 125,093
Total 3,041.045 1,559.075
Germany 1,044,837 132.292
United States 492.270 627,347
Paints, Dyes, Inks 763,412 264,009
Germany 326.980 33,508
United Kingdom 285.500 135.630
United Slates 85,687 77,978
Explosives 922,954 563,841
Germany 180,482 14,471
United Kingdom 346,010 148,282
United States 235.932 390.682
Varnishes 171,301 81,182
United Kingdom 62.017 47,190
United States 52,700 25.357
Industrial Oils 1,079,310 523,830
Germany 166,195 31.463
United Kingdom 439,305 122,616
United States 456.088 358,988
Crude Petroleum 4,405.727 3,712,768
United States 3,500,395 2,640,056
Naphtha Petroleum. Gasoline. Kerosene,
Paraffin, for Industrial Purposes 1,078,253 633,288
United States 1,061,825 620.592
Paraffin Wax 558,657 612.873
Germany 302,887 8.354
United States 143.643 560.329
Sheet and Plate Glass 272,880 72,782
Belgium 151,386 6.347
United States 1,030 42,555
Paper, Cardboard, and Manufactures of. . . 3.581,027 1,905,781
Germany 1,959.087 241.419
United States 463.573 413.164
The extent to which the present prosperity of the
country has reacted upon the purchases of chemicals
and allied products from the United States can be
readily traced in the next table, in which gratifying
gains are indicated for almost every item. The sales
of American chemicals, drugs, and perfumery in the
fiscal year 191 7 easily surpass the German total previous
to t*he war. Over $1,000,000 worth of business is
noted for the "All other" group alone, and it is re-
grettable that further details are not available as to
the articles included in that classification. The sub-
stantial gain in the imports of American dyes is an
interesting and encouraging feature, as is the gain in
receipts of American paper. Certainly it should be pos-
sible to retain much of this trade when the war is over.
Details of the imports from the United States are
shown in the following table, which is based upon offi-
cial American statistics for the fiscal years 1 9 1 4 and 1 9 1 7 :
American Products Sold in Chile
Articles 1914
Aluminum and manufactures $ 1 ,938
Asphaltum and manufactures 50.347
Babhitt metal 1 1 . 23 1
Blacking, shoe paste, etc 18,506
Celluloid and manufactures 117
Cement, hydraulic 35 ,807
Chemicals, drugs, dyes, etc.:
Acids:
Sulfuric 48 , 277
All other 3,415
Baking powder 10,663
Bark extract for tanning 251
Calcium carbide 72.289
Copper sulfate 1.385
Dyes and dyestuffs 893
Medicines, patent and proprietary 200,918
Petroleum jelly, etc 840
Roots, herbs, barks 77
Soda salts and preparations
All other 68 ,365
Clay, fire 58
Explosives:
Cartridges, loaded 45,220
Dynamite 107,087
Gunpowder 5,270
All other 15.134
Glass and glassware 40 , 224
Glucose 14.808
Grease :
Lubricating 78,326
Soap stocks, and other 1 , 882
India-rubber manufactures 139.256
Ink 12.408
Leather, patent 56,305
Metal polish 2,028
Naval stores 68 , 897
Oilcloth and linoleum:
For floors 1.117
All other 9.855
Oils:
Animal 2.872
Mineral:
Crude 118.500
Gas and fuel 1.365.661
Illuminating 1.028.155
Lubricating, etc 418.279
Gasoline 166, 724
Other light 12.412
Vegetable:
Cottonseed 436 . 672
Linseed 2 . 598
Other fixed 11,982
Volatile 217
Paints, pigments, etc.:
Dry colors 64
Ready-mixed paints 26 , 829
Varnishes 10.712
White lead 725
Zinc oxide
All other (including crayons) 22 . 763
Paper and manufactures 233 .603
D and wax 92.098
Paste 203
Perfumery, cosmetics, etc 25,437
Photographic goods:
Moton-pictore films 5.268
Other sensitized goods 18,213
Plumbago and manufactures 2,297
Quicksilver
Soap:
Toilet 91 .330
All other 16.290
Sugar, refined 687
Wax, manufactures of I , 1 45
1917
17.197
30.090
61,936
51 ,145
8.285
112.397
37.827
71.869
25.676
21.963
78.296
38.828
110.646
305.611
20.320
22.014
211.691
1,038,531
9,340
74.861
968.765
10.266
1.192.023
290,753
18.182
121.209
36.184
714.571
39.781
313.639
4.136
164.848
6.291
67,224
2.826.963
399.860
561,225
97.955
462,703
257. 948
31.197
148.343
14,386
27,982
55,912
14.108
5.632
102.737
1,188,139
577.644
3.599
51.844
13.904
46.902
409
127,790
9,618
6.687
Oct., 1918
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
807
Chile sent to the United States about $45,000,000
■worth of sodium nitrate and an equal amount of copper
«in 191 7, and it would be a difficult matter to over-
estimate the vital importance of these two materials
to the cause of the Allies. The $4,000,000 worth of
iodine was another valuable contribution, as was the
$2,000,000 worth of tungsten ore. The shipments of
tin ore and bismuth are to be credited to Bolivia,
however, as they merely pass through Chile. The im-
portance of Chile as a reservoir of war materials is
■made clear in the following table, which is based upon
American statistics for the fiscal years 19 14 and 1917:
Chilean Products Sold in the United States
Articles 1914
Antimony ore $ 8
Bismuth
Bones, hoofs, horns
Chemicals, drugs, dyes, etc.:
Argols
Iodine, crude or resublimed 433 , 293
Potash:
Nitrate
Salts of
Soda, nitrate 17, 808 , 763
AU other
Copper:
Ore 1 ,974,429
Concentrates
Matte and regulus 2,004,898
Unrefined, black, etc
Refined, in bars, etc 2,145,748
Glue and glue size 607
Hide cuttings, raw
India rubber, unmanufactured
Iron ore 7 , 829
Lead ore 91 ,994
Paper and products
Platinum
Tanning materials: Quebracho wood
Tin:
Ore
Bars, etc
Tungsten-bearing ore
Wax:
Beeswax 36,975
Vegetable
Zinc, pigs
1917
461,462
11,627
13,040
77,720
18,751
44,231.240
51,279
4,840,321
40,764
2,645,973
35,779.947
2,501,685
67,810
3,841
392,624
50,145
178,503
7,640
62,981
37,445
2,708,373
24,401
2,013,411
157,212
8,063
485
PEBU
Mining and agriculture are the chief industries of
Peru. The mineral resources are varied and ex-
tensive, including copper, gold, silver, lead, quicksilver,
coal, bismuth, vanadium, tungsten, nickel, iron, sulfur,
antimony, petroleum, salt, zinc, borax, cobalt, gypsum,
asbestos, ocher, kaolin, molybdenite, manganese,
magnesia, mica, peat, and various marbles. Copper is
extensively worked at present, with American capital
heavily interested, but the silver output is also important,
as it has been since the sixteenth century. Few of the
other minerals are produced in anything like important
quantities, so that it can be safely said that even to-
day the mineral industry is only in its infancy.
Considering the proportion of the country that is
' either mountainous or desert, agriculture is sur-
prisingly well developed, the principal products being
sugar cane, cotton, coca, rice, and grapes. The total
value of the crops of the country can be placed some-
where between 40 and 50 million dollars.
The manufacturing industries are not well de-
veloped, although the output of the sugar mills is now
considerable and the domestic supplies of cotton and
wool have led to the development of a prosperous
textile industry.
Industrial chemicals are not required in large
quantities, but there is a steady demand for many
of the finer chemicals. In 1913 the imports of chemi-
cals, drugs, medicines, and pharmaceutical supplies
amounted to slightly more than $1,000,000, which was
divided fairly evenly among American, German,
French, and English manufacturers, the Americans
leading with $291,000. In 1916 the imports were
nearly $1,500,000, of which American manufacturers
furnished very nearly $1,000,000 worth. American
goods have always been in good demand in Peru, a
circumstance that is usually explained as being a
natural consequence of extensive investments of
, American capital in the mining industries of the
country.
As will be seen in the following table, which is a
compilation from official Peruvian statistics, none of
the articles usually classed as chemicals is imported
to the extent of $500,000 annually; in fact, patent
medicines are the only item exceeding $300,000 in
value. It will be noticed, however, that the American
share of the imports has been substantially increased
as a result of war conditions and there is no con-
vincing reason why this business should not be re-
tained and expanded when normal conditions are re-
stored.
Of the classes of goods that can be considered as
allied chemical products, "colors, paints, varnishes,
oils, and gums" were imported in 1916 to the extent
of more than $2,000,000, the United States having
almost a monopoly of the trade. Mineral oils are the
most important item in this group. Explosives and
paper are both important, American manufacturers
now dominating the market.
The table is based on statistics for the calendar
years 1913 and 1916, the last normal year and the
latest available war year. These figures should be
used only as a general guide in estimating the extent
of the markets and the relative share of the principal
competing countries in the trade.
Peruvian Imports op Chemicals and Allied Products
Articles 1913 1916
Chemicals, Drugs, etc.
Acids:
Sulfuric $ 5,161 $ 60,103
United Kingdom 307 20
United States 2,209 60,083
Tartaric 10.673 13,962
Germany 5,261
United States 31 6,942
Disinfectants, prepared 24,536 35,715
Germany 3 , 205
United States 18,205 35,355
Glycerin 6,029 7.135
United Kingdom 2,468 260
United States 64 6,255
Medicines, proprietary 348,950 327,343
France 108,037 54.763
United States 162,078 236,749
Methyl alcohol 21,180 4,547
Germany 21,180
United Kingdom 4,544
Quinine 131.437 90,747
France 49.790 8,972
United States 2,229 34,008
Soda ash 20,295 28.477
United Kingdom 17.378 13.071
United States 1.165 15.263
Soda, bicarbonate of 12,080 50,566
United Kingdom 6,159 2,551
UnitedStates 5.084 24,839
Soda, caustic 36,608 67.629
United Kingdom 25.980 8.319
UnitedStates 9,266 59.247
Sulfur 19,434 49.070
Italy 12.635 10,740
UnitedStates 292 29,855
Colors, Paints. Varnishes, Oils, and Gums. . 1,772,828 2,198.913
Germany 420,371 820
United Kingdom 301,602 277,591
UnitedStates 894,878 1.770.555
8o8
I III: JOURNAL OF INDUSTRIAL AM) ENGINEERING CHEMISTRY Vol. 10. No. 10
1916
$ 938.582
886.390
755.816
755.816
1 ,312,900
74,980
10.000
127.823
787.851
307,641
900
5,621
>86
HI,'/
70
V><>
V4'<
.'i
,;,,
90
268
53
S.sv
4
s4.>
«
025
14
1917
276
$ 17,605
,949
13.500
,526
19.896
275
3,329
121
8,434
,902
125,367
Peruvian Imports, lire. (Concluded)
Articles 19 13
Explosives $ 516,851
United States 201 ,221
Dynamite, etc 325 ,512
United States 160,317
Paper, Cardboard and Office Supplies
Total imports 914, 862
France 54.044
Germany 403 , 723
United Kingdom 104,637
United States 234,000
Newsprint paper 189,386
Germany 128,355
Norway
Sweden
United States 56,894
Book and lithographic paper 78,897
Germany 33,734
United Kingdom 1 5 , 964
United States 10,618
Sheet and Plate Glass 28,781
Belgium 24.956
United Kingdom 1 ,158
United States 199
The character of chemicals and allied products sold
in Peruvian markets by American manufacturers can
be determined more accurately from the following
table, which is based upon official American statistics
for the fiscal years 1914 and 191 7:
American Products Sold in Peru
Articles 19
Aluminum and manufactures $
Babbitt metal 4
Blacking, shoe paste, etc 4
Candles
Celluloid and manufactures
Cement, hydraulic 109
Chemicals, drugs, dyes, etc.:
Acids:
Sulfuric 4
Allother
Baking powder 1
Calcium carbide 22
Copper sulfate
Dyes and dyestuffs 2
Medicines, patent and proprietary 197
Petroleum jelly, etc
Roots, herbs, barks
Soda salts and preparations
All other 81
Chewing gum
Explosives:
Cartridges, loaded 17
Dynamite 56
Gunpowder
All other 26
Flavoring extracts and fruit juices
Glass and glassware 18
Glue
Grease:
Lubricating 24
Soap stock and other 3
India-rubber manufactures 44
Ink 3
Leather, patent 17
Lime
Naval stores:
Rosin 22
Tar, turpentine, pitch
Turpentine, spirits 17
Oilcloth and linoleum 1
Oils:
Animal
Mineral:
Gas and fuel
Illuminating 73
Lubricating, etc 67
All other 262
Vegetable
Cottonseed
Linseed
Other fixed '2
Volatile
Paints, pigments, etc.:
Dry colors 5
Ready-mixed paints 12
Zinc, oxide
All other (including crayons) 2
Paper and manufactures 80
ind paraffin was 22
Perfumery, cosmetics, etc 44
Photographic goods:
Exposed motion-picture films
I >thrt sensitized goods 12
Plumbago and manufactures
Soap:
Toilet 6
All other IS
Stearin, vegetable
Sueir and molasses
Wax and manufactures
21,274
31,729
3.604
19,364
4,523
94,775
245,373
7,497
5.317
80,892
377,924
5,475
47.577
219.721
45,925
382.487
7,738
156.485
3,347
17,912
9,773
156.593
23.427
100,962
3,183
34,257
4.807
32.923
17.535
89.563
i.t.4:7
144.283
565
8,042
26,318
28,753
3.176
11.670
14.384
2.096
53.060
7.773
16.822
Copper is easily the most important of the ma-
terials now shipped to the United States by Peru, as
the next table shows, the exports having been greatly
stimulated by the war. Other important items are
cane sugar, mineral oil, tungsten ore, and India rubber.
The tin originates in Bolivia. The following table is
compiled from American statistics for the fiscal years
1 9 14 and 191 7:
Peruvian Products Sold in the United States
Articles 1914
Antimony ore $
Chemicals, drugs, dyes, etc.:
Colors or dyes
Glycerin, crude
Soda, cyanide
Copper:
On 751,582
Concentrates
Matte, regulus, etc 866.2! 1
Unrefined, in bars, etc 6.59
India rubber, etc.:
Balata
Gutta-percha
India rubber 427,002
Lead
Oils:
Crude mineral 506,535
Refined mineral:
Benzine, gasoline, naphtha 867,020
All other
Sugar, cane 181,519
Tin:
Ore
Bars, etc
Tungsten-bearing ore
Wax : Beeswax
Zinc
1917
S 5.378
6.456
2,930
2,190
833,085
60,778
306.939
20,684,121
4.400
1.275
: .227.776
1,395,453
146.514
3.576.707
18.115
6.688
1 .073.001
5.411
2,720
BOLIVIA
Bolivia's wealth lies in mineral deposits, and it is
estimated that more than $2,000,000,000 worth of
metals have been taken from the country since the com-
ing of the Spaniards in the sixteenth century. Gold and
silver were formerly recovered in immense quantities,
but of the total mineral production of $27,000,000 in
191 2, over $23,000,000 was tin. The silver output
the same year was something more than a million and a
half, while the gold production was practically nil.
Nearly $1,000,000 worth of bismuth was recovered,
which represents a large part of the world's production.
As a source of tin Bolivia is now second to the Malay
peninsula. The immense forests have not been
exploited nor has agriculture been developed, although
there are unlimited possibilities in that direction.
Aside from the reduction of tin ore there is very little
activity that can be classed as manufacturing.
Naturally there is little demand for chemicals or
chemical products, but such imports as were recorded
by the Government for 1913 and 1915 are shown in the
following table. There seems to be little possibility
of developing a trade in these lines in the near future.
Bolivian Imports of Chemicals and Allied Products
Articles 1913
Chemical Products $ 49 . 830
Un
9 , 356
4.876
1 62 . 704
lited States
Prepared Medicines
Germany
United States
PERFUMERY AND CoSMETICS
Germany
United Slates
S" w-s
United Kingdom
United States
1 'yes, Varnishes 127.619
Germany 61,811
United States 6,272
Explosives 446.316
Germany 362, 705
United States 5.143
58 , 295
17 . 291
13.022
109,687
4.814
1915
I
3 . 295
4.391
19,340
390
2,161
M.737
5.844
20.870
2.847
2 . 665
312.090
329
143.130
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Bolivian Imports, Etc. {Concluded)
Articles 1913
Mineral Oils and Their Derivatives $ 86,403
Germany 20,533
United States 21,116
Vegetable Oils, Edible 14 , 1 24
Italy 4,536
United States 521
Oils, Other 47,232
Germany 14,823
United States 11,146
Sheet and Plate Glass 46,664
Germany 21,078
United States 5,129
Glassware 103 . 845
Germany 53,500
United States 6,576
Paper and Cardboard (except Wall Paper) 167 ,391
Germany 70,353
United States 15,742
Manufacture op Paper (except Books) 31, 914
Germany 1 5 , 562
United States 414
1915
4234.630
7,288
118,683
17,870
6,590
4,048
8,456
48
6,254
18,337
121
9.437
21.518
3.232
6,261
91.012
6,598
28,790
14,138
1,629
1,516
How the war has affected what little trade American
manufacturers have with Bolivia can be ascertained
from the following table, which is compiled from
American statistics for the fiscal years 1914 and 191 7:
American Products Sold in Bolivia
Articles 1914 1917
Blacking, shoe paste, etc $ 1,136 $ 4,642
Candles ... 3,841
Cement, hydraulic ... 1,781
Chemicals, drugs, dyes, etc.:
Acids 119 4,423
Calcium carbide 573 364
Medicines, patent and proprietary 23 , 792 1 3 , 208
Soda salts and preparations ... 9.561
AU other 4,600 29,334
Explosives:
Cartridges, loaded 6,622 23,768
Dynamite 72,044
Gunpowder ... 12,556
Allother 26 42,217
American Products Sold in Bolivia (Concluded)
Articles 1914 1917
Glass and glassware $ 7,895 $19,469
Grease, lubricating 1 ,933 5,464
India-rubber manufactures ... 31 ,618
Leather, patent 1 ,475 5,024
Oils:
Refined mineral:
Gasoline, etc 1 ,998 4,494
Illuminating 16,647 22, 199
Lubricating, etc 20 , 583 36 , 026
Naphthas, etc 1 , 998 59 , 797
Vegetable:
Cottonseed 22 6, 123
Linseed 233 2,353
AU other 187 6,862
Paints, pigments, etc.:
Ready-mixed paints 2,647 1 ,236
White lead ... 23,688
Allother 1,619 7,095
Paper and manufactures 83,227 66,405
Paraffin, etc 720 85,045
Perfumeries, cosmetics, etc 1 ,830 3,685
Soap:
Toilet 7,050 15,914
Other 330 5,781
Sugar, refined 6 817
The statistics supplied by our own Government do
not show many imports from Bolivia, as shipments
are made from the Pacific and Atlantic ports of neigh-
boring countries and consequently credited to them.-
Of the nearly $3,000,000 worth of tin ore imported
into the United States during the fiscal year 1917,
practically all was credited to Chile in our statistics.
Such imports jumped to $10,000,000 in 1918. Imports
of bismuth were valued at $196,000 in 191 7, of which
$32,000 worth is credited to Argentina, Chile, and
Uruguay, and is obviously of Bolivian origin. The
preliminary statistics for the fiscal year 1918 do not
show imports of bismuth.
ORIGINAL PAPERS
VALUATION OF RAW SUGARS*
By W. D. Hornb
In the sugar trade it has long been customary to
buy and sell raw sugars on their polarization, adopting
usually a basis of 96 ° for centrifugal sugars and 89 °
for muscovado and molasses sugars. For every de-
gree above the basis a certain additional increase is
paid, while for each degree below the basis a double
deduction is made.
This system, while based on practical considera-
tions and having much to recommend it, is still far
from satisfactory, because it does not take sufficient
account of the many influences on refining of sugars
introduced by their endless variations.
Efforts have therefore been made in recent years
to attempt a rough standardization of raw sugars on
the part of some of the advanced manufacturers. Such
methods consist of grading the sugars according to
the size of grain, hardness of grain, cleanliness of solu-
tion, odor, and reaction, as well as polarization and
moisture, with perhaps some other determinations.
Admirable as these efforts are, they still fall far
short of what is desired, for they are based on
assumptions which frequently are not borne out in
practice and entirely overlook many important varia-
1 Read before the Division of Industrial Chemists and Chemical Engi-
neers, 56th Meeting of the Amcriran Chemical Society, September 10 to 13,
1918.
tions in raw sugars which radically affect their value
for refining purposes.
It is the object of this paper to direct attention to
the practical considerations involved in valuation of
raw sugars for refining purposes and to suggest some
amplifications of the tests applied, with the hope that
it may lead to a full discussion of the subject and in
the belief that closer attention to the points involved
must inevitably lead to greater efficiency of manufac-
ture with a consequent decrease of wasteful operation
in both manufacture and refining.
The refining value of a raw sugar depends upon its
content of sucrose and the availability of that sucrose,
as modified by the nature and quantity of the impuri-
ties. The nature of the impurities will determine the
ease of their separation from the sucrose during re-
fining.
Refining consists principally of (1) affination or
washing the residual mother liquor of the raw sugar
massecuite from the solid grain of the sugar; (2)
defecation and filtration, to remove insoluble sub-
stances and some soluble impurities from the solution
of the washed sugar or from the dilute washings; (3)
decolorization by boneblack or other means; (4)
crystallization and separation of pure sugar from the
other constituents.
The response of any raw sugars to tests for the first
three of these operations can be determined readily
8io
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
by operations herein described, giving a far closer
grading of the sugar in its refining value than by the
data at present supplied.
The proposed tests are novel only in some details
and in their immediate application to a precise valua-
tion of raw sugars on a strictly mathematical and
therefore scientific basis.
The object of washing the raw sugar is to remove
the film of low-testing molasses from the surface of
the grains. A 96 ° polarizing sugar is usually crys-
tallized from a solution having a purity of something
less than 80, and the separation of the sucrose in crys-
tals leaves a mother liquor of between 60 and 70
purity. Purging the massecuite in centrifugals re-
moves, it is true, a large part of this syrup, but unless
the sugar crystals are sprayed with water or a sugar
solution in the centrifugal machine, an appreciable
amount of this mother liquor remains adherent to
the crystals.
As the object of refining is to separate the impuri-
ties from the sugar as promptly and thoroughly as
possible, the first operation of refining consists of
washing this residual mother liquor from the faces
of the sugar crystals, and the condition of the crystals
is a factor of great importance in this purification. An
even grain of large size is the easiest to cleanse. Small
crystals present relatively more surface than larger
ones, carrying more syrup, requiring larger amounts
of wash water, and present greater resistance to the
purging of the sugar. They also dissolve more freely
in the wash water or sugar solutions used for mixing
and washing, thus decreasing the yield of washed sugar
and increasing the amount of washings. This carries
relatively pure sugar off into impure washings and
increases the labor of its recovery. Small grained
sugars are slow to purge and are a detriment to rapid
work.
Clustered grain is another objectionable feature as
these conglomerates hold a certain amount of low
mother liquor which refuses to wash out.
The purity of the grain itself is of fundamental
importance for if that is not of high test, no amount
of washing will yield a washed sugar of the desired
quality.
All raw centrifugal sugars should be boiled from
clean solutions of sufficient purity to insure a nucleus
of the purest type, ranging over 99 in test. This can
ie done by starting grain on concentrated juice,
building up later if need be with syrups or mother
liquors from other sugars.
If a second or third sugar is used as seed grain the
resulting crystals will contain more impurity and can
never be washed up to the highest purity.
One of the best attempts at regulating the produc-
tion of raw sugar so as to meet reasonable require-
ments of refiners, lias been made by the Cuban-Amer-
ican Sugar Company. Their tests include size of
grain, taking a diameter of a little less than a milli-
meter as standard; hardness of grain, as observed
when rolled between the thumb and finger; odor,
divided into normal, musty, fruity, and sour; cleanli-
ness, as indicated by the milligrams of insoluble mat-
ter per 100 g., or by the turbidity of 5 g. dissolved in
25 cc. of water, as well as polarization and moisture.
The hardness of grain is at best a questionable fac-
tor. Its solubility is what counts, and the smaller
it is the more it dissolves. The refiner wants to know
what yield will be had of washed sugar in washing
any particular sample and how pure the washed sugar
will be. The more directly and accurately these
facts can be determined, the more useful the informa-
tion will be.
In working out this question the matter of first im-
portance was to adopt the proper liquid for washing
the raw sugar. Water is not suitable as it dissolves
too much of the grain. A pure sugar solution has
the objection of tending to obscure the difference
between high and low sugars through adding to each
approximately the same absolute amount instead
of the same relative amount of pure sugar. What
I have found to be more satisfactory is a saturated
solution of the raw sugar itself. This has the advan-
tage of dissolving none of the grain and removing prac-
tically all of the mother liquor from the crystals,
and finally of altering to a minimum degree the purity
of the washed sugar. The only other method would
be to use an alcohol washing method or its equiva-
lent, or to use a syrup or molasses obtained by working
back and washing several times, both of which are
too slow. The low molasses also becomes too viscous
to use to advantage.
The method used is to mix 100 g. of the raw sugar
with 45 cc. of water, shake 10 min. to saturate, let
settle, and decant 92 cc. of the resulting solution upon
200 g. of the raw sugar. This is well mixed into a
magma and purged in a small laboratory centrifugal.
In the experiments here referred to, a 5-in. cyclone
centrifugal has been used, with which about '/i min.
is needed to get up full speed. Two minutes' steady
running after this is all that is needed, making about
9 revolutions of the handle shaft each 10 seconds.
The sugar is thus made comparatively dry, and the
yield of washed sugar is found by weighing the basket
with the purged sugar in it.
The sugar is then removed, dried 2 hrs. at 9S0 C.
in a water-jacketed air bath, and polarized. A good
centrifugal sugar, not mixed with seconds, will polarize
about 99.4, which, of course, is the purity of the
washed crystals, and the ordinary centrifugal sugars,
such as constitute the greater part of the present-day
supply, will have a purity of at least 99 °. This is in
exact accord with refinery practice, showing that the
method above described gives as pure a washed sugar
as that obtained under working conditions, where
clear water is used in the final washing in the centrif-
ugals.
Washing an ordinary 96° centrifugal sugar yields
washings of 75 ° to 8o° purity, or thereabouts, and it
is highly desirable that all of the impurities possible
should be separated from the grain and forced into
the syrup, for these two are handled separately and
each additional pound of impurities that hangs back
in the washed sugar necessitates just so much extra
work for its final elimination. A pound of impuri-
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
811
ties will lose about 0.4 of its mass in the boneblack,
and carry with its remainder about 0.4 lb. of sugar
into residual syrup, having a purity of about 400.
In washings of 80° purity only about 2V2 boilings or
crystallizations are necessary to effect this separa-
tion, whereas in washed sugar of 98 ° purity 6 or
7 boilings and crystallizations with all the corre-
lated operations will be necessary to eliminate the im-
purities. In a washed sugar of 98 ° purity, therefore,,
as compared with one of 99 ° purity taken as standard,
there will be 1 per cent of the mass which will have
to be boiled, etc., four extra times. It follows that
each 1 per cent of impurities above the normal 1 per
cent left in the washed sugar costs the refiner 1 per
cent X 4 X the cost of boiling, etc., X price per lb. of
raw sugar above the basic price of raw sugar, and
should be valued accordingly. Conversely, a sugar
washing up to 99.5° purity under standard conditions
is o. 5 per cent X 4 X boiling cost X price per lb. of
raw sugar less expensive to refine than the normal and
should be valued in accordance.
The second point to be taken into account is the
amount of defecation required and the speed of fil-
tration. These two items are rather closely related,
as no raw sugar solutions will filter clear unless defeca-
ting material be added to flocculate the fine suspended
impurities into masses sufficiently large to be caught
in the meshes of the filter cloth or other medium em-
ployed. Raw sugars require differing amounts of
defecant and consume widely varying lengths of time
for nitration.
It has always been customary to neutralize any
acidity with lime added in a thin cream. Formerly
the flocculation required was obtained by adding blood
from slaughter houses to the solution before heating
to the coagulating point of serum, then raising the
temperature and causing a strong flocculation.
Later, phosphoric acid and acid phosphate of lime
came into vogue and these, neutralized with lime,
proved very satisfactory when using filtering bags.
But the rapid work done in the beet sugar industry in
filtering carbonate of lime in filter presses could not
be followed in sugar refining on phosphate of lime
because this precipitate is soft and chokes up the
cloths when subjected to the high pressure necessarily
used in the filter press.
Now, in the past few years, a suitable defecant for
use in filtering sugar solutions through filter presses
has been found in the great deposits of infusorial
earth at Lompoc, Cal. One vein of this deposit,
after special processes of treatment, is now being largely
used, under the name of Filtercel, by nearly all the
refiners of the country. But despite the most careful
treatment in defecation, some raw sugars will filter
very slowly, delaying the operations of a refinery
sometimes in an exaggerated and very costly manner.
Such sugars are commonly called gummy, and fre-
quently indeed they give an excessive amount of pre-
cipitate when treated, in solution, with an excess of
alcohol and a little acetic acid. These sugars are in
fact very common and their objectionable quality is
quite evidently due to the improper defecation of raw
cane juice, a matter that is capable of nearly complete
correction, and that at almost no added expense.
Some raw sugars, on the other hand, filter very slowly,
although containing no excessive gummy matter,
probably from high sulfates, from clay, and other
causes.
In order to determine the relative filterability of a
raw sugar, it has been found best to use a 45 per cent
solution defecated with the minimum amount of acid
calcium phosphate and made slightly alkaline with a
standard sucrate of lime. Into 18. 1 cc. of this solu-
tion, representing 10 g. of raw sugar, introduce 0.2
cc. of a solution of acid calcium phosphate made up
to contain 1 per cent P2O5. This will represent 0.02
per cent P2O5 on the dry sugar. Then add saccharate
of lime standardized against the P205 solution so as
to balance it volume for volume when using phenol-
phthalein, until the solution is just faintly alkaline to
litmus. This is heated to boiling in a test tube and
allowed to settle while inclined at 45 °. Other tubes
are rapidly prepared in succession, using 0.03 per
cent P2O5, 0.04 per cent, and so on, noting the mini-
mum amount which gives a clear supernatant liquor.
After thus determining the minimum amount of
defecant that will give a clear solution by this pre-
liminary trial, one adds the indicated amount of acid
phosphate and lime to 100 cc. of the 45° Brix sugar
solution, heats gradually to 1900 F., lets stand half
a minute off the hot surface, and pours slowly in a
small stream upon the top of the triple thickness of
a 6-in. bag filter cloth folded like a filter paper in a
3-in. perforated brass cone, with about 625 holes per
sq. in., setting loosely by means of attached lugs, in a
vulcanite funnel with no stem. In about 3/< minute,
when the transfer is complete, the cloth is closely cov-
ered with a watch glass. The time is observed which
is required for the filtration of 70 cc. If the cloth is
of the right structure this filtrate will appear clear.
Excessive amounts of defecant retard rather then
aid filtration.
In the refinery the column of liquor constantly
rises in the bags, while in this test the column, after
the short period of introduction, constantly sinks,
so that conditions are quite different, and while they
cannot be directly compared, there is found to be this
relation — that the slower the solution is to filter in
the refinery the longer the time required for 70 cc. to
pass through the small filter cloth. In sugar solu-
tions that filter freely this test portion will run through
in 5 min. or less. In medium sugars from 5 to 10
min. will be taken, while poor sugars require 10 to
15 min., and bad samples take from 15 to 20 min.,
or even longer.
As a very slow filtering sugar may easily increase
the time of filtration in the refinery to 120 pel <nt
of the normal, it follows that time lost may be ap-
proximated by adding 7 per cent to the normal time
1 additional 5 min. in the experimental filtra-
tion test. The percentage of excess time multiplied
by the price of a pound of raw sugar multiplied by
the cost of normal filtration will give approximately
the correction to be deducted from the basic price
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. Xo. 10
to arrive at the refining value of a slow filtering
sugar.
The third item to be taken into account as affecting
the value of a raw sugar is its readiness to yield up
its color on filtration through boneblack or on sub-
jection to any other decolorizing process. After all,
refining sugar is principally decolorizing it, and any
system of standardization or valuation of raws which
ignores this important feature is lacking in one of the
essential details.
Sugars may be of a wide range of shades and from
many causes, as the variety of cane, burnt cane,
caramelization during manufacture, over-liming, work-
ing back molasses and second or third product sugars,
contamination by iron salts, and so on. Some of these
coloring matters are more easily absorbed than others
and their absorption by different agents varies widely.
For instance, the natural color of cane juice is only
slightly absorbed by boneblack, while Norit absorbs
it quite freely; and this latter agent takes up 95 parts
of color due to the action of lime on invert sugar as
easily as it absorbs 23 parts of color due to caramel.
These and other considerations render an empirical
test desirable, based on general common practice.
Such a determination of the decolorability of a raw
sugar by boneblack, for instance, may be arrived at
by dissolving 10 g. of raw sugar in 30 cc. of water,
adding 0.25 g. of Filtered and 2 g. of the best bone-
black ground finer than 60 mesh, bringing all gently
to a boil, and filtering through paper. A similar test,
made as the first is, but without boneblack, affords the
basis of comparison. After reading the colors of the
filtrates either against a tintometer standard or by
comparing the depths of columns to give equal colors,
one may readily calculate the amount of color absorbed
by the boneblack.
It will be found that a fair average sugar will yield
about 75 per cent of its color in this test, and any
greater amount yielded means a proportional economy
in char work required, while a smaller absorption
designates a larger amount of char work that will be
required. One can easily calculate the amount to be
added to or deducted from the basic price of a sugar
to arrive at its value in respect to filterability. Thus
a sugar giving up only 60 per cent of color instead of
75 per cent should have ls/so of the normal char filter-
ing expense deducted from the basic price to recom-
pense for the extra expense that will be entailed in
its char filtration.
Other factors might be taken into account, as the
amount of ash in the raw sugar, but as under present
conditions it is of less importance how much melassi-
genic ash there is than how much time and labor will
have to be expended in refining the sugar, these fac-
tors may, for the present, be disregarded.
The extra refining expenses enumerated in the above
examples are very small, it is true, and would occur
in relatively few cases, but with upward of $600,000
worth of raw sugar entering the port of New York
alone, daily, even small decimals add up to large aggre-
gates and are certainly worth taking into account.
Just now there is so ready a market for all raw sugar
that competition in its sale is slight, but when the
present stress is over and Europe resumes her large
production there will be a great surplus, with corre-
sponding competition to sell. Then the purchaser
will pick and choose what suits him best, and it is the
part of caution for the raw-sugar maker to consider
what class of sugars will be most desired and to manage
his manufacture accordingly. It is in the hope of
assisting in this very particular discrimination that
these suggestions are presented.
Yonkers, New York
ON THE PREPARATION OF AN ACTIVE DECOLORIZING
CARBON FROM KELP1
By F. W. Zerban and E. C. Freela_sd
Dr. J. W. Turrentine, in charge of the United States
Experimental Kelp Potash Plant at Summerland,
California, has for several years been engaged in work-
ing out methods for the commercial utilization of the
giant kelps of the Pacific Coast. During the course
of his investigations it occurred to him that the char
obtained in the manufacturing process used might
perhaps be converted into a decolorizing carbon. It
appears, however, that this question was not taken up
actively, until one of the authors of this article con-
ceived the same idea, while engaged in a study on
carbons that might be used in the cane sugar indus-
try. At his request, Dr. Turrentine sent him some
dried kelp to experiment with. In the first test
the kelp, after thorough drying and grinding, was
carbonized in an iron retort provided with an outlet
for gases, until no more fumes were given off. The
char was then transferred to a closed iron receptacle
and heated for 2 hrs. to a bright red heat. It
was then cooled, boiled out with hydrochloric acid,
washed with water, and dried. Upon examination
it was found that the resulting carbon reduced the
color of a molasses test solution to about one-third
of that obtained by using an equal quantity of our
standard carbon, Norit. A sample of kelp char, also
received from Dr. Turrentine, when treated in a similar
manner as the dried kelp, produced only a very poor
carbon. We therefore decided to investigate this
matter more thoroughly, and at our request Dr. Tur-
rentine very kindly furnished us an ample supply
of raw material for our further experiments, and we
wish to express to him our thanks for this courtesy,
as well as for the great interest he has taken in the
progress of our work. The material received con-
sisted of three different samples. The first, A. was
kelp (Macrocystis pyrifera) dried in a rotary kiln;
the second, B, was "incinerated"' kelp, prepared as
described below; and the third, C, was a sample made
by subjecting kelp to destructive distillation. The
last sample was kindly sent to us through Dr. Spencer,
who was investigating the destructive distillation
of kelp at the Forest Products Laboratory, Madison,
Wisconsin. None of the three samples had been
leached with water.
1 Presented before the Division of Industrial Chemists and Chemical
Engineers at the 56th Meeting of the American Chemical Society, Cleveland,
September 10 to 1J, 1918.
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
813
Upon investigation it was found that there are three
factors which have an important effect on the proper-
ties of the final product sought. First of these is the
particular point in the process at which the soluble
salts and other ash constituents are removed. The
second is the method by which the material is carbon-
ized. We used two different ways with Sample A.
In one experiment it was charred in an open iron
saucepan over a gas ring burner, until fumes ceased
to come off and the material was thoroughly carbon-
ized. In other tests the process was conducted in a
half gallon, heavy iron retort with a descending iron
condensing tube about V2 in. in diameter and 3 ft.
long. This was heated over a gas ring burner. Sam-
ple B, which was a char, had been prepared by feeding
dried kelp into a revolving "incinerator," setting it on
fire, and after it had been heated sufficiently, cooling
it rapidly by quenching. Sample C was only partly
carbonized, having undergone destructive distillation
at a temperature not exceeding 314° C.
The third factor is the temperature to which the
char, obtained by carbonization, is heated in a closed
receptacle. We effected this final heating in an iron
cylinder made from a nipple of 2-in. pipe, closed at
both ends by screwed-on iron caps. This cylinder
was placed in a muffle furnace commonly used for
making ash determinations in sugar products, and
which produces a maximum heat of about 8oo° to
900° C.
The three factors mentioned will be taken up in
detail in this paper. The decolorizing effect on sugar
products of the various carbons made was determined
by the following method: 5 g. of the carbon under
examination are added to 200 cc. of a 3 per cent solu-
tion of a stock sample of low-grade molasses. The solu-
tion is brought just to the boiling point and at once
filtered through a folded filter. The decolorized solu-
tion is then compared colorimetrically with one ob-
tained under the same conditions, but using 5 g. of
Norit instead of the carbon. The color of the solu-
tion obtained by means of Norit is used as a standard
and is called " 1." Carbons more effective than Norit
will give figures below "1" and those less effective
figures above "1". The reciprocals of the figures
give a direct measure of the effectiveness of the car-
bon as compared with Norit.
EFFECT OF LEACHING
A part of each sample, A, B, and C, was boiled out
several times with water, thoroughly drained, and again
dried. Parallel experiments were then made with
both leached and unleached material. The following
table gives the tests and their results:
Color op Solution Decolorized
with Carbon from
Leached Not leached
before before
Treatment heating heating
A, charred in retort, heated to bright red heat in
closed iron cylinder, boiled out with water 5.00 2.86
A, charred, heated to bright red heat, boiled out
with acid, then water 2. 78 1 . 25
B, heated to bright red heat, boiled out with water. 2.56 1.37
B, heated to bright red heat, boiled out with acid,
then water 1.47 0.34
C, heated to bright red heat, boiled out with water. 3.57 3.33
C, heated to bright red heat, boiled out with acid,
then water 1.85 1.37
The table shows that the better carbon is always ob-
tained from the unleached material, and, in fact, the
only carbon that is better than Norit, and consider-
ably so, was prepared from material that was not
treated with any solvent until after it had been brought
to red heat. We may conclude from this that if our
object is to make an active carbon, none of the min-
eral matter must be removed before heating the ma-
terial to red heat.
EFFECT OF METHOD OF CARBONIZATION
The way in which the kelp is carbonized is almost of
as great importance as the question of leaching. The
different methods of charring have already been de-
scribed above. It is very difficult to carbonize the
kelp in the iron retort always under the same condi-
tions on account of varying gas pressure and because
the condensing tube often gets more or less clogged
with tarry products, thus preventing the free escape
of the fumes. The effect of these factors which were
not under control is strikingly shown in the figures
below.
Treatment Color
A, carbonized in an open saucepan, then heated to bright red
heat in closed cylinder, boiled out with acid, then water 0.28
A, carbonized in iron retort, then heated to bright red heat, boiled
out with acid, then water 0.31
Same, other experiment 0 . 50
Same, other experiment 0 . 75
Same, other experiment 1 . 25
B, heated to bright red heat, boiled out with acid, then water. . . 0.34
C, heated to bright red heat, boiled out with acid, then water. . . 1.37
C, first completely carbonized in open saucepan, heated to bright
red heat, boiled out with acid, then water 1 .70
These experiments show that the best results are ob-
tained when the raw material is carbonized quickly
at a comparatively high temperature and in such a
way that the fumes can freely escape. Carboniza-
tion alone, howevei , is not sufficient to make an active
decolorizing carbon, as is shown by the fact that Sam-
ple B itself, without first being heated to red heat,
produced a color of 3 . 70 when extracted with water,
and of 1. 56 when extracted with acid and then washed
with water. Sample C gave 3.85 and 1.72, respec-
tively.
EFFECT OF TEMPERATURE TO WHICH THE MATERIAL
IS HEATED AFTER CARBONIZATION
Three series of experiments were made to test
this question, two (1 to 4 and 5 to 8) with char ob-
tained by carbonizing Sample A in the iron retort at
low temperature, and another with Sample B as re-
ceived (9 to 11).
No. Treatment Color
1 A. carbonized in iron retort, heated to full red heat, boiled
out with water 2.86
2 A, carbonized, heated to medium red heat, boiled out with
water 3 . 23
3 A, carbonized, heated to low red heat, boiled out with water. 3.57
4 A, carbonized, heated to barely red heat, boiled out with
water 4.17
5 A, carbonized, heated to full red heat, boiled out with acid,
then water 1 . 25
6 A. carbonized, heated to medium red heat, boiled out with
acid, then water ■ ■ 1-52
7 A, carbonized, heated to low red heat, boiled out with acid,
then water 1-47
8 A, carbonized, heated to barely red heat, boiled out with
acid, then water 1.72
9 II, heated to full red heat, boiled out with acid, then water
0.34 and 0.30, average 0.32
10 B, heated to medium red heat, boiled out with acid, then
water 0 . 62
1 1 11, heated to low red heat, boiled out with acid, then with
water 1 . 43
iM
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
We find that within the temperatures at which tests
were made the best carbon is obtained by heating to
the highest temperature, full red heat. It is possible
and even probable that still better carbons might be
prepared by heating to even higher temperatures,
but this would hardly be of practical interest. One
experiment was made in which a quantity of B was
heated in a clay crucible in a Fletcher furnace, but
observation showed that the temperature was not any
higher than we could obtain with the iron cylinder
in the muffle furnace. The resulting carbon, after
washing with acid and water, produced a color
of 0.36, which is very close to the 0.32 shown in the
above table for the muffle heated carbon.
Another experiment was carried out in order to
see whether a good carbon could not be made in one
operation. The iron cylinder described above was
filled with dried kelp, and one of the caps was only
screwed on loosely, so that the fumes might escape,
without giving the air free access to the char. After
heating to full red heat the carbon was boiled out
with acid, and washed with water. It produced a
color of 0.75, and was therefore much less effective
than the carbon produced in two operations.
We have also found that it is not necessary to ex-
tract the carbon directly with hydrochloric acid.
The water-soluble salts can first be removed with this
solvent, and the greater part of the remaining ash
is then dissolved with hydrochloric acid, after which
the acid is again washed out with water.
Summarizing briefly, our tests have shown that a
carbon which has a much greater decolorizing power
than Norit can be prepared in the laboratory by quickly
carbonizing dried Pacific Coast kelp in such a way that
the fumes can freely escape. After they cease to come off,
the char is transferred to a closed iron receptacle and
heated for 2 hrs. or so to red heat. Instead of
charring dried kelp, "incinerated" kelp may be used
directly. The carbon is then boiled out either with
dilute hydrochloric acid, or firet with water and then
acid. This is again washed out with water, and the
carbon dried. It remains to be seen whether the
process can be worked successfully and economically
on a large scale, and whether the price to be gotten
for the finished product will warrant its manufac-
ture. The most logical place to work out the first
problem is the United States Experimental Kelp
Potash Plant in California, and we hope that the
Bureau of Soils may be willing and able to take up
this project.
The great decolorizing power of the kelp carbon is
probably due to two factors. We had found before
that active decolorizing carbons can be prepared
from cellulose materials by first impregnating them
willi either infusible substances like lime, alumina,
silica, or else with such substances as chlorides, etc.,
which are volatile at the temperature at which the
carbon is made. In all these cases the carbon must
be heated to red heat to get good results, and the im-
pregnating substances must then be removed with proper
solvents. In the particular case of potassium chloride
as impregnating substance the carbon obtained was
rather poor, and the potassium chloride content of
the kelp alone would not explain the decolorizing
power of the kelp carbon. There is also too little in-
fusible ash to account for it. However, a distinguish-
ing feature of kelp is its high nitrogen content, and it
seems reasonable to suppose that this is largely re-
sponsible for the great effect of kelp carbon. The
great decolorizing power of carbons made from highly
nitrogenous materials, like blood charcoal, or the
carbon made from the residues of the manufacture
of ferrocyanide and from similar materials has long
been well known. We noticed that in every case
where we obtained a good carbon from kelp, prussian
blue was formed when the carbon coming from the
muffle was extracted with hydrochloric acid. It im-
parted to the wash waters a deep blue color, being
dissolved in colloidal form. The r61e played by the
nitrogen is not known definitely, but the effect of its
presence is quite plain.
SUMMARY
It is shown in this paper that under proper condi-
tions a decolorizing carbon much more effective than
Norit can be prepared from Pacific Coast kelp. The
factors affecting the decolorizing power of the carbon
are discussed, and a method for making the most
effective carbon is described.
Louisiana Sugar Experiment Station
New Orleans, Louisiana
THE ROLE OF OXIDASES AND OF LRON IN THE COLOR
CHANGES OF SUGAR CANE JUICE1
By F. W. Zerban
If the methods now being used in the manufacture
of white sugar directly from the cane are to be placed
on a strictly scientific basis, it will be necessary to
gain a more accurate knowledge of the coloring mat-
ters which have to be removed or the formation of
which has to be avoided. A great deal of work has
already been done in this direction, but much more
still remains to be done. Any such investigation must
first take into consideration the coloring matter found
in the cane itself and in the raw juice obtained from
it by applying pressure or diffusion.
Previous investigators have found that the cane
contains chlorophyll, saccharetin, and, in the case of
dark-colored canes, also anthocyanin. Neither the
chlorophyll nor the saccharetin dissolve in the juice
upon milling, but pass into it mechanically with the
finely divided bagasse. They therefore do not affect
the color of the juice itself, except in the form of solid
suspended particles, and do not make their presence
felt until the juice is treated with lime, an excess of
which causes the saccharetin to turn yellow. An-
thocyanin, however, is quite soluble in the raw juice,
and this is the reason why dark-colored canes give
a darker juice than light-colored ones.
But all these facts do not explain the dark color
of raw juice from light-colored canes. C. A. Browne*
nted before the Division of Agricultural and Food Chemistry
at the 56th Meeting of the American Chemical Society, Cleveland, Sep-
tember 10 to 13, 1918.
'Louisiana Bulletin, 76, 249; 91, 17.
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
815
states that the darkening of raw cane juice is due to the
effect of an oxidizing enzyme, closely related to oenoxy-
dase, upon certain polyphenols present in the juice.
This enzyme was found to act upon hydroquinone,
but not on tyrosin. Browne concluded from this
that tyrosinase was absent in cane juice. However,
he found a peroxidase in some cases.
Previously, Raciborski1 had discovered two oxidizing
enzymes in cane, but did not investigate their connec-
tion with the darkening of cane juices. He found in the
growing parts of the cane an oxidase (a laccase) which
turned tincture of guaiac blue in the absence of hydro-
gen peroxide. It was very unstable, soon losing its
oxidizing action upon standing, and being destroyed
rapidly by heating above 6o°. But besides this lac-
case he detected in all parts of the cane, young or old,
an enzyme giving a dark blue coloration with tincture
of guaiac to which hydrogen peroxide had been added.
This enzyme was therefore what we now term a peroxi-
dase. It was found to be very stable, and resistant to
temperatures of 00 ° to 95°. He called this substance
leptomin. Further tests showed it to be present in
all the higher plants investigated, and Raciborski
drew from this the conclusion that his leptomin per-
formed an important function in the life of all higher
plants, being comparable to the hemoglobin of the
animal kingdom.
Prinsen-Geerligs found in 19052 that the gray color
of certain sugars is associated with the presence in
them of small quantities of iron, and he suggested
that the iron was in the form of a saccharate. In
1913 Shilstone2 again called attention to the fact that
the iron, of which practically all modern sugar ma-
chinery is made, wa,s responsible for the dark color of
certain sugars, and I. F. Morse3 made a similar sug-
gestion. Shilstone also recognized the fact that the
iron must be in the form of extremely dark-colored
compounds, because otherwise the very great effect
of mere traces of iron could not be explained. He
suggested that the iron was combined with "organic
acids." It remained for Schneller4 to show what
particular class of organic iron compounds could cause
the grayish tint of sugars and the abnormally dark
color of other sugar products. Schneller based his
explanation on the discovery by Szymanski6 and by
Browne5 of "tannins" in cane, i. e., of aromatic com-
pounds giving the well-known color reaction with ferric
salts, and which need not necessarily be true tannins
in the chemical sense of the word, but may be any
of the numerous polyphenols or phenolcarbonic acids.
As a further support of his explanation, Schneller
called attention to the researches of Gonnermann7 and of
Grafe8 on the darkening of beet juices. Both of these
authors had concluded from their investigations that
the dark color of beet juices is caused by the action
1 Archie/ ». d. Java-Suikerind., No. 8, 1906.
• Louisiana Planter, 49, 402.
• Modern Sugar Planter, No. 6, 43.
• Louisiana Bulletin, 167.
• Her. dcr Vers.-Stat. far Zuckerrohr in West Java, 2, 13.
• Louisiana Bulletin, 91, 9.
' Z. Ver. D. Zuckerind., 67, 1068.
• Oesttrr.-Ung. Z. Zuckerind., 37, 55.
of tyrosinase on pyrocatechin in the presence of fer-
rous salts. According to Gonnermann, the pyro-
catechin which both he and Grafe found in beet juices
is not present as such in the beet itself, but is formed,
as soon as the juice is extracted, by the action of tyro-
sinase on the tyrosin of the beet.
In view of these facts Schneller's explanation seemed
so plausible that it was decided to test it further, and
to see whether the dark color of cane juices could be
experimentally explained on the basis of Schneller's
hypothesis. It was decided to make the necessary
tests with material as free as possible from the natural
coloring matters of the cane which we have enumerated
above. For this reason we used young cane shoots
from which the leaves were entirely removed, and which
therefore contained practically no chlorophyll. Neither
could they contain any anthocyanin, and the presence
of any saccharetin could not make itself felt to any ex-
tent, because it does 'not dissolve in the natural juice.
The young shoots have the further advantage that
they are rich in "tannin," and that the color reactions
would therefore be more pronounced.
We first undertook the identification of the oxidizing
enzymes of the cane, and a study of the effects of iron
salts. The nature of the "tannins" will form the
subject of a later paper.
A young cane shoot was ground to pulp with a little
water in a porcelain mortar, and we were surprised
to find that the color of the solution obtained was en-
tirely unlike that of a mill juice. It was dark brown,
instead of the characteristic muddy green color of mill
juice. This at once suggested that the iron of the mill
had something to do with the color of the mill juice.
In a second test we added a crystal of ferrous sulfate,
the size of a pin-head, to the water in which the cane
was macerated, and we at once obtained a dark green
juice, exactly of the same tint as mill juice, only more
pronounced. It might be objected here that the cane
itself contains iron. This is perfectly true, but it is
well known that the iron is in organic combination
and not in ionized form.
We would conclude from these tests that the brown
color obtained in the first instance is due to the action
of oxidases on the polyphenols, while in the second
case the ferrous salt reacts with both the oxidase and
the polyphenols yet unattacked. The result will be
the green color due to the reaction of ferric salts with
certain polyphenols which will entirely mask the
brown color of the oxidation products of polyphenols,
to study this question further, the following
experiments were made:
Six flasks were prepared, with equal quantities of water in
each.
Test i — A earn; shoot was cut up into fine chilis, and they
were dropped directly into the water. The mixture was then
allowed to stand, with frequent stirring. The juice gradually
turned dark brown.
Test 2 — Same as Test I, but water was first heated to boiling
and was kept boiling while the cane slices were dropped in.
This juice remained colorless for days.
-Same as Test I, except that 15 mg. of iron in the form
of ferrous sulfate were dissolved in the water, before the cane
idded. The juice rapidly turned -i muddy green to a
I I ilaek.
8i6
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. 10
Test 4 — Same as Test i, except that 15 mg. of iron in the form that they rapidly turn greenish black, and all of the
of ferric chloride were dissolved in the water before adding the . . - , assumes a green color,
cane. Similar result as in lest 3. j r
Test 5— Same as Test 2, except that after short boiling the Having ascertained the exact r61e played by the
flask was rapidly cooled in running water. Then 15 mg. of iron iron, the next step was to identify the oxidizing en-
as ferrous sulfate were added. The juice remained colorless for present in the young shoots. Previous work
some time, but gradually became green, as the ferrous iron was ***"» l"ac"1 J 6
oxidized. along this line has already been mentioned. Browne s
Test 6 — Same as Test 5, but substituting ferric chloride for results showing the absence of tyrosinase seemed
the ferrous sulfate. Juice at once became dark green after addi- surpi.ism„ jn v,ew 0f the fact that the writer found
tion of the ferric chloride solution. . . , . ...
tyrosm in cane.1 However, for this very reason tyro-
The results clearly show that the color of a raw sinase could not readily be identified by the addition of
juice depends on several factors, viz., the presence or tyrosin to the juice. It was therefore necessary to look
absence of oxidizing enzymes, the presence or absence for tyrosinase with the aid of other reactions. Be-
of iron salts, and the form in which any iron salts are sides, not much reliance can be placed on any identi-
present. The result of Test 1 is due to the effect of fixation of enzymes made on the basis of tests with
the oxidizing enzymes on the polyphenols of the cane. cane juice, or even with solutions obtained by drop-
. Material Not Extracted With Alcohol . Material Extracted With Alcohol •
No addition Acid Alkaline No addition Acid Alkaline
No. Test Reagent A B C D E F
1 Water Dark, muddy brown Brownish yellow Dark.muddybrown Very slight dark- No change Very slight dark-
ening ening
2 Pyrocatechin. 1 per Quickly turns golden Quickly lemon-yel- Quickly turns pink- Darkens very Same as D, but less Same as D, but
cent soln. . . .' yellow, darkens to low, darkens to ish yellow, dark- quickly through quickly more quickly
medium brown brownish yellow ens to dark brown yellow
3 Resorcinol, I per No change No change No change No change No change No change
4 Hydroquinone 1 per Purple, darkens to Light purple, much Turns purple rapid- Purple, darkens to Same as D, but less Same as D. but
cent soln ' brown lighter than A ly, darkens to pur- brown quickly more quickly
, plish brown
5 Pyrogallol, 1 per Golden yellow, dark- Golden yellow. Turns yellow rapid- Like A Like B Like C
cent soln ens to brownish lighter than A ly and soon dark-
yellow ens to brown
6 Phloroglucinol, 1 per No change No change No change No change N'o change No change
7 Guaiacol, ' " 1 " per Purplish pink Light pink Purple Turns purple Lighter than D Darker than D
cent soln quickly
8 Paracresoi, 1 per Brownish yellow Reddish brown Brownish yellow Pinkish yellow No darkening. Yellowish red
cent soln turns milky
9 Paracresoi 0 1 per Reddish brown Brownish yellow Dark reddish brown Orange-red No darkening Red. next morning
cent soln. plus cry- blue.with copper-
stal of glycocoll. . . colored reflex
10 Tincture of guaiae. . Blue Blue
1 1 Tannin, 1 per cent Light yellow Very light yellow Yellow No change No change No change
12 Tyrosin, 1 per cent Dark, muddy brown Brownish yellow Greenish black Muddy gray No change Muddy gTay
soln
In Test 2 the enzymes are destroyed by boiling, and P^g cane slices directly into the test solutions, be-
since there were no iron ions present, the juice did cause the polyphenols present in the cane are also
not change at all. Test 3 is a duplicate of the one acted upon by the enzymes, and the reactions are thus
already described and discussed above. In Test 4 liable t0 be obscured. A more reliable method consists
there is no need for the oxidase to act upon the iron in dropping thin slices of the material into strong alco-
salt because it is already in the ferric form. The color hoi contained in a mortar and macerating them with
of a juice extracted in the presence of iron salts will a pestle. The alcohol precipitates the enzymes,
depend on the quantity of these salts. When this is while the polyphenols go into solution. The alcohol
infinitesimally small the brown color of the oxidation is then filtered off rapidly, the residual pulp dried
products of the polyphenols will overbalance the green quickly between filter paper, and the remaining pulp
color of the polyphenol-iron compounds. As the may now be used for carrying out the tests with the
iron gradually increases we get mixtures of green and various polyphenol solutions.
brown, and finally the green will become the dominating Several series of experiments were made, both by
color. This is reached with only very small quantities dropping thin slices of cane shoots directly into the
of iron. In Test 5 the enzymes are eliminated by water solutions of the various reagents, and also by
boiling. The juice therefore contains only unoxidized using the alcohol-extracted pulp in the same way. In
polyphenols, as in Test 2. They give no reaction with every case parallel tests were made in solutions slightly
ferrous salts, but as the oxygen of the air gradually acidified with acetic acid, and in others made slightly
oxidizes the iron to the trivalent form, the color of alkaline with sodium bicarbonate. In every experi-
the phenol-iron compound appears. In Test 6 this ment a drop of toluene was added to the test solution,
happens at once after the ferric salt is added. The preceding table gives the results of these experi-
Now we can readily understand why cane juice ments.
that has not come in contact with iron turns brown The results show that the tests in which the material
(Test 1), and why juice obtained by the mill in the was not extracted with alcohol in some cases gave
sugar factory turns green (Test 3). We have found, characteristic reactions, while in others they were more
when passing young cane shoots through a clean labora- affected by the polyphenols naturally present in the
tory mill, that the first part of the juice is brown, but cane than by the test reagents used. This is espe-
soon the particles of fiber in direct contact with the cially marked in the tests with paracresoi. Nos. 8
iron Of the mill form enough Organic ferrous salt SO ■ Original Communication, 8th fat Conp. App. Chem.. 8, 103.
Oct., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
817
and 9. Here the water solutions gave in every case
colorations similar to those obtained in the absence of
the phenols used as reagents, and the tint was only
slightly influenced by the latter. But the alcohol-ex-
tracted pulp gave in these cases, very characteristic
reactions which clearly show that the cane shoots
contain not only a laccase (8E, 9E), but also tyro-
sinase (8D, 8F, 9D, and especially 9F, which is such a
characteristic reaction that it cannot be mistaken).
The presence of a laccase is further shown by the tests
with hydroquinone, pyrogallol, guaiacol, and tincture
of guaiac. The effect on pyrocatechin may be due to
both laccase and tyrosinase, as pyrocatechin seems to
be acted upon by both of these enzymes. The re-
action obtained with tyrosin itself was not very charac-
teristic, for reasons already explained above, and also
on account of the well-known interference with this
reaction by other substances, particularly amido
acids, which often have either an inhibitory effect on
tyrosinase, or may entirely change the color produced.
Tests for oxidases with potassium iodide-starch solu-
tion also gave positive results with both extracted and
unextracted pulp. This reaction is not due to nitrites,
because boiled juices do not give it, nor is it obtained
in the presence of N / 2 sulfuric acid.
The activity of both laccase and tyrosinase dimin-
ishes very rapidly, as was already pointed out by
Browne and by Raciborski. But the peroxidase reac-
tion with tincture of guaiac and hydrogen peroxide
could be obtained in juices that had been kept for
weeks, preserved with toluene. In the light of Bach
and Chodat's theory of oxidases this may be due to
the fact that the organic peroxide part of the oxidase
is quickly used up when acting upon the polyphenols
also contained in the can« itself, but that the peroxidase
part of the oxidase is much more stable.
Since the amount of tyrosin found in the cane by
the writer was extremely small, it would appear
that the dark brown color of cane juices in the absence
of^iron is due largely to the effect of the laccase upon
the polyphenols of the cane, and only in small part
to that of the tyrosinase upon tyrosin. The reaction
is therefore greatly different from that taking place
in beet juices.
The question as to the nature of the polyphenols
has so far not been taken up. Schneller suggested pyro-
catechin from analogy with the beet and from the
green iron reaction. During the past grinding season
several pounds of eyes which are rich in polyphenols
were cut off from sugar canes, and dropped directly
into alcohol. Cane tops also were sliced and treated
in the same way. But in spite of these precautions
the materials, which were kept in the laboratory, after
several months' standing, had darkened so much that
it was found impossible to isolate any polyphenols
from them in a pure state. So far we have been un-
able, to find any pyrocatechin in these solutions,
although the positive result of Wolff's test1 would point
to the possibility that pyrocatechin or some related
substance is present in the sugar cane. We intend to
approach this problem by a different method and hope
positively to identify any polyphenols or phenolcar-
bonic acids.
SUMMARY
The presence in young cane shoots of a laccase, of
tyrosinase, and of peroxidase has been established.
It is shown that the dark brown color of cane juices
obtained in the absence of iron is due to the action of
the laccase upon the polyphenols present in the cane,
and to a small extent, to that of the tyrosinase upon
the tyrosin of the cane. The dark green color of cane
juices from the factory mill is due to the interaction
of the laccase, the polyphenols of the cane, and
of the ferrous salts formed by the action of the organic
acids of the cane upon the iron of the mill. The fer-
rous salts are rapidly oxidized by the oxidases of the
cane to the ferric state, and these give the character-
istic dark-colored compounds with the polyphenols
of the cane.
Louisiana Sugar Experiment Station
New Orleans, Lou
LABORATORY AND PLANT
METHODS OF ANALYSIS USED IN THE COAL-TAR
INDUSTRY. II— DISTILLED TARS AND PITCHES
By J. M. Weiss
Received August 20, 19 IS
In Paper I of this series1 the author presented the
testing methods of The Barrett Company for crude
tar together with introductory matter to which we
would refer the reader of this paper All references
to previous tests noted in this paper refer to the pre-
ceding paper.1
DISTILLED TAE TESTS
test C2 — water. Identical with B2.
test C3 — specific gravity (pycnometer). Iden-
tical with B5.
test C4 — specific gravity (platinum plan). Iden-
tical with B6.
1 Tnis Journal, 10 (1918), 732.
test C5 — insoluble in benzol. Identical with B7.
test c6 — viscosity.- Identical with Bio.
test C7 — consistency (schutte)
apparatus — Schutte penetrometer (see Fig. IV). !
Stop watch.
method — The collar shall be filled by placing it
upon a flat tin roofing disk which has been coated
with a thin film of vaseline and pouring an excess of
material into the collar. After cooling and contrac-
tion the excess material shall be cut off level with the
upper edge of the plug by means of a heated knife
blade. The collar shall be then immersed in water
of the required temperature and left at that tem-
perature for 15 min. The collar with roofing disk
attached shall be screwed into the tube while the tube
' Ann. inn. Pasteur, SI, 92.
1 Figures arc numbered consecutively in this series of articles.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
T.nDlic
Fig, IV — Assembly of Schutte Penetrometer
is in position. The water bath, shall just cover the
shoulder of the tube. The tube shall be filled with
water of the required temperature and the roofing
disk removed by slipping it sideways. The time
(measured by a stop watch) from the slipping off of
the disk to the sudden drop of the water in the tube,
shall be noted and reported in seconds.
precautions — Take extreme care to keep the water
bath within 0.50 F. of the required temperature.
See that the thermometer used for taking this tem-
perature is of tested accuracy. Note that the thread
on the collar is so cut that it screws into the tube to an
exact depth of l/t in. Plug the small holes at the
top of the tube around the handle with wax or pitch
to prevent leakage of water during the test.
accuracy — ±5 per cent.
notes — As the bitumen is displaced from the plug
there is a very slight and gradual fall of water in the
>tube. The end-point is, however, a sharp and sud-
den drop and is unmistakable.
If no temperature for the test is specified, the tem-
perature (in even io° F., *. e., 400, 500, 6o°, etc.), at
which the test gives results nearest to 100 seconds,
should be selected.
TEST C8 — CONSISTENCY (FLOAT)1
apparatus — Float tester (see Fig. V). Brass plate,
5X8 cm. Stop watch.
method — The brass collar shall be placed with the
small end down on the brass plate which should
be previously amalgamated with mercury by rub-
bing it first with .1 dilute solution of a mercury salt
and then with metallic mercury. Sufficient of the
material to be tested shall then be melted in a suita-
1 Adapted from Bulletin 314, Office of Public Roads.
ble container, care being taken to prevent loss by
volatilization or formation of air bubbles. The ma-
terial shall then be poured into the collar in a thin
stream until slightly more than level with the top.
The surplus shall be removed, after cooling to room
temperature, by means of a steel spatula, the blade
of which has been slightly heated. The collar with
plate attached shall then be placed in water at 50 C.
and allowed to remain at that temperature for at least
15 minutes. A suitable water bath shall be filled
'A full of water, placed over a burner and brought to
the temperature at which it is desired to make the test.
This temperature shall not be allowed to vary during
the test more than 0.50 C. from the required point.
The brass plate shall be removed from the collar and
the latter with contents shall be screwed into the
aluminum float, which shall then be immediately
floated on the carefully regulated warm bath. As the
plug of bituminous material becomes warm and fluid,
it is gradually forced upward and out of the collar
until the entrance of water causes the collar to sink.
Unless otherwise specified, the time in seconds (noted
by a stop watch) from placing the float in water to the
time the water breaks through the material shall be re-
ported as the consistency of the material.
precautions — No test should be recorded if water
finds its way into the float through the thread of the
plug. This can be avoided by thoroughly coating
the thread with grease or vaseline.
notes — In certain specifications it is required to
take the time from placing the float in water until
the float sinks. This may make a difference of 5 to
10 seconds in the result. Tests are ordinarily made
at 500 C. At ioo° C. the test is not at all sensitive
for distilled tars.
F10. V — Assembly of Float Tester
Oct., IQlS
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
819
TEST C9 DISTILLATION1
apparatus — See Fig. VI.
Flask: The distillation flask shall be a 250 cc.
Engler distilling flask, having the following dimen-
sions:
Diameter of bulb 8.0cm
Length of neck 15.0 cm
Diameter of neck 1.7cm
Surface of material to lower side of tubulature 11.0
Length of tubulature 15.0
Diameter of tubulature 0.9
Angle of tubulature 75°
A variation of 3 per cent from the above measure-
ments shall be considered allowable.
Thermometer: The thermometer shall conform to
the following requirements:
The thermometer shall be made of thermometric
glass of a quality equivalent to suitable grades of Jena
or Corning. It shall be thoroughly annealed.
It shall be filled above the mercury with inert gas
which will not act chemically on or contaminate the
mercury. The pressure of the gas shall be sufficient
to prevent separation of the mercury column at all
temperatures of the scale. There shall be a reservoir
above the final graduation large enough so that the
pressure will not become excessive at the highest tem-
perature. The thermometer shall be finished at the
top with a small glass ring or button suitable for at-
taching a tag. Each thermometer shall have for
identification the maker's name, a serial number, and
the letters "A. S. T. M. Distillation."
The thermometer shall be graduated from o° to
400 ° C. at intervals of 1° C. Every fifth graduation
shall be longer than the intermediate ones, and every
tenth graduation beginning at zero shall be numbered.
The graduation marks and numbers shall be clear-
cut and distinct.
The thermometer shall conform to the following
dimensions:
Total length, maximum, 385 mm.
Diameter of stem, 7 mm.; permissible variation, 0.5 mm.
Diameter of bulb, minimum, 5 mm.; and shall not exceed diameter of
stem.
Length of bulb, 12.5 mm.; permissible variation, 2.5 mm.
Distance, 0° to bottom of bulb, 30 mm.; permissible variation, 5 mm.
Distance, 0" to 400°, 295 mm.; permissible variation, 10 mm.
The accuracy of the thermometer when delivered
to the purchaser shall be such that when tested at
full immersion the maximum error from o° to 2000 C.
shall not exceed 0.50; from 2000 to 300° C, it shall
not exceed i° C; from 3000 to 375 ° C, it shall not ex-
ceed 1.5° C.
The sensitiveness of the thermometer shall be such
that when cooled to a temperature of 74 ° below the
boiling point of water at the barometric pressure
at the time of test and plunged into free flow of steam,
the meniscus shall pass the point io° below the boil-
ing point of water in not more than 6 seconds.
Condenser: The condenser tube shall have the
following dimensions:
Adapter 70 mm.
Length of straight tube 185 mm.
Width of tube 12-15 mm.
Width of adapter end of tube 20-25 mm
1 See "Standard Method for Distillation of BituminouB Materials
Suitable for Road Treatment." A. S. T. M. D-20-I6. published in 1916,
A. S. T. M. Standards, pages 540, el seq.
Stands: Two iron stands shall be provided, one
with a universal clamp for holding the condenser, and
one with a light grip arm with a cork-lined clamp for
holding the flask.
Burner and Shield: A Bunsen burner shall be
provided, with a tin shield 20 cm. long by 9 cm. in
diameter. The shield shall have a small hole for ob-
serving the flame.
Cylinders: The cylinders used in collecting the
distillate shall have a capacity of 25 cc. and shall be
graduated in 0.1 cc.
method — The apparatus shall be set up as shown in
Fig. VI, the thermometer being placed so that the
top of the bulb is opposite the middle of the tubula-
ture. All connections shall be tight.
Fig. VI — Assembly for Distillation Test
A. S. T. M. D-20-16
Distilled Tars
If the presence of water is suspected or known, the
material shall be dehydrated before the test is made
(see B3).
One hundred cubic centimeters (see note) of the
dehydrated material to be tested shall be placed in
a tared flask and weighed. After adjusting the ther-
mometer, shield, condenser, etc., the distillation
is commenced, the rate being so regulated that 1 cc.
passes over every minute. The receiver is changed
as the mercury column just passes the fractionating
point.
The following fractions should be reported:
Start of distillation to 1 10° C.
110° to 170° C.
170° to 235° C.
235° to 270° C. •
270° to 300° C.
Residue
To determine the amount of residue, the flask is
weighed again when distillation is complete. During
the distillation the condenser tube shall be warmed
when necessary to prevent the deposition of any
sublimate. The percentages of fractions shall be
reported both by weight and by volume.
note — It is usually impractical to accurately
measure ioo cc. of the materials used for distillation.
Therefore, the weight corresponding to ioo cc. should
820
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 10
be calculated from the predetermined specific gravity
and this amount weighed into the flask. For exam-
ple, if the specific gravity is i . 189, the operator should
weigh out 1 18. 9 g. for the test.
PITCH TESTS
TEST D2 SPECIFIC GRAVITY (PLATINUM PAN)
This is identical with B6 with the special note that
care must be taken to prevent the formation of air
bubbles on the pitch when immersed in water.
TEST D3 SPECIFIC GRAVITY (PYCNOMETER)
This is identical with B5 with the same modifying
note as given under D2.
TEST D4 SPECIFIC GRAVITY (SUSPENDED CUBE)
apparatus — Chemical balance.
Wooden bridge: Usually supplied with balances.
This consists of a small wooden beaker support which
holds a beaker over the balance pan and at the same
time allows the pan to oscillate freely without con-
tact with the bridge at any point.
method — A lump of pitch shall be suspended
from the hook above the left-hand pan of the bal-
ance by means of a fine waxed silk thread in such a
manner that the cube is about one inch above the
pan and its weight noted. The bridge shall be ap-
plied with a beaker of freshly-boiled distilled water
at a temperature of about 130 C. (55° F.). The lump
of pitch (still suspended from the hook) shall be im-
mersed in the water, the temperature allowed to rise
to 15.5° C. (6o° F.), and the weight in water noted.
The weight of the pitch in air divided by its loss of
weight in water gives the specific gravity.
precautions — When weights are taken see that the
balance pan swings freely and does not touch the
bridge or beaker. See that the pitch cube is free from
air bubbles.
TEST D5 INSOLUBLE IN BENZOL (FREE CARBON)
All matter as to apparatus, method, precautions,
and accuracy given under B7 (except as noted below)
apply to this test on this material.
special note — If the pitch is hard enough, grinding
the material taken for test will be advantageous in
aiding the subsequent solution. It is well to examine
the carbon residue for foreign matter, such as wood
slivers, pieces of bagging, etc. If such foreign matter
is present, the test should be rejected. The require-
ment (as given under B7) to pass the material hot
through a 30-mesh sieve does not apply to these ma-
terials.
TEST D6 — WAXES MELTING POINT
apparatus — See Fig. VII.
Pitch mould. Hook made of No. 12 B. and S. gauge
copper wire (diam. 0.0808 in.). Beaker, 600 cc,
Griffin's low form.
Thermometer: The thermometer shall conform
to the following specifications:
I "' J length 370 to 400*mm.
Diameter 6.5 to 7.5 mm.
Iinlli length Not over 14 mm.
Bulb diameter 4.5 lo 5.5 mm
The scale shall start not less than 75 mm. above
the bottom of the bulb and extend over a distance
of 240 to 270 mm. The graduations shall be from
o° to 8o° C. in Vs° C. and shall be clear cut and dis-
tinct. '
The thermometer shall be correct to 0.250 C. as de-
termined by comparison at full immersion with a simi-
lar thermometer calibrated at full immersion by the
Bureau of Standards.
The thermometer shall be furnished with an ex-
pansion chamber at the top and have a ring for
attaching tags. It shall be made of a suitable quality
of glass and so annealed as not to change its readings
under conditions of use.
Fig. VII — Assembly of Test for Water Melting Point
method — (a) Pitches having melting points between
43° C. and 77° C.(no° 10170°^.). Acleanshaped
half-inch cube of pitch shall be formed in the mould
and placed on the hook of wire (see Fig. VII for detail
of method of placing the cube on the wire). The ap-
paratus shall be assembled as shown in Fig. VII, placing
400 cc. of freshly-boiled distilled water at 15. 50 C.
in the beaker.
The thermometer shall be placed so that the bottom
of the bulb is level with the bottom of the cube of
pitch and shall be immediately contiguous to, but not
touching, the cube.
The pitch cube shall be suspended so that its bot-
tom is one inch above the bottom of the beaker and
allowed to remain in the water at 15. 5 °, C. for 5
min. before starting the test. Heat shall then be
applied in such a manner that the temperature of the
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
821
water is raised 5° C. (9° F.) each minute. The tem-
perature recorded by the thermometer at the instant
the pitch touches the bottom of the beaker shall be
reported as the melting point.
(b) Pitches having melting points below 43 ° C.
(110° F.). These shall be tested exactly as under a,
except that the water at the start shall be 4° C. (400 F.)
and the cube shall be allowed to remain 5 min. at this
temperature before starting to apply the heat.
precautions — The use of boiled distilled water is
essential, as otherwise air bubbles may form on the
cube and retard its sinking. The rate of rise must
be uniform and not averaged over the period of the
test. All tests where the rise is not uniform shall be
rejected. A variation of not more than ±0.5° C.
for any minute period after the first three is the max-
imum allowable.
ACCURACY ±I°F.
notes — Pitches of the a range of consistency can
ordinarily be molded at room temperature, but, if
necessary, cold or hot water can be used to harden or
soften them. Pitches of the b range can be con-
veniently formed in water of about 40 C. (400 F.).
A sheet of paper placed on the bottom of the 600 cc.
beaker and conveniently weighted will prevent the
pitch from sticking to the beaker when it drops off,
thereby saving considerable time and trouble in clean-
ing.
This method shall not be used on pitches above
770 C. (170° F.), water melting point. Such pitches
shall be tested as under D7.
TEST D7 AIR MELTING POINT
apparatus — Melting point oven (see Fig. VIII).
Tripod: The oven shall be mounted on a suitable
tripod of such size that it supports the outer edge
only of the oven, leaving the bottom exposed directly
to the heat of the burner.
Burner: A Tyrell burner of type A. H. T. 22884,
E. & A. 1462 shall be used for heating. It shall be
provided with a suitable chimney (A. H. T. 22984,
E. & A. 1590).
Hooks: Made of No. 12 B. and S. gauge copper
wire (diam. 0.0808 in.).
Copper Cup: This shall be of about 50 cc. capacity,
in size i1/: in. deep, by 1V2 in. diameter. It shall be
provided with a wooden handle (see Fig. VIII).
Thermometer: This shall conform to the following
specifications:
Total length 380 to 385 mm.
Diameter of stem .* 6.5 to 7.5 mm.
Bulb length Not over 1 4 mm.
Bulb diameter 4 . 5 to 5 . 5 mm.
The graduations of the scale shall be from 30° to 1600
C. in '/i0 C. and shall be clear cut and distinct. The
30 ° mark shall be at least 75 mm. above the bottom of
the bulb. The length between the 30 ° mark and the
1600 mark shall be between 230 mm. and 275 mm.
The thermometer shall be correct to o.25°C. as de-
termined by comparison at full immersion with a simi-
lar thermometer calibrated at full immersion by the
Bureau of Standards.
The thermometer shall be furnished with an
expansion chamber at the top and have a ring for
attaching tags. It shall be made of a suitable quality
of glass and so annealed as not to change its readings
under conditions of use. It is desirable not to have a
supplementary bulb above the main bulb, but if this
is done, such supplementary bulb must not be separated
from the main bulb by a distance of more than 2 mm.
Aif Melting-Point Test (for Pitches)
method — The copper cup (see Fig. VIII) shall be half
filled with pitch and carefully heated until melted.
The cube shall then be formed by pouring- into the
mould and allowing to cool. The cube shall be sus-
pended in the oven on a hook of proper length so that
its center rests on a level with an imaginary line run-
ning through the centers of the observation windows.
The bottom of the thermometer bulb shall be level
with the bottom of the cube of pitch. The tempera-
ture of the oven is raised exactly 50 C. (90 F.) each
minute and the temperature recorded by the thermom-
eter at the instant the pitch drops to the bottom of
the oven shall be taken as the melting point.
precautions— Care shall be taken to avoid notice-
able evolution of vapors in the heating and melting
of the pitch. If necessary an oil bath may be used.
The apparatus should be set up in a place free from
drafts and if necessary protected by means of a
shield set apart from the apparatus. The oven itself
must not be lagged.
The rate of rise must be uniform and not averaged
over the period of the test. Any tests where the rise
is not uniform shall be rejected.
A variation (after the first 3 min. of the
test) of ±1° C. is the maximum allowable. Not over
II 1"' run in the oven at the same time,
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
and these shall not be pitches with melting points
more than 5° C. (o° F.) apart. The cubes shall be
close to but not touching the thermometer and equi-
distant from it.
I-Plan
H-Elevation
HI.-S[.cTioNTinoi)(in Center Line
'"^>
Fie. IX — Detail of Shield for Air Melting-Point Test
notes — This method shall be used only on pitches
melting above 77° C. (1700 F.). To make results by
this method comparable with result obtained in
water, 6.5° C. (12° F.) may be added to the ob-
served melting point, but the results of melting-point
tests must always be reported in terms of the method
by which the test is made.
In a laboratory free from drafts a shield is not
necessary. If one is needed, a convenient type which
can be easily constructed is shown in Fig. IX.
TEST DIO EVAPORATION
apparatus — Copper drying oven, 8 in. X 8 in. X
10 in., A. H. T. 41500, E. & A. 3030. The oven shall
be completely covered inside and out with Vs in.
asbestos board, excepting the outer bottom surface.
The door of the oven shall also be covered inside and
out with the same thickness of asbestos. The shelf of
the oven shall be 2.5 in. above the bottom of the
oven.
Evaporating dishes: These shall be made of pure
nickel. They shall be 2 in. inside diameter at the
bottom and Vis in. high, tapering at the top to a
diameter of 2l/s in. (see Fig. X). They shall be
provided with a suitable handle of the same ma-
terial.
Thermometer: This shall be graduated from o° to
300° C. in i° C. and of such a length that when placed
in position the ioo° C. mark will be within 10° C.
above the cork. This requires a total length of 300
to 350 mm. with the ioo° mark about 140 cm. from
the bottom of the bulb. The thermometer before
use shall be checked at full immersion against a ther-
mometer calibrated at full immersion by the Bureau
of Standards, and the readings used thereby cor-
rected.
Burner: The oven shall be heated by a Tyrell
burner (A. H. T. 22884, E. & A. 1462), provided with
a chimney of the type A. H. T. 22984, E. & A. 1590.
Assembly of apparatus: Shown in Fig. X. Each
dish shall be placed on a round l/t-'m. asbestos pad of
approximately the same diameter as the dish. The
bulb of the thermometer shall rest in a pan of suitable
high-flash oil, on a similar asbestos pad. The pan in
which the thermometer bulb is inserted shall be higher
than the others and need not be made of nickel. The
height shall be such that the thermometer bulb is
completely immersed in the oil. Not more than 4
pans, including the one with the thermometer, shall
be run in the oven at one time. The pans shall be
arranged symmetrically with respect to the center of
the shelf of the oven.
method — Approximately 10 g. of pitch shall be
weighed into a dish, placed in the oven, held at 163 °
C. (325° F.) ±2° C. for 7 hrs., removed, allowed to
cool in a desiccator, and the loss of weight noted.
precautions^ — The oven should be set up in a
place free from drafts and should be regulated to
temperature before the dishes are inserted.
note — Where the laboratory has a reasonably
uniform gas pressure, it is advisable to have a burner
of the A. H. T. 22860 type permanently connected
by iron pipe under the oven and provided with a shut-
off cock. The regulation of the burner can then be
left in the same adjustment between tests, thereby
obviating all but minor adjustments during the test.
test dii — SLIDE
apparatus — Water-jacketed oven (of type A. H. T.
Fie. X — Assembly of Drying and Evaporating Oven
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
823
41508, E. & A. 4876), size 10 in. X 12 in. Slide
plate (see Fig. XI). Pitch mould (see Fig. IV).
Cube op p
Fig. XI — Assembly op Slide Test
method — A half-inch cube of pitch such as used for
the melting-point test shall be placed at the top of
one of the depressions in the corrugated plate, warmed
slightly, and pressed down so as to present a rounded
top, care being taken to keep the lower edge intact.
A mark shall be made on the adjoining ridge parallel
to the lower edge of the cube, which shall then be
placed in the oven and held at 40 ° C. for 7 hrs.
The temperature shall be measured by a thermometer
whose bulb is 1 in. above the center of the upper
surface of the slide plate, and whose scale is such
that the effective range may be observed outside of
the oven. After the 7-hr. period has elapsed, the
plate shall be removed from the "oven and a second
mark made from the ridge parallel to the furthest
point the pitch has reached. The linear distance be-
tween the two marks shall be reported as the slide.
note — Very soft pitches which may run beyond
the end of the slide must be observed from time to
time and the time interval at which they reach the
end of the slide noted.
The Barrett Company
17 Battery Place, New York City
A CONVENIENT ELECTRIC HEATER FOR USE IN THE
ANALYTICAL DISTILLATION OF GASOLINE1
By E. W". Dean
Received May 14, 1918
INTRODUCTION
A recent technical paper2 of the Bureau of Mines
recommends and describes a method for the analytical
distillation of gasoline. The discussion published
deals only with such details as are essential to the
accuracy and uniformity of the method and for the
sake of simplicity omits matters which concern only
ease and convenience in manipulation.
1 Published by permission of the Director of the U. S. B
' E. W. Dean, '•Motor Gasoline, Properties, Laboratory M
Testing, iind Practical Specifications," Bureau of Mines, Technical Paper
No 166 (1917), 27 pp. Sec also Am. Soc. Test Mat. YtM Hook 1915,
pp. 568-569; Part I, Committee Reports, 16 (1916), S 1 8-521 .
One of the important requirements of the method
is that the distillation be conducted at a fixed and
uniform rate. To fulfil this requirement it is neces-
sary to employ a source of heat that can be accurately
regulated and that is not subject to uncontrollable
fluctuation. The procedure commonly employed in
petroleum-testing laboratories involves the use of a
gas burner equipped with gas and air regulating de-
vices and protected from air currents by an enclosing
screen or shield. In the laboratories of the Bureau
there has been employed instead a special electric
heater which has proven so advantageous that a de-
scription is now being offered for general informa-
tion.
DISADVANTAGES OF GAS AND ALCOHOL BURNERS
Testing laboratories generally use a source of heat
for gasoline distillation, either gas or alcohol burn-
ers. The former are generally preferred, although
there is now on the market at least one type of special
large alcohol lamp1 that the Bureau knows to be
satisfactory.
The chief disadvan-
tage of all flame heaters
is the difficulty in keep-
ing them under proper
control. Both accurate
regulation and freedom
from fluctuation are dif-
ficult to attain. More-
over, ordinary gas
burners are not de-
signed for the partic-
ular requirements of
gasoline distillation and ^
though more satis-
factory types2 are un-
doubtedly used by
many laboratories they
are at best less satis-
factory than electric
heaters. In addition
to difficulties in regu-
lating and shielding,
there are considerable
losses of heat to the
surrounding air and to Flt, x
parts of the apparatus Special sas burner designed and em-
... , ., , , ployed for gasoline distillation by the
that Should not be Atlantic Refining Company Burner is
, 4. ,j -..Av.^^rtii,, Tt,:« composed of a special bronze casting
heated externally. I hlS equipped with sensitive needle valve and
psranp of hpnt mnv a screw adjustment for the regulation of
escape OI neat. m.iy tneair.gasnliTture. The various features
Drove a Source of dis- appear as follows: a-gaa Inlet; 6-gas
r regulating valve; c = air inlet: a = screw
comfort to the Operator adjustment controlling air supply; e =
,.,.,, . gauze cap to prevent flame "striking
and IS liable tO intrO- back"; /= mica chimney for protection of
, ...... flame against drafts
duce minor possibilities
of variation in the results of an analysis. Finally
the use of flame heaters for the distillation of volatile
liable liquids introduces an clement of danger
M Ml 1 , % the C. J. Tagliahue Manufacturing Co., Brooklyn, N. Y.
i burner with which the Bureau is familiar
is a type In PhikuJ Iphia laboratory of the Atlantic Refining Company,
Indneaa of Chief Chemial P.C, Roblnaon, of this company,
present state of devclop-
lo I'*ig. I of this paper
824
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
which, though slight when the operator is skilful and
careful, is nevertheless a marked disadvantage.
ADVANTAGES AND DISADVANTAGES OF ELECTRIC HEATERS
The chief advantages of electric heaters have been
indicated indirectly through mention of the disadvan-
tages of flame heaters. The two vital elements of
superiority are better regulation and freedom from
uncontrollable fluctuation. In addition a well-de-
signed electric heater delivers heat almost exclusively
to the liquid that is being distilled, thereby increas-
ing the comfort of the operator and avoiding possi-
bilities of error due to transfer of heat to the ther-
mometer bulb through any other medium than the
condensing gasoline vapor. Finally, the danger of
breakage of flasks, and of fire, either in case of break-
age or through ignition of uncondensed gasoline vapor,
is reduced to a minimum.
The chief disadvantages of electric heaters are rela-
tively high cost and difficulty in obtaining equipment
of satisfactory type. Heaters such as are used by
the Bureau are not at present obtainable in the market,
but it is believed that manufacturers will supply them
if a demand exists. They can be made readily by
the user by following the description given in the
present paper though this involves some little mechan-
ical work and possible difficulty in procuring nickel-
chromium wire, which is at present sold u nder a licensing
system. The cost of electric heaters is moreover
bound to be several times that of gas or alcohol burn-
ers and there is also an up-keep cost to be taken into
account as the resistance elements are subject to
gradual deterioration. The convenience and effi1-
ciency of electric heaters is, however, believed to
more than compensate for these disadvantages.
GENERAL PRINCIPLES INVOLVED IN THE BUREAU OF
MINES HEATER
The type of heater designed by the Bureau of Mines
involves no elements of novelty and is simply the re-
sult of applying well-recognized principles of electric
furnace construction to the requirements of the pres-
ent type of work. The fact that only a small portion
of the surface of the distilling flask can be heated (a
circle 1V4 in. in diameter), renders it necessary to
use a heater which is actually a small furnace. Owing
to the fact that heat is transmitted through an air
space instead of by actual contact with the glass the
resistance element operates at a relatively high tem-
perature. It has not been found, however, that the
limits of durability of either the wire or the insulating
materials have been exceeded.
The gasoline distillation heater is actually a small
electric furnace with a heating element in the form of
an inverted cone. The resistance material is ordinary
nickel-chromium alloy wire. Electrical insulation is
effected by a supporting cone of alundum. Thermal
insulation is obtained by jacketing the heating ele-
ment with kieselguhr composition, enclosed in a tight
metal box with a cover of hard asbestos board.1
1 Transit* sold by the H. W. Tohns-Manville Co.
CONSTRUCTION OF HEATERS
The heaters used by the Bureau have been con-
structed in its own laboratories and it is realized that
they probably lack much of mechanical perfection.
They have, however, been perfectly satisfactory in
use and as the interest of the Bureau has been in
service rendered rather than in details and methods
of construction, no experiments along the line of
mechanical improvement have been attempted since
the first heaters of the present type were put in use.
The following description is offered simply as a record
of experience and not with the idea that it represents
either the only or the best way of accomplishing the
desired purpose.
HEATING ELEMENT
materials — H eaters have been made with
two common grades of nickel-chromium resistance
wire,1 each of which has been found satisfactory. It
has not yet been determined whether the longer life
or higher grades of the same type of material (such as
Chromel A or Nichrome II) would be sufficient to
warrant the greater cost. Alundum cement2 has
proven entirely satisfactory as electrical insulating
material.
shape and size of the heating element — The
first heating elements made proved satisfactory in
the matter of shape and size and no experiments were
made to ascertain if some other design might be bet-
ter. The conical form was adopted principally be-
cause it suited the method of hand manufacture.
Dimensions of the cone appear in the following para-
graph.
method of construction — Heating elements are
built on a conical wooden core (see Fig. II), consisting
of two parts, the
cone proper and
a removable base,
which when in posi-
tion acts as a sup-
porting flange for
the alundum cement.
The cone is 2Z % in.
high and i'/« m- in
diameter at the base.
The flange projects
about */«. of an inch.
A number of small
holes are drilled
in the cone, the
pIG 11 arrangement being
Showing the conical wooden form used such that they fall
aking heating elements. The helix of . , ,.
in place by on a spiral line
the wood. , ■ . . e
making six turns of
even pitch. Wire brads are set in these holes to hold
the resistance wire in position while the alundum
cement is being applied.
The resistance wire is wound on a mandrel of about
'. s in. diameter, and the helix thus obtained stretched
1 Nichrome. sold by the Driver-Harris Co., Harrison. N. J.. Chromel C.
sold by the Hoskins Co., Detroit. Mich.
' Manufactured by the Norton Co.. Worcester. Mass
Scale in inches
in maki
resistance wire
brads inserted
Oct.. 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
825
to a length of about 26 in. It is then placed on the
cone, where it is held in position by the brads. The
ends of the wire are made fast by twisting them se-
curely around brads at the apex and the base of the
cone. The arrangement is shown in Fig. II.
Experience has indicated that heating elements may
be satisfactorily constructed, using sizes and quanti-
ties of wire indicated by the following tabulation:
Voltage B. and S. gauge Feet of
of Current of wire to be u
110 24 20
220 27 +0
Resistance
rire in Ohms Amperes
ed (approximate) carried
30 3.6
120 1.8
The full-load capacity of heaters for either voltage
is about 400 watts. It is of course understood that
these figures are only roughly approximate and that
they make no attempt to take account of the minor
variations introduced by the use of wire of slightly
different composition and by decrease in wattage at
higher temperatures.
After attaching the wire to the well-greased mold
a thick paste, made by mixing alundum cement with
water, is applied. The layer should be about 3/8
Mn. thick and the cement should be well worked in
between the turns of the helix. It is not, however,
necessary to get it between the individual turns of
wire as these are sufficiently insulated by the coating
of oxide that forms on the wire. The alun'dum is
allowed to dry and harden for at least a day at ordinary
atmospheric conditions. Rapid drying occasionally
results in the development of cracks, which may also
be caused by the use of alundum paste containing
too much water. After this drying the heating ele-
ment is removed from the wooden core. This is ac-
complished by pulling out the wire brads, removing
the base of the mold, and then screwing it on again
after inserting a gasket which bears on the alundum
mass. At this stage the latter is deficient in mechan-
ical strength and must be handled with care. It is
' next smoothed up with a thin paste of cement and
dried for several hours at a temperature of ioo° to
1500 C. Finally it is fired in a muffle furnace at a
temperature of 7000 to ooo° C, or, lacking the use
of a satisfactory furnace, it may be cautiously brought
to a red heat by connecting it with a properly regulated
electrical current. It is then hard and of a strength
about equivalent to that of ordinary stoneware.
supporting case — The Bureau has used as sup-
porting cases stout brass boxes with tops of hard as-
bestos (Transite) board. The dimensions and gen-
eral construction of the box and assembled heater are
shown in Fig. III.
insulating materials — The insulating material
preferred by the Bureau of Mines is a kieselguhr
composition sold in the form of bricks.' The bricks
are shaped roughly to the desired inside and outside
form, the interstices being filled with brick dust.
Shredded asbestos, plain kieselguhr, or magnesia
might, if desired, be used instead.
assembling of heater — The heating element is
attached to the Transite top of the box, as shown in
1 Nonpareil bricks, made by the Armstrong Cork Co., Pittsburgh, I'a.
Fig. Ill
Plan and section of the complete heater showing: a = heating
element; 4=wire attaching heating element to the cover of the
insulating case; c = silica or porcelain tube insulating the electrical
lead coming from the apex of the cone; d = screws to which the
supporting wire b is attached; £=binding posts connecting with the
heating element; /= transite top of the supporting case; j? = kiesel-
guhr composition used for heat insulation; h= metal enclosing
box; 1 = opening through which heat is delivered, to the distilling
flask.
Fig. III. The cover is fastened to the metal box
with small "stove nuts" screwed through the asbestos
and the projecting metal flange.
regulating rheostats
In the Bureau the heaters have been used connected
in series with regulating rheostats of the slide wire
type. It has not been found satisfactory to secure
regulation by the procedure of turning the current
intermittently on and off. Satisfactory results have
been obtained by the use of rheostats that permitted
reduction of the heat delivered to about a third of
the full-load maximum. Rheostats having the fol-
lowing minimum ratings have been found satisfac-
tory: For no-volt current, 25 ohms resi t;
3.6 amperes carrying capacity; for 220-volt current,
100 ohms resistance and 1.8 amperes carrying capacity.
826
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10 No.
The rheostats used by the Bureau have cost between
$9 and $10 apiece, but it is possible that cheaper
equipment capable of giving adequate service may
be obtainable in the market. Water rheostats might
be employed, and were at one time in service in the
Bureau. They are, however, of the nature of a make-
shift.
DETAILS OF OPERATION
The type of heater described is designed for the
distillation of gasoline and should not be employed
for high-boiling liquids. The surface from which heat
is delivered is too small for such petroleum products
as kerosene, and for this type of work it would be de-
sirable to construct a heating element with larger
radiating surface.
Heating elements are of course subject to deteriora-
tion in the course of time but the Bureau does not
know what their actual life is. As yet none of the
heaters have burned out while being used with gaso-
line, although as indicated above rapid deterioration
occurred when kerosene was distilled. Probably, also
rapid deterioration will ensue if a heater is left for a
considerable period of time at full current consumption
without any liquid to distil. It is, however, desirable
to warm heaters up before beginning a distillation, as
they come to heat only after 10 or 15 min., and time can
be saved with the first distillation of a series if the
electric current is turned on before the other prelimi-
nary operations of making a distillation are begun.
The current should not be left on between distillations
of a series.
SUMMARY
The general requirements for methods of heating
in the analytical distillation of gasoline have been
discussed briefly. The inherent disadvantages of
flame heaters have been indicated and a convenient
electric heater used in the Petroleum Laboratories
of the Bureau of Mines has been described in detail.
Chemical Section, Petroleum Division
U. S. Bureau of Mines, Pittsburgh
FOURTH NATIONAL EXPOSITION OF CHEMICAL ENGINEERS
The Fourth National Exposition of Chemical Industries, held
in the Grand Central Palace, New York City, September 23-28,
1918, has now become a part of the history of the American
chemical industry during this remarkable period of expansion.
The carrying out of the program as originally planned was made
possible through the recognition by the War Department of the
direct bearing of the Exposition upon the military program,
and the results of Exposition Week have abundantly justified this
sympathetic cooperation.
The increased number of exhibitors of chemical products and
machinery completely filled the vacant spaces caused by the
withdrawal of support by the Railroad Administration of the
railways' program for industrial development through chemical
surveys.
A striking feature of many exhibits was the evident thought
taken to give the lay public a clear understanding of the rela-
tions between various lines of manufacture. The recompense
for such effort lay in the thoughtful study given to these ex-
hibits by visitors. Several exhibitors displayed attractive
booths, though engaged now solely upon war problems, with no
opportunity for sales through the usual channels of commerce.
The symposiums on important phases of the industry brought
together a mass of well-digested material which constitutes a
distinct addition to chemical literature. Once again the daily
press has effectively supported the Exposition. Through the
reports of the proceedings, as well as through the large at-
tendance, the function of the Exposition in moulding a
sympathetic public opinion has been realized.
At a joint meeting of the Managers and the Advisory Com-
mittee it was decided to hold the Fifth Exposition at Chicago,
in the Coliseum and its Annex, during September 19:9
— [Editor.]
OPENING ADDRESSES
September 23, 1918
PERMANENT CHEMICAL INDEPENDENCE
By Charles H. Herty
Chairman Advisory Committee of the Chemical Exposition
This annual assemblage of the products of American chem-
ical industry and of the mechanical appliances by which these
products are manufactured provides fitting occasion for a stock-
taking of past accomplishments and a care-taking for the perma-
nency of those additions to our national wealth whereby economic
independence may be assured. To secure this independence
it is essential that there should be close cooperation between
the chemist and the American people, which can only be brought
about when the chemist takes the people into his full confidence
regarding the problems whose successful solution is a matter
of joint responsibility. By the presentation of these exhibits
and by open discussion of the problems confronting the industry,
a sympathetic understanding is produced which creates a sound,
intelligent public opinion, which is the greatest asset any industry'
can possess.
The number of exhibitors continues to grow, in keeping with
the continued expansion of the industry throughout the nation
The only disappointment is tin- setting aside by the Railroad
Administration of the large plans which had been inaugurated
by the industrial departments of the several railroads for pre-
senting here a marvelous display of those natural resources
of this country which still await the touch of the chemist to
rise to their true dignity as invaluable assets. It has been
deemed necessary to eliminate during war times this most prom-
ising and well-inaugurated line of development. This back-
ward step is a matter of keen regret, taken, strange to say,
just at a time when, for economic efficiency, increase rather
than curtailment of such development was to be expected,
and when the call for the chemist was insistent from all other
centers of industrial life. It is sincerely to be hoped that maturer
consideration will result in a reversal of this gravely erroneous
policy.
MEASURES OF EXPANSION
In taking stock of the chemical industry first thought turns
naturally to tin matter of available capital. The amount of capi-
tal accessions has continued to grow. During the first eight
months of 191S, $59,164,000 was added, making the aggregate
authorized capital invested in the industry since August 1,
1914, the date of the outbreak of the war, S3S6, 967,000.
These figures do not include, of course, the investments made
In- tin- National Government in the great chemical plants whose
output is used solely for war purposes. The total production
of these plants si ts our Government apart as the largest manu-
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
>27
facturer of chemicals in the world. In the after-war period
when the story may be told of the rapidity of construction and
of the enormous output of these plants it will add a brilliant
chapter to the romance of chemistry. Meanwhile we can rest
content in the assurance that the great army which we are now
hurrying to Europe will be abundantly supplied.
Perhaps the picture of the growth of the industry can best
be gathered from a few figures concerning our export trade,
for export statistics indicate production in excess of domestic
needs, great as these demands have been during the past year.
Four items have been selected, three because of their fundamental
character, and one on account of the rapidity of its develop-'
ment.
Exports 1913/1914 1917/1918
Sulfuricacid 12.000.000 lbs. 68.000.000 lbs.
Caustic soda and soda ash Negligible 334 . 000 , 000 lbs.
Benzol Negligible 25,000,000 lbs.
Dyes, dyestuffs and dyewoods $357 , 000 $17, 000 . 000
Doubtless in future years these figures will appear diminu-
tive, but at the present they constitute an inspiring hope for
that future.
A fair measure of the increasing participation of the Govern-
ment in chemical activity is shown in the supplemental ap-
propriation estimates submitted by the War Department to
Congress on September 17, 1918. Aside from the great appro-
priations for explosives, there has been requested for the Chem-
ical Warfare Service, the recently organized division having to
do solely with offensive and defensive gas warfare, $198,704,000,
a sum greater than was asked for the clothing of the increased
army we are now raising. Germany began poison gas warfare;
within the next twelve months it will have more than its fill
of it.
PUBLIC SUPPORT
The present status of the American chemical industry and its
prospects for the future must prove gratifying to all good citi-
zens of this republic, but these prospects can never be fully
realized unless the work of the chemist is supported by sound and
loyal public opinion, which, in turn, will eventually manifest
itself in the form of a thoroughly sympathetic attitude on the
part of official representatives of that public opinion.
The stress of war preparations and the great part we feel
that we are destined to play in the decision have aroused a whole-
some national pride, which should contribute to the develop-
ment of an atmosphere of good will! America must make good!
America can make good! America shall make good! These
thoughts fill the minds of our people to-day. The craze for
"imported goods" which has so often palsied industrial effort
is now being supplanted by pride in domestic achievement.
Certainly the label "Made in Germany" no longer exerts its
hypnotic influence over the masses of the world. Yet German
propaganda is insidious, is ever present, and must constantly
be combated if we are to gain that measure of national self-
containedness in essential industries which will guard us against
a recurrence of the economic tribulations which characterized
the period immediately following the blockading of German
ports. The chief centers of that disturbance were coal-tar
chemicals (dyes and medicinals) and potash; and I beg to ask
your serious attention to certain conditions attending the ef-
forts to create these industries in this country.
DYES AND GAS WARFARE
No word is needed concerning the marvelous development of
the dye indu itry. It is here to-day for your inspection. Nor
111. .1 1 dwi 11 upon tin- close relation of this industry to that of
high explosives. That point has already sunk deep into our
national consciousness. It was appreciation of this relation
perhaps even more than economic need, which brought together
producers and consumers in a unique display of unanimity which
procured from Congress a protective tariff and anti-dumping
legislation guaranteeing life for the young industry.
There was an additional argument for such legislation, how-
ever, undreamed of by any of us at that time. We had not
entered the war and gave no thought to the efforts which
might be required of us in the matter of poison gas production.
But when our authorities, following our entrance into the war,
determined to meet the Germans with their own weapons and
on a scale far greater then they had ever contemplated, it be-
came necessary to make use of every available means for manu-
facture of toxic material. The great plants planned for Govern-
ment construction and operation were not sufficient for the pro-
gram. I am violating no confidence in telling you that at this
juncture the Government turned to the young dye industry
for plants and trained organizations to augment its poison gas
output, and splendidly has the young industry responded.
For military reasons I am advised not to mention specific plants
or the products manufactured therein, but with official sanction
I may say that five dyestuff plants are now participating in the
production of this material, while many others are contributing
indirectly to the same end. The plants were suited to the
needs, staffs and workmen were familiar with this kind of work,
and the conversion to the new role was thus enabled quickly
to be made.
In view of the adaptability of the dyestuff industry to such
serious national needs, it is difficult to be patient with many
of our mercantile establishments which still insist upon placard-
ing their counters with signs such as "The color of these goods
cannot be guaranteed." What a sweet morsel of comfort these
placards are to the enemy, in effect an effort to preserve the
market for him by our own people, if such they are! Was
it ever the practice to guarantee all colors? Certainly not, for
even before the war nine-tenths of the dyes used were not fast
and did not need to be. Moreover, are our merchants not yet
aware of the conditions which led for a time to the uncertainties
as to color fastness? Do they not know that in the period of
acute shortage of German dyes, before the American industry
was started, many German dyes were used for purposes never
intended, and so gave bad results, in most cases falsely attributed
to American origin, and so when remaining German stocks ap-
proached depletion, and the American products began to ap-
pear on the markets, these were likewise used in ways never in-
tended, with equally as poor results as in the case of the misuse
of the German dyes? With the present adequate domestic
production, these matters are correcting themselves. Public
sentiment can, and I believe will, make an end of the disloyal
placards.
NEEDED LEGISLATION
Assurance of the future of the coal-tar chemical industry lies
not only with our people as a whole but even more directly with
their representatives in Congress, for it must not be forgotten
that legislation stands to-day, as a result of the enactment of
the 1916 General Revenue Bill, which is directly in favor of
the German industry, at the risk of the very life of the American
industry. Every phase of the domestic industry has been studied
by the Tariff Commission, and, according to a recent statement
of a representative of the Commission, its report to Congress
will be published soon after the passage of the Revenue Bill.
While nothing is known of the character of this report, T am
confident that when the results of this impartial study of the in-
dustry are presented to Congress the same unanimous vote
will characterize the correction of errors of existing legislation
as has just marked the passage by the House of the $8,000,-
000,000 revenue measure. But the time for action is short, if
1 the great military victory in 1919 to which all look
forward with supreme confidence. No opportunity must be
afforded for the practice of industrial infiltration which may
lap the verj Foundations of the coal-tar chemical industry.
In this connection may I suggest the legislative correction of
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
an error for which we chemists are primarily responsible. In
the existing Act intermediates are assessed one-half the duties
of finished dyes, which ratio was adopted by Congress upon our
recommendation. Experience has shown that this differentia-
tion is a mistake. The difficult stage of production is from the
crudes to the intermediates, far more difficult than from the
intermediates to the finished dyes. And it is in the field of inter-
mediates that dyestuffs, high explosives, and medicinals meet
upon common ground. Furthermore, it is evident that when
these industries bear the brunt of foreign attack the enemy
will take advantage of questions of definition to avoid the higher
duties, or will seek to accomplish the same purpose by shipping
the lower-assessed intermediates for assemblage here into fin-
ished dyes by simple processes requiring little outlay. Justifica-
tion of this contention is furnished by the following extract (page
22) from the "Census of Dyes and Coal-Tar Chemicals, 1917"
just issued by the Tariff Commission:
"With these exceptions the American dye industry was
based entirely on imported intermediates. * * * * This
peculiar situation was due primarily to the provisions of the
tariff laws of 1897, 1909, and 1913, which have consistently placed
a higher duty on dyes than on intermediates. In general, the
German industry dominated the field, and the Americans were
unable to compete. It happens, however, that in the making
of certain dyes the last chemical step of transforming the inter-
mediate into the finished dyes is a comparatively simple and
cheap process. As the rate of duty on intermediates was lower
than that on the finished dyes, the margin in some instances
was sufficient to make it profitable to avoid paying the higher
duty on dyes, by importing the intermediates and completing
the manufacture of the dy'es in the United States."
Knowing therefore where the attack will be made, would it
not be the part of wisdom for us to strengthen our forces at this
point by legislation which will place all of these products on
the same dutiable basis?
COAL-TAR MEDICINALS
Coal-tar dyes have received an abnormal amount of atten-
tion from our people and our press. Of equal importance and of
far greater meaning to the comfort and well-being of our people
are the coal-tar medicinals. In spite of unfavorable legisla-
tion our manufacturers have worthily met their responsibilities
in this field. Especially is this noted in the recent statements
of Government officers that the needs of our Army for these
materials have been fully met by our home output. Congress,
I am again confident, will correct the unevenness in legislation
which hangs as a life-threat over this line of production.
Congressional action, however, will not suffice in itself, for,
in the matter of medicinals, we are particularly susceptible to
our prejudices. A well-advertised name frequently means
more to us than a knowledge of quality. In this connection it
has been amazing to note a persistent campaign of newspaper
advertising, seeking to convince our people that only tablets
of aspirin stamped with the magic word "Bayer" (A German
name! In such times as these!) give assurance of genuine
acetylsalicylic acid. These tablets are "made on the banks of
the Hudson," but in the plant of an enemy-owned corporation
now controlled by the Alien Property Custodian. This
particular brand of material, no longer patented, sells
to day in large quantities and at a price greatly above
that of the same substance manufactured by American
firms, whose product has been shown by official tests to
be of equal purity The most remarkable feature of this
advertising campaign is that it is being carried on by American
directors, appointed liv tin- Alien Property Custodian, and with
thi Unerican directorship emphasized in the advertising matter,
thereby beclouding the main issue of enemy ownership. Zeal
in trusteeship is of course commendable, but a campaign of
misrepresentation and of exploitation is reprehensible. Good
faith does not demand the piling up of undue profits for the
benefit of Germany after the war. We do not need such assets
for settlement of war claims, for according to recently published
figures the value of German property already seized in this
country is fifty times that of American property seized in Ger-
many. Away with any such flaunting of false German supe-
riority. The public should rebuke it, and follow the example
of pharmacist de Haven, of West Chester, who was recently re-
ported in the press to have burned his large stock of aspirin
manufactured by the enemy-owned corporation, and then "tele-
• graphed for a fresh supply from a real American firm!"
INDEPENDENCE IN POTASH SUPPLIES
The blockade of German ports produced a great shortage not
only of coal-tar chemicals, but also of potash for fertilizers. In
many respects the two situations were closely analogous, the
acute shortage, the complete dependence, and the consequent
sharp rise in prices. In the case of the coal-tar products the
situation was met by a prompt union of forces on the part of
producers and consumers, the latter being largely New England,
mill men who would not shy at the matter of protection of a
home industry by tariff. The chief consumers of potash, how-
ever, are the cotton planters of our Southern states, and, among
these, advocacy of a protective tariff was unthinkable. Pro-
ducers and consumers therefore failed to get together for the I
common fight against foreign dependence.
The abundance of raw material is just as favorable for a domes-
tic potash industry as was the case in the coal-tar chemical in-
dustry. The brines of Nebraska, now yielding 60 per cent of
our present production; Searles Lake in California, estimated
to contain from 10 to 20 million tons of potash; the giant kelps
of the Pacific Coast, with their remarkable power of selective
potash extraction from sea water; the alunite of Utah; precipi-
tated cement dust, with an estimated possibility of 50,000 tons
of potash per annum ; the dust from blast furnaces, with a possi-
ble yield of 200,000 to 300,000 tons per year; the potash rich
silicates, such as the green sands of New Jersey and the Carters-
ville slates of Georgia — wherever we turn, potash is at hand,
in forms, however, too slowly available for plant food, but
awaiting the skill of the chemist backed by necessary capital. J
In spite of the lack of cooperation during the past three
years some progress has been made. The 1000 tons of KjOA
produced in 1915 was increased to 9,720 tons in 1916 and to
32,000 tons in 1917. Much fundamental investigation has
been carried out, and the promise for the future is hopefuL'j
Success can be predicted if producers and consumers get to- I
gether, and if public opinion is aroused to the fact that failure *
to secure national independence in this matter vitally affects^
the entire nation. The Mining Bill, as modified by Senator
Henderson, and now before the Senate, may prove the solution. ;
It may be that protective duties or direct subsidy will be called
for, or possibly the relief from war taxation of capital invested
in this industry — whatever the cost and whatever the method
adopted, Government assistance is needed and may be secured
if the demand is nation-wide. Independence in potash can be
assured if this country makes up its mind that it will no longer^*
be dependent upon Germany for its supplies, but its mind must
be made up quickly. This is one of the most urgent qi:
in both its economic and its political aspects, before this country
to-day. We cannot afford to neglect it.
THE EXPOSITION IN WAR AND IN PEACE
By F. J. Tomb
President American Electrochemical Society
During the past four years we all must agree that the chemical
industry of America has passed through the most important
period of its history. This has been a war not only between
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
829
efficiently organized armies and nations but between efficiently
organized industries. Our chemical industry to-day is pitted
against the chemical industry of Germany and one has only
to study this great Exposition to be convinced that the American
chemist is going to measure up to his opportunity. At the
beginning of the war our industry was highly organized in special
fields but it lacked symmetrical development. It was un-
balanced. It lacked self-containedness and coordination. It
has taken the war to enable the chemical industry to find itself
and it has likewise taken the war to enable this country to dis-
cover that it has a great chemical industry and to recognize
it as a great national asset; and it must be said that one of the
big forces which have worked toward the progress of chemistry
and toward public recognition of chemistry in America has been
this Exposition. We give all honor to the men whose foresight
and energy made this possible.
In this big forward movement of the past four years the electro-
chemist has played a large part. America has long enjoyed a
supremacy in electrochemistry, but in spite of the strong position
of the industry before the war no one would have dared to predict
the expansion which the war would demand of us. It has called
for chlorine, cyanamid, air nitrates, and phosphorus in vast
quantities. It has required the ferro-alloy industry, the elec-
trode industry, the abrasive industry to quadruple their outputs.
As a single example, consider briefly the contribution of electro-
chemistry and electrometallurgy to the aircraft program. The
airplane motor has a crank case and pistons of aluminum. Its
crank shaft and engine parts subject to the greatest strains are
all composed of chrome alloy steel. All of these parts are
brought to mechanical perfection and made interchangeable by
being finished to a fraction of a thousandth of an inch by means
of the modern grinding wheel made from electric furnace
abrasives. Calcium carbide and its derivative acetylene are
making possible an ample supply of cellulose acetate for air-
plane dope. When the aviator trains his machine gun on an
enemy plane his firing is made effective by tracer bullets of
magnesium or phosphorus. When our bombing planes begin to
carry the war into Germany it will be with bombs perhaps of
ammonium nitrate or picric acid or other high explosives all
depending largely in their manufacture on electrochemical
reagents. Without the pioneer work of Hall, Acheson, Willson,
Bradley and others, the present aircraft program would be im-
possible of achievement.
Then there is gas warfare, the very basis of which is chlorine.
Germany has long been a nation of chemists and when she
planned a war of frightfulness it followed as a matter of course
that she should seek to make it also a war of chemical frightful-
ness. Much as we deplore it, therefore, we have been forced to
throw our best energies to the solution of the problems of gas
warfare. It is interesting to note that chlorine, the product
of the electrolytic cell, is the basis of mustard gas, chlorpicrin,
phosgene,, and almost all of the important war gases. Thus
does electrochemistry enter fundamentally into the modern
military machine.
It is important for us to remember that while we are working
to develop our industry to a point where it will meet the de-
mands of the war, our work is only begun. If this is in a measure
a chemists' war, we must work to see that afterwards w( bavi
peace. After the war will come bigger problems and
bigger responsibilities and no one has a bigger opportunity than
the chemist to make life better and to serve his fellow-man, We
have the problems of the conservation and proper utilization
of our resources, the elimination of wastes, the problem of food-
stuffs, clothing, and sanitation. All these problems and many
others touch the every -day life of the people and arc preeminently
the problems of the chemist. Fortunately the nation is coming
to realize to what an extent it depends in war and in peace
on the work of the chemist. By the establishment of the
Chemical Warfare Service our place in the military organization
has been definitely recognized. We want the same recognition
in the councils of the nation after the war. We want the Govern-
ment to recognize the value of scientific methods in legislation
and administration and we will look to this Exposition in future
years as one of the forces which will visualize to the rest of the
country the role of the American chemist.
THE IMPORTANCE OF PRACTICAL CHEMISTRY
By G. W. Thompson
President American Institute of Chemical Engineers
This National Exposition of Chemical Industries, the fourth
that has been held, is a growing illustration of the advantage to
our industries which chemistry has afforded. The growth of our
industries of all kinds has been greatly assisted by chemists.
Strictly speaking, all industries are chemical industries, but
some industries are more obviously chemical industries than
others. This Exposition has, naturally, more to do with the in-
dustries which are obviously chemical, but the general proposi-
tion that all industries are dependent upon chemical processes
should be emphasized, even if in each case the connection is not
obvious to the unthinking man.
We learn by adversity. This war has taught us that all
industry is more or less chemical in its character. The fact
that the assistance of chemistry has been particularly demanded
during the last four years has been due to the fact that our
most powerful enemy has been perhaps a little wiser than we
have been in the past, and we, seeing the extent to which
chemistry could be of service to a nation, both in war and in
peace, have learned a lesson, although our education in this
respect may not be complete. If chemistry has been of great
assistance to us during this war, how much more will it be of
assistance to us when the war is over and we are again in com-
petition with a great commercial enemy who earlier than us
learned the lesson of which I am speaking. The few remarks
that I have to make to-day are in the direction of trying to im-
press upon our people the necessity of learning this lesson more
completely, learning it from day to day, learning it with respect
to war and with respect to peace.
Every one needs instruction along this line, but I will address
myself particularly first to those who control manufacturing
operations, second, to the universities and colleges where chem-
ists are taught, and, third, to chemists themselves. Those who
control manufacturing operations must learn more fully and com-
pletely the need of chemical knowledge for the perfection of
industry, the need of chemists in their organization. Our uni-
versities and colleges must learn that however valuable pure
chemistry may be as an interesting study and for the purpose
of training the mind, the most important thing that chemistry
does is to be found in its application; that while it is extremely
interesting and upbuilding to think in terms of atoms and mole-
cules, it is equally important to think in terms of large quantities
of the chemical components that enter into reactions. Chem-
ists must learn more fully and completely the need of applying
their knowledge to chemical processes conducted on a large scale.
Permit me to elaborate my appeal for a greater education of
these three groups of individuals. Again, let me speak to those
who are at the head of concerns that control manufacturing
operations. They will, without doubt, agree to the broad
academic statement that I have already made, that all manu-
facturing industries are chemical to a greater or less degree
and that for their successful prosecution the chemist is an essen-
tial factor. Some manufacturers are more progressive than
others in this respect, and they arc the ones who have nude tin
greatest success in recent years. This academic statement, how-
ever, is to be valued by its application. Manufacturers need
chemists and they should do everything in their power to secure
a supply of the best chemists possible. The progress of manu-
»30
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
facturing is dependent upon the development of chemical knowl-
edge, and the manufacturers should give their assistance in every
way in their power to the development of chemical knowledge.
Manufacturers can do a great deal to help the universities and
colleges in developing more efficient methods of instruction.
They can do this by calling university and college professors
into their councils and developing the practical sides of these
professors so that the students in their charge will be developed
along lines which will be useful to industry. The teacher in
chemistry who is not in touch with practical manufacturing
operations cannot properly instruct the student under him and
build him up so as to make him capable, on graduation, of enter-
ing into the industries and applying his knowledge to their fur-
therance. Practical business men often distrust college pro-
fessors. They say that they are theoretical and visionary.
This in many cases is due to the fact that the practical business
man has a narrow vision. Sometimes it may be true that in-
structors in chemistry have not a practical turn of mind. Whether
this view of practical business men is true or not, the remedy is
in their hands, and if they will see their broad duty, they
will throw open their plants more freely to instructors in chem-
istry and make the education of chemists a part of their organ-
ized plan. In other words, our colleges and universities must
be used by our manufacturers and our manufacturing plants
must be opened to use by our universities and colleges.
Now, let me address another word to our educational institu-
tions. They are not entirely free from criticism. It is my
opinion that the educational institutions of this country should
give honorary degrees to men who have accomplished big things
in the industrial world. The practice in many of these institu-
tions is to give degrees only to those who have done original
work in what is called pure science, but which work may be of no
immediate practical use. It is my opinion that the man who
discovers by hard labor things of practical value in the chemical
world is deserving of some recognition from our colleges for his
contribution to practical science. I believe that our universities
and colleges should, all of them, turn more to the practical as-
pects of education. Many of them think only of its cultural
side. Culture is desirable; no one questions this; but culture is
not incompatible with an education that suits a man for the
practical affairs of life. It is absurd to say that a man, to be
successful in the business world, must be a boor, for its corollary
is that the man of culture cannot succeed in the business world.
Culture with an education that will make the student of prac-
tical use is what we want, and the educational institution that
thinks only of culture is about as badly off as the educational
institution that thinks only of the practical affairs of life. Our
educational institutions should keep in touch with manufactur-
ing operations, and instructors in chemistry should keep their
feet upon the earth, even if we cannot expect them at all times
to keep their heads out of the clouds.
Since this war started it has been a wonderful thing to see
how chemists generally have offered themselves to our Govern-
ment in the hope that they would be able to help in solving
the practical problems confronting it. Many instructors of
academic chemistry descended from their exalted positions and
attempted to handle problems which they by experience have
been unfitted to solve. All honor to these men; we do not
criticise them, and have only praise to offer for their self-sacri-
fice. How much better would it have been, however, if these
men had been better acquainted with the practical matters with
which they became intrusted. They came nobly to our country's
assistance. They broke down the barriers with which they were
surrounded, and it is a delicious hope that when peace arrives
they will not allow these barriers again to be erected
To chemists generally 1 address tilts word: You li.ive the powei
of influencing the opinion of those who control industries and the
opinion of those who control the policy of our educational iusti
tutions. I would ask you to insist upon it that the manufac-
turers of our country and our educational institutions get closer
together and that between them there be opened up wide avenues
of intercourse. The result will be that each will be modified.
Our industries will be influenced by our educational institutions,
and our educational institutions will have breathed into them
some of the life of the business world.
We all know that this Exposition is to be a success, but success
in the best sense of the term involves the power of growth.
Success does not consist only in the doing of single definite things,
but in the bigger sense means the doing of a series of definite
things, each member of the series being of a greater value than
that which immediately preceded it. My few remarks are
directed to the desire that chemists and chemical industries, and
expositions of this kind will have such vitality and growing
power that each succeeding achievement will surpass that which
preceded it, in a progressive and developing series.
CONFERENCE ON ACIDS AND CHEMICALS
September 24, 1918
DEVELOPMENT IN NITKIC ACID MANUFACTURE IN THE
UNITED STATES SINCE IO14
By E. J. Pranke. of the American Cyanamid Company
The production of nitric acid in 191 4, according to the Census
of Manufactures, was 78,589 tons of nitric acid of average
strength and 112,124 tons of mixed acid. According to other
data given in the census, these figures represent about 89,000
tons of 100 per cent nitric acid. All of this acid was produced
from nitrate of soda, consuming about 160,000 tons of nitrate.
The pre-war importation of nitrate of soda amounted to about
560,000 tons per annum; hence the normal consumption for
purposes other than the manufacture of nitric acid was about
400,000 tons.
The present rate of importation is about 1,600,000 tons of
nitrate per annum. Since very little is going into storage and
the total consumption for purposes other than nitric acid manu-
facture has increased but slightly, if at all, it may be estimated
that at least 1,000,000 tons of nitrate per annum are being con-
verted into nitric acid at the present time. This is equivalent to
650,000 tons of 100 per cent nitric acid of which nearly five-
sixths is being used for the manufacture of military explosives.
The building of the new nitrate of soda acid plants has offered
an excellent opportunity for the introduction of many improve-
ments. The Dutch ovens under the retorts have been dis-
placed by modern fire boxes provided with a proper arch. This
change has effected a saving in coal consumption of approxi-
mately 25 per cent. The chemical stoneware from the retorts
to the condensers and the glass condenser tubes have been dis-
placed by acid-proof, high-silica iron, such as Duriron and
Tantiron. The volvic-ware saucers in the towers have also been
displaced by acid-proof iron. The chemical ware- from the
condensers to the absorption towers, and the glass lines for
circulation of acid at the sides and top of the towers, however,
are retained. The absorption tower capacity has been increased
about 40 per cent by the addition of more towers. Spiral rings
for tower packing have taken the place of the ordinary form of
packing.
Important changes have also been made in operation. The
average charge of 5,000 lbs. of nitrate per retort has been in-
creased to about 7,500 lbs. The retorts, instead of being
operated in batches, are now operated in rotation. Instead of
3 runs per retort per day the usual practice is now 2 runs per
day. Temperatures are also controlled more carefully than
in the past.
The result of these improvements is an increase in the amount
of nitrogen recovered as acid from an average of about 78-80
per cent to about 92-94 per cent of the nitrogen in the nitrate
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
831
of soda. At the same time the labor requirement has been
somewhat decreased.
A good beginning also has been made in the recovery of nitrose
gases produced in the various nitration operations. In some
of the systems that have been devised as much as one-half
of the fumes are being recovered. The collection of the gases
from the many nitration units, however, is still a serious problem.
While the aggregate amount of acid that is being recovered is
large, it represents only a small fraction of the acid gases that
are being wasted. In the ordinary nitration operation as carried
out at present about one-tenth or one-twelfth of the nitric acid is
wasted in the wash waters, while on an average about one-
eighth is lost as fumes, of which one-half is recovered in plants
that are equipped with recovery systems.
Nitric acid by direct combustion of air by the arc process has
not had any important development as yet in America. Three
small plants, more or less on an experimental scale, have been
built in the United States and operated for short periods. The
production of these plants thus far has been negligible. The
total annual capacity probably does not exceed two or three
thousand tons of nitric acid per annum.
Nitric acid by the oxidation of ammonia has received a con-
siderable and important development since the outbreak of the
war. In 1914 there were no ammonia oxidation plants in this
country. At the present time there are under construction
ammonia oxidation plants with a capacity equal to about
225,000 tons of 100 per cent nitric acid per annum.
The first commercial-sized oxidation plant was established in
July 1916, at the Ammo-Phos Works of the American Cyanamid
Company, at Warners, New Jersey. Six catalyzer units were
installed, each with a presumed capacity of 14 lbs. nitric acid
per hour. Improvements in the design of the catalyzer and in
methods of operation have brought the capacity to over 40
lbs. of nitric acid per hour. The catalyzer used is a single
fine platinum gauze with an area of about 2 sq. ft., electrically
heated. Over a period of 2 years two of these units have supplied
the nitric requirements of the 60,000 ton sulfuric acid chamber
plant at this works. The ammonia is taken directly from
cyanamid autoclaves producing about 30 tons of ammonia gas
per day, used mainly for aqua ammonia manufacture. This
plant has served for several months as a training school for the
instruction of operatives for the Government cyanamid-nitrates
plants. Hence, more extensive records are available than
would normally be the case. As an example of the normal oper-
ation of the catalyzers on ammonia taken directly from the auto-
clave mains, the following figures are quoted verbatim from the
records for the week July 13 to 19, 1918. Each value is the
average of determinations of two chemists working independ-
ently, with the exception of those marked (*) which are de-
terminations of one chemist only.
Catalyzer No
. S
Catalyzer No.
6
Date
Time
Efficiency
Date
Time
Efficiency
July 13
2.35 a.m.
96.2
July 13
5.30 a.m.
90.0
July 13
8.40 a.m.
98.5
July 13
1.10 P.M.
93.0
July 13
5.20 p.m.
93.1
July 13
8.40 P.M.
93.4
July 13
11.50 p.m.
96.0
July 14
2.50 a.m.
93.0
July 14
5.50 A.M.
97.4
July 14
1.00 P.M.
94.2
July 14
5.10 p.m.
94.8
July 14
10.15 p.m.
93.2
July 15
10.35 a.m.
95.0
July 15
8. 15 A.M.
95.6
July 15
5. 15 P.M.
95.8
July 15
2.30 P.M.
90.7
July 16
1.50 A.M.
95.4
July 15
11.30 p.m.
92.6
July 16
11.20 A.M.
95.4
July 16
s 00 a K.
90.0
July 17
1.10 A K.
92.1
July 16
8.25 P.M.
93.0*
July 17
1.00 P.M.
92.3
July 17
9. JO t m
K)
July 18
12.50 a.m.
93.4
July 17
94.0
July 18
10.55 am.
92.6
July 18
7.40 A.M.
92.0
July IK
8.00 p.m.
91.9
July 18
5. 10 p.m.
91.6*
July 19
9.50 a.m.
93.6
July 19
4.15 A.M.
93.0
Averase for week
94.5
1
92.5
The cyanamid-nitrates plant at Muscle Shoals, Alabama, will
use the ell Cl ted, single gauze catalyzer. It will produce
approximately <;o,ixki tons of 1 nitric acid per annum.
The plant is expected to go into operation aboul November 1,
1918. The cyanamid-nitrates plant neat Cincinnati and the
one near Toledo, Ohio, will also use the same process, each
producing at one-half the above rate. They are expected to be
in operation early next spring.
The Government experimental plant at Sheffield, Alabama,
known as Nitrate Plant No. 1, which wi 1 make about 15,000
tons of nitric acid per annum, has adopted a non-electrically
heated multiple screen, consisting of several layers of platinum
gauze, welded together at points, and rolled into the form of a
cylinder. The ammonia-air mixture flows outwards through the
screen at a rate several times as fast as with the electrically
heated single screen. After the oxidation has been started by
external application of heat the temperature is self-sustaining
from the heat of reaction.
In view of the perfect control obtainable with electrical
heating, the cost of the electric energy consumed, amounting
to about one-third of one per cent of the present market value
of the nitric acid, may be regarded as negligible. As to the single
versus the multiple screen the efficiencies cited above as examples
of normal operation of electrically heated single screens are be-
lieved to represent the highest standards yet attained in the
practical operation of ammonia catalyzers.
It is understood that the Semet-Solvay Company has an
ammonia oxidation plant at Syracuse, New York, using the
multiple screen without electrical heating. This plant is pro-
ducing several tons of sodium nitrite per day. Information
regarding efficiencies is not available.
In addition to the plants above mentioned the Navy De-
partment, about two months ago, decided to build a plant at
Indian Head, Maryland, for fixing nitrogen by the modified
Haber process used at Plant No. 1. All the ammonia produced
will be oxidized to nitric acid, yielding about 30,000 tons per
annum.
Considerable work is also being done on the use of catalyzers
to hasten the conversion of the nitrose gases obtained from the
catalyzers into nitric acid. The object is to reduce the amount
of space required for reaction chambers. The experiments
along this line show promise of early success.
The nitric acid producing rate in the spring of 19 19 will be
about 650,000 tons from nitrate of soda and about 225,000
tons by oxidation of ammonia obtained from the air, a total of
875,000 tons of 100 per cent nitric acid. This is about nine
times the pre-war normal consumption. In 1914 the industrial
explosives industry consumed about 50,000 tons per annum,
while all other uses took only about 40,000 tons. The only
notable increase in consuming ability since 191 4, aside from
military explosives, has been in the dye industry. In 1917 it
was estimated that 30,000 tons of dyes were produced in America,
equal to the total 1914 consumption. The production will
probably increase somewhat further, but at most could hardly
consume more than 30,000 or 40,000 tons of concentrated nitric
acid. With a producing rate of 875,000 tons and a consuming
ability in peace times of 125,000 or possibly 150,000 tons, it is
evident that over four-fifths of the nitric acid producing capacity
will have to be shut down as soon as peace conditions are estab-
lished.
The successful development of the ammonia oxidation process
raises the question whether this may not become the principal
source of nitric acid in the future. While a categorical state-
ment cannot be made, some of the major factors may at least
be pointed out. The cost of converting nitrate of soda to con-
centrated nitric acid is just about equal to the cost of converting
autoclave ammonia gas to concentrated nitric acid, interest and
depreciation included in both cases. Ammonia gas, however,
is a cheaper form of nitrogen than is nitrate of soda. It is
cheaper by the amount of sulfuric acid required to fix the
ammonia gas in the form of sulfate of ammonia, for nitrate
id 'ill.it. ..I ammonia in the past have always sold at
about the same price pei 1 nd of nitrogen They will probably
832
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
be sold on a competitive basis after the war, or if there is any
difference, the ammonium form will probably be the cheaper.
The differential between ammonia gas and sulfate of ammonia,
then, will make a difference of about 15 to 20 per cent in the cost
of the nitric acid, in favor of ammonia oxidation. The fact
that the nitrate of soda acid plants are being amortized during the
war and are conveniently located for peace-time industrial uses,
while new ammonia oxidation plants would have to be built at
these same points in order to avoid transporting acid, is rel-
atively not very important, because the interest and deprecia-
tion charge saved by amortization of the nitrate of soda acid
plants is only about 4 per cent of the normal cost of the acid.
The decisive factor will probably be simply the question whether
the difference in cost of acid by the two processes is a sufficient
incentive to overcome the inertia of human nature against
changing existing practices.
POTASH SYMPOSIUM
September 25, 1918
RECOVERY OF POTASH FROM KELP
By C. A. Higoins. of the Hercules Powder Company
The recovery of potash from kelp, and the utilization of kelp
ashes, principally as a fertilizer, is an art that has long been
practiced. Many centuries before the German Syndicate
began to market potash salts from their Stassfurt mines, the
crofters around the rocky shores of Scotland and the northern
coast of France had burned the drift kelp as a fuel, and scattered
the ashes over their land as a fertilizer. The great success which
resulted from the use of this kelp ash on the land caused a rapid
expansion in the business of kelp harvesting, until about the
beginning of the 19th century quite a flourishing industry had
already sprung up.
The opening up of the German potash mines, however, about
the middle of the 19th century, began to flood the market with
potash at a price far below that at which the old kelp burners
could produce it, and although the kelp potash industry still
struggled along in isolated parts of the coast among the Scottish
crofters, and to some extent in Japan, it may be said that the
German production killed the kelp industry, which had up to
that time attained fairly considerable proportions.
The outbreak of the present war, however, drove potash users
to look for new sources of supply, and naturally one of the first
to come to their attention was kelp. Previous to the outbreak
of the war many writers had drawn attention to the huge per-
ennial beds of kelp which grow practically uninterrupted all
along our coastal waters on the Pacific side, from the Mexican
line to Alaska, and around the scattered groups of islands which
lie close to the California shore. These vast fields of kelp
seemed to offer inexhaustible supplies of potash, which according
to the preliminary survey made by the Government, bade fair
to supply far more than the normal requirements of our country'
for the indispensable muriate of potash. All that remained
was to devise economical means for harvesting these vast beds
and drying and reducing the kelp to a suitable condition for
transportation and use as a fertilizer. Within a few months,
therefore, of the cutting off of the German muriate, various
large companies were prospecting the Pacific Coast for suitable
sites on which to erect plants for the harvesting and extraction
of potash from the Pacific kelp.
The earliest attempts at harvesting were very crude and in-
volved a good deal of manual labor. Men in flat-bottom SCOWS
would reap the weed by hand with large sickle knives and Durn
it in a rather primitive way. The ash was afterwards sold to
the big fertilizer companies at a price based upon the potash
content, which generally ranged around 15 per cent K ( > I. .iter.
however, modern methods were installed for the harvesting of
kelp. Large flat-bottom, steam or gasoline propelled scows
were equipped with a 1necl1auic.1l reaping device and baud con-
veyors which cut the kelp and conveyed it in one operation into
the tanks aboard the harvesting vessel, at very much less expense
than that involved in the old method of hand cutting. These
harvesters, when filled, then proceeded to shore under thr-ir own
power and discharged their contents into hoppers at the plant,
which in turn fed series of mechanical dryers, where the kelp
leaves were dried and partly incinerated by passage through
revolving drums heated by oil burners. The dried incinerated
kelp leaves were next ground and sacked, and were then ready
to be shipped to the fertilizer factory. Some attention is paid
in the drying process to insure that a minimum of the potash
and nitrogen content of the kelp is lost by the destructive dis-
tillation effect of the drying equipment. That, briefly, is the
method now in use in plants where potash is considered as the
only valuable constituent of the kelp. Experience has shown,
however, that this process of producing potash and realizing
the values of kelp is very expensive, and will exist possibly just
so long as the war and the present high price of potash last.
A few figures will show the status of the kelp ash industry in
this regard. Using the modern harvesting methods that I have
already briefly touched upon, experience shows that it costs
around Si. 10 to harvest and bring a ton of kelp leaves ashore.
Analyses show that the average potash content of the raw kelp I
as harvested in California coastal waters is about 1.3 per cent
K-O, which means that it costs about S85.00 to bring in the green
kelp equivalent to 2000 lbs. 100 per cent KsO. To this, of
course, must be added the cost of drying these kelp leave;, which
contain about 90 per cent of moisture, and by reason of their
gelatinous and cellular structure present quite a problem in
desiccation. All indications seem to point very clearly to the
fact, therefore, that any industry which looks to the production
of potash from kelp on a permanent peace-time basis must
reduce its costs very considerably, or produce valuable by-
products in the same process which in turn will effect a reduction
in the cost of the potash.
Along these lines certain investigators have suggested, as
far back as a century ago, that the peculiar algin bodies present
in kelp might be profitably recovered and used in certain opera-
tions in place of gelatin, for the sizing of paper and textiles,
the proofing of cloth, and in the production of rubber substitutes
and admixtures. Another interesting suggestion is that of Prof. ,
T. C. Frye, who made a conserve by first leaching out the potash 9
and soluble salts and afterwards soaking the kelp in cane sugar
solution flavored with lemon. In Japan a kind of sour pickle ■
with vinegar is made from the fleshy parts of the kelp. The
kelp fiber when compressed and dried also forms a hard sub-
stance resembling ebonite or vulcanized fiber, and at least
one concern is working along these lines at the present time.
The production of by-product iodine from kelp, however, has
long been a practical proposition, although hampered somewhat
by the competition of by-product iodine from the Chilean
nitrate fields
The biggest practical advance in the economical production
of potash from kelp was made in the year 19 15, when the Hercules
Powder Company started the construction of large gasoline-
propelled marine kelp harvesters and a factory near San Diego,
California. This equipment was designed primarily for the
production of acetone, potash, and iodine from kelp Kelp
as a source of acetone was something entirely new to the chemical
industry, and chemists all over the world have watched the
growth and development of the undertaking with great interest.
The plant since its inception has rapidly increased the number
and range of its products and has placed upon the market some
new materials which are full of industrial promise.
Reduced to its simplest terms, the basic principle of this
process of kelp reduction lies in the destruction of the cellular
tissue of the kelp leaf by fermentation, bringing the potash
into solution, and producing acetic acid as the product of the
Oct., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
833
Acbtatb OP Limb
Muriats op Potash
_r\
r
Calcium Acbtatb
Calcium Proprionatb
Calcium Butyratb
Calcium Valerate, Etc.
y\.
Potassium Iodidr
Acbtatb op Limb
Muriats op Potash
Muriate
of
Potash
Acetone
Oil3
Ethyl
Esters
Organic
Adda
Algin
Common
Salt
fermentation of the kelp leaf. The acetic acid is neutralized
with limestone, giving calcium acetate, potash, and iodides
in the solution.
The products chart (Fig. 1) will give a general idea of the
operations at this plant and will serve as an introduction to the
more detailed descriptions of processes which follow. With this
I think we can outline quite clearly the principal steps involved
and the products produced in the fermentation of kelp. The
kelp is harvested, brought to the plant, and pumped from the
tank barges into the fermentation vats, where it is allowed to
ferment until the kelp leaf goes into solution and a liquor is
obtained which on evaporation and concentration yields, at
various stages, three intermediate salts.
The first intermediate product, consisting of a mixture of
acetate of lime and muriate of potash, is heated in regular
acetone retorts. This produces acetone from the acetate,
leaving as residue muriate of potash and calcium carbonate,
from which the high-grade muriate is separated by leaching
and subsequent crystallization. The fractionation of the crude
acetone yields a certain amount of light and heavy acetone
oils, in addition to the C. P. acetone.
Intermediate product No. 2, consisting of the calcium salts
of the higher fatty acids, is mixed with alcohol and sulfuric
acid and the corresponding ethyl esters and produced by the well-
known methods. These esters are easily separated by fractiona-
tion. Ethyl acetate, ethyl propionate, and ethyl butyrate
from this source in commercial quantities are now on the market
and are finding very extensive application as solvents in the
soluble cotton industry, in the manufacture of artificial leather,
etc., etc.
Intermediate product No. 3, consisting principally of potas-
sium iodide, is treated with chlorine and the precipitated iodine
dried and resublimed.
The last of the final products is algin. This substance is at
the present time being produced from at the residual unfermented
leaves which are screened from the fermentation vats. These
leaves are treated with sodium carbonate which extracts the
algin in the form of a soluble sodium salt which is afterwards
precipitated and purified. So far but little progress has been
made in the commercial development of the use of this algin
as an article of commerce. The perfection of extraction manu-
facturing methods, however, and the increasing cost of gelatin
and vegetable gums lead to the conclusion that this material
may find a very extensive use in the future.
In addition to the foregoing, valuable products promising
experiments are now in progress whereby ammonia, valeric and
caproic acids are being recovered as by-products in the fer-
mentation of kelp. Nitrogen combined as ammonia exists to
the extent of about 0.2 per cent in kelp, and is left in the liquor
after fermentation of the leaf. Isovaleric acid is much needed
at the present time in the treatment of nervous disorders, the
supply of the valerian root from which the medicinal valerates
were formerly made having been almost entirely cut off.
Sufficient has been said I think to indicate that the kelp
industry from being conceived solely as a source of fertilizer
potash will eventually develop along the lines of fine chemicals
with high-grade muriate somewhat in the position of a by-
product. It is doubtful whether the total potash production
of all the kelp-harvesting concerns at the present time amounts
to more than about 25 tons a day on the basis of 80 per cent
muriate of potash. Of this, more than half is of a high grade
of purity, about 95 per cent KC1, and is produced not by the
original method involving the incineration of the kelp, but by the
fermentation process already referred to.1
CONCLUSION
It may be a little early to speak definitely of the future
of the kelp industry and its bearing on potash. Certain it is
that with kelp reduction factories extending all along the Pacific
Coast our domestic demands for potash cannot be met thereby.
Certain it is too that kelp, solely as a source of potash, will never
compete with unrestricted supplies from Europe or even with the
potash recovered in modern cement or blast furnace practice.
The utilization of kelp in such a way, however, as to realize
on all the other possible values of kelp, some of which we have
touched upon within the brief limits of this paper, may help
to render the users of high-grade potash for chemical purposes
outside of the fertilizer trade independent of foreign supplies.
' At this point there were exhibited about 300 ft. of cinema film and
some 30 lantern slides showing kelp harvesting machines at work and the
operation and equipment of the factory.
834
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 10
RECOVERY OF POTASH FROM IRON BLAST FURNACES AND
CEMENT KILNS BY ELECTRICAL PRECIPITATION •
By Linn Bradley, of the Research Corporation, New York City
The subject of potash recovery is becoming of more universal
interest to the public as well as to the technical man. The
daily press and the magazines frequently refer to what is being
done and to what should be done in this country in order to
offset and decisively defeat the Kaiser and his followers. Re-
cently several news items and editorials have appeared in the
metropolitan press calling our attention to what is being done
in England toward making their country independent of Ger-
many, and it appears that the British Government has furnished
large sums of money to assist in recovering potash from their
iron blast-furnace gases. It is predicted that this source will
enable England to obtain enough potash to equal her entire pre-
war importation from Germany. France is reported to be as
keenly awake to the possibilities along this line and we may see
the time when France will be recovering large quantities of pot-
ash from iron ores which Germany has made such strenuous
efforts to control. However, it is not surprising that interest
in potash should increase, when we consider that this is the one
big economic weapon which Germany has relied upon to regain
her place in the sun after the war. She boasts that all coun-
tries will have to depend on her for potash. She claims that
other countries cannot produce potash to compete with that
supplied by Germany. But in this, as in many other instances,
her reasoning is based on lack of information as to facts and
possibilities.
The recovery of potash in this country is making rapid strides.
The industry may be roughly divided into those plants in which
the recovered potash is the main product and those in which the
potash is recovered as a by-product. In this paper the latter
phase will be considered, as it is believed that while the largest
immediate tonnage may be obtained from desert lakes, kelp,
alunite, and a few other sources, nevertheless a study of the
economic problems will show that the surest way of making our
potash industry a permanent and enduring one, able to supply
all of our requirements, even against German competition, is to
develop and rely upon the by-product potash.
After the installation of the Cottrell process at the plant of
the Riverside Portland Cement Company in California was
placed in operation for the purpose of eliminating the dust
nuisance, it was noticed that the material collected in various
parts of the precipitator differed in fineness. Natural inquis-
itiveness then called for an analysis of these products to deter-
mine if any impurities in the raw mix had become concentrated
in any portion of the dust. The alkalies increased with the
fineness of the material as shown by screen analyses. At that
time considerable light fume was escaping from the precipitator
exits and the suggestion was made and urged that some of this
material be collected and analyzed as it might show even higher
alkali content, since having been interested in agricultural and
fertilizer problems it seemed to some of us that potash might
be found in the escaping fume in percentages such as would
warrant its recovery. Thus the first commercial potash-recov-
ering plant in this country was established. The engineer in
charge of this work was \Y A. Schmidt, of Los Angeles. Since
that time a number of improvements have been developed and
the commercial success of the potash plant at Riverside has been
the cause of several other cement companies installing potash
recovery plants.
Early in 1912 the Research Corporation, of New York, started
to develop the Cottrell process and apply it to various plants
in the eastern portion of the United States. Shortlv after work
had been begun, a paper was read and a demonstration given
at a meeting of the local section of the American' ChBMICAI,
Society near Allentown, Pa. The next day arrangements were
made for a visit to the South Bethlehem plant of tin- Bethlehem
Steel Company. Having in mind the experiences of the River-
' "side cement plant, curiosity was aroused by the appearance of
the gases coming from the tall brick stack connected to the
boilers. An investigation was undertaken by Mr. R. J. Wysor,
and this resulted in extensive investigations thereafter to deter-
mine the possibility of cleaning these gases by the Cottrell pro-
cess and recovering whatever of value could be obtained from
the collected material. Mr. Wysor has published a very able
and valuable article in the Transactions of the American Insti-
tute of Mining Engineers (1917) giving a great deal of data
on ores, fluxes, slags, potash balances, and other items directly
related to the recovery of potash as a by-product of blast fur-
naces. His paper probably served as an inspiration for much
of the work which has been undertaken abroad.
Analyses of iron ores, cokes, limestones, and dolomites show a
wide variation in potash content, and it is therefore advisable
for one interested to make sure that his raw materials are suffi-
ciently rich to warrant a potash recovery plant. Furnaces which
produce a large tonnage of slag per ton of iron on account of the
iron content of the furnace charge will, of course, carry more
potash into the slag than furnaces which produce a relatively
small volume of slag, other things being equal, except for com-
position of the charge. Some iron ores carry as high as 60 per
cent of iron and are practically devoid of potash. Some cokes
have a low ash and are low in potash. Some limestones and
some dolomites may be quite pure. If, therefore, the ores are
uniform and properly prepared and the fuel and flux are prop-
erly proportioned, the slag volume will be small and the potash
in the gases may likewise be negligible. On the other hand, if
the iron ore carries as much as two or even one per cent of pot-
ash (KjO) and the coke ratio is high, and it and the flux contains
as much as 0.25 to o . 50 per cent of potash, quite a large quantity
of potash will be volatilized and carried off by the gases from
which it can be recovered. The high temperature in the blast
furnace and the length of time under treatment allows the
silicates to be decomposed more readily than in a cement kiln
where the temperatures are not so high. The potentialities of
the by-product recovery' from blast furnaces would, therefore,
seem to surpass the possibilities of the Portland cement indus-
try in this regard.
Numerous attempts have heretofore been made to recover
potash from silicate rocks. The investment and operating cost,
especially for fuel, are hard to overcome if one endeavors to
volatilize the potash and recover it and nothing else. It there-
fore seems that the best way to recover the potash from these
silicates by heat treatment is to charge these silicates into exist-
ing furnaces along with the regular charge and recover the pot-
ash as a by-product, thus eliminating the investment and oper-
ating cost for new and separate furnaces. This would be profit-
able up to a certain point, beyond which, however, this prac-
tice would not be desirable.
Since the investigations referred to were begun at South
Bethlehem, numerous other furnaces have been investigated and
potash balances made. Iron ores have been found in abundance
in Alabama which carry from 1 to as high as 3 per cent in pot-
ash and carry enough iron to make them highly suitable for
this purpose. The following tables show the results of one
investigation :
Analyses op Materials
Material Fe SiOi AfcOi CaO MgO Ash Carbon NsuO KiO
Ore No. 1 46.36 17.42 4.19 S. 0.1 8.33 0.62 1.27
Ore No. 2 54.69 12.78 3.49 4.04 6.00 0.39 0.74
Slone 1.56 0.58 46.24 7.25 0.64 0.26
Coke 5.82 3.49 0.510.24 13.0186.15 0.39 0.32
Charged into Blast FtntNACB
Lbs. per Tot.il Per cent
Materials ton iron lbs. KiO of total
Ore No. 1 3115 39.56 61.0
Ore No. 2 1168 8.65 I "> .'
Stone 1440 3.74 5.8
Coke 4050 12.97 20.0
Total 9773 64.92 100. 0
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Summary
Total K2O charged into furnace per ton of iron pro-
duced • 64 . 92 lbs.
Lost in slag per ton of iro.-. produced 1 1 . 60 lbs.
Lost as fume from gas leaks per ton of iron produced
(estimated) 1.16 lbs.
Total potash recoverable from gases per ton of iron
produced 52. 16 lbs.
Total potash in dust in gases as per analyses 34. 1 1 per cent
Water-soluble potash in dust in gases as per analyses 32. 10 per cent
Portion of total potash in dust, which is water-soluble 94. 1 1 per cent
Total water-soluble potash recoverable per ton of iron
by collecting the dust in the flue gases 49.09 lbs.
Total water-soluble potash as above per 500 tons iron
per day 24545.00 lbs.
Total water-soluble potash as above per year of 350
days
Portion of total potash charged into furnace which is
lecoverable from gases in water-soluble condition. .
Safe estimate of above amount recoverable in opera-
ting practice
Safe estimate of above amount recoverable as above
per year of 350 days
4295.37 tons
75.62 per cent
80.00 percent
3436.29 tons
A study of the above figures will show that it is desirable to
keep the potash content of the raw materials up to the highest
point and to keep the slag volume and potash content as low as
possible. It is clear that if the slag volume remained constant,
as well as its analysis, that if only 11.6 lbs. of potash had been
contained in the furnace charge there would have been nothing
available for collection. With suitable slag volume and potash
content and a rich potash charge the recovery of potash in quan-
tities worth while is readily accomplished. Sodium chloride has
been found helpful in liberating the potash in such way that it
is recoverable in the dust in a water-soluble form. While work-
ing at a cupola furnace in which sash weights were made from
old tin cans and other metal waste, it was found that the use
of common salt greatly increased the fume volume and density
and this later was shown to be due to the fact that chlorides of
lead, tin, and zinc were formed and readily volatilized as such.
The use of salt has been extended to cement kiln practice and to
other uses in connection with the recovery of silver, lead, and
zinc from low-grade ores and tailings, the values being recovered
from the gases after volatilization as chlorides.
Consideration of data such as presented in the tables given
herein resulted in an effort being made to find raw materials
suitable for making iron and yet carrying high percentages of
potash. Samples of ores, fluxes, and cokes were obtained from
a number of furnaces and other sources, and later on this work
was carried on much more extensively by the Bureau of Soils
of the Department of Agriculture and by the Bureau of Mines,
Department of Interior. It is probable that Mr. Frederick
Brown, of the Bureau of Soils, has now collected data on nearly
all of the raw materials available for iron making and that if
such data were made public in the near future, it would be of
great assistance in connection with the problems under con-
sideration. Personal efforts to find materials such as described
developed the fact that in the eastern part of Alabama there is
a very large tonnage of iron ores carrying in some cases an aver-
age of 1 per cent of potash and in other instances an average
of about j . 80 per cent of K2O, several analyses showing a con-
tent of over 3 per cent of K20. I am indebted to Dr. J. S.
Grasty for having brought these ores to my attention and for
much of the data on their iron and potash content as given later
in this paper. Mr. M. W. Bush, president of the Shelby Iron
Company, has also contributed data on the iron situation of the
South and the values of these iron ores in furnace operations.
I have examined these properties and have interviewed blast
furnace operators who have used them in their furnaces and
hold the opinion that they constitute an asset of importance to
the nation as well as to interested parties. They should receive
the consideration of the Government in connection with our
war problems and likewise our post-war problems so as to assist
in rendering our country absolutely independent of ('•
The ores carry an average of from 48 to 52 per cent of iron, are
very uniform, easily mined and shipped as they are directly on
the railroad, and operate satisfactorily in the furnace, produi ing
good iron at low cost. Their potash content also acts as a
desulfurizer, thus improving the grade of iron. The phosphorus
content is very low.
The following table has been compiled to show the economic
importance of these ores as a source of potash, the figures having
been based on experience at several other furnaces as well as on
the data obtained in connection with these particular ores and
at various iron furnaces in the South. The table has been sub-
mitted to experienced iron blast-furnace operators for sugges-
tions and criticisms. For comparison, other ores have been
included in the table. The composition of the high-potash iron
ore has been taken from the average of over 1000 tons of such
ore shipped to furnaces on which K20 was determined for each
car of this particular shipment.
SiOi AI1O1
CaO
K.O
Fe
Per cent Per cent
Per cent
Per cent
Per cent
0.3
0.3
1.7
53.0
0.3
0.0
No. 1 Giay 19 2 4.8
1.3
1.8
»9.8
No. 2 Red 15.0 4.0
17.0
0.2
36.0
No. 3 Brown 19.5 3.8
6.0
0.2
.
42.0
4398
6039
5212
46.07
-54.
35
46.87
Coke required for 1 ton iron, pounds.. . .
2700
3900
3000
28.29
35.
I '
26.98
Stone required for 1 ton iron, pounds. . .
2448
1159
2909
Percentage of burden
25.64
10.
+ f
25.15
Total potash constant of burden per ton
99.5
29.
s7
33.97
Deduct for losses in slag and else-
10.4
15.
6
14.0
Total potash collectible from gases,
89.1
13.
W
19.97
Slag volume per ton iron, pounds....
2715
3290
3090
Total potash in gases per day (500 tons
44550
6985
9985
Total potash in gases per 350-day year,
7796
1222
1747
Assume 80 per cent recovery, this equals
6237
978
1406
Value per annum at $500 per ton of
K20 $3
118500
489000
703000
Value per annum at $100 per ton of
EjO
623700
97800
140600
The total production of pig iron in this country is such that
about 200 furnaces of such sizes as referred to above would be
needed to meet our requirements if the furnaces were of the
same capacity and the lower potash ores are used. Also it is
easy to see that we now have sufficient furnace capacity to pro-
duce annually over 1,500,000 tons of potash, far in excess of our
pre-war requirements, provided ores such as No. 1 are employed.
The difficulty lies in the fact that we have not found that all
furnace burdens carry the amount of potash shown under the
No. 1 column. If the furnace charges and operations could be
adapted so that one-fifth of the amount, or 300,000 tons, could be
produced, this would meet our needs without assistance from any
other source. The three constituents of the charge, ore, stone,
and coke, contain more or less potash. By using those raw mate-
rials which carry more than usual amounts of potash, our recov-
eries can be considerably augmented. In cases where ores are
smelted which are excessively limey, feldspar, potash-bearing
slate, or other potash-bearing silicates could be fed into the
furnace and thus increase the potash content of the furnace bur-
den.
Mr. H. E- Brown, a chemical engineer of New York City, has
developed a process fcr making a special cement from the slag
obtained from a blast furnace and at the same time recovering
water-soluble potash from the gases. He charges limestone,
coke, and feldspar into the furnace. Now if iron ores of suitable
kind could be used for a portion of the raw material, it might be
possible to produce potash from the gases, also pig iron, and a
slag which could be readily converted into a marketable cement.
As tin market varies with the supply and price, the furnace
charge could be varied so as to increase the potash and reduce
the iron, or vice versa. The process has been developed to the
extent that both potash and the special cement can be produced,
but investigations looking to a reduction in the operating cost
have Hot been completed.. It appears, however, that with an
assured market for the cement at fair prices, the process can be
operated successfully and show a good return on tin invi stmeot,
836
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
especially when the price for potash is high. In this connection,
it seems that consideration might well be given to the use of
powdered coal introduced through the tuyeres and thus reduce
the coke required, possibly doing away with it altogether. It
would materially reduce operating costs and increase production
and recoveries.
It is natural to look to feldspar and other potash-bearing
silicates for our potash. The cost of mining and grinding feld-
spar is one obstacle to be overcome which is not an obstacle for
instance in the Cambrian slates of Georgia. It has been sug-
gested also that efforts be made to recover potash from the
tailings dumps in the Cripple Creek District of Colorado, these
tailings carrying as high as 7 per cent of K>0. I n vestigations as
to the feasibility of this are now under way. Sufficient progress
has not yet been made, however, to warrant any very optimistic
statements. The fuel cost and the necessity for a long freight
haul to the fertilizer-consuming districts are large items to
overcome.
Serecites and Cambrian potash-bearing slates have been lo-
cated in Georgia which carry potash in considerable quantity,
several deposits analyzing as high as 8 or 9 per cent. Laboratory
investigations have shown that the potash in these raw mate-
rials was more readily rendered water-soluble or volatilized by
treatment with salt in a rotary kiln than the potash from feld-
spar. Furthermore, the amount of lime required to be added to
the charge before the potash is liberated appears to be much
less than required for feldspar. The cost of production is much
less than in the case of feldspar and the cost of grinding is very
much less and altogether these slates are much better adapted
for the purpose here discussed than feldspar is. Dr. T. P. May-
nard, of Atlanta, Georgia, who conducted these researches and
developed the properties, reports that there is an enormous ton-
nage available. It is also reported that a company has been
treating this material in a rotary kiln, adding 200 to 300 lbs. of
salt per ton of raw material, volatilizing a good portion of the
potash, and converting a large percentage of the balance into a
water-soluble compound in the powdered calcines. One part
limestone is used with two parts of ground slate. Freight rates
should be very low since this material is located very close to a
large market, namely, the cotton fields of Georgia and Alabama.
Engineers state that cotton grows prolifically on these lands
without any additional fertilizer, indicating the ease with which
the potash is made available.
In all of the cases mentioned above, potash is volatilized and
must be recovered from the gases. The Cottrell process has met
with excellent success in this phase of potash recovery problems.
The field of application which has been developed the farthest
is in the recovery of potash from cement kiln gases. Several
plants are now in successful operation and at the present time a
considerable tonnage is being obtained in this manner. Other
plants are under construction and the outlook for a much larger
tonnage is very favorable. In The American Fertilizer for Au-
gust 31, 1918, John J Porter, General Manager, Security Ce-
ment and Lime Company, of Hagerstown, Maryland, in an
article entitled "The Recovery of Potash as a By-Product in
the Manufacture of Portland Cement," gives a great deal of
valuable information concerning this problem. The following
is quoted from that article:
Estimating Potash Recovery — For the benefit of those who may
wish to figure on their own conditions, I give the following
method of calculating the probable recovery of potash.
Let A = per cent potash in raw mix
Let B = per cent potash in clinker
600A — 380B
Let C = per cent liberation
600A
I.i I 1' = lbs. of potash recombined per bbl clinker (= 0.7 to
.5 depending on fuel consumption and per cent ash in coal)'
Let P = percent potash precipitated in 11 ■
Assume 600 lbs. of raw mix actually used to make one bbl. of
clinker,
Then, r
Lbs. of potash entering kilns per bbl. of clinker = 600A
Lbs. of potash volatilized in kilns per bbl. clinker = 600
AC
Lbs. of water-soluble potash entering treaters per bbl. clinker
= 600AC-F
Lbs. of water-soluble potash collected in treaters per bbl. clinker
= (600AC-F; = P
*****
The cost of collecting potash at Security is now running about
as follows:
Per Unit
of Potash
Collection, including labor, power, repairs and laboratory fO !4
Packing and shipping 0.08
Total operating cost, exclusive of depreciation, royalty, and salt
addition $0 22
The cost of the salt addition is about $0.25 per unit of potash but this
is not a necessary element of cost and can be omitted whenever price condi-
tions become such as to give an unsatisfactory margin of profits.
The article then goes on to show that from a 3000-bbl. cement
plant, the operating profit per annum on the potash alone comes
to about $458,000, the raw mix having 0.75 per cent of potash.
The article is quite complete and those interested are referred
to it for further details. The Bureau of Soils published the
results of their survey of cement plants. The data given indi-
cate that this industry can be counted on to furnish 80,000 to
100,000 tons of potash annually. By using materials which are
higher in potash content, such as feldspar, serecite. or slate in
part, the yield of potash can be materially increased. The addi-
tional cost for raw material should be weighed against the greater
financial return from the plant operation as a whole and not
allow first cost per ton of material to govern. The utilization
of existing cement kilns and equipment for the manufacture of
cement as a by-product, placing special emphasis on the potash
yield and profits therefrom, should be urged by all citizens, and
this should be more emphatically urged for the recovery of pot-
ash from blast-furnace gases. The feat of obtaining all of our
potash from existing industries by recovering the by-products
will be typically American and worthy of our "Yankee inge-
nuity." The by-product method will enable us to compete with
potash from any other source, and the Kaiser's vain boast that
all countries will be compelled to submit to his will because
they must have his potash, shall receive its proper answer. It
is not difficult to recall that the by-products of our packing
house industries constitutes the source of a large tonnage of our
fertilizers, whereas a few years ago these materials were annoy-
ing left-overs, difficult to dispose of.
Referring again to the iron industry and its relation to the
potash question, it should be pointed out that in the Alabama
district there is an abundance of excellent coal, labor is plentiful
and cheap, and the climatic conditions are such that the district
may be considered an all-year one as far as operating is concerned.
Then when it is realized that there is immediately at hand an
enormous tonnage of high-grade iron ore which carries such a
large potash content and that the South produces our cotton and
therefore is the large consumer of potash and thus provides a
large market within a few miles, the economic importance of
this situation can be better appreciated. Other iron ores con-
tain potash, some of which may justify recovery plants, and we
should be on the lookout for such material, keeping in mind that
our goal is to obtain our potash as a by-product at such a cost
as will enable us to ignore Germany forever and thus make the
dreams of the American chemist and engineer come true.
Tin South produces pig iron cheaper than any other district
in normal times. In fact their furnaces must do this in order
to stay in the market. The South does not yet consume as
much iron and steel products as its population justifies and
therefore their iron must carry a high freight charge if it is
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
837
shipped North to the larger markets. The manufacture of cast
iron pipe has, however, grown to a large industry. In the future
more and more iron and steel will be consumed locally as it is
evident that the South is coming into its own very rapidly.
The additional profit which can be obtained from the potash
will be of great assistance in keeping their iron furnaces in blast
when the market sags. The South has a very fortunate combina-
tion of labor, raw materials, climate, and a large and near fer-
tilizer market.
In France and in Great Britain the national governments have
taken an active interest in the possibilities along the lines herein
pointed out. It has been reported that investigations, extend-
ing over a period of three years, have shown that Great Britain
can produce enough potash to satisfy all her requirements.
The British Potash Company, Limited, has recently been organ-
ized for this purpose and the British Government has undertaken
to provide at least half of the total capital required. The funds
necessary for the enormous scale operations contemplated will
be more than an individual would be anxious to supply in these
times. Another reason is that the British Government is fully
awake to the importance of the potash to their national interests.
It does not seem that our own Government should falter or lag
in this field, but on the contrary should immediately make com-
prehensive plans and take energetic action of such a character
as will insure the proper solution of the problems under discus-
sion. At the present time individuals shy at putting their money
into a new enterprise which requires much labor and material
without having adequate assurance that their efforts will meet
with success. In order to do this, the full and continuing sup-
port of the Government must be had. Priorities, labor, ma-
terial, and fuel allocation play an all-important part, and on
top of this the new industry is handicapped by having to face
an enormous taxation before the plant is fully paid for from
earnings, and there is no positive assurance that potash will long
remain above the pre-war level. Surely this situation should
be corrected promptly. It seems ridiculous that the United
States should be playing the role of food granary for ourselves
and our Allies, also raising the cotton which is so necessary in
connection with the war, and yet be doing nothing to provide
the potash either for food purposes or for the cotton, except
the limited and inadequate efforts due to private initiative. It
ought to be emphasized that potash is a subject which should be
understood and appreciated by everyone in the nation, and that
it should be considered primarily from the national point of
view. Does any one of us imagine that there is such ignorance
of potash in Germany as exists among our own citizens? No,
they have learned that potash is the big German raw material
and economic weapon which they counted upon and are still
counting on to help the Kaiser impose his will on you and on
me. This must be defeated!
To all those who are assisting in the solution of the problem,
I would state that we should soon take steps to solve our post-
war problems. The question of the market conditions which
will prevail is ever before us. Germany will do all within her
power after peace is declared to break down that which will
have been built up, the same as she has destroyed the beautiful
cities of France. She will endeavor to regain control of the
potash situation in this country. Even now she prob-
ably has her propaganda all prepared and ready for launching.
One need not be surprised to learn that she has agents in the
various Governmental departments and bureaus in Washington
ever ready to interfere with efforts being made by our tech-
nical and business men. Even now we hear rumors to the
effect that potash is not a plant food and is not needed for
cotton, potatoes, and various other crops. Careful investiga-
tion of the southern cotton fields should be convincing evidence
that this may be another piece of German propaganda. It is
difficult to check up these rumors, but all of us should be on
guard against these German efforts. It would be to the national
interest in the broadest way for this country to take steps to
forever exclude every ounce of German potash. Tariff, price
control, and other methods should be earnestly considered.
The farmer must be made to realize that he dare not use German
potash even if he might obtain it a little bit cheaper than the local
product. In other words he must not be a potash slacker. The
politician hates to take any action which would have a harmful
effect on the farmer vote, so we may look for strong opposition
when legislation is urged for protection of the new potash indus-
try. It will be short-sighted of our Congressmen to fail or
neglect to fully protect this industry. It should be remembered
that Germany will continually strive to break down any bar-
riers which may have been erected, and it therefore behooves us
to band ourselves together in an alliance which could fittingly
be called the American Potash Alliance and see to it that our
interests are at all times being taken care of. In unity there is
strength, therefore let all parties interested form such an alli-
ance and immediately organize and institute efforts to have the
proper legislation passed, and also to conduct a publicity and an
educational campaign throughout the country and, generally,
to serve the combined interests of those who assist in rendering
our country free from the Kaiser as far as potash is concerned.
The hearty and active cooperation of the various technical so-
cieties should be readily obtained, and I commend these sugges-
tions for the formation of the American Potash Alliance to their
attention. The author would be pleased to hear from all who
approve this suggestion.
BIBLIOGRAPHY
Articles from Miscellaneous Sources
Gale, "Our Mineral Supplies — Potash," U. S. Geol. Surv.,
Bull. 666-iV".
1 Gale, "Potash in 1916 — Part II," TJ. S. Geol. Surv., Mineral
Resources of the United States, 1916.
Ross, Merz and Wagner, "The Recovery of Potash as a By-
product in the Cement Industry," TJ. S. Dept. Agr., Bull. 572.
Porter, "The Recovery of Potash as By-Product in the Manu-
facture of Portland Cement." Paper presented at Chicago Meet-
ing of the Portland Cement Association, Sept. 10 to 13, 191 7-
Wysor, "Potash as a By-Product from the Blast Furnace,"
Trans. Am. Inst, of Mining Eng., 56, 257. To this article is ap-
pended a bibliography; also see discussion of article on pages
288-302.
Stockbridge, "The Potash Famine," World's Work, May 1918.
"Potash in Maryland Becomes a Reality," Baltimore Morning
Sun, May 18, 1918.
Articles from Metallurgical and Chemical Engineering
Koepping, "Can an American Potash Industry be Established?"
December I, 19 16.
de Beers, "Development of our Potash Industry," December
1, 1916.
"Glimpses of New Pacific Coast Industries in the Making,"
November 1, 1916.
"Potash from Cement Mills." June 1, 1917.
"Potash from Cement at Riverside Portland Cement Com-
pany, July 1, 191 7-
Meade, "Possibilities of Developing an American Potash In-
dustry," July 15, 1917-
Buck, "Bibliography on the Extraction of Potash from Com-
plex Minerals— Feldspar, Lcucite, etc.," January 1, 1918.
Articles from "This Journal"
Haff and Schwartz, "A Practical Revision of the Cobalt
Nitrate Method for the Determination of Potash," August 1917-
Ross and Merz, "Recovery of Water-Soluble I'otash as a By-
Product in the Cemenl hldustry," November 1917.
Anderson and Mestell, "The Volatilization of Potash from
Cement Materials," March 1917.
838
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
Articles from the Manufacturers Record
Catlett, "Possibilities in Potash Production from Fumes of
Cement Kilns,'' February 24, 1916.
v atlett, "The Blast Furnace as a Potash Producer," May 11,
1916.
"Potash-Making Possible in Iron Production," May 11, 1916.
"Recovery of Potash at Security Cement Plant,'' May 11,
1916.
"Widespread Interest in Potash as By-Product in Iron Pro-
duction," May 18, 1916.
"Potash in Iron-Making as Viewed by Government Experts,"
May 25, 1916. Also letter from Catlett in same issue.
"Bethlehem Company Saving Potash as By-Product," June 8,
1916.
Grasty, "Southern Iron Ores as a Source of Potash," Septem-
ber 14, 19:6.
Burchard, "Potash as a By-Product in Cement and Iron In-
dustries," September 14, 1916.
"Potash as a By-Product in Cement- and Iron-Making," March
22, 1917.
Catlett, "Potash from Alabama Gray Ores," March 29, 191 7.
"Potash as a By-Product in Cement," August 26, 1917.
Wilmer, "100,000 Tons of Potash Obtainable from Cement
Dust Every Year," April 25, 1918.
"Large Potash Recovery at Clinehlield Cement Plant,'' May
2, 1918.
Hicks, "Production of Potash in the United States," June 20,
1918.
Catlett, "Potash as a National Asset against Germany's
Damnation Plans," July 4, 1918.
"How We Can Become Wholly Independent of German Pot-
ash," August 15, 1918.
"American Potash for American Farmers," August 22, 1918.
"Potash Potentialities in America which if Utilized Would
Make Us Independent of Germany," Open Letter to President,
August 29, 191 8.
"Potash Question and Its Bearing upon Peace Terms," Let-
ter from Dr. Maynard and Editorial Comment, September 5,
1918.
See also the Manufacturers Record of September 12, 1918, and
that of September 19, 1918, for a number of articles on potash.
POTASH FROM DESERT LAKES AND ALUNITE
By J. W. Hornsev. Consulting Engineer, Summit, N. J.
The arbitrary action taken by the German government some
years ago in forcing Americans who had purchased interests in
German potash works to join the German Potash Syndicate and
the lack of tact displayed by those who handled the situation
for Germany, created so much ill feeling that altogether it
brought about the determination upon the part of the United
States Government and of American buyers to find some
source of potash other than the German, and plans were there-
upon made for both governmental and independent searches.
Fortunately for this country when war was declared in 19 14
these searches had developed a large amount of valuable data.
Both the Geological Survey and the Bureau of Soils were
granted appropriations and began active work which has proven
to be of considerable value The independent investigators made
a somewhat more comprehensive survey without going quite so
exhaustively into details, except where it seemed reasonably cer-
tain that a commercially workable supply would in found.
All probable sources '>f supply were investigated, including
feldspar, kelp, desert lakes, leucite, and alunite. It was evident
from the start that potash could nut be produced profitably at
ante war prices from certain of these materials without the pro
duction and sale of by-products, and for some of these by-prod-
ucts there was only a limited market. In other eases a some-
what more careful study of the subject showed that potash was
unquestionably the by-product.
This work has, however, definitely resulted in the development of
a permanent potash industry in this country, and I say perma-
nent advisedly. Some of the plants will, undoubtedly, be able
to continue after the war.
DESERT LAKES
Investigation of many of the lakes of western deserts showed
such percentages of potash as to make it improbable that potash
could be produced commercially in competition with Germany
at tin- price then prevailing.
seari.es lake — Early in 19 12 a company which had acquired
control of Searles Lake found that their deposit contained a
considerable percentage of potash, apparently in the form of
chloride. This so-called lake consists of a deposit of crystals,
resulting from the evaporation of a prehistoric lake which was
at least 600 ft. deep when it ceased to overflow. In the course
of time, as evaporation under desert conditions continued, the
lower portion of the valley became filled with crystals permeated
with a saturated brine. This body of crystals has been exhaus-
tively investigated by the drilling of wells and its limitations are
now well known. This crystalline body, averaging 75 ft. deep,
has an area of 25 sq. mi. That portion near the edge is covered
with mud, but 121 '; sq. mi. are uncovered, and here the crystal
body is smooth, hard, and solid enough to carry any weight.
It is, however, not dense, but composed of crystals varying in
size from, say l/< in cubes, to the equivalent of 4 in. cubes.
This mass of crystals is formed with openings and interstices
between them, approximating 40 per cent of the contents of the
crystal body.
This interstitial space is filled with a brine saturated with the
salts of which the crystals are formed, comprising the chloride of
potassium and the carbonate, borate, sulfate, and chloride of
sodium. As these voids extend throughout the entire crystal
body they form unobstructed channels through the deposit, and
owing to the well-known principle of the diffusion of salts in
solution, the brirle is virtually uniform in composition through
the entire crystal body Analyses of many samples taken at
widely separated points have given substantially the same re-
sult. The following is a typical analysis given in the form of
the usual hypothetical combination, but which to-day in view of
the large amount of work done on this deposit, can hardly be
called hypothetical:
Per cent
NajB.OT.lOHiO 2.92
N*a:C(>, 4.92
NaCI 15.84
N'.SO. 6.72
K.C1 4.36
Total Solids 34.76
Repeated analyses of brine taken from various parts of the
il< posit by pumping continuously 24 hrs. per day for periods of
30 days show that near the center of the deposit the potash
content calculated as KC1 will gradually increase from about
4 75 per nut to 5.25 per cent. In one case at the end of 30
days it showed 5 40 per cent Near the edge of the deposit
the pcrccntagi gradually lowered from about 4.75 per cent to
4.00 per cent
A composite sample made up of 52 samples of the crystals
taken from widely separated points and from various depths
showed 5 00 per cent of potash calculated as KC1. Obviously
this shows the lirim to be saturated with potash and before its
potash content can be lowered by pumping, the potash in the
crystals will be dissolved.
The average level of the brine is 1 in. below the surface of the
crystals, in consequence of which the surface crystals are al-
ways wet, and in the intensely hot desert atmosphere this is
Followed by a very high rate of the evaporation, which in turn
is compensated for by a constant inflow of water from the sur-
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
839
rounding mountains, entering the crystal body at the bottom and
flowing through the valley beneath an impervious clay layer.
The raw material in this case is the brine, and the mining cost
is that of pumping. The separation of the various salts is
greatly simplified by the differences in their relative solubilities.
Potassium chloride and borax are much more soluble in hot
water than in cold, while the solubilities of the other salts do
not vary greatly with the temperature of the solution.
The question is often raised as to the total tonnage of potash
in Searles Lake. It is not difficult to calculate with a greater
degree of accuracy than would be possible in most mineral de-
posits. The following facts are known :
The deposit covers 25 sq. mi.
The average depth is 75 ft.
The volume occupied by crystals is 60 per cent.
The volume occupied by brine is 40 per cent.
The weight of 1 gal. is 10.738 lbs.
The average analysis of the brine shows a potash content of
4.36 per cent.
It seems perfectly safe and conservative to say that Searles
Lake in the brine alone contains 30,000,000 tons of potassium
chloride, calculated as 100 per cent pure.
The first company to produce potash from Searles Lake brine
was the American Trona Corporation. Their operations have
proven to be profitable and they will undoubtedly be able to
compete with Germany after the war.
great salt lake— This is still a body of water or brine and
has not progressed nearly so far in the process of desiccation as
Searles Lake. It has, however, for some time been looked upon
as a possible source of potash. In fact, the Diamond Match
Company has had a plant in operation there for the past 2 or 3
years, and has recently doubled its output. The Virginia-Caro-
lina Chemical Company, in cooperation with the Inland Crystal
Salt Company of Salt Lake City, have also built a plant. How-
ever, the composition of the waters of the lake is such that a very
large amount of evaporation is necessary before the bitter liquors
are sufficiently saturated with potash to make them workable.
The primary evaporation is effected in open air, clay-lined ponds,
during which considerable quantities of sodium chloride are
thrown out. The bitter liquor remaining is then worked up for
the separation of potash, which is effected by evaporation, heat-
ing, and cooling, and depends upon the varying relative solu-
bilities of the different salts. The principal difficulty encoun-
tered is to bring about a satisfactory separation of magnesium
chloride. The total output from Great Salt Lake is so small
that it is unlikely to become an important factor in the market.
other American lakes — There are a number of lakes in the
western deserts which are possible sources of potash, among
them Owens, Abert, and Summer lakes. But these all require
so large an amount of evaporation and contain contaminating
salts of such a character that up to date nothing has been done
commercially for the production of potash from them.
pintados deposit in chile — About 60 miles from the coast
and directly on the railroad in northern Chile is a deposit which,
while it cannot be correctly called a lake is essentially the same,
and contains several hundred thousands of tons of workable pot-
ash in the form of a crystal body directly on the surface, aver-
aging about 18 in. deep and covering many thousands of acres.
The average analysis will show about 5 per cent of KaO. This
potash upon leaching and crystallization can be recovered as
the muriate, or, if mixed with the raw material from which
sodium nitrate is made and which immediately joins this de-
posit, can be recovered as the nitrate.
While this deposit is not in the United States, it is 1000 miles
nearer to New York by water than California and is located where
labor and other conditions are so favorable as to offset the high
price of fuel. The climate is better than at some points in our
western deserts and the country has a stable government.
Revolutions are unknown and there has been less change in their
constitution and general governmental methods during the past
century than in the United States, England, France, or any other
large country.
ALUNITE
Many centuries ago alunite was mined in Smyrna and for
about 400 years in Italy and was used for the production of pot-
ash alum. When the search for potash began in this country
it was felt that a deposit of alunite might be found and that it
might be used as a source of potash rather than potash alum.
About this time such a deposit was discovered in Southern Utah,
a few miles from Marysvale. Later it seemed that it would
be necessary to discover some means of refining the alumina
before potash could be produced in competition with Germany.
However, early in 1915, when the price of potash had risen to
what seemed impossible figures, Mr. Howard F. Chappell and
his associates, of the Mineral Products Corporation, decided to
build a plant, and this has been in continuous and successful
operation for 3 years, except for two shut-downs of 1 or 2 months
each, caused by fires. They are now producing and shipping
about 600 tons of sulfate per month, and the product is consider-
ably better than 90 per cent pure.
Several formulas are given by various authorities to indicate
the chemical composition of alunite as a double sulfate of potas-
sium and aluminum, of which the following are representative:
KjSOLsCAlaO^O^^HzO; (K,Na),(Al2OH)3,(S04)2; K(AIOH),,
(SO,),,3H20.
The first of the above formulas appears to be more nearly cor-
rect, i. e., for the alunite now being worked at the town of Alu-
nite near Marysvale. Several methods have been proposed for
the treatment of an ore of this character for the production of
potash, but probably the simplest one is that employed in this
plant where the ore is calcined at approximately 1000° C. This
drives off water of crystallization and sulfuric acid, leaving
water-soluble potassium sulfate and alumina. Upon leaching
and evaporation of the resulting solution, potash is recovered as
sulfate with a very small percentage of soda and some infinitely
fine alumina which has passed through the filter cloths.
The alunite from the Mineral Products Corporation's mine is
of a distinctly crystalline nature and from 96 to 97 per cent
pure alunite. There are other large deposits nearby but they
are more nearly amorphous in appearance and carry more silica
which seems to interfere with the calcination and also with the
subsequent refining of the alumina.
The alumina residue, containing any silica present in the ore,
is now discarded; but it is planned later to refine and use it.
It has been discovered that the silica content may be reduced
to less than one-half of one per cent by calcination with pro-
ducer gas instead of pulverized coal and separation of .the alu-
mina from the silica by flotation. The average silica content of
the ore used by Mr. Chappell's company is 3V2 per cent. The
loss on ignition is approximately 40 per cent and the raw ore
contains an average of approximately 10 per cent of K20, or
i8'A per cent of KsS04. The plant is operated profitably, and
by reason of improvements and refinements which have grad-
ually been developed, will, it is believed, be able to compete
with Germany after the war.
POTASH FROM SEARLES LAKE
By AlprBD db Ropp, Jr., of the American Trona Corporation
Searles Lake Basin1 is a broad, roughly circular valley or de-
pression 8 to 10 miles from east to west and 20 to 25 miles from
north to south, bordered by the abruptly rising slope of the sur-
' For the topographical description of the Searles Lake Basin and its
porous salt bed, we are indebted to Dull. 880-L, written by Hoyt S. Gale
iled States Geological Survey. His description of Searles Lake
and the surrounding country is the clearest aod most comprehensive of any
that have come to our notice.
840
I 111: JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. \o. «
Map of Q«
Ftg. 1
, Searles, Panaraitit ;
od Death Valley Basins
rounding ranges. This Basin lies between the Argus Range on
the west and northwest, and the Slate Range on the east, the
latter a narrow, rocky wall, which divides it from the larger and
deeper depression of the Panamint Valley.
The Searles Lake Basin was, during a part of the glacial epoch,
occupied by at least one deep lake, whose traces are still so dis-
tinct as to be indisputable.
While the waters stood at their highest position, the Searles
Basin was flooded to a depth of 635 to 640 ft. above the level
of the present valley bottom, and the lake extended back through
the Salt Wells Valley to join with a broad, shallow lake that
flooded the greater part of the Indian Wells Valley.
With the lowering of the water level less than 75 ft., the di-
vide in the volcanic peaks between Indian Wells Valley and Salt
Wells Valley became an actual division between two distinct
water bodies, and for a time here also there was a period of over-
flow from Indian Wells Valley to the lower waters in the Searles
Basin, in the same way that Owens Valley overflowed and
spilled its waters into Indian Wells Lake. These are facts
attested to by the records of the ancient shore lines and water
channels
The determined elevation of the lowest part of the present
salt flat in the main Searles Basin is 1617.6 ft above sea level
F10. 2
Cross Section of Owens, Searles, Panamint and Death V*U
Ld
t/1 l£
z < £
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- - " 5 I -1
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in
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Oct., 191S
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
841,
Pump House She
Fig. 4
ing Transformer He
and Manifolds
The Owens Lake, during a period of former greater water
supply, overflowed the divide at the south end of its basin and
its surplus waters flooded in turn a succession of lower basins,
of which the Searles Basin was one of the largest.
The Owens waters, after passing the Haiwee Divide, dropped
some 1500 ft. in about 30 miles to Indian Wells Valley, and then
spread out in a broad and relatively shallow sheet of water.
This, in turn, also overflowed, its waters passing by way of Salt
Wells Valley and a rock-cut gorge at the lower end of that val-
ley into the Searles Basin.
Eventually, the waters rose in the Searles Basin to such a
height that all three of these valleys were submerged in one
continuous body of water. The maximum water level in this
basin was clearly determined by the elevation of an outlet pass
on the south side of the basin, whence its surplus waters flowed
into the extreme south end of Panamint Valley.
In the Panamint Basin a history similar in some respects to
that of the Searles Basin was repeated: the waters rose until
the height of the lowest outlet was reached, and as they evidently
remained stationary at about that level for a relatively long
period, it is presumed that this level was determined by the
overflow of its surplus waters.
The most distinctive feature of this desert basin is the im-
mense sheet of solid white salts that lie exposed on its bottom.
It is to this salt deposit that the name Searles Lake has been
generally applied. So far as known at present, the deposit is
unique in this country in the variety of its saline minerals.
Fig. 3 shows two cross sections of the crystal body. These
were plotted from data obtained from the numerous wells which
were drilled by the California Trona Company to comply with
— "^
General View of Pipe Line between Pump House and Plant
the assessment work necessary to hold its claims. Some 300
wells were thus drilled.
As may be seen, the crystal body underlies the surrounding
mud flats found along the shore of Searles Lake.
The area of salt crust in the Searles Basin is some 12 sq. mi.
in extent, and averages from 65 to 75 ft. in depth. The forma-
tion of the crystal body is such that the brine with which it is
associated is absolutely free-flowing, and nowhere, even by
extended pumping operations, have we been able to lower the
level of the brine in the lake at any one spot to a noticeable
extent.
The main or central salt deposit is a firm but extremely por-
ous bed of salt crystals, so hard and compact that roads are built
on the same; teams and motor trucks have no difficulty in driv-
ing over its surface; and even the concrete foundations of the
American Trona Corporation's pump house were laid on the
surface of the crystal body. The road built out to the pump
Fig. 6
View of plant from west showing from left to right: 2 Urine Stor.ige Tanks of 500 000 gals each. 1 Spray Pond. 1 Boiler House with 8 Il.ihcock
and Wilcox Boilers of 500 h. p. each. 2 Concrete Stacks, 150 ft. high and 9 ft in diameter in the clear 2 Evaporator Houses for housing two triple-
effect 22 ft. in diameter and two double 1 ffect 16 ft. in diameter Manistee vacuum pins 1 Waste Silt Cones, which at present are being replaced by
Dorr Classifiers for washing the tailing salts and recovering some 10 to 15 tons of potash which w;is formerly lost. 1 Crystallizing House. 180 ft wide
and 800 ft long, ft is in this building that the new process for recovering potash from the concentrated pan liquors, as well as the new borax refinery,
will be located.
842
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. id* No.
Pflfi B|p«T-9ipi7r
\&m 'in 1 nv
Fio. 7
A Triple-Effect Unit of Manistee Vacut
1 Pans
house is some 3 V2 mi. long. Between 19,000 and 20,000 ft.
of 10-in. iron pipe connects the pumps with two storage tanks
of 500,000 gal. capacity each.
The pipe line is laid on concrete piers; it is insulated against
changes in temperature by a 2-in. layer of hair felt and a i-in.
layer of wool felt, the insulation being protected against the
elements by a thin sheet of black iron, which is fastened by
narrow iron straps.
Fio. 9
Evaporator leg pipe and tailings elevator. These tailing salt
elevators handle. rouKhly, ,VSO tons 01 waste salts per 24 hrs. These
■aid are dropped by gravity into waste silt eones from which thev are
flushed with brackish water back on to the lake.
i^y
g9m
L^L^Enf^
k \
0
r
Fig. 8
Upper Flue Sheet of a 22 ft. Maniste
Vacuum Pan
The first 15 to 20 feet of the crystal body is composed of
cubical halite and will analyze 90 per cent (or better) NaCl on
a dry basis. Below this are alternating and irregular layers of
salts, respectively high in Trona (a sesquicarbonate of soda),
sodium chloride, and sodium sulfate. The potash content of
these layers is very irregular, layers of potash-bearing crystals
having been discovered by various drilling operations which ran
from 14 to 30 plus per cent potassium chloride. The average
potash content of the crystal body is, roughly, 4 per cent potas-
sium chloride.
In a report made to the American Trona Corporation by
Charles S. Lee it is estimated that the crystal body contains
110,000 "million gallons," or 594,000,000 tons of brine. This
does not include any incoming waters from either underground
or surface sources. This brine will average 4 per cent potas-
Fio. 10
Pumps for transferring partially concentrated pan liquors from
one evaporator to another. In the background may be seen the Pelton-
Doble water-wheel-driven pump with its act of connections for filling and
draining the vacuum pans It has a capacity of 6000 gal per rain The
suction and discharge'openings are 16 in. in diameter.
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
843
Fig. 11
Set of six valves connected to filling pump by opening any two of
which the pans may cither be filled with raw brine prior to starting a run;
drained into large storage vats prior to boiling out (which in the present
cycle is done after every run of 36 hrs.; filled with brackish water for
boiling out to clean pans; or drained of same after boiling out has been
accomplished.
sium chloride. The potash contained in this brine alone amounts
to 23,760,000 tons of potassium chloride.
The average brine pumped by the American Trona Corpora-
tion has the following composition:
Per cent
Na 1 1 .00
K 2.50
CI 12.50
COj 2.65
SO. 4.65
B 0.35
In view of the process in use, the brine is given the following
arbitrary composition, based on the above values:
Per cent
NaCl 16.50
NajSOi 6.90
Na.COi 4.70
NaiB.Or 1 . SO
KC1 4.75
Specific gravity 1 . 290 at 30° C.
All the COj is figured as normal carbonate, although the brine
contains some bicarbonate.
This brine is pumped to the plant from wells drilled in the
crystal body of Searles Lake. The pumping equipment consists
of two all- iron centrifugal pumps capable of delivering 750,000 gal.
of brine each to the company's storage tanks per 24 hrs. The
pumps are connected by short manifolds to the 6 wells drilled
through the crystal body.
The pump house, and a raised road on which is operated
narrow gauge, gasoline locomotive and dump cars, are built
directly on the surface of the crystal body. The brine is pumped
to storage tanks and from them directly to the evaporators. It
passes first through a 16-ft. Manistee vacuum pan, which is
used merely as a pre-heater. From this it is pumped to three
pans of the same type, which are operated in triple effect. These
pans stand 86 ft. high and are 22 ft. in diameter. The calandria
or steam belt is comprised in the first section above the working
floor, which is 30 ft. above the ground floor of the building.
Rotary jet condenser us*--d on high-vacuum pan showing reduction
gears and 500 h. p. Terry steam turbine for driving same. Booster pump
for removing cooling and condensed waters in the background.
Fig. 13
Working floor of evaporator house. This shows a triple-effect unit
of 22 ft Manistee vacuum pans as they appear when completed- They
arc insulated with 2 in corrugated air-cell asbestos. On top of this is
spread a layer of plaster about 1 in. thick, and on top of this is a cover-
ing of 10 oz duck, the whole being finished off with a coiting of white
paint. In the distance may be seen a part of the 16 ft single-effect pan
now used as a pie-heater for the raw brine fed to No. 3 pan.
The pans are numbered (see Fig. 7) from left to right, 3, 2, and
1. No. 3 is the low-temperature, high- vacuum pan and it is
into this pan that the brine, after the pre-heating in the single-
effect 16-ft. Manistee pan, is pumped, together with a propor-
tionate amount of mother liquor from the pumps in the crys-
tallizing house. The liquors pass from No. 3 pan through the
li iii No. 2 pan into the high-temperature, low-vacuum
No. 1 pan in a steady How. Prom No, i pan the new concen-
trated liquors, having a specific gravity of 1.385 to 1.390, are
pumped over to the crystallizing house. Exhaust steam from
Terry steam turbines is fed to No. I vacuum pan from a mixing
drum.
*44
THE jaURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
\ To the left of No. 3 pan is shown a rotary jet condenser. This
■pump, operated by a 500 h. p. Terry steam turbine, functions
bo'th as a vacuum pump and condenser, handling the vapors
from No. 3 pan. The condensed vapors and cooling waters are
pumped from the condenser and returned to the spray pond by
an auxiliary booster pump. Some 7000 gal. of condensed and
cooling waters are forced through the sprays every minute.
The pans handle from 200,000 to 250,000 gal. of raw brine and
about 100,000 gal. of mother liquor per 24 hrs. This total of
300,000 to 350,000 gal. of liquor is concentrated to about 100,000
gal. of "concentrated liquor" before being sent to the crystallizing
house to cool.
Fig. 8 illustrates the upper flue sheet on one of these 22-ft.
Manistee vacuum pans. The men shown in the photograph are
expanding the 6-ft. charcoal iron flues (2 in. in diameter) into
the upper flue sheet of the calandria. One 22-ft. pan contains
some 3V5 mi- of such flues.
Inte
Fig. 14
■ of crystallizing house. This shows two of four rows of crys-
tallizing vats. These vats are 54 ft. long, 15 ft. wide, and 6 ft. deep.
They hold 30.000 gal. of concentrated liquor. An average of 15 tons of
crude potaph salts is taken from each vat. There are 36 such vats in use
for the one unit which is now operating.
A propeller shaft, extending through the length of the pan
from the top of the pan to well below the calandria, and making
30 revolutions per minute increases the circulation of the heavy
pan liquors through the flues. Foaming is kept down by the
addition of a medium heavy mineral oil.
During the boiling, sodium chloride, sodium sulfate, and sodium
carbonate are salted out. These tailing salts drop to the
bottom of the vacuum pans and are removed by salt elevators of
the regular Manistee type. The elevators discharge their salts
into waste salt cones, from which they are washed away by
water.
Machinery is being installed by Dr. H. \V. Morse, Technical
Manager, by which we will recover 95 per cent of the potash
formerly carried away by these waste salts. This will increase
our output by some 10 tons (or better) of potassium chloride
per unit per 24 hrs. Operating under the old system this
was previously lost to us.
The liquor in the pans is boiled down to the point where potas-
sium chloride begins to salt out, and is then sent to crystallizing
vats in this condition at a temperature of 90° to 95° C.
The triple effect pans are operated with constant flow, liquor
entering the pan next the vacuum pump (where the vacuum is
ind the boiling point lowest) and passing in a constant
flow from this pan through the intermediate pan to the final
high temperature, low vacuum pan, and from this pan to the
crystallizing vats.
The temperatures and vacuums are about as follows:
Pan Vacuum Temperature
No. In. Deg. C.
4 24.5 72
3 (Of triple- I 24.5 72
2 J effect - 21.0 86
1 /units ) 12.5 102
Cooling and crystallization takes place in crystallizing vats
whose dimensions are 54 x 16 x 6 ft. There are 36 such vats in
the unit now operating, and the day's run of hot concentrated
liquor tills from 3 to 4 of these. The vats cool for about 8 days,
and the liquor, now nearly at atmospheric temperature, is then
drained off.
The crystal crop is shoveled into a traveling box and is car-
ried to a drain floor, where it is allowed to lie for about a week
or so before shipment.
The following table gives the average composition of raw
brine, concentrated liquor, mother liquor returned to the sys-
tem, and crude potash salts ready for shipment:
Concen- Crude
Raw trated Mother Potash
Brine Liquor Liquor Salts
NasB.Cb, per cent 1.50 8.81 7.82 10 91
NaiCOi, per cent. 4.70 10.82 10.53 1.70
NaCl. per cent... 16.50 9.67 9.43 10.93
NaiSO*. per cent. 6.90 2.58 2.08 0.44
KC1, per cent... . 4.75 14.87 10.82 66.34
H2O, per cent ... ... 9.66
Total 34.35 46.75 40.68 99.98
Sp. Gr 1.290 (30° C.) 1 .384 (38° C.) 1 .362 (34" C.)
The American Trona Corporation is producing to date some
1800 tons of crude potash salts per month. Additional equip-
ment, such as a nearly completed second unit together with a
300-ton ice plant1 for refrigerating purposes and new methods
for treating the concentrated liquor (devised under the direction
of Dr. H. W. Morse), will enable the American Trona Corpora-
tion to produce by the end of October some 4500 tons of potash
salts a month, analyzing from 75 to 80 per cent potassium
chloride and containing less than 3.5 per cent borax, figured as
anhydrous sodium tetraborate.
By the first of 1919 the American Trona Corporation will be
producing some 40 to 50 tons of refined borax daily, analyzing
99.50 per cent N^I^Oi.ioHiO (crystal borax).
SYMPOSIUM ON CERAMICS
September 26, 1918
RECENT DEVELOPMENTS IN CERAMICS:
By A. V. BUEININ'GER
Bureau of Standards, Pittsburgh
One of the most important functions of the ceramic industries
is the supply of refractories for the metallurgical operations of
the country, steam power plants, by-product coke ovens, gas
plants, glass works, and many other purposes too numerous to
enumerate here. The demand for these products has been
enormous and has been met by the refractories industries in a
very satisfactory manner. Although at times the need of No.
1 fire bricks has been greater than the production, such a con-
dition does not exist at the present time, owing to the expansion
of this branch of the industry. In many instances the extraor-
dinaiy demand was caused, in part, by the unwillingness of
consumers to use anything but No. 1 refractories even for pur-
poses where lower grade products would serve equally well.
Fire bricks of the lower refractory grades are available in abun-
dance, especially since a considerable number of face and building
brick plants have taken up the production of this type of ware.
One of the urgent needs in this connection is the establishment
of a classification and specifications for the several grades of clay
refractories. This task is being undertaken at the present time
by the War Industries Board. The work of standardizing the
1 The equipment in this refrigerating unit consists of three 100-ton
De La Vergne ice machines, driven by three Corliss engines of 300 h. p.
1 By permission of the Director of the Bureau of Standards.
Oct., 191!
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
shapes of fire brick has already been accomplished in a satisfac-
tory manner.
The demand for silica bricks has been greatly increased through
the development of the by-product coke oven. Meeting this
demand involves not only large quantity production of these
refractories, but high quality as well. It is necessary that the
transformation of the quartz to cristobalite be largely com-
pleted, as indicated by the lowering of the specific gravity to a
value of not more than 2 .38, and that the product possess good
mechanical strength, corresponding to an average modulus of
rupture of about 500 lbs. per sq. in. These requirements are
exacting and may not always be met in bricks made from silica
rock other than quartzite. Certain materials, like chert and
flint, transform to cristobalite more rapidly than quartzite, but
do not yield as strong a product. Sandstones usually transform
more slowly and likewise tend to give inferior strength.
The manufacture of silica refractories is certain to expand still
more, both in the Eastern States and in the Middle West. If
the war continues for any considerable period, additional emer-
gency production in connection with the erection of new coke
oven plants will certainly be necessary.
Difficulties have been met in supplying the basic magnesite
refractories from the available American materials. This has
been due to the nature of our magnesite, which differs from the
Austrian ore in being very low in iron oxide and sometimes
higher in lime. This makes it necessary to add the iron syn-
thetically, a procedure which adds to the cost of production,
since it requires intimate blending and grinding of the mixture
and a higher calcination temperature than is needed with the
European raw material. In addition, the magnesite must be
transported across the continent from California or Washington.
The latter state produces at the present time large quantities of
magnesite quite low in lime and the quality of the material is of
a character which is making it possible to reduce operations to a
uniform practice. It has been found possible also to replace
magnesite bricks in certain operations by bauxite refractories.
The production of magnesia spinal refractories of the compo-
sition MgOAl203 has made a beginning, and it is not unlikely
that for many purposes it will prove a very desirable material.
There has naturally been a shortage of chromite refractories,
even though the quantities really needed are small. This has
been overcome by the use of thinner partings and in many cases
by doing away with this refractory entirely, without, apparently,
any serious effects
Much has been said on the question of graphite crucibles.
The graphite problem is undoubtedly the more important one in
this connection. It is a difficult matter to replace Ceylon graph-
ite altogether with the domestic mineral. In the first place the
greater density of the imported material, 2.25, which imparts
to it the characteristic resistance to oxidation, its foliated struc-
ture, and the low ash content of the best grades combine to make it
extremely satisfactory for the purpose of crucible making. This
graphite can be bonded together with a comparatively small
amount of clay, since the surface factor per unit weight is smaller
than for that of any other kind of graphite. This point may be
illustrated by the volumes occupied by the same weight of sev-
eral types of graphite. Thus, 100 g. of ground Ceylon graphite
after thorough shaking occupies a volume of 90.7 cc, Canadian
graphite iiy.6 cc , and Alabama graphite 152.0 cc. In other
words, it would be impossible to make graphite mixtures of
maximum carbon content from the two American materials.
Since they offer a much larger surface the amount of clay used
must be greater. From this it follows that the ultimate density
and thermal conductivity are certain to be lower. To what
extent American flake graphite can be admixed with the Ceylon
graphite remains to be seen. The writer has seen mixtures in
which the flake added amounted to 20 per cent of the total
graphite content and gave fair foundry results. It might be
possible, however, to perfect processes which will enable the
crucible maker to employ larger percentages of domestic graph-
ite, and at the same time secure practically the same results as
with Ceylon graphite. On the other hand, there is no reason
why a large quantity of domestic graphite should not be used
in the making of stoppers and similar articles. The comparison
made between the Ceylon and flake graphite is, of course, rela-
tive, and refers to crucible value obtained per dollar at the
present time. If this country could no longer obtain Ceylon
graphite, the production of metal certainly would not be dimin-
ished in any way as we could get along very well with flake and
amorphus graphite, furnace carbon and coke.
The lack of the German Klingenberg clay for crucible making
is not as serious a matter as has been thought. It has been
shown conclusively that it can be replaced both by English and
American ball clays.
Similarly, the German Gross Almerode clay used in the mak-
ing of glass pots has been replaced by American clays and syn-
thetic mixtures in a very satisfactory manner. In fact, it is
quite probable that the new techniques now being developed
will yield results superior to those formerly obtained with the
use of imported clay. The shaking up caused by the war will,
in the end, be of distinct service to the glass refractories indus-
try. At the same time, the glass industry will gain in pot
service through the realization that the control of the heating-up
process of the pots in the arches is essential in preventing loss.
Special clay refractories have been developed also with refer-
ence to improved thermal insulation, including materials highly
refractory, light in weight, and possessed of good insulating
qualities. The saving in fuel consumption and weight through
the use of such products is bound to be considerable.
The manufacture of hard-fire, true porcelain has received a
powerful impetus through the war. Three plants are already
operating successfully on the production of chemical porcelain
and are making rapid strides with respect to quality. The
manufacture of hard porcelain tableware on a large scale is to
be begun in the very near future. It is very fortunate that the
pioneers in this work have realized the importance of putting
their production on a firm basis with reference to foreign com-
petition. By the use of automatic machinery, mechanical dry-
ers, and tunnel kilns, they will be enabled to meet foreign com-
petitors on equal terms. The plants now in course of construc-
tion excel all European potteries in the elimination of unnecessary
labor cost and expenditure of fuel. The development of a hard-
fire porcelain industry is, indeed, a national duty. It would be
preposterous and humiliating to contemplate any further de-
pendence on Germany and Austria for these products. By
establishing this industry we shall be in position to seek the
South American markets to which we have a fair right.
The demand for ordinary tableware at the present time is
greater than has ever been known before and difficulty is being
experienced in supplying the requirements of the Army and
Navy and at the same time those of the country. The simpler
shapes such as cups and mugs are now being produced by the
one-fire process, which incidentally results in an appreciable
saving of fuel.
Porcelains for special purposes have been dewlope.l Mice,'.-,
fully. Thus, the National Bureau of Standards has introduced
the manufacture of the refractory Marquardt porcelain, essen-
tially sillimanite, formerly produced by the Royal Porcelain
Manufactory at Berlin and used so largely for pyrometer tubes
and similar articles. Likewise, we have succeeded in making
porcelains possessing remarkably li i k '» electrical resistance at
temperatures. Several of the bodies produced in the
Pittsburgh Laboratory of the Bureau of Standards showed a
Ohm per cc. at 7800 C. and at the same
time a coefficient of thermal expansion of only 3.81 X io pei
degree C. between the temperature range 300 to 40)0 C. The
846
THE JOURNAL OF INDUSTRIAL AXD ENGINEERING CHEMISTRY Vol. 10, Xo. 10
same materials showed none of the variation in thermal expan-
sion common to most porcelains, the coefficient remaining prac-
tically constant throughout the range 30° to 5200 C. It is
evident that such properties, coupled with good mechanical
strength, are essential for such uses as aeroplane spark plugs.
There is every reason to believe that the principles thus worked
out will greatly assist in producing special grades of electrical
porcelain for use under severe conditions. These developments
have been assisted greatly through the use of the petrographic
microscope in the study of porcelain structures.
The manufacture of electrical porcelain is undergoing improve-
ments at a more rapid rate than ever before in the history of
this industry. The methods of preparation are more thorough,
the details of shaping are being studied more carefully, the dry-
ing process is being controlled with greater accuracy, and the
methods of testing developed towards more exact differentiation
as to quality. The casting process is finding application to an
increasing extent. Further developments are to be expected
with reference to the composition and firing of electrical porce-
lain, based on more recent studies on the subject of the function
of feldspar as an electrolyte and the volume changes induced by
the transformation of quartz to its several crystalline modifica-
tions.
Considerable work is being done also with regard to the com-
plete survey of the resources of the country in kaolins and ball
clays for use in the ceramic and paper industries, through the
agencies of the Association of State Geologists, the Bureau of
Mines, the United States Geological Survey, the American
Ceramic Society, and the Bureau of Standards. It is believed
that this survey will enable us to take stock of our resources
with the final object of making ourselves independent of any
foreign sources. A considerable number of new clay deposits
have been located within the past two years, to say nothing of
glass sand and other ceramic raw materials.
One of the clay industries vital in the prosecution of the war
is the manufacture of chemical stoneware. The production of
this type of ware requires particular skill, owing to the compli-
cated designs, large size, and the necessity of the tight fitting
of the pieces. But few realize the magnitude of the task which
confronted this industry, especially when handicapped by short-
age in labor, fuel, and other necessities. It is very gratifying,
indeed, to be able to say that the stoneware manufacturers have
met the situation so well and have been able to supply the needs
of the chemical industries. This statement applies equally to
the manufacturers of acid-proof, enameled cast iron, and sheet
steel, products which have played an important role in recent
chemical developments.
Another industry having a direct bearing upon war work is
that engaged in the manufacture of abrasives and grinding
wheels. The rapid growth of this branch of manufacture 3nd
its technical development are characteristic of America. Its
work has been done with such quiet efficiency and it has met
the demands of the present conditions so promptly that but few
realize the magnitude and importance of its accomplishments.
Research has played a large part in this development and to
the utilization of scientific facts we owe the highly specialized
grinding tools made available for large production, as well as
for the most delicate processes, such as the grinding of optical
lenses.
The industries engaged in the production of ceramic struc-
tural materials have naturally been hard hit by the decrease in
building activities and by the fuel orders. The manufacturers
of building bricks, hollow tiles, sewer pipe, paving bricks, terra
cotta, floor and wall tile, etc, are endeavoring to hold their or-
ganizations together. In districts where war activity prevails
the plants are operating to capacity, in others new branches of
manufacture have been taken up, such as the production of
refractories, crucibles, and certain specialties for war use. But
even under such conditions interesting developments are taking
place. Much attention is being given to the question of fuel
economy through more rapid firing and the utilization of waste
heat. New applications of clay are being found, such as the use
of crushed, vesicular, vitrified brick material as an aggregate for
concrete, having the advantage of light weight, low thermal
conductivity, and constancy of volume when heated.
With reference to the glass industry the three most interesting
developments are those relating to the optical, colored (signal),
and the resistant or chemical glasses. When it is realized that
at the beginning of the war but little optical glass was being
produced in the United States, the rapid development of the art
presents an inspiring example. The necessity of war brought
together the manufacturers on the one hand and scientific and
technical organizations like the Geophysical Laboratory of the
Carnegie Institute and the Bureau of Standards on the other.
Although some of the manufacturers had brought their furnace
practice to a very satisfactory state it was not realized fully
that the raw materials must be practically free from iron, sulfur,
chlorine, and other impurities. Likewise methods for the rapid
examination of the glass were lacking, so that frequently poor
glass was brought to the grinding and polishing rooms of the
optical shops and again, good product was by chance rejected.
The necessity of temperature measurement and control was not
fully realized and the method of stirring had not been brought
to a satisfactory development. At the same time the com-
mercial glass pots were the source of much grief, due to their
high iron content which discolored the glass in the absence of
decolorizers which are not allowable, and their failure to resist
the corrosive action of the flint and barium glasses. These
things have been overcome to a very large extent.
Through the use of sand of great purity and constant checking
of the composition of the other constituents the primary diffi-
culties have been removed. The composition of the glasses has
been correlated with the optical properties, the index of refrac-
tion, the dispersion value, and the light absorption. Time-tem-
perature schedules have been worked out for the melting and
cooling periods and satisfactory stirring machines designed.
Rapid inspection even of the glass in lump form is now possible
by the use of immersion methods and examination with mono-
chromatic light in addition to the examination through the
polished edges of blocks.
The pot problem has been solved through the use of white
burning clays like the kaolins and even more satisfactorily by
the production of se mi- or true-porcelain pots. Containers of
the latter type are now being made in several works and have
proven eminently useful. In fact, it has been possible to melt
in such pots dense barium crown glasses which have proven
exceedingly destructive to the ordinary types of refractory
material.
The annealing process is being studied by a number of work-
ers and some interesting information has already been obtained.
It might be said, then, that in the United States we have mas-
tered the essentials of the production of optical glass and about
seven types are being manufactured commercially. Problems
dealing with the cutting down of the losses due to certain optical
phenomena, etc., of course, still remain, and it is to be expected
that continued progress w-ill be made in this art.
It is a source of pleasure to note the fact that scientific and
technical researches dealing with the technology of silicates are
being continued at the present time, even though they have
more or less bearing upon conditions brought about by the war.
We are mastering more and more the control of the class of dis-
persed systems represented by clays floated in water, their
drying behavior, and the changes which they undergo upon
vitrification and fusion by resorting to the methods of the scien-
tific investigator.
In this brief survey it has not been possible to emphasize
Oct., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
847
some of the more important technical advances, nor is it
permissible at this time to dwell upon certain developments,
such as a new role played by clay in chemistry, but it is hoped
that this hasty contribution may afford some conception as to
the activities in the ceramic industries.
CARBORUNDUM REFRACTORIES
By S. C. LlNBARGER
Ceramic Engineer, The Carborundum Co., Niagara Falls, N. Y.
Ever since its inception one of the vital problems of the
ceramic industry has been the question of suitable refractory
materials, both for use in its own factories and as a product
which will meet the demands of the other industries which re-
quire the highest grade of refractories. These materials must
have sufficient strength under normal conditions to carry the
weight of the structure of which they are an integral part and
must, furthermore, have sufficient refractoriness to carry this
same load under the extreme heat conditions to which they are
subjected.
It has always been customary to regard heat insulation in a
refractory material equally desirable with resistance to fusion,
probably because these properties are intimately associated in
the case of the common type of fire brick or saggar mix of the
aluminous silicate type which are highly refractory and are such
poor conductors of heat that in comparison with metallic sub-
stances they can safely be classed as heat insulators. However,
only a superficial study of the problems involved in the burning
of ware in saggars or muffle kilns reveals the fact that heat con-
ductivity of the refractories used, besides being highly desirable,
is a potent factor in the economical operation of the process.
For many years men connected with all branches of the clay-
working industry have been seeking a more effective means of
burning clay products in a shorter time and with less fuel. Es-
pecially is this true, and the need for it was never greater than
at the present time when the vital needs of the country must
be met with a maximum of fuel economy. Most of the efforts
have been along the line of improving kiln design so that the
maximum amount of heat is extracted from the gases of combus-
tion before they pass into the stack. In most cases this is accom-
plished by passing the gases from the hot zone cr chamber over
ware in other zones which is at a much lower temperature, and
thereby gradually raising the temperature of the ware by the
utilization of the sensible heat of the gases after they leave the
combustion zone. All agree that when ware is being burned at
a high maturing temperature one of the vital points of fuel
economy is to get as much as is possible of the heat of the gases
transferred from them to the ware.
In the pottery and allied industries where the ware is burned
in saggars or by setting on shelves or bats, a solution of this prob-
lem resolves itself into the proper selection and utilization of a
refractory material which will more quickly and more easily
absorb the heat from the surrounding gases and transmit and
deliver it to the center of the bearing structure. The essential
physical properties which govern the selection of the best refrac-
tory for this purpose are strength, specific heat, thermal con-
ductivity, and emissivity. Of course in connection with these
it must have the required refractoriness and be able to with-
stand the necessary handling without breakage.
The clement of strength, both transverse and compressive, is
one of the properties which is too often overlooked in the selec-
tion of the proper refractory material. By using a material of
high mechanical strength, both under normal and heat condi-
tions, not only is the loss by breakage materially reduced, but
primarily the walls of the building material can be very much
thinner, with the consequence that the heat is conducted to the
ware much more readily, to say nothing of the saving in kiln
space and the smaller amount of heat required to bring the
building material up to the maturing temperature of the kiln.
The specific heat of the refractory is the important physical
property required in calculating the number of thermal units
that are really wasted in bringing the large mass of the support-
ing material from normal temperature up to the finishing tem-
perature of the kiln. In some instances where the weight of
the bats and saggers is equal to or more than the weight of the
ware which it protects and supports, it means a considerable
item in the burning cost.
As a concrete example of the exact factors involved in the
transfer of heat from the hot kiln gases to the ware, let us con-
sider the specific case of a plant which is burning ware in sag-
gars, the saggars being set in stacks so arranged in the kiln that
their entire peripheral surface is exposed to the kiln gases. The
spaces between the saggar stacks can be assumed to be chimneys
and the velocity of the gases through them will depend upon
their size and shape and also upon the draft of the kiln. Assume:
1 — That the turbulence is such as to make a fairly uniform
temperature in the kiln at any point on one of a system of sur-
faces which is symmetrical about the gas passage; and
2 — That the average temperature on these surfaces is the aver-
age of the temperature of the gases at ingress and egress.
It is evident that these hypotheses mean that the turbulence
is controlled by some finite law and that a graph indicating the
temperature gradient through the kiln would be a straight line.
These hypotheses hold fairly well if the motion of the gases is
so slow as to make the turbulence negligible or if the motion of
the hot gases is so great as to make the turbulence very great.
The quantity of heat then that will pass through the walls of the
supporting refractory medium in a given time and be delivered
to the center of the saggars will depend upon the excess temper-
ature of the gases over the ware and the thermal conductivity
of the refractory and will be a direct function of the emissivity
of it.
When heat waves strike a body some of them are absorbed and
some of them reflected, unless the body be what is known as a
black body, in which case all of the heat rays are absorbed. All
other bodies absorb a definite percentage of the heat waves
which strike their surfaces and reflect the rest, the exact ratio
of conduction and radiation being dependent upon the surface
and the character of the body. This ratio for any material is
what is known as the emissivity factor of that material. Under
like conditions the same ratios hold true for the radiation of heat
units from any solid body into a gaseous medium. The emis-
sivity factor for any substance can then be determined experi-
mentally by finding the radiation per second per unit surface
area per degree difference in temperature. As the quantity of
heat that will cross the boundary plane between the solid and
the gas per unit time is dependent upon a factor other than the
thermal conductivity of the solid, it is readily observed that the
emissivity factor of the refractory which is usually neglected is
an important consideration in the absorption of the greatest
amount of the sensible heat from the gases which come in con-
tact with it.
Crystallized silicon carbide or carborundum, as it is most com-
monly called, has long been recognized as having unique phys-
ical properties which make it peculiarly adaptable in the construc-
tion of highly refractory materials. However, up to the present
time it has not had a very wide application in this field owing
to its high price and also to the lack of sufficient quantities to
supply other than the abrasive industry, which of course is its
field of primary importance.
At the present time there are two types of crystallized carbo-
rundum refractories which have been highly developed. The
first type which goes under the trade names of "Refrax" and
"Silfrax," depending upon whether the crystallization of the
aggregate is large or small, is made according to patents which
I cover the silicklizing of mixtures of carbon and silicon
carbide or carbon forms and their subsequent conversion into
848
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
carborundum by subjecting the carbon to silicon-containing
vapors at the heat of the electric furnace. The carbon is con-
verted into carbide of silicou forming a dense interstitial binder
or matrix between the crystals. Of course there are many
modifications of this process but the essential characteristic of
this type of refractory is that the final products obtained are
pure silicon carbide.
The other type which is known as "Cartofrax" is the type
most generally applicable for use in the ceramic industries. It
is made by bonding graded crystallized carbide of silicon grains
with various percentages of a mixture of special refractory clays
or other bonding substances.
When bonded with even a high percentage of clay binder,
brick which contain carborundum give very great refractory
values. However, since the refractoriness of a conglomerate
refractory mass is a direct function of the amount and character
of the least refractory constituent, it is recognized that the ideal
condition to be obtained is that the amount of binding material
used be the least which is consistent with the requisite strength ;
and that the vitrification temperature of the binder be as high
as is commercially practicable. Mixtures of grits and methods of
bonding are employed which insure a very dense body of low-
porosity with but a minute percentage of refractory clay binder
and at the same time allow the manufacture of large and intri-
cate shapes.
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product of that particular class of refractory. No attempt was
made to compare different brands of the same material.
Table I
Compressive
Specific Thermal Strength. Lbs.
Material Heat Conductivity per sq. in.
Fire Brick 0.192 0.0034 1,050
Saggar Mix 0.187 0.0033 1.340
nesite 0.220 0.0071 4.800
Chrome 0.174 0.0067 3.900
Refrax 0.162 0.0275 12.500
Carbofrax 0.180 0.0243 14.700
Silica 0.191 0.0020 2.300
A comparison of the thermal conductivities of the materials
reveals the fact that the carbofrax brick will conduct about three
times as much heat as magnesite, seven times as much as the
saggar mix, and twelve times as much as a silica brick in the
same period of time.
Fig. II graphically represents the relative efficiencies of vari-
ous refractory' materials as obtained by using the values of
specific heat, thermal conductivity, and emissivity in the formula
for the law governing the transmission of heat from a gas to the
interior of a solid body. The table is arbitrarily based with the
abscissas representing relative efficiencies while the ordinates
give difference of temperature. A study of the results demon-
strates that the materials with a high emissivity factor and high
coefficient of heat conductivity show several times the efficiency
of those with correspondingly lower values with the same thick-
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Fig. I
Rtiatire Efficiency
Fie. II
Experimentation has shown that crystalline silicon carbide
forms at 18400 C. and dissociates at 2240° C. into its elements,
the silicon being volatilized and the carbon remaining as graphite.
No softening or fusing occurs below the dissociation temperature
which is shown by the sharp and perfect forms of graphite pseu-
domorphs or skeletons which are left when silicon carbide dis-
sociates. This is in direct contrast to most other refractories,
such as silica, chrome, and fireclay brick, which soften at a tem-
perature several hundred degrees lower than their fusion
point.
Fig I shows tin' emissivity curves of several common rcfrac-
tories The curves for this factor were accurately plotted from
results obtained by very complex experimental methods winch
are too cumbersome to describe in this paper. It will be noted
that the emissivity of both classes of crystallized carborundum
brick is much higher than either magnesite or chrome brick and
almost double that Of clay brick at a temperature of 200° C. and
higher.
Table 1 shows the results of some tests made- on the most
common types of refractory materials. The specimens tested
were selected at random as being representative of the average
ness of wall Compressive tests of the materials show that the
carborundum refractories have a load-carrying capacity over
ten times as great as the saggar mixture under normal tem-
peratures Under heat conditions this ratio are considerably in-
creased because there is absolutely no softening of this class of
material at 13500 C, while the saggar mix at the same temper-
ature shows a deformation with a load of 50 lbs. per sq. in. In
fact, blocks of bonded silicon carbide are used as bearing blocks
in making load tests on refractories at high temperatures. It
would then be possible to use refractories for supporting ware
in kilns with walls one-tenth as thick as are ordinarily used with
the aluminous silicate type of refractories. Since the
amount of heat transmitted by a solid is inversely proportional
to its thickness, the efficiency already demonstrated by high
thermal conductivity and emissivity would be multiplied by ten.
Aside from the importance of fuel economy, the high thermal
conductivity and heat capacity of crystallized carborundum im-
part to refractories made from it the property of withstanding
the most sudden temperature changes because any variance in
tin- temperature of the surface is quickly communicated to the
whole mass and the heat is rapidly dissipated. Thus, the
Oct.. 191S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
S40
molecular work resulting from it is uniform, and refractory
shapes of this type can be subjected to the most sudden
variations of temperature without being cracked or dis-
integrated.
As silicon carbide is not subject to any molecular changes
being formed at 18500 C. in a crystalline state, and has an
extremely low coefficient of expansion, no porous structure is
necessary and a high density can therefore be obtained. This is
not possible with most refractories since they contain ingredi-
ents which have one or more allotropic forms and must be made
open and porous to withstand successfully the internal stresses.
The low coefficient of expansion and high density of carbo-
rundum brick permits the construction of solid structures in
places where the leakage of heat and gases through cracks in
the walls due to alternate contraction and expansion is a detri-
ment to the successful operation of the process.
In an effort to obtain the complete combustion of a fuel there
is a growing tendency to increase the temperature of the fire-
boxes or furnaces. Ordinary firebrick, even of the best grade,
fuse under the high temperatures developed and are attacked
by the fluid ashes of the coal. This fluid ash which so violently
attacks fireclay brick forms a brownish coating or glaze over
the exposed portion of the carborundum brick which is unat-
tacked by any additional fluid ash which is formed in the fire-
box. Owing to their extreme hardness this type of brick does
not suffer from deterioration as do the common refractories
when struck by the tools of the firemen during the process of
cleaning the fires.
Carborundum is manufactured by passing an electric current
through a mixture of sawdust, sand, and coke in a long rectan-
gular resistance furnace. By the utilization of an enormous
amount of electrical energy, the central portion of the furnace
is brought up to about 22000 C, at which temperature the silica
is volatilized. One molecule of silicon combines with one of
carbon, forming a core of pure crystallized silicon carbide be-
tween the electrodes in opposite ends of the furnace. Imme-
diately surrounding this is a zone of the amorphous variety of
carborundum which is commercially known as firesand. Chem-
ically it is a mixture of several silico-carbides which vary in com-
position from SijCaO to Si$CeO. This represents a partial reduc-
tion of silica by carbon or a solid solution of silicon carbide in
silica.
This material is also highly refractory but, owing to its lower
heat of formation and lack of definite crystalline structure, it is
not as stable under extremely high temperature as the crystal-
line variety. However, it has a wide application in places where
a higher degree of refractoriness is required than can be obtained
in the best grade of fireclay brick.
Finely ground firesand when mixed with a bonding material,
such as kaolin or high-grade plastic fireclay, makes a refractory
which can be moulded in place or plastered over the surface of
a lower grade refractory to protect it from the cutting action of
impinging flames. Owing to the fact that even the intense re-
ducing heat of an oil flame does not cause any modification of
the firesand, it has come to be a recognized material for the
linings of brass furnaces of all types. It is also used as a pro-
tective coating for the brickwoik of furnaces, bag and baffle
walls, and the walls of potter's kilns. For this work it is mixed
with water and sodium silicate, and often a small amount of
clay to increase the adhesion, and applied to the walls in a slip
condition.
Refractory materials made of mixtures containing silicon car-
bide are now being used in various capacities in the ceramic as
well as the metallurgical industries. When the thermal effi-
ciency and the increased permanancc of structures made from it
are recognized it promises to have a much wider application in
the burning of ceramic wares.
SYMPOSIUM ON METAL INDUSTRIES
September 27, 1918
THE PYROPHORIC ALLOY INDUSTRY
By Alcan Hirsch, Consulting Chemist. New York City
The pyrophoric alloy industry is a very young industry and
is intimately associated with the rare earth industry which is
also a comparatively young one. In order to make the situa-
tion clear, it will be necessary to briefly outline the meaning,
foundation, and history of the rare earth industry. The term
. means the industries which mine, separate, purify, and use the
earthy metals or salts of metals formerly considered rare, i. e.,
cerium, lanthanum, didymium, yttrium, zirconium, and tho-
rium. The rare earth industry was founded in 1885 by an
Austrian, Baron Auer von Welsbach, who while investigating
certain ores noted the brilliant light-emitting qualities of their
oxides, and invented the incandescent gas mantle. This gas
mantle was made from oxides of lanthanum and zirconium to
which a little cerium oxide was added. Welsbach secured pat-
ents in various countries and sold them to investors. About
1887 the industry took root in the United States with the forma-
tion of the Welsbach Light Company. The early gas mantles
proved somewhat of a disappointment. Welsbach was in dan-
ger of being discredited and pushed his research further, par
ticularly investigating ores of thorium. The early mantles gave
only about 10 candle power per cu. ft. of gas, but the use of
thorium salts considerably improved this, and purer and still
purer thorium salts were tried until finally the salts were made
so pure that they emitted no light at all. To make a long
story short, it was found that while thoria should be the main
and almost the whole constituent of a mantle, the presence of
1 or 2 per cent of other oxides, chiefly cerium oxide, was essential
to high light-emissive value. This leads us to the present incan-
descent gas mantle, with which we are only indirectly concerned
in so far as its production leads to the making of by-products
from which pyrophoric alloy is produced.
The original sources of thoria (thorite) found in Norway proved
totally insufficient in quantity to supply the demand of thoria
for use in gas mantles. The manufacturers of gas mantles,
therefore, turned to monazite sand, found rather plentifully in
Brazil and India and to some degree in North Carolina as a source
of thoria. About 15 to 30 per cent of monazite sand is phos-
phoric acid, and most of the rest is made up of various oxides
of the rare earths, 20 to 30 per cent cerium oxide, 20 to 30 per
cent oxides of lanthanum and didymium in varying proportions,
and small percentages of the yttrium and zirconium oxides. All of
these are practically useless in any quantity in the gas mantle busi-
ness. It is the 2 to 10 per cent of thorium oxide, generally about
6 per cent, for which the monazite sand is bought and worked
up. More than a quarter of a million pounds a year of thorium
oxide is made in the United States from about 5,000,000 lbs. of
monazite sand with the by-product mostly wasted. This by-
product of so-called "cerium oxides" or "mixed rare earth metal
oxides" is considerably more than 1,000,000 lbs. per annum, and
this by-product constitutes the raw material for making pyro-
phoric alloy.
It should here be made clear that what is called "metallic
cerium" and used as such is really a mixture of cerium, lantha-
num, didymium, samarium, etc., all very closely allied and very
similar metals. It is not necessary to separate them, but the
salts for making the metal must be purified. The process for
making metallic cerium and the like is described in U. S. Patent
1,273,223, patented July 23, 1918, to Alcan Hirsch and Marx
Hirsch, inventors.
The metal is made in an electric furnace by electrolysis which
consists in passing an electric current in a certain manner through
a molten salt of the metals to be produced, called the electrolyte.
The first problem is, therefore, the making of 1 1 1 electrolyte.
We have found tli.it to Secure an electrolyte suitable for the
850
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
prolonged, regular commercial production of metallic cerium,
certain peculiar precautions are necessary. We have found that
certain rather limited ranges of temperatures are required for
efficiently performing the two classes of work to be carried out
in the electrolytic cell, and these are denominated "separating
temperature" and "agglomerating temperature." The electro-
lyte is prepared preferably by utilizing the oxides described
above which are the by-product from the incandescent gas man-
tle industry. These oxides are preferably dissolved in commer-
cial hydrochloric acid, reasonably free of sulfuric acid and sul-
fates, using during the solution process as little heat as possible,
and preferably maintaining an excess of the oxides so as to make
the chlorides of the metal. The resulting chloride liquor consists
not of cerium chloride, but of a mixture of the chlorides of cerium,
lanthanum, didymium, samarium, yttrium, thorium, and other
rare earth metals, of which cerium is the chief single con-
stituent.
Contrary to common belief, the general purity of this solution
is immaterial, but the percentages of sulfur and phosphorus
compounds on the one hand, or of chlorine carriers of dual
valency, such as iron and aluminum compounds, on the other
hand, should each be reduced below 3 per cent. Addition of an
excess of cerium oxide may be used to throw out the iron and
aluminum, and calcium chloride, or better barium chloride, may
be used to throw out the sulfur and phosphorus compounds.
The solution is then clarified, preferably hot by filtration or
settling, and evaporated to dryness. The preparation of elec-
trolyte should be so carried out as to secure the proper tension
conditions between the fused electrolyte and the fused metal
when produced in the electrolytic bath. An excess of certain
impurities including oxy-chlorinated products, such as cerium
oxy-chloride, I believe tends to so far reduce the surface tension
between the metal and electrolyte in the electrolytic bath and
alter the viscosity as to produce emulsification or colloidal solu-
tion of metal in the fused electrolyte and prevent amalgamation
of the metal in the bath. The oxy-chlorides may be removed
in either of two ways.
(1) The chloride solution obtained as above may be evap-
orated to solidification, and then fused in an atmosphere of
hydrochloric acid gas to produce complete dehydration while
preventing oxidation by the air, or decomposed steam, from the
electrolyte, the aqueous acid in the vapors being, if desired,
condensed hot and separated, and the concentrated hydrochloric
acid gas may be dried and used over again, or may be recovered
with water as hydrochloric acid.
(2) The known method of making for electrolysis the
double chloride of sodium and cerium does not yield a desirable
electrolyte. If, however, about 15 per cent sodium or potas-
sium chloride (insufficient to make the double salt) and 15 per
cent of ammonium chloride by weight, based on the dry weight,
of the dissolved rare earth chlorides, are both added to the
chlorides after the excess of iron, aluminum, sulfur, and phos-
phorus impurities are removed and before the evaporation, the
solution may then be evaporated to dryness and the dehydration
carried through to fusion of the chloride without the production
of characteristics resulting in objectionable tension phenomena
in the electrolytic bath when the material is later subjected to
electrolysis. The ammonium chloride is volatilized in the above
treatment, and forms a chlorinating agent as does the hydro-
chloric acid gas in the first way, and may be similarly recovered
and re-introduced into the process. When the electrolyte formed
in this way is subjected to electrolysis, the alkali metal chloride
accumulates in the electrolytic cell, and after the removal of the
metallic cerium or mischmetall, it may be thrown away or dis-
solved in hydrochloric acid, clarified, purified as above explained,
and added to fresh electrolyte being prepared.
The electrolysis is preferably carried out in pots of similar
cast iron, although it may be carried out in suitable clay
crucibles, about 1 ft. in diameter and 12 to 18 in.
deep, usually set in brickwork and externally heated. Heat
should not be applied to the sides of the pot, as would or-
dinarily be the case. It should be applied almost wholly to the
bottom of the pot, so as to regulate its intensity and volume.
It is very objectionable to fill the pot with fused electrolyte, as
is described in experimental literature. We begin the electrol-
ysis with a nearly empty pot, heat a small amount of electro-
lyte with the outside gas flame nearly to fusion, and apply the
electric current to complete the fusion. Thereafter continue
the electrolysis and the gradual addition of electrolyte, building
up the charge in the pot continuously by gradual increase in
the contents of the pot, until it is practically full, and a termina-
tion of the run is brought about. Either carbon or graphite
anodes may be used, but they each show a critical density,
that is. one above which current may pass without valuable
effect. For graphite this is about 6 to 7 amperes per sq. in. of
anode surface, and for carbon about 5V2 amperes per sq. in. of
anode surface. Furthermore, we find it desirable to maintain a
relation between current density at the anode and at the cathode,
the latter being about '/< to '/i of the former, in order to secure
a desirable electrical circulating and heating effect. By adding
solid lumps of electrolyte to the bath, the temperature of the
cell is regulated when it becomes slightly too hot and this also
contributes a portion, at least, of the fresh electrolyte required
for building up the charge which is being decomposed.
As the run approaches 2+ to 26 hrs. in duration, if electro-
lyte made according to the second way is used, the sodium salt
accumulates in the charge to such an extent that it becomes
advisable to terminate the run. We have found that certain
precaution for this termination is necessary to secure good yields
of metal. Therefore, preparatory to shutting down the run, we
turn on the heating torch full blast, and we also increase the
current, stirring up the charge in the cell thoroughly about every
half hour for the last two or three hours of the run. The contents
of the cell should be in a nice liquid condition if the electrolysis
has been properly carried out. The current may be shut off,
the anode taken out, and the bath gently but thoroughly stirred
for about 5 min., care being taken to cease stirring well before
the bath begins to stiffen up at all. If iron pots are used, it is
generally most practical to break up the pot after cooling, in
order to separate the button of metal from the electrolyte.
This relatively pure mixed metal or mischmetall is soft and
does not spark easily on scratching. Consequently, to make
pyrophoric alloy it must be made harder, and it is, therefore,
alloyed with about 30 per cent of other metals, chiefly iron, to
make the commercial sparking metal or pyrophoric alloy which
is formed into small pieces to make the "flints" used in making
lighters, igniters, mechanical fuses, etc. The alloy enters into
commerce in the form of small strips, rectangular or round, of
varying lengths, varying from 200 to 2000 pieces to the pound.
The most general form is a round piece approximately about
', t in. in diameter and Ys in. long, of which there are from
1500 to 2000 pieces to the pound.
In this connection, I might mention that the manufacture of
these small pieces, the only form in which mischmetall is sale-
able, is a most difficult operation, requiring what is comparable
to equipment for the manufacture of fine jewelry-
Baron Auer von Welsbach developed the improvement of
hardening the relatively soft metal with iron, in order to make
a hard metal which would emit sparks when scratched. He took
out patents on this invention the world over. The German and
English patents wore litigated and held restricted to the use of
iron and its equivalent in substantially the 30 per cent amount
named. This is to say that in Germany and England the court
held that Welsbach was entitled to protection only on the iron
alloys. The United States courts have sustained the patent
much more broadly to include any cerium-containing materia
Oct.. 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
hardened with any alloyed metal to make the pyrophoric alloy.
When Baron Auer von Welsbach and his associates developed
the pyrophoric alloy business, they did not form separate com-
panies in each country, but centralized the manufacture of cer-
ium and pyrophoric alloy in the Treibacher Chemische Gesell-
schaft of Treibach, Austria (a part of the rare earth cartel or
trust). As stated above, they established branches of this Aus-
trian company, namely, the Treibacher Chemische Gesellschaft
in England, France, Russia, United States, etc., for the purpose
of alloying the metal to meet local requirements and selling the
alloy. It was not until some time after the first attack on
France that a pound of cerium was made anywhere in the world
outside of the Central Powers so far as I can learn, and then
such cerium was made by the New Process Metals Company,
which company operates under our basic patent on metallic
cerium. Therefore, to reiterate somewhat for the sake of clear-
ness, until the start of the European war the pyrophoric alloy
business of the world was operated as follows:
The German and Austrian rare earth gas mantle cartel or
trust turned over to the Treibacher Chemische Gesellschaft a
large part of their cerium residues, which the Treibacher Com-
pany made into metallic cerium. This metallic cerium the Trei-
bacher Company exported to its branches in France, England,
United States, etc , which branches alloyed the metallic cerium
with about 30 per cent of iron and other metals, and made the
alloy into small pieces, selling these pieces of alloy to the manu-
facturers of pocket lighters, miners' lamps, gas lighters, etc.
The business of marketing the small pieces of pyrophoric alloy
was protected by the patent under discussion which has been
contested, and, as stated, very broadly sustained in this country.
The American branch of the Treibacher Chemische Gesellschaft
was established about 1907, and handled all the pyrophoric
alloy business in this country.
After August 1914, the efficiency of the British Navy made it
impossible for the Treibacher Chemische Gesellschaft to deliver
cerium metal to its agency in the United States. They tried by
every means to secure cerium metal from Austria, even trying
to import it by the submarine Deutschland, but were unsuccessful.
In 1915 the American agency of the Treibacher Chemische
Gesellschaft got in touch with a chemical company in this coun-
try and tried to have this company produce metallic cerium for
them. The company, after working several months, was wholly
unable to do so. The president of this chemical company then
learned that I had secured my degree from the University of
Wisconsin as the result of experimental work on the electrolytic
preparation of metallic cerium, and engaged my firm to work
out a process for the commercial manufacture of this metal.
With me in our joint laboratories were associated my brother and
other assistants. After several months of intensive work in the
laboratory, metallic cerium was commercially produced of satis-
factory quality and in regular quantity, and thereafter the New
Process Metals Company was formed which manufactured and
sold this material. From that time until April 19 17 the New
Process Metals Company furnished metallic cerium to the
American branch of the Treibacher Chemische Gesellschaft
located in New York City.
In April 19 17 the manager of the American branch of the
Treibacher Chemische Gesellschaft formally notified t
Process Metals Company that he personally, doing business as
the American Pyrophor Company, had purchased the business
of the Treibacher Chemische Gesellschaft. From April until
December 191 7 the New Process Metals Company further furnished
metallic cerium to this manager doing business as the American
Pyrophor Company.
After war against Austria was declared, the propei 1
American Pyrophor Company, or the Treibachei Chemische
Gesellschaft, which ever you choose to call it, was taken over
by the Alien Property Custodian of the United States.
From the foregoing it is seen that the New Process Metals
Company developed the cerium business in America. From
shortly after the start of the war until the autumn of 1917 it was
the only company in the world, outside of the Central Powers,
making metallic cerium, and the pyrophoric alloy made from
this product supplied the needs of the armies and civil popula-
tions of Russia, France, England, South America, United States,
etc. In this connection, it is interesting to note that the cerium
lighters have been extensively used in the trenches, first because
of the great scarcity of matches in Europe, and second because of
the effect of dampness on matches We are glad to be able to
say that for several years prior to 1918 we supplied the British
and French armies with their requirements of pyrophoric alloy.
Now this metal, we understand, is being made in France.
The future of the pyrophoric metal business in this country
is an interesting field for speculation. We hope to be able to
maintain this business to some degree at least. Frankly, it is
our potential ability to market our alloy in the form of lighters
upon which we rely for the maintenance of our company and
it is our hope that our lighter facilities will become so economical
as to enable us to successfully meet Austrian competition after
the war.
THE FERRO-ALLOYS
By J. W. Richards, Professor of Metallurgy, Lehigh University
A large industry has grown up within the last 50 years, most
of it within the last 25 years, which furnishes to steel makers
alloys of iron with some of the rarer metals, in order to intro-
duce these rare metals into steel. Such alloys are known as
ferro-alloys, because they all contain iron (ferrum); some of
them, however, contain more of the rare metal than iron. They
were originally made in crucibles, cupolas, or blast furnaces, but
are now being made principally in electric furnaces, and their
manufacture is one of the principal electric furnace industries.
They are of great importance to the steel industry. The steel
maker uses them for one of two purposes: (1) As reagents to
take oxygen out of melted steel and thus ensure sound solid
castings (ferromanganese, ferrosilicon, ferro-aluminum) or (2 )
to put into the steel a small or large percentage of the rare metal
(ferromanganese, ferrochromium, ferrotungsten, ferromolybde-
num, ferrovanadium, ferrotitanium, ferro-uranium, ferroboron).
Let us discuss these two uses. Melted steel, just before taking
from the furnace, always contains some oxygen dissolved in it
(like the dissolved gas in charged soda water). If this is not
removed, the casting made is more or less unsound from cavities
or blow-holes. The addition of a small amount of an clement
or metal with a high affinity for oxygen removes this oxygen and
makes the casting sound. Manganese (1 per cent or less) is
the cheapest and most generally used reagent for accomplishing
this; silicon (Vs per cent or less) is more powerful but also
more expensive, and is often used to supplement the action of
manganese; aluminum (0.1 per cent or less) is still more power-
ful and still more expensive, and is used in very small quantities
k a final addition to complete the action of the manganese and
silicon. All steel makers use one, two or all three of these re-
agents; manganese and silicon in the form of ferro-alloys, alum-
inum more often as the pure metal, but ferro-aluminum is some-
times used.
The second use is to make special steels, that is, steels contain-
ing such quantities of the rare metal as give to them properties
different from plain carbon <lized by manganese,
silicon, or aluminum. Tims we may make manganese steel by
putting in [2 to 14 pet cent of manganese, making a very tough,
hard tee! act < is used in mining and grinding machinery,
burglar-proof vauH 1, eti ; 1 hromium (2 to 4 per cent) makes a
very hard tool steel; tungsten (15 to 25 per cent) makes high-
speed tool steel, which cuts iron while red hot; molybdenum (6
852
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
to 10 per cent) has powers similar to tungsten, and is also used
in steel for lining large guns. Vanadium ('/io to '/» Per cent)
makes a very strong steel which resists shock extremely well, as
when used for automobile axles; titanium, uranium, and boron
impart valuable properties not so easily described. Every one
of these materials is used for producing some specific result which
is not produced by any other; sometimes combinations of two,
three, or four are used in one steel, producing a particular com-
bination of special properties for some special purpose. Some
of these materials cost $5 per lb., and the special steels produced
cost up to $2.50 per lb., but their particularly valuable proper-
ties justify the expense. The value of these special steels to the
industries, and particularly for military purposes, is very great,
so great that the supply of ferro-alloys for their manufacture is
an important factor in winning the war.
FERROMANGANESE
This is the oldest of the ferro-alloys. Its manufacture was
begun about 50 years ago. It was first made in crucibles, had
for a long time been made in blast furnaces, but is now being
produced in many places in electric furnaces. It is made with
30 to 85 per cent manganese, 3 to 5 per cent carbon, a little
silicon, and the rest iron. The rich grades, 75 to 85 per cent,
are preferred by the steel maker, but they require rich manga-
nese ores for their manufacture. The United States has very
little rich manganese ore, but large quantities of low-grade ores; .
one of the present burdens of the steel maker is to use low-grade
ferromanganese, in order that we may not have to use ships for
importing the high-grade ores from Brazil.
The usual manufacture in blast furnaces is wasteful of both
fuel and manganese; the furnace must be run hot and slowly,
with very hot blast in order to reduce the manganese oxide ore
as completely as possible and not waste manganese in the slag.
Yet, in spite of all efforts, from 15 to 25 per cent of the man-
ganese going into the furnace escapes reduction and is lost in
the slag. This waste of fuel and manganese has led to the use
of the electric furnace, in which fuel is required only as a chem-
ical reagent and not to produce heat, thus saving about two-
thirds of the fuel requirements of the blast furnace, while the
higher temperature available causes the extraction of manganese
to reach 90 per cent, i. e., slag losses drop down to 10 per cent
or less. Against these economies must be set the considerable
expense for electric power and the smaller scale on which the
furnaces run. At the present high prices of coke and manganese
ore, and in view of the scarcity of manganese and the high price
of ferromanganese, the electric ferromanganese industry is able
to exist and make large profits. Whether it can do so when
normal conditions return, after the war, is questionable; it is to
be hoped that it will be able to do so, because of the economy
which it undoubtedly possesses in regard to fuel and manganese.
Steel producers use ferromanganese particularly for making
the low-carbon or soft steels, because they can thus introduce
the required manganese for deoxidation without putting in con-
siderable carbon. For higher carbon steels spiegeleisen (15 to
20 per cent manganese), a cheap blast furnace alloy, can be used,
and is being used at present wherever practicable, in order to
save ferromanganese. The best practice with either spiegeleisen
or ferromanganese is to melt them in a small electric furnace,
and tap from it the required weight to be added to the heat of
steel. The melted alloy mixes quicker with and reacts more
actively upon the melted steel, while less of it is necessary be-
cause less is oxidized by the furnace gases. The saving in man-
ganese by the use of the electrically melted ferro is alone suffi-
cient to justify the expense of melting it in an electric furnace,
while better and more homogeneous steel is produced.
FERROSH.ICON
This alloy may run 15 to 90 per cent silicon, but the most
commonly used is the so per cent grade. It is made from or-
dinary silica (quartz or sand), reduced by carbon in the presence
of iron ore or scrap iron. The blast furnace is able to make only
the lowest (15 per cent) grade, because silica (SiO*) is excep-
tionally difficult to reduce, and under conditions which would
reduce 99 per cent of the iron ore in a furnace, or 75 per cent of
the manganese ore, only 15 to 20 per cent of the silica present
can be reduced, and only a low-grade silicon alloy produced.
The higher grades must all be produced in the electric furnace.
The raw materials are ordinary silica, the most abundant
metallic oxide on the earth's surface, iron ore or scrap iron (iron
or steel turnings or punchings), and coke. Electric furnaces up
to 10,000 h. p. have been operated on ferrosilicon (50 per cent
grade). At the high temperature required, a not inconsiderable
proportion of the reduced silicon vaporizes, and burns outside
the furnace to a white silica smoke. This can be largely pre-
vented by skilful furnace supervision. In normal times, the 50
per cent alloy sells at S45 to $50 per ton, which is a low price
for an alloy so difficult to produce.
Steel producers use ferrosilicon principally for the great ac-
tivity with which the silicon removes dissolved oxygen from the
steel. It is about four times as active as manganese in thus
reducing blow-holes and producing sound castings. It is usual,
however, to use manganese first to do the bulk of the deoxida-
tion, and silicon afterwards, to finish up the reaction completely.
It is particularly useful in making sound steel castings which
are cast into their ultimate form and do not have to be worked
into shape, because a slight excess of silicon may make the steel
hard to forge or roll, whereas an excess of manganese does not
have so bad an effect on the working qualities. A particular
kind of steel called silicon steel carries 1 to 2 per cent of silicon
and yet forges well; this would be classed as a special steel.
The ferrosilicon industry has attained large proportions in
countries where electric power is cheap, particularly, therefore,
in Switzerland, the French Alps, Norway, Canada, and parts
of the United States. Under present conditions it is even prof-
itably run where electric power is relatively dear, as at Anniston,
Alabama, and Baltimore, Md. It is a large, interesting, and
rapidly growing industry.
FERRO-ALUMINUM
This alloy, with 10 to 20 percent of aluminum, was made in
the electric furnace and used in considerable quantity in steel
about 1885-88, but was displaced by pure aluminum as the
latter became cheaper. Aluminum is about 7 times as powerful
as silicon and 28 times as strong as manganese in acting upon the
oxygen dissolved in steel; therefore only minute quantities are
necessary, say 1 oz. or up to a maximum of 1 lb. of aluminum per
ton of steel. Its use gives the finishing touch to the deoxidation
of the steel.
About 1885 the Cowles Brothers, operating the first large
electrical furnaces run in America, at Lockport, N. Y., made and
sold considerable quantities of ferro-aluminum, selling the alu-
minum in it at the rate of about $2.00 per lb., while the pure metal
was then costing S5.00. When, a few years later, pure aluminum,
sold for 50 cents per lb., the steel makers turned to using the
pure metal instead of the ferro-aluminum, and at the present
time aluminum is so used in practically every steel works in the
world.
There seems to me a distinct opportunity for makers of ferro-
alloys to revive the manufacture and sale of ferro-aluminum.
Such great advances have been made in the construction and
operation of large electric furnaces since 1890, and so much
.experience has been had in reducing the difficult oxides to ferro-
alloys, that the production of 50 per cent ferro-aluminum at say
Si 00 per ton may be a distinct electric furnace possibility. That
would furnish the contained aluminum at about 10 cents per
lb., as aga nst 30 cents for the commercial aluminum now used.
The alloy should be broken up small before using and thrown in
the 1 unner or on the bottom of the ladle, in order that the melted
steel may quickly dissolve it as it runs into the ladle.
Oct., 1 91 8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
853
Such ferro-aluminum would require bauxite (aluminum ore)^
with iron ore or scrap iron for its manufacture, but there are
large deposits of low-grade bauxite rich in iron in Southern
France, which could be reduced directly to the alloy, without
any additions, and thus furnish very cheap raw material for the
operation.
In conclusion, ferro-aluminum is not now being made, but its
electric furnace production is a real possibility.
FERROCHROMIUM
Ferrochromium is used for making what is familiarly (but
erroneously) called "chrome steel." It makes steel exceedingly
hard. Very hard cutting tools, and armor plates to keep out
projectiles, are made of it. Only 2 to 4 per cent of chromium
may be used.
Several grades are made in the electric furnace, depending on
the per cent of chromium (25 to 75 per cent), and the content of
carbon (2 to 8 per cent). This alloy takes up carbon so actively
in the furnace that it has to be treated subsequently to remove
the carbon, down to what can be endured by the steel into which
it is introduced.
The raw material for its manufacture is a black ore known as
chrotnite, an oxide of both chromium and iron. If this is mixed
with carbon and smelted in the electric furnace, it reduces di-
rectly to ferrochromium alloy (often misnamed "ferrochrome"),
and highly saturated with carbon (6 to 10 per cent). Steel mak-
ers want lower carbon than this, so the alloy is re-melted in
another furnace, with more chromite, and the excess of carbon
oxidized out. The low-carbon alloy sells for 2 to 3 times the
price of the high-carbon crude material.
The cutting off of importations of high-grade chromite ore
from Asia Minor has led to intense prospecting in the United
States for chromite. Fair material has been found in many
places, and at present our country is nearly independent of for-
eign sources of the ore.
FERROTUNGSTEN
Tungsten (also called "wolfram") imparts curious and valu-
able properties to steel. A small amount (2 to 5 per cent) has
been used for half a century or more, to make the steel self-hard-
ening; that is, a tool of this steel need only be allowed to cool
in the air, and it becomes hard, without the ordinary quenching
or chilling operation. Larger proportions (10 to 25 per cent)
make a steel which stays hard even when red hot. A tool of
this material can be run so fast on a lathe, for instance, that it
gets red hot from the friction and work, yet keeps hard and keeps
on cutting. It is called "high-speed tool steel," and its use alone
has more than doubled the output capacity of the machine shops
of the world.
The ore used is either wolframite, a black oxide of iron and
tungsten, or scheelite, a white oxide of calcium and tungsten.
It is found in considerable quantities in Colorado, and some
other western states, and imports of this ore have not been
necessary during the war. In this respect we are much more
favorably situated than the European nations. A plentiful sup-
ply of tungsten ore may indeed be regarded as a large factor in
the production of cannon and fire arms and all kinds of machin-
ery, and therefore a considerable factor in winning the war.
FERROMOLYBDENUM
Molybdenum has only recently come into large use in steel.
Its action being somewhat similar to tungsten, scarcity of the
latter metal, particularly in Europe, has led to the manufacture
of fcrromolybdcnum on a comparatively large scale.
The ores are widely distributed but not very plentiful. Mol-
ybdenum sulfide, the mineral molybdenite, looks almost exactly
like shiny graphite, but it is a shade lighter in color and
twice as heavy. It occurs usually as flakes in granite rock, and
might easily be mistaken for graphite. Lead molybdate, the
mineral wulfenite, is a compound of lead and molybdenum ox-
ides, a yellow to red mineral very prettily crystallized in thin
square plates. It occurs abundantly in a few lead mines in the
West. It is usually first treated to extract its lead, and the
residue then worked for molybdenum. The sulfide used to be
roasted to molybdenum oxide, and this reduced by carbon in
the presence of iron ore or scrap iron in an electric furnace. It
is now smelted directly in the electric furnace with carbon and
a large excess of lime along with iron ore or scrap iron. Ferro
with 50 to 60 per cent of molybdenum is tapped from the fur-
nace like other ferro-alloys, but with molybdenum up to 80
per cent the alloy has such a high melting point that it cannot
be tapped out without freezing; it is necessary to make a fur-
nace full of this alloy and then let the furnace cool down and
take it apart, taking out a large mass of solidified alloy; the
furnace is then rebuilt.
The large use of molybdenum in steel has been so recent that
not much has been made public about it. Rumor says that
the large German guns (the "Black Berthas"), which bombarded
Liege, were lined with molybdenum steel (6 to 7 per cent)
to increase their resistance to erosion. It seems certain that
Germany drew considerable supplies of molybdenite from Nor-
way to compensate for shortage of tungsten for high-speed tool
steel. Parts of guns, gun carriages, motors, and automobiles
have also been made of molybdenum steel of most excellent
quality. Canada has been especially active in the manufacture
of ferromolybdenum, most of which it exported to Europe.
This alloy is therefore another preeminently valuable war ma-
terial.
FERROVANADIUM
Without vanadium the modern automobile or auto truck
would be a much weaker machine. When steel is desired to
withstand the heaviest shocks and vibration, nothing is quite
so effective as adding vanadium. This is another comparatively
rare metal, found principally in the radium ores of Colorado
and as a black sulfide on the highlands of Peru. The canary-
yellow Colorado ore is treated for radium, and the residues for
vanadium and uranium. The United States Government (Bu-
reau of Mines) operates this process for the radium supply.
The black ore of Peru is rich and unusual; it is a sulfide with
some asphaltic matter, and it is roasted and gotten into the
condition of iron-vanadium oxide before reduction. The oxides
are best reduced by metallic aluminum. Vanadium oxide plus
aluminum produces vanadium plus aluminum oxide slag. This
is the well-known thermit (Goldschmidt) method of reduction.
Electric furnace reduction by carbon is not advantageous be-
cause of the large amount of carbon taken up by the alloy;
powdered silicon is therefore put into the charge as the reduc-
ing agent, together with iron, lime, and fluorspar, and then a 30
to 40 per cent vanadium alloy is obtained with seldom over 1
per cent of carbon, a very desirable composition (R. M.
Keeney ) .
Only small amounts of vanadium are necessary in improving
the steel; 0.1 to 0.4 per cent are. the usual quantities. This is
fortunate, because the vanadium costs $5 per lb. and over.
Metallurgists suspect that part of the improvement of the steel
may be due to the vanadium combining with and removing
nitrogen dissolved in the melted steel. This is probably true,
yet some advantage undoubtedly must be ascribed to the final
vanadium content in the steel; both avenues of improvement
function. Steels thus treated are unusually resistant to shock
and alternate stresses, making them very useful for axles, cranks,
piston rods, and such severe service.
FERROTITANIUM
Titanium is an abundant element in nature. It occurs in
immense amounts as a double oxide of titanium and iron, known
as ilimuite, or titanic iron ore. This ore can be reduced directly
by carbon, in electric furnaces, to ferrotitaiiium. The reduc-
854
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
tion proceeds more easily if some aluminum is put in as a reduc-
ing agent, but this is expensive and unnecessary. The alloy
running 15 to 25 per cent titanium is sold for use in steel, as a
refining agent to remove oxygen and nitrogen, Thousands of
tons of steel for rails have been thus treated, the tests showing
considerable improvement in the mechanical properties by the
use of quite small amounts (o. 10 to 0.20 per cent) of titanium.
Only one firm in America makes this alloy, and its use in steel
has not yet gained universal approval.
FERROBORON
This is another alloy whose valuable qualities have not yet
been entirely determined. Roron is the metallic base of borax,
which is a sodium boron oxide. Borax is very difficult to reduce
to the metallic state. Another raw material, not so abundant,
is colemanite, containing lime and boron oxide. Many attempts
have been made, none very successfully, to reduce this with
iron oxide to ferroboron. The American Borax Company offered
a prize, for several years, for a process which would accomplish
this. Boron oxide occurs rarely in nature, but it can be
manufactured from borax and colemanite. When the oxide is
obtained, this can be combined with iron oxide and the resultant
boron-iron compound reduced by carbon in the electric furnace
to ferroboron. Small quantities of this alloy have thus been
manufactured.
Experiments on steel have shown that ferroboron acts some-
what similarly to ferrovanadium. Experiments in France showed
remarkably strong and tough steels were thus made, using 0.5
to 2 per cent of boron. The results have not been properly
followed up, partly on account of the difficulty in getting ferro-
boron ; no one, as yet, has taken up its regular manufacture, and
steel makers can hardly be blamed, in these stirring times, for not
having as yet thoroughly explored its possibilities as an addi-
tion to steel.
FERRO-URANIUM
This is the latest of the ferro-alloys to enter the lists. Uranium
is a very heavy and, chemically, very active element. It is
found in small quantity as a black oxide, the mineral pitch-
blende, the mineral in which radium was first discovered. It is
found more abundantly in the Colorado radium ore, a bright
yellow oxide and silicate of vanadium, uranium, and lime. After
extracting the radium and vanadium, the uranium remains in
the residues as a by-product, usually as a soda-uranium com-
pound. This is treated so that uranium oxide is obtained, and
this can be reduced by carbon in an electric furnace in the pres-
ence of iron ore or scrap iron, to ferro-uraniutn (30 to 60 per
cent). The recovery of uranium is not high (50 to 70 per cent),
the rest being lost in the slag. Mr. R. M. Keeney has recently
described these processes in detail, for the first time, in the
August bulletin of the American Institute of Mining Engineers.
The results of tests showing the influence of uranium on steel
arc not yet completely known. Some firms have claimed for it
wonderful strengthening power and resistance to shock. The
subject is now receiving expert attention from steel makers and
valuable results arc confidently expected.
CONCLUSION
The ferro alloys are exceedingly important materials to the
steel maker, either in the making of ordinary steel or for pro-
ducing special alloy steels. They are indispensable to the steel
industry. They are important factors in producing both or-
dinary and tine steels, and therefore in winning the war. The
country well supplied with them has a great advantage over the
country in which they are scarce. They are deserving of all the
expert attention which they are receiving from the War Indus-
tries Board, the steel makers, and the economists. The posses-
sion by the United Stales of large supplies and resources in the
ferro-alloys line will be one of the important factors in determin-
ing the quick ending of the war.
SYMPOSIUM ON INDUSTRIAL ORGANIC CHEMISTRY
September 28, 1918
ADVANCES IN INDUSTRIAL ORGANIC CHEMISTRY SINCE THE
BEGINNING OF THE WAR
By Samuel P. Sadtler
Consulting Chemist, Philadelphia
Many ordinarily intelligent people with no special acquaint-
ance with scientific matters will confess to having had the belief
that the United States had no established chemical industries
at the outbreak of the present great world war, or if we had
any, they did not cover the field of what is known as organic
chemistry. Organic chemistry was to them the field of coal-tar
dyes and synthetic medicines, and was not this the peculiar and
exclusive domain of the German chemical manufacturer? We
rather think that this expresses the actual knowledge on the
subject on the part of our non-scientific newspaper and maga-
zine writers at the outbreak of the war.
However, the elements which go to favor the establishing of a
chemical industry are a wealth of raw materials and a market
for the manufactured product, and with these the cooperation
of intelligent chemical effort and capital. All four of these
elements existed in the United States and the result of their
cooperation had already been quite effective long before the
beginning of the war in giving us flourishing chemical industries
based upon organic raw materials and involving applications of
organic chemistry. When we recall the great wealth of this
country in petroleum and asphalt, in all varieties of coal, in vege-
table and animal oils and fats, in cereals of all kinds, and in
fibers of indispensable character, we would be surprised if flour-
ishing chemical industries had not been established.
Let us briefly view some of these industrial organic develop-
ments as they existed prior to 1914.
The American petroleum industry easily ranked as the first
in importance in supplying the world with the various products
of mineral oil.
Of a total annual world's production in 1914 of over 400,000,-
000 bbls., the United States produced 265,762,000 bbls., or just
about two-thirds, while Russia, the next in rank, produced
67,000,000 bbls., or 16.7 per cent of the total amount.
But it is not only the raw material production that is to be
considered. By far the larger proportion of this crude oil was
refined in the United States and from it were made gasoline,
kerosene, lubricating oils in great variety, paraffin and paraffin
candles, vaseline and similar products. These products were
not alone for the American market but went all over the world.
We also had a great and well-developed industry in the
extraction, refining, and working-up of vegetable and animal
fats and oils. A peculiarly American industry was the cotton-
seed oil and cake industry. Hundreds of mills throughout our
southern states were devoted to the crushing of the seed and
the preparation of the cake, while the refining of the oil and the
making of the finest edible products were carried out in large
plants. The enormous production of lard and lard oil by our
great packing companies and the preparation of oleo oil for
foreign shipment was also an important and well established
American industry. As a side product, the extraction and re-
fining of glycerin had also become well established and the
American soap industry was also well developed and a large
export business already inaugurated.
The utilization of linseed oil for paint oils and in the manu-
facture of linoleum and oil cloth had also reached a high devel-
opment at tin- hands of American technologists.
The great naval stores industries involving the production and
utilization of American turpentine and rosin had also been well
developed auel many minor chemical industries based upon
them. America was also one of the largest consumers in the
world of rubber, and thanks to the manufacture of all classes of
rubber and water-proofed goods and to the utilization for automo-
bile tires, the working of rubber had been extensively developed
Oct., 1018
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
855
The refining of sugar, in part produced in the United States
and the neighboring West India Islands, and in part from im-
ported European raw beet sugar, had become an extensive
industry with the most modern of plant equipment and under
scientific chemical control.
As America is in large degree the granary of the world in its
production of cereal foods, we had large chemical industries
already occupied with the preparation of the special classes of
food products of cereal origin. One of the best instances of a
distinctively American industry developed from American ma-
terial is the corn products industry. From the maize or Indian
corn is produced corn starch for food purposes, and for technical
purposes, glucose or commercial dextrose, corn or maize oil, and
commercial dextrines. This industry has been developed from
a distinctively American cereal and on lines quite peculiar to it
as an industry of American growth.
Turning to the textile industries, we have as an American
production, one of the world's most useful fibers, viz., the cotton
fiber. I have already referred to its peculiar by-product, the
cotton seed, and its utilization. However, we have many im-
portant industries utilizing the cotton fiber in which its bleach-
ing, dyeing, and other treatment are controlled by accurate
chemical knowledge and practice.
The textile industries using wool and silk as well as cotton
have also attained a high development in the United States and
the chemical side involving the cleansing and after-treatment of
the fibers has been thoroughly worked out.
The products of destructive distillation remain to be spoken
of. Our American wood distillation industry will be specially
presented by another speaker during this Exposition and so I
will pass this by. Coal distillation for gas making had been
practiced by the most accurate scientific methods and great
varieties of special gas-making processes had been developed.
It will be remembered that the Lowe water-gas process was an
American invention which has been copied and adopted since
in various other countries. However, we were slow to discard
the old wasteful beehive oven for coking of coal for by-product
ovens which collect the valuable residuals including gas, tar,
and ammonia. The production of coal-tar crude ingredients
was therefore only moderately developed and of what we term
the 'intermediates" for the color industry hardly at all.
An American dye color industry using imported intermediates
therefore existed, but it existed under difficulty and played but
a subordinate part in supplying the American market with the
dyes required for our textile industries.
This brief survey shows that it is a great mistake to assume
that there were no organic chemical industries existing in this
country in 1914 at the outbreak of the war. Nevertheless, the
general public knew little of the chemist and his actual or poten-
tial value to industry or commerce. Capital, which frequently
made large investments in mining and similar enterprises, many
of which were largely speculative, had not made the acquaint-
ance of the chemist to any notable extent, perhaps because the
language of chemical reactions was something foreign to its
experience or training and hence distrusted. The war came and
we soon learned how great a disturbance such a great war could
be to the world's commerce in which the United States played
a vitally important part. We also learned promptly how chcm-
ical industries were the foundation stones for this great com-
merce. It soon developed that war in its modern form was
based upon the chemical activity and scientific development of a
country and then the chemist began, as it has been repeatedly
said, to come into his own.
Our special topic therefore is to note briefly how our American
chemical industries, and in particular those involving organic
chemistry, have responded to this war impulse and demand in
the four years that have elapsed since the beginning of the war
in I'm 1
Our petroleum industry, which we have shown was already in
a highly developed state, had important problems at once pre-
sented to it. Great as was our refining capacity, it was utterly
inadequate to produce in normal course the quantities of gaso-
line that were required. Besides the growing automobile con-
sumption, the war demands for motor trucks and for aeroplane
and tractor engines came as an added load on the industry.
Because of the demoralization of the Russian oil production and
the German occupation of Roumania, the whole gasoline supply
for the allied nations has to come from America. To meet this
demand we have in addition to what may be called "straight
refinery" gasoline, blended ' 'casing head" gasoline and "cracked"
gasoline. Under the pressure of the great demand, large quan-
tities of volatile hydrocarbons are washed out by suitable sol-
vents or condensed out of natural gas and then blended with
heavy naphtha to bring down the gravity to a proper average.
Such a gasoline will necessarily have a wide volatility range,
but is available for most uses that the normal refinery gasoline
is. Most of the areas producing natural gas are available for
this gasoline extraction but it has developed particularly in
West Virginia, in Oklahoma, and in California. It is furnishing
a rapidly increasing amount of gasoline yearly. The third source
of gasoline mentioned is from special cracking processes and it
is this class of processes which have been attracting the most
interest and giving the greatest promise of large results. The
whole subject was discussed from a theoretical and historical
point of view in Bulletin 1 14 of the Bureau of Mines by Rittman,
Dutton, and Dean. Since the date of that publication in 19 16,
a great deal additional has been published in the journals and
much has been done in a practical way. The Burton process
adopted by the Standard Oil Company is now in operation on a
large scale in several of the largest refineries of that Company;
the Rittman process has been tried on a working scale, although
not yet developed to a final form for large scale production; the
McAfee process of decomposition in the presence of aluminum
chloride as catalyst has been developed by the Gulf Refining
Company, and the Snelling process has also been brought for-
ward. That heavy petroleum oils can be cracked So as to pro-
duce much light oil or gasoline is beyond question, but the prob-
lem is to avoid the production of large proportions of unsaturated
hydrocarbons which require acid treatment in the product.
McAfee claims to avoid this production of unsaturated com-
pounds and that his gasoline requires no acid treatment, but
the success of his process is dependent on the economical recovery
of the anhydrous aluminum chloride available for use. Enor-
mous quantities of other special petroleum products have also
been called for by reason of war demands, such as high-grade
lubricating oils. I had brought to me for testing some time
back a "recoil oil," required by the Government for use with
heavy guns, which with a high viscosity had to stand a cold test
of-5°F. (— 2o°C.).
Then the demands of the English and the United States Navy
for fuel oil has drawn upon the Mexican oil fields, as well as those
of Louisiana and Texas, and pushed production to the maximum.
Meanwhile a new raw material has been brought to notice
that is capable of adding enormously to our available petroleum
supplies in the oil shales of Western Colorado and Eastern Utah,
the deposits also being found to some extent in Nevada, Wyom-
ing, and Montana. These shales readily yield by distillation a
crude oil capable of furnishing gasoline, kerosene, and paraffin
and in addition large amounts of ammonia, so that sulfate of
ammonia may be obtained as a by-product. In Bulletin 691 -B
of tin- United States Geological Survey, D. K. Winchester has
dea ribed this occurrence and jives records of distillation. These
shales arc said to be lilo the Scotch shales but richer in oil.
With the gradual exhaustion of the oil fields they will prove a
welcome addition,
The vegetable and animal oil markets have been greatly
856
THE JO-URN A L OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
affected by the war and the industries based upon them have
been changed in a revolutionary way in many cases. The first
cause may be said to have been the export embargo established
Ijv Great Britain upon all glycerin-containing oils with the be-
ginning of the war. Following this came a shortage in the
cottonseed crop in 1915 and the introduction of soy bean culture
in the South. As the refined cottonseed oil took more and more
the position of an edible oil, commanding correspondingly higher
prices, the soy bean oil took its place for industrial uses, for soap
and paint manufacturers, and as a constituent of compound
lard and oleomargarine. The soy bean cake has also been
readily taken up for stock feed and for fertilizer. The soy bean
contains more protein than either cotton seed or peanuts, as
much fat as cotton seed, and only one fourth as much fiber as
cotton seed or peanuts.
It has a lower iodine number than linseed oil and is slow in
drying, so that it cannot completely replace linseed oil in the
paint industry but can be admixed with it. Besides the pro-
duction in the South, which according to Government reports
in the year 191 7 was from 531,000 acres, we have had an enor-
mous development of the soy bean oil importation as the follow-
ing figures will show. Importation for year 1914, 12,500,000
lbs.; for 191 7, 264,900,000 lbs.; and for 1918, 336,824,646 lbs.
Most of this coming from Manchuria enters Seattle and other
Pacific coast ports. All available storage facilities at Seattle and
other coast points have been overtaxed in the handling of this
supply.
Another great development in oil supplies has come from the
greatly increased production of peanut oil. This has come to
the fore as a salad oil and for soap making. The crop in the
United States rose from 3,500,000 bu. before the war to
40,000,000 bu. in 19 16. For 1917, the Government reports show
that 3,277,000 acres were devoted to its culture in the South,
and for the year of 1918 it is estimated in the state of Texas alone
3,000,000 acres will be devoted to it. The importations have
also increased sixfold since 1914, now amounting to over 8,000.000
gal.
A year ago we had no castor beans grown in this country to
speak of, to-day we have at Government instigation hundreds of
thousands of acres devoted to it in Florida and elsewhere and the
product contracted for by the Government. As illustrating the
greatly increased demand for oils capable of yielding food prod-
ucts we may also note the remarkable growth in the coconut
oil and copra importations. In 1914 the importations of coco-
nut oil amounted to 74,386,213 lbs , in 1918 it had grown to
289,194,853 lbs.; of copra for the expressing of coconut oil we
imported 45,437,155 lbs. in 1914 and in 1918, 486,996,112 lbs.
Similar changes have taken place in the fish-oil markets with
the decrease in the menhaden catch due to the commandeering
of fishing boats and scarcity of men to man them Through our
Pacific ports chiefly are imported quantities of dogfish, hali-
but, salmon, sardine, shark, tuna fish, candlefish, and walrus
oils, largely new to the market, while whale oil, seal oil, and por-
poise oils are again appearing in large quantities. These fish
oils have moreover an added value as sources of supply since
■the general application of the hydrogenation process whereby
they can be changed into hardened fats without offensive odor
and of the greatest value as soap stock and for glycerin pro-
duction.
With regard to the increased production of glycerin because
of the war demand I have no figures, but it has been very great,
SO that the use of glycerin in pharmaceutical preparations has
been discouraged in order to conserve the glycerin for nitro-
glycerin production and for export to our allies, 21,000,000 lbs.
having been exported in 1918.
In the field of essential oils there are a few items of interest
to note. With the Study of wood turpentines as distinguished
from gum turpentine it has been recognized that spruce-wood
turpentine, now a waste product of the sulfite process of making
paper pulp, has a peculiar composition. It consists largely of
one aromatic hydrocarbon, cymene (iso-propyl-methyl-benzene ).
On subjecting this to the Friedel and Crafts reaction with alu-
minum chloride in the presence of an excess of benzene, toluene
and cumene (propyl -benzene) are formed. The toluene is read-
ily converted into TXT (trinitrotoluene) and the cumene
may be oxidized directly into benzoic acid. The work as re-
ported in This Journal for May 1918 is still in a purely exper-
imental stage but it has much promise.
One of the newer uses of essential oils which has particularly
stimulated the production in the last few years of pine oil in
the South is for the ore flotation process. The concentration
of both copper and zinc ores in the United States as in other
parts of the world is now effected by agitating the finely pulver-
ized ore with water in the presence of a small quantity of oil.
While fatty oils, mineral oils, coal-tar and wood-tar creosotes
have been used, certain essential oils have been found to be
specially adapted for this treatment. In this country pine oils,
both steam-distilled and destructively distilled have been espe-
cially used and quite an industry in these oils has developed.
The magnitude of our copper and zinc production is such that
although the amount of oil used in this flotation is relatively
small (less than 1 per cent on the ore) the aggregate consump-
tion of oil is very' large.
The war demand has greatly increased the call for rubber
goods of all kinds, especially automobile tires, and consequently
the consumption of crude rubber has grown rapidly. The im-
portations of rubber in 1914 amounted to 132,000,000 lbs. but
grew to 390,000,000 lbs. in 191 8. The exports of rubber boots
and shoes amounted to Si, 113,495 for 1914 and to 55,774,341
in 19 18; the automobile tire exports were valued at $4,068,639
in 1914 and at $15,128,294 in 1918.
In this connection reference may be made to the greatly in-
creased demand for organic solvents and the work done to meet
this demand. The most important work of this kind is prob-
ably the production of acetone and similar solvents from the
Pacific Coast kelp by the Hercules Powder Company, and this
fortunately we will have specially presented at this time in a
paper dealing fully with the subject.
Another promising line is the manufacture of amyl acetate
from petroleum pentane recently described in This Journal.1
This work has been carried out at the Mellon Institute in Pitts-
burgh, Pa. The use of these organic solvents is manifold, but
we may note the extensive use of pyroxylin solvents and the
greatly increased use of lacquers of this description in the last
four years. From aeroplane wing dope to artificial leather we
have a variety of utilizations and some of these have grown to
extensive industries within the past few years.
Closely allied to this industry is the artificial silk industry,
one variety of which is made from a nitrated cotton or pyroxylin.
Besides this variety we have the viscose variety, the cellulose
acetate, and the cuprammouium artificial silk. The develop-
ment of these products has been very great in this country in
recent years, both for films and for artificial silk as a fiber in-
creasingly used in the textile trade.
Industrial alcohol production has developed greatly in the
past few years and numerous new plants have been established
for its production from a variety of sources. Much attention
has been given to a revival of the Classen process for hydrolyz-
ing the cellulose of sawdust and fermenting the sugar produced
therefrom. I have no reliable information, however, as to whether
the difficulties which developed when it was first tried in this
country some years ago have been sufficiently overcome to make
it a dependable manufacturing process although it has attracted
much newspaper attention. More reliable are the processes
based upon the use of low-grade molasses and cereals of various
• This Jchrnal, 10 (1918). 511.
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
857
kinds and a large production, at present taken over by the muni-
tion manufacturers, has been the result.
In addition to this direct war use much alcohol is made for
denaturing and use in the manufacture of pharmaceutical prod-
ucts. Some 27 denaturing formulas have been allowed by the
United States Internal Revenue Office and these adapt it for use in
a wide variety of cases where tax-paid pure alcohol is inadmissible
on account of its cost. This form of utilization is not of tem-
porary character as is the use in munitions manufacture, but is
destined to grow and require an increasing amount of alcohol
properly denatured.
We come now to the industry which may be said to be the
touchstone of our ability to achieve results under difficult con-
ditions when confronted with an imperative necessity, viz., the
building up on American soil from American raw materials with
American capital and American chemical effort an independent
dyestuff industry. In speaking of the conditions in the United
States in 1914, I said that we had a small dyestuff industry,
working under trade difficulties, for the most part with imported
intermediates. There were, to be exact, five manufacturers,
large and small, of dyestuffs in 1914. The tariff census of coal-
tar products, as reported for 191 7, shows that there were at that
time in the United States 81 establishments engaged in the
manufacture of coal-tar dyes and 117 firms manufacturing inter-
mediates. While these figures are striking and cannot fail to
arrest attention, it is only when we look more fully into the
details that we get an adequate understanding of the great in-
dustrial achievement that has been wrought in the last four
years.
First, as to our dependence upon foreign sources, chiefly Ger-
man, for our dyestuffs at the beginning of the war in 1914: we
were then making in this country a bare one-fifth of our needs
out of foreign materials and had neither crudes nor intermediates
to speak of. Dye imports from Germany in 1914 were valued
at $5,965,537; in 1916 they were valued at $849; in 1917 at
$464,499; and in 1918 at $3,048. The relatively large amount
for 1917 represents shipments held at first in Great Britain but
released later on appeal. Do we still import any dyestuffs?
Yes. There are two reasons for importing, from Switzerland
a:nl Great Britain mainly, certain dye colors.
The new American dye industry did not at once attempt to
duplicate the 900 or more supposedly distinct synthetic dyes of
the German dealers, but took up the most important classes and
produced a moderate number of representative dyes covering
as far as possible the coloring or tinctorial needs of the textile
trade, and some of the finer shades are still missing, hence the
Swiss importations.
The other reason and perhaps the more important one was
that Congress, in the enactment of our present tariff law, cut
off the ad valorem duty on indigo and alizarine products, which
caused manufacturers to leave the production of these very im-
portant products until they had covered the need in the other
groups more fully.
However, synthetic indigo of American manufacture is already
on the market and there will be three sources of supply for it in
1918, one of which promises to supply at least one-half of what
the American trade will need for the year. Similarly artificial
alizarine of American manufacture, made in Brooklyn, X. V.,
will be available in large quantities from this time on.
Meanwhile approximately three-fourths of the dyestuffs
heeded are being produced and some colors in such quantity
that an export trade has been started. Let us note that for the
year ending June 1916 the exports of all varieties of dyestuffs,
aniline dyes, logwood extract, and all others totalled $5,102,002
in value, but the bulk of these wire vegetable colors. In i9'7.
the valuation of the exports had leaped to Si 1,709,287, with an
increasing amount of such colors as sulfur black and the simpler
aniline colors. In 1918, and this shows the quality as well as
quantity of development, the total exports of dyestuffs were
valued at $16,92 1,888. Of this, total aniline colors make $7,298,-
298, logwood extract $2,339,480, and all other $7,284,110. It
will be noted that the aniline colors alone exceeded in value the
dyestuff importations from Germany in 1914.
But the main market for which these dyes are being made,
and for the permanent relief of which a great American industry
has been created is the United States market and the way in
which this has been done is deserving of a more detailed exam-
ination.
1 With the shutting off of the foreign sources of supply in 1914,
not only was the need of an American dye industry made clear,
but the manufacture of munitions and the filling of foreign orders
for the same called for coal-tar products. The manufacture of
phenol, of picric acid, and of trinitrotoluol all demanded an im-
mediate supply of coal-tar crudes. So the gas works, the by-
product coke ovens, and the tar distillers all united to increase
and intensify production. I need only refer to the lists of such
great companies as the Semet-Solvay Company, the United Gas
Improvement Company, and the Barrett Manufacturing Com-
pany as illustrating the achievements in this production of coal-
tar crudes. For the increased production of benzol and toluol
the Ordnance -Division of the War Department has also started
to establish plants for by-product coal distillation because of its
special needs. However, for the dyestuff manufacture we go
from the coal-tar crudes to the "intermediates." Some of these
require very special apparatus for their manufacture and it was
these that had not been made in this country prior to 1914.
Our chemical apparatus manufacturers (several of whom are
very well represented in this exposition) responded to the call
for this apparatus and gradually these important products,
mostly new to American trade, were supplied. The tariff cen-
sus of 1917 states that the production of intermediates for that
year was contributed to by 117 firms and that the production
amounted to 322,650,531 lbs. valued at $106,942,918.- These
figures, however, involve considerable duplications because of the
use of some as the starting point in making others. That the
amounts of many are very large is, however, shown by the state-
ment published by the National Aniline and Chemical Company
that their Marcus Hook works has a producing capacity of an-
iline oil five times as great as the total consumption in this
country prior to the war, and that this company is now the
largest producer of aniline oil in the world.
The cooperation of producers of coal tar and its "crudes"
with the manufacturers of "intermediates" and the dyestuff
manufacturers was obviously a very desirable thing in the build-
ing up of the new industry and establishing it on a firm founda-
tion. Such cooperation has been planned in the organization of
our largest American dye manufacturing company. As they
announce in their statement, "the various plants of this com-
pany are engaged in producing everything necessary for dye
manufacturing, commencing with the basic raw materials or
'crudes' derived directly from coal with the acids and other
chemicals converting these crudes into dye 'intermediates,'
which arc also used for explosives and the manufacture finally
of the several classes of dyes demanded by the industries."
In this combination we have the Semet-Solvay Company,
the Barrett Manufacturing Company, the General Chemical
! 1 roductS Company furnishing ''crudes"
and "intermediates," and the Schoellkopf Aniline and Chemical
Works, Buffalo, N. Y., the \V. Beckers Aniline and I
Works, Brooklyn, X.Y., the Century Color Corporation, Nutley,
N. J., and the Standard Aniline Products Company, Wappingcrs
Palls, X v., producing "intermediates" and finished "dye
colors." All the raw materials are the product of American fac-
tor* as well as the finished products.
The "infc 1 mi diati 1" listed by the National Aniline and Chem.
858
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. 10
ical Company amount to 58 distinct substances and the dyes
named to nearly 200.
Other of our American color manufacturers have additional dis-
tinctive dye colors as well as many which are the equivalents
of those in the list referred to — truly a satisfactory showing for
what is practically a newly created industry at the end of the
fourth year since the start was made.
The Tariff Census of 1917 before referred to makes the fol-
lowing statement:
The annual production was reported for the following groups
of products made in whole or in part from material derived from
coal tar; 45,977,246 lbs. of dyes valued at $57. 796,027; 5.092,558
lbs. of color lakes valued at $2,764,064; 2,236,161 lbs. of medicinal
chemicals valued at $5,560,237; 779,416 lbs. of flavors valued at
$1,862,456; 263,068 lbs. of photographic chemicals valued at
$602,281 ; and 19,545 lbs. of perfume material valued at $125,960.
Of course the manufacture of munitions begun on allied ac-
count and continued later by the Ordnance Department on our
own account, means the production of numerous organic com-
pounds on a scale totally beyond any previous experience.
Picric acid, trinitrotoluol, nitrocellulose and nitroglycerin for
smokeless powder, fulminate powders, and other preparations
are manufactured by tons, but as this is a war industry and not
one that will continue, we have omitted it from our discussion.
CONCLUSION
What is the outlook for industrial organic chemistry in
the immediate future in this country? I would say that
it is most encouraging. The exigencies of the war in Europe
have caused a widespread search for independent sources of raw
materials and with very satisfactory results in many cases. Our
large corporations have established research laboratories with
the best up-to-date equipment and have planned real and thor-
oughgoing research in a broad intelligent spirit which does not
ask for hasty results but emphasizes the wish for thoroughness.
Our Government has recognized in a very satisfactory way its
need of chemical service and has thus publicly endorsed the
fundamental importance of the chemist in industrial achievement.
Capital has come forward willingly in support of properly planned
chemical undertakings and thus made the establishment of new in-
dustries possible in a way far beyond what had been possible before
the war period. Lastly, the disturbed condition of all European
trade relations has made it possible for the United States to
inaugurate very promising export business in quarters not pre-
viously practical or only so under conditions distinctly unfavor-
able.
These new achievements we have every reason to expect to
continue in future and no doubt with added momentum.
SOLVENTS FROM KELP
By C. A. HlGOtNS, of the Hercules Powder Company
The serious shortage of acetate of lime and its derivatives is
now causing solvent users considerable anxiety. The past four
years have seen a tremendous increase in the demand for ace-
tone, acetic acid, acetic anhydride, etc., for purely war purposes,
and this has caused a corresponding diminution in the quantity
available for commercial uses. Since the war, acetate of lime
has increased to three or four times its normal pre-war price,
and its solvent derivatives such as acetone, ethyl methyl ketone,
acetone oil, acetic acid, ethyl acetate, etc . have advanced cor-
respondingly.
Considerable interest has accordingly been shown in the huge
kelp or seaweed fermentation plant built and now being operated
by the Hercules Powder Company on the coast of Southern
California, where acetone, ketones, and a long Hue of acetate
derivatives air being obtained from kelp. This factory, so
far as I know, is the only one of its kind in existence, Tin
data are therefore rather limited and resolve themselves into a de-
scription of the methods and results obtained at this factory by
the Hercules Powder Company.
You will realize, therefore, there is no historical background
to the manufacture of solvents from kelp. There is, however,
record of experiments carried out by Stenhouse in the year 1851,
when he produced acetate of lime by allowing kelp to ferment
under suitable conditions. While his experiments as re-
corded in the Philosophical Magazine and Journal of Science did
not have any immediate practical application, they contained
the germ of an idea which found manufacturing expression about
the year 1915.
The attention of potash users was rather focused at this time
on the huge beds of perennial kelp which stretch along the
Pacific coast. About this time, too, the Hercules Powder Com-
pany needed acetone, and needed it from an entirely new source.
We needed it to make smokeless powder for the British Govern-
ment. Experimental work was immediately started on the pro-
duction of acetate salts by the fermentation of kelp. Shortly
afterwards ground was broken for a factory capable of producing
acetone and ketones from kelp at the rate of about 3 to 4 tons a
day with potash and iodine as valuable by-products.
The Hercules process of producing solvents and their inter-
mediates from kelp is really very simple. The kelp is mowed
and garnered from the marine beds by special harvesting boats.
It is then macerated and pumped to the tank at the factory on
shore, where it is diluted and allowed to ferment at about 90° F.
with the addition of finely ground limestone to neutralize the
acids formed in the fermentation. After a period of about 15
days, the leafy structure of the kelp has been entirely destroyed
and a liquor is obtained containing chiefly acetate of lime,
muriate of potash, and iodides in solution. The crude salts
recovered therefrom by evaporation are heated in retorts to
obtain acetone and the muriate of potash is recovered by leach-
ing and crystallization.
That is the process in its essentials and stripped of all its
details. A glance at the products chart (page 833) will show,
however, that a great many new and additional products have
been isolated. In addition to the acetone, ketones, potash, and
iodine already referred to, the higher acids of the acetic series
are also being produced, together with their ethyl alcohol esters.
The fermentation of kelp by the Hercules method is produc-
tive, therefore, of not only acetate salts, but also of propionates,
butyrates, valerates, and even of the higher acids of this series.
It is this series of salts which by conversion into their ethyl
esters is providing the trade with an entirely new source of
ethyl acetate and an entirely new series of amyl acetate sub-
stitutes in the ethyl propionate and ethyl butyrate, which latter
have never before been made in commercial quantities for the
solvent trade.
The principal solvent product of a kelp fermentation plant
along the lines developed by the Hercules process must neces-
sarily be acetone and the higher ketones. This is explained by
the fact that the bulk of the salts obtained in the evaporation
of the fermented kelp liquor already mentioned consists of a
mixture of acetate of lime and muriate of potash. By far the
simplest and most economical way of separating this mixture
or realizing the values of both salts is to heat the mixed salt in
retorts. Acetone is thereby obtained, and muriate of potash
and calcium carbonate is left behind as residue. The potash
is leached from the insoluble calcium carbonate and recovered
by crystallization.
In the process of concentrating the fermented liquor, however,
a scum collects on the surface of the liquid. This scum con-
sists of a mixture of calcium acetate, propionate, butyrate. \ .il-
. all of which are less soluble in hot than in cold solu-
tion. This scum holds very little of the potash ami can accord-
ingly be used in the manufacture of solvents such as esters,
where the recovery of any residual potash salt would be difficult.
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
8 59
Use is therefore made of this scum or "taffy," as it is called by
the workmen on account of its plastic nature when hot, in the
manufacture of solvent esters which are in such demand in the
soluble cotton and lacquer industries. The taffy is mixed with
ethyl alcohol and sulfuric acid and the resultant esters separated
by fractionation.
A word now as to the nature and uses of these solvent esters.
Ethyl acetate is an old friend among us. Its use as a solvent
of soluble cotton or nitrocellulose in the manufacture of imita-
tion leather, in finishing celluloid, and in a thousand and one
other directions are too widely known to need mention. Ethyl
propionate and butyrate are not so widely known. Several in-
vestigators have mentioned their excellence as solvents for nitro-
cellulose gums, resins, etc. Worden, in his "Nitrocellulose In-
dustry" mentions this fact and states that the only bar to their
use is the high price, or that they are not commercially obtain-
able. Ethyl propionate boils at 100° C. and appears to resemble
in its properties a mixture of ethyl acetate with about 10 to 20
per cent amyl acetate. Ethyl butyrate boils around 1200 C.
and resembles amyl acetate very closely in its physical prop-
erties. These two esters now produced for the first time in
large quantities will doubtless find wide application in the sol-
uble cotton celluloid, artificial leather, paint and varnish
trades, where neutral solvents of pleasant odor and possessing
a moderately slow rate of evaporation are desired. The use of
these esters is also contributing materially at the present time
to the War Industries Board's program for the conservation of
acetate of lime
Special mention might be made of the valerates, caproates,
etc., which are now being isolated in this process. Valerian and
its salts and esters are well known to the drug and pharmaceu-
tical trade, to whom a new source at this time will be welcome,
while the esters of these acids will doubtless be much sought
after by the essence and perfume trade.
The kelp industry is in its infancy, and although somewhat of
a war baby, it has in it the makings of a vigorous adult. Her-
alded as the savior of potash users, it has come to the aid of
users of high-grade solvents and pharmaceuticals, and bids fair
in the future to continue to develop new and valuable organic
chemicals.
WOOD WASTE AS A SOURCE OF ETHYL ALCOHOL
By G. H. Tomlinson
Manager, Kinzinger Bruce and Co., Ltd., Niagara Falls, Ontario
For some years we have been hearing more and more regarding
waste wood as a source of ethyl alcohol. The amount which is
thus being made, however, is still but a fraction of the nation's
supply and within the past few years has not been extended,
irrespective of the great and increasing demand which the war
has developed.
It may be advanced that sufficient capital is available and
competent technical skill can be secured and if the proposition
is therefore all that has been claimed, the question naturally
occurs, why has more rapid progress not been made? Is the
proposition fundamentally unsound or does it still offer the very
considerable possibilities which have been predicted?
We all realize the distance to be traveled between the discov-
ery of a chemical reaction and its successful commercial develop-
ment and application. In this case, as a matter of fact, 100
years have already elapsed. The pitfalls to be crossed, both
technical and commercial, are legion, and the more unusual,
attractive, or revolutionary the proposition may be, the more
difficult may its pathway become. Premature development and
extravagant or unsound exploitation can prostitute an under-
taking, no matter how promising it may be, and when this occurs
in connection with a process, which has not been already estab-
lished, disaster is invited.
I think I may safely say that such a condition of prostitution
represents the present status of this particular industry, and
explains to a large extent its present position of apparent stag-
nation, even at this time when its further development should
offer such unusual opportunities.
In this connection the several company flotations which have
occurred have been initiated by promoters having no particular
interest in the business itself. This has resulted in only a small
portion of the relatively large amount of capital which has been
raised in connection with the undertaking filtering through for
its actual development. Adequate research has not been under-
taken, the plants, which already have been constructed, have
been started prematurely in locations having little regard to the
commercial conditions involved, all in order that a rapid showing
might be realized, and a quick turn made by the promoters.
Any complete consideration of this aspect of the proposition can
only lead to the conclusion that the miracle is that anything has
survived. The fact, however, that several million gallons of
alcohol have actually been produced from this source, and that
at least two plants have been operating more or less contin-
uously over a period of years, irrespective of the technical and
commercial handicaps from which they still suffer, justifies the
belief that ultimate success is established, and that the under-
taking offers much promise for the future.
It was originally assumed that almost every sawmill repre-
sented a possible location for the establishment of such a plant.
Since there were almost innumerable sawmills at which the dis-
position of wood waste was a problem, even constituting in most
an element of expense, it was also assumed that this material
could be purchased at a purely nominal figure. It therefore
seemed logical that favorable contracts for wood waste could be
made and having sufficient capital, the company controlling the
process could establish an endless chain of plants producing
ethyl alcohol, and thus soon secure entire control of the alcohol
market.
On this basis and plan the business was projected. It was
soon Tound, however, that while there was no question regarding
the number of sawmills or the extent of the waste wood which
is produced, there are nevertheless, very few at which condi-
tions are entirely favorable for the establishment of the exten-
sive plant which the manufacture of ethyl alcohol requires.
The life of the lumbering operations may be uncertain, the water
supply deficient, labor or transportation conditions unfavorable,
or any one of a number of such factors may be found which
jeopardize success.
The fact that sawdust and all the other forms of waste wood
are so bulky and difficult to handle precludes transportation,
and therefore confines its processing to the point at which its
production occurs. When approached, the lumberman who has
a suitable location soon recognizes the advantage which he
enjoys, and any outside company wishing to do business must
pay his price; and if once established, has no other source of
supply. It can at once be seen that any large or general devel-
opment along these lines was impractical and bound to fail.
In the manufacture of our lumber we know that many millions
of tons of waste wood are annually produced, and the potential
asset which this waste represents is being recognized. If any
considerable part of this, however, can be converted into alco-
hol, there is probably no more important industrial use which
it can be made to serve. That this can be done in a limited way
has now been completely proved, but in order to great!
its application, the development, it would seem, must follow
different commercial lines from those along which the start WM
made.
The process which has been developed naturally divides itself
into two very distinct and separate steps: We first convert a
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THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
certain portion of the wood, amounting to a maximum of about
28 per cent, into soluble carbohydrates which are then separated
in the form of a clear solution which normally contains from
10 to 12 per cent. As a second step, we have the fermentation
and distillation of this product for the production of ethyl
alcohol. It is not essential that both of these operations be
conducted at one point, since the sugar solution can be evapo-
rated, and then becomes quite the equivalent of cane molasses,
which at present constitutes the principal source of our alcohol
supply. Molasses, as we know, is transported to, and assem-
bled at the most favorable locations for alcohol production,
there to be manufactured on the largest scale. Applying this
same principle, we immediately find that the scope of the wood
process is greatly extended. Not only can wood waste be util-
ized at those comparatively few locations at which suitable
conditions for the manufacture and distribution of alcohol are
found, but almost every sawmill with an assured capacity for a
reasonable period can be considered as a possibility. At the
most desirable locations, complete installations for manufactur-
ing alcohol can, of course, be made; at the others, molasses plants
can be installed and their product transported to existing dis-
tilleries, or to new ones at which the product of several such
units can be assembled and used.
The investment required for such a molasses plant is small
compared with that which the complete distillery involves, and
the importance of this in extending the scope of the undertaking
can at once be seen. Furthermore, smaller units can be operated
economically, less skilled labor is required, and it does not come
under the exacting regulations and control of the Internal
Revenue Department, as is the case if alcohol is produced.
Furthermore, if the molasses product is sold to those already
engaged in the distilling business, many market and other trade
difliculties are removed which only those having experience in
the alcohol business fully appreciate and which the smaller pro-
ducer might be unable to overcome.
It would seem, however, that proper headway cannot be made
in the carrying out of such a plan unless the lumbermen them-
selves assume the initiative, or at least give it their most sym-
pathetic cooperation and support
Such a plant, to operate to the greatest economy, should
preferably constitute a part of the lumber operation itself, being
operated under the same management and on the same prem-
ises, thus avoiding all unnecessary handling and storing, as well
as duplication of equipment or staff. In addition to this, the
lumberman, controlling as he does the raw material, can alone
determine and regulate its most economical disposition and use,
and unless he is financially interested in the subsidiary com-
pany, its supply of raw material can never be fully assured.
The lumbermen, however, are naturally cautious about engag-
ing in enterprises apart from their regular trade. In the past
numerous by-product ventures which have been taken up in
connection with the lumber industry have failed and very few
have succeeded. That this has been due either to their being
entirely impractical or to incompetent technical advice is prob-
ably true, but nevertheless these failures have seriously retarded
others from embarking in the like.
In this case, however, the uncertain and costly experimental
expense has already been borne by those who have been blazing
the trail, and the success of the enterprise, from its technical as-
pects at least, is demonstrated. It now remains for some one
to make a fresh start and thus step in and take advantage of
the mistakes of the past. If this is done along sound business
lines by one of our progressive lumber concerns, complete com-
mercial success appears inevitable. Should it be found that
progress along these lines is blocked, as the result of patents,
those controlling such patents would be well advised to accept
an equitable royalty in order that a proper start should be made.
Once this step is taken, others will follow, and real headway
will then be made.
From the lumberman's point of view, the production of
molasses should offer a very strong appeal. While there are at
least several profitable uses to which his waste can be applied,
aside from its use as fuel, the others, as far as I know, demand
sorting or selection. In the case of producing molasses or alco-
hol, any part, or all, of his waste can be used, even including
that which constitutes his fuel supply, since the residue left after
extracting the sugars, representing 70 per cent of the original
amount, is not depreciated in fuel value. In other words, that
portion which is actual waste and is being destroyed can be
combined with the amount being burned for fuel, and 70 per
cent of this total still be available for power development. In
considering and comparing the values extracted, it is therefore
necessary to consider also the much larger tonnage which this
process utilizes. The cost of production compared with the cost
of cane molasses is, however, the vital element upon which this
development must ultimately depend.
In June 1913, the costs given below were obtained in the
alcohol plant then operated by the Standard Alcohol Company
at Fullerton, La. The actual cost of this plant at that time
amounted to $456,920.56. Of this sum, about S200,ooo.oo
represented the expenditure for the plant and equipment in-
volved in the conversion of the wood into sugar and the separa-
tion of this in the form of a solution. The balance was required
to provide the necessary plant and faciUties for fermenting
and distilling the latter and converting it into alcohol.
Operations were conducted 22 days, at three-fourths capacity.
During this time 6,125 tons of green waste wood, containing 48
per cent moisture, were processed, giving a yield of 1,688,600
gal. of sugar solution averaging in strength 10.3 per cent.
The cost of processing this, exclusive of the cost of the wood,
but including all other material, labor, power, factory and over-
head expense, together with proper allowances for depreciation,
amounted to a total of $5,371.56 or 31.8 cents per hundred gal-
lons of the strength stated. To convert this into molasses the
cost of the equipment for this purpose would have to be added
to the cost of the plant and the cost of its operation to that of
the product. Since the residue from the process, however, sup-
plies the necessary fuel, this concentration can be affected at
very little cost.
Assuming a concentration of 8 to 1, the resulting 12V1 gal- of
molasses which 100 gal of the dilute solution will yield, may be
figured at 2.5 cents per gal. or say 3 cents, including the evap-
oration. This is, of course, a lowrer figure than that at which
cane molasses has been sold in recent years and very much
lower than any price which may be expected to prevail in the
future. What this price may be is problematical, but 12 cents
is probably none too high.
When we compare the fermentable contents of the product of
this run with that of cane molasses, the showing is not so favor-
able. During the month the average production of spirit
amounted to only 4.87 proof gal. per 100 gal. of dilute solution.
Using this same percentage, a gallon of wood molasses would
yield only 0.39 gal. of proof spirit, whereas cane molasses yields
practically gallon for gallon. This gives a cost of 7.7 cents
for wood molasses to yield the spirit given by a gallon of cane
molasses. While even on this basis it appears that a profit is
fully assured, the result which this comparison gives is far from
representing the best which can be obtained since the quality
of this product was poor. From the figures given it can be
calculated that only about 8.5 per cent of the dry wood was
converted into sugars which were fermented, although approx-
imately 24 per cent of the wood was extracted in the solution
obtained. It his been repeatedly demonstrated, however, on
both large and small scale experimental operations, that 26 to
28 per cent of the wood can be converted into water-soluble
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
carbohydrates as a result of simple acid hydrolysis and that
under the best conditions over 80 per cent of this is obtainable
in the form of fermentable sugar. In place of realizing this
result, not over 50 per cent of the water-soluble carbohydrates
obtained has actually been fermentable in the product of the
plant which I have mentioned, and the average has been less.
It remains to translate such experimental results, depending
as they do upon the conduct and control of the chemical reac-
tions involved, into commercial practice. To do this requires
little change in the mechanical methods of handling which were
used at Fullerton and largely developed by myself. The mechan-
ical efficiency of these is indicated by the very low per gallon
cost which I have given and which there is no reason to believe
should be increased in effecting the much more complete hydrol-
ysis which it is easily possible to obtain. That this has not
already been done, I attribute principally to patent conflict
which has directed this development along unnatural lines in
the effort to avoid infringement and permit exploitation. In
undertaking any new installations, however, if full advantage is
taken of existing knowledge and the experiences of the past, the
production of a wood molasses equal to cane molasses in ferment-
able value is assured, and at a cost per gallon which certainly
should not exceed that of the low-grade Fullerton product which
we have considered.
The lumberman already can see a limit to his timber supply,
and is rapidly being forced, for this reason, to recognize the
necessity of conserving all that is left. Nevertheless, he is still
burning 50 per cent of his logs either under his boilers, or in
his refuse destroyer. Every ton of this waste can be made to
yield over 30 gal. of molasses without disturbing in any way
existing methods of operation, unless it be that of the expensive
destroyer which every large sawmill still maintains. Allowing
but 3 cents per gal. profit on the molasses which can thus be
made, this would be equivalent to an additional profit of almost
$2.00 per thousand feet of lumber, an amount probably quite
equal to the average profit normally realized on the lumber itself.
In this, it would appear that we may have an almost unlimited
source of molasses within our reach which the distiller can
readily convert into the highest grade of ethyl alcohol without
any, or little, modification in the equipment which he already
has at hand.
With drastic prohibition as a probability of the future, as well
as the necessity of conserving everything which can be used,
either directly or indirectly, for food, this should offer a means
by which the distilling business can readjust itself to meet these
conditions, and at the same time provide alcohol in such quan-
tities and on such a basis that its much wider industrial applica-
tion becomes a possibility, with all the consequent commercial
advantages to which this would lead.
With proper cooperation to this end between the lumber and
distilling interests, it should be possible to rapidly realize this
condition to their mutual advantage, and at the same time
release for other use the immense quantities of food products
now used for alcohol production.
When the facts which I have attempted so inadequately to
present are more fully recognized and the proposition is taken
in hand by those having a vital interest in its development and
success, it may be expected to become a business of the greatest
magnitude and importance, and wood waste should become the
principal source of ethyl alcohol.
CURRENT INDUSTRIAL NEWS
By A. McMillan, 24 Weitend Park St, Glasgow. Scotland
IRON AND STEEL INDUSTRY IN JAPAN
The British Commissioner at Seoul writes that, in order to
encourage the iron industry in Corea, exemption from import
duty on coal, machinery and implements imported for the use
of iron foundries, has been announced by the Governor Gen-
eral. The total quantity of iron ore now obtained in Corea is
put at some 200,000 tons a year and a large output of pig iron
and steel is expected from the new foundries in the Chinnampo
district which are now on the point of completion. The annual
output of pig iron from the new Mitsubishi Foundry there, which
has just started operations, is estimated at 100,000 tons, of
which 50,000 tons will be made into steel.
many other such articles. Jewelry, cutlery, glassware and
fancy goods are also in demand.
GOODS IN DEMAND IN AUSTRALIA
It seems scarcely necessary to enumerate the very large
variety of goods which have been getting in short supply in
the Commonwealth, says the Times Trade Supplement, as a
result of the interference with normal trade. Australian im-
porters would now welcome the largest possible consignments
of building materials, ironmongery, tools, locks, aluminum
ware, hollow ware, and hardware lines generally. It may,
therefore be imagined what the demand will amount to when
building operations are resumed after the war. Again, in con-
nection with the expansion of industry generally, which has been
mentioned above, eager inquiries have been in the market for
some time past for all lines of industrial chemicals used by brew-
ers, tanners, soap manufacturers, textile mills, photographers,
etc., including such articles as litharge, tartaric acid, citric
acid, soda, dyes, waxes. As regards soft materials, an absolute
shortage of silk goods was reported recently from Sydney,
while buyers in that city and in Melbourne have been clamoring
for means of replenishing their stocks of cotton piece goods,
woolen goods, linings, handkerchiefs, shirtings, hosiery, and
JUTE PRODUCTION IN CHINA
According to returns of the Chinese Maritime Customs, the
export of jute from China amounted to 94.481 piculs (picul =
'33l/a lbs.) in 1916. Of this amount 67,000 picu's were shipped
from Tientsin, North China, 15,000 from Hankow, Central
China, and 13,000 from South China. A small amount was also
exported from Manchuria. It is probable, however, that a
considerable proportion, if not all, of this jute is in reality "Abu-
tilon" hemp, the two plants being constantly confused by the
Chinese. The Ministry of Agriculture can give no informa-
tion which locates the area of production of jute with any ac-
curacy. According to catalog of the Vienna Exhibition, jute
fiber is produced in China and is exported from Shanghai.
It is also mentioned as being cultivated near Canton, in the
Province of Szechuan and in the Vangtse Valley.
CRANES AND TRANSPORTERS
In a catalog issued by Sir William Arrol & Co., Ltd., Glasgow,
illustrations and short descriptions are given of shipbuilding
cranes and shipbuilding berth equipment manufactured by them.
The first part deals with various types of derrick and tower
cranes, and the pictures represent installations of such machines
in various important shipyards at home and abroad, while the
second gives brief descriptions of various arrangements of
cranes for building and fitting out ships in covered and uncov-
ered berths in which the Olympic and her s ster ships were con-
structed. Another list from the same firm shows installations
of different types of Temperley transporters — some mono-rail,
Others fixed, others moving on rails, and others designed to be
fitted in ships— which have been erected ill various parts of
the world for handling coal and other materials.
86 a
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
NATURAL INDIGO INDUSTRY
With the cutting off of the synthetic indigo supplies from
Germany since the outbreak of war, the natural indigo industry
has come into its own and the cultivation of the crop has
considerably increased. While the total area under this crop
in 1914-15 was only 148,400 acres, in 1915-16 it rose to 353,100
acres, and in 1916-17 to 756,400 acres. The greatest increase,
both absolute and relative, occurs in the Madras Presidency
and in the United Provinces, where the industry is mainly in
the hands of small holders and the dye manufactured is of in-
ferior quality. In Bihar, where a superior dye is manufac-
tured, mainly in large factories, the increase of area in 1916-17
was about 33 per cent as compared with 1915-16. The yield
of indigo increased from 55,000 cwt. in 1915-16 to 95,000 cwt.
in 1916-17, Madras contributing two-thirds of the total pro-
duction. Both the average and the output in 1 916-17 were,
however, only half of what they were in 1895, when the syn-
thetic product came into the market. The forecast for 1917-
18 puts the average at 690,000 acres and the output at 87,000
cwt. The future of the indigo industry, says the Board of
Trade Journal, depends (1) on a good and sufficient supply of
seed, (2) on an increase in the output of green leaf, (3) on im-
provement of manufacture, (4) on organization in marketing,
{5) on elimination of the practice of adulteration.
REFRACTORY MATERIAL FROM BAUXITE
At the Sheffield meeting of the Refractory Material Section
of the Ceramic Society, a paper was read by Dr. A. Bigot on
"Corindite" which is described as a new refractory and abrasive
material. Corindite is obtained by heating a mixture of bauxite
and anthracite in a cupola, the heat developed by the reac-
tion being such that the mass fuses in successive layers. The
point of fusion of corindite from French white bauxite taken
from the War Department is 1950° C, a point higher than the
melting point of the bauxite. The crushed corindite, accord-
ing to the Client. Trade Journal, 62 (191 8), 431, is mixed
with refractory binders, finely pulverized, such as bauxite,
kaolinic clay, etc. Binding of the material with such bases
as lime, magnesia, and calcined dolomite must be avoided as
these lower the fusing point of the mixture. The corindite
can be suitably moistened and mechanically mixed and
is then employed as an ordinary refractory mixture for
making firebricks. The dried bricks are baked between
135°° C. and 1400° C. and undergo no shrinkage. Be-
tween 1700 and 1730° C. they lengthen by about 0.5 per cent.
Above 17500 C. they begin to undergo a shrinkage attaining
3 per cent at 1850° C. The porosity depends on the mechan-
ical composition of the mixture and on the compression it varies
from 9 to 12 per cent. The product is said to be three and a
half times more resistant to wear than good magnesia bricks.
Refractory products based on fused bauxite are attacked by
slag and scoria in the same way as refractory matter made from
iron-fused bauxite. The action of slag and scoria is being in-
vestigated but results are not yet completed. Tests have been
carried out with white bauxite from Inland and these seem to
give as good results as the French bauxite in many respects,
but refractory power is a little less, due to a smaller proportion
of alumina in the Irish bauxite .
SUBSTITUTE FOR SHELLAC
it has been Found that naph-
thol resin can be used as a substitute for shellac and that the
products of condensation of a and ,; naphthol have a number
icteristics in common with shellac, such as capacity for
taking a polish and suitability for use as an alcohol varnish,
and as an insulating material. The substitutes are particularly
useful if the residues are cleaned by filtering from an alcoholic
solution, the alcohol being distilled from the filtrate.
ELECTRICITY IN SILK INDUSTRY
The application of electrical methods in the weaving indus-
try and especially in connection with silk are discussed by
M. Ch. Vallet in L'industrie Electrique. The chief advantage
is said to be the avoidance of breakage of the fine threads,
which appears to be inseparable from the use of steam and gas
engines. The essential factor is regularity of speed and the
better results secured in this respect through the electric drive
have led to an increase of 5 to 20 per cent. The question of the
best arrangement of drive receives some consideration. Gen-
erally speaking, the author inclines to the view that control by
groups is preferable in a workshop where a large number of
machines are working on identical processes.
VEGETABLE OILS IN JAPAN
According to a report from the British representative at
Shimonoscki, a new company for the exploitation of vegetable
oils, established in July 1917, with a capital of Ssoo.ooo, has
completed the first section of its works at Warkamatsu, and
manufacturing operations will be started shortly. In Japan,
the oil industry is still in its infancy. The better qualities of
glycerin, soap and paint are still imported, while imports of
Manchurian bean oil are valued at over $500,000 annually. It
is evident, therefore, that there is an important future for the
industry. The consumption of raw material will, it is stated,
be 100 tons per day, or approximately 30,000 tons per year,
and will consist principally of soy beans. The output of bean
cake and bean oil is expected to be 24,000 tons and 4,200 tons,
respectively. On the completion of the second section of the
works, the consumption of soy beans will be 150 tons daily,
or 45,000 tons annually, and the output of bean cake 37,000
tons and bean oil 6300 tons. The land for a third section is
being prepared and on this site will be erected works for cake
crushing, for the manufacture of stearic oil, glycerin, soap,
candles, etc. The output of the works will be all taken by
the Mitsui Bussan Kaisha under a contract. The refined oil
will be exported and the bean cake sold to Japanese fanners.
ALUMINUM
Writing upon the supply of aluminum in Switzerland, Metall
und Erz, of March last, stated that the war had given a power-
ful impetus to the aluminum industry in all countries. As a
substitute for other metals and for new uses, that metal is in
great and increasing demand. Hence its production was be-
coming one of the great industries of the world. The annual
report of the Swiss Co., at Neuhausen, shows that the output
has increased greatly during the past year and that means of
production are being taken to meet the growing demands.
Five million francs have been set aside out of the gross profits
for the year to provide additional water power with a view to
an extension of the works.
A NEW HEAT INSULATOR
A new heat-insulating material is being produced in Sweden,
says Electrician, 81 (1918), 2ik\ which is said to be promising.
The chief constituent in this new material is a kind of fine clay
found on the island of Mars. This "Molera," as it is termed.
is very porous and each grain appears to be hollow. This fact
is no doubt largely responsible for the good heat-insulating
properties. After it has been burnt the molera becomes c.\-
tremely light and therefore a poor conductor of heat. Be-
fore it is burned, however, it is mixed with cork, bricks of the
mixture being burned while the cork is consumed. The new-
insulator is said to be primarily suitable for covering steam
pipes and boilers, but may also have uses for the production
of sound-proof chambers and as a medium to check the trans-
mission of vibration.
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
863
SCIENTIFIC SOCIETIES
FIFTY-SIXTH MEETING AMERICAN CHEMICAL SOCIETY
CLEVELAND, SEPTEMBER O-13, 1918
PROGRAM OF PAPERS
GENERAL SESSION1
Address of Welcome. A. W. Smith.
Response. H. S. Miner.
The American Chemist's Place in Warfare. Charles L. Parsons, Chair-
man Committee on War Service for Chemists.
The Work of the Chemical Section of the War Industries Board. Chas.
H. MacDowell, Director of Chemicals Division, War Industries Board.
War Disturbances and Peace Readjustments in the Chemical Industries.
GrinnELL Jones, Chemist, Tariff Commission.
Chemical Warfare Research. Wilder D. Bancroft, Chemical Warfare
Service.
The Place of the University in Chemical War Work. Edward W. Wash-
burn, National Research Council.
President's Address —A Retrospect and an Application. William H.
Nichols.
AGRICULTURAL AND FOOD CHEMISTRY DIVISION
T. J. Bryan, Chairman F. F. Flanders, Secretary
1. Some Chemical and Economic Aspects of the American Food Supply.
H. C. Sherman.
2. The Role of Oxidases and of Iron in the Color Changes of Sugar Cane
Juice. F. W. Zerban. (See p. 814, this issue )
3. A Centrifugal Method for the Separation of Cottage Cheese Curd from
Buttermilk. A. E. Perkins.
4. Influence of Conditions upon the Polarizing Constants of Sugar Cane
Products. C. A. Browne.
5. The Effect of Manganese on the Growth of Wheat; Basic Slag a Source
of Manganese. (Lantern.) J. S. McHargub.
6. A Comparison of Barium Sulfate Results on Feeds and Feces by the
Benedict Wet Solution Method (Wolf and Ostenberg) with the
Modified Sodium Peroxide Method, Silica Being Removed. J. O.
Halverson.
7. The Thermo-Stability of the Water-Soluble Vitamines. A. D. Emmbtt
and G. Oeschger.
BIOLOGICAL CHEMISTRY DIVISION
W. J. V. Osterhoht, Chairman I. K. Phelps, Secretary
I — Special Program on Plant Chemistry
1. A Contribution to the Classification of Peat Based on Botanical Com-
position, Physical and Chemical Characteristics. Quality and Value
of Important Types of Peat Material. A. P. Dachnowski.
2. The Effect.of Temperature and Aeration on Carbohydrate Changes in
Sweet Corn. C. O. Appleman.
3. The Comparative Respiratory Activity of Stored Cereals. (Lantern.)
C. H. Bailey and G. M. Gurjar.
4. Imbibition by Seeds. R. A. Gortner.
5. The Pectin Relations of Sclerotinia cinerea. J. J. Willaman.
6. The Nutrition of Sclerotinia cinerea: Evidence of the Existence of a
Growth-Promoting Substance. J. J. Willaman.
7. Effect of Low Concentration by Sulfur Dioxide on the Protein Content
of Plants. P. J. OGara.
8. Physiological Balance in the Soil Solution. R. P. Hibbard.
H— Papers
1. The Effect of Thymol-Chloroform Solution as a Preservative on the
Chlorine Content of Urine. J. O. Halverson and J. A. Schulz.
2. Influence of Hydrogen-Ion Concentration upon the Enzyme Activity of
Three Typical Amylases. H. C. Sherman, A. W. Thomas and M.
E. Baldwin
3. The Composition and the Nutritive Value of the Corn Plant at Different
Stages of Growth. (Lantern.) H. S. Grindley and H. C. Eck-
stein
4. ViUmine Studies. I. Some Observations on the Catalase Activity of
Tissues in Avian Polyneuritis. (Lantern ) R. Adams Dutcher.
5. On the Forms of Nitrogen in "Protein-Free Milk." Cornelia Kbn-
6. The Determination of Tyrosin in Proteins. C. O. Johns and D. B.
7. The Elimination of Tartrates. G. E. Simpson.
8. Salmon Oils. M R Daughters and F. W. Nestbll.
9. Absorption Index of Protoplasm for Fluorite Rays. W T B
10. The Localization of the Physiological Effects of Radiation Within the
Celt W. T. Bovie.
11. Sensitization of Protoplasm to Heat by Actinic Radiation. W. T.
Bovie.
12. The Mechanics of the Physiological Action of Rays. W. T. Bovie.
13. The Rate of Recovery from the Action of Fluorite Radiation. W. T.
Bovte.
14. Action of Enzymes upon Starches of Different Origin. H. C. Sher-
man, Florence Walker and Mary C. Caldwell.
15. Efficiency of the Proteins of Cereal Grains in Adult Human Nutrition.
H. C Sherman, E. Osterberg, J. C. Winters and V. Philips.
16. Reduction of the Quantity of Human Nitrogen Formed in the Hydrolysis
of the Nitrogenous Constituents of Feeding-Stuffs. (Lantern.) H.
C. Eckstein and H. S. Grindley.
17. Composition of "Glidine" by Nitrogen Distribution into Seven Groups.
(Lantern.) H. C. Eckstein and H. S. Grindley.
18. The Nitrogen Metabolism of Two-Year Old Steers. (Lantern.)
Sleeter Bull and H. S. Grindley.
19. Vitamine Studies, n. Does Water-Soluble Vitamine Function as a
Catalase Activator? R. A Dutcher and F. A. Collatz.
20. Vitamine Studies. HI. Observations on the Curative Properties of
Honey, Nectar, and Corn Pollen in Avian Polyneuritis. R. A.
Dutcher.
21. The "Gold Numbers" of "Protalbinic" and "Lysalbinic" Acids. R. A.
Gortner.
22. On the Origin of the Humin Formed by the Acid Hydrolysis of Proteins.
IV. Humins from Substituted Indoles. R. A. Gortner.
23. The Nutritive Value of Cocoanut Globulin and Cocoanut Press Cake.
C. O. Johns and A. J. Finks.
24. The Nutritive Value of the Proteins of the Chinese Velvet Bean. C. O.
Johns and A. J. Finks.
25. The Hydrolysis of Arachin. C. O. Johns and D. B. Jones.
26. A Preliminary Report upon Some Halophilic Bacteria. E. LeFevrb
and L. A. Round.
27. The Zinc Content of Some Food Products. V. Birckner.
28. Investigation of the Kjeldahl Method for Determining Nitrogen. Vn.
The Determination of Nitrogen in Aromatic Nitro Compounds.
(Read by title.) I. K. Phelps and H. W. Daudt.
29. The Estimation of Tartaric Acid after Separation from Citric and
Succinic Acids. I. K. Phelps and H. E. Palmer.
30. The Utilization of Waste Fruits in Vinegar Making. L. A. Round
and E. LeFevre.
31. The Protein Extract of Ragweed Pollen. F. W. Heyl.
32. Standardization of Amylolytic Digestion. (Preliminary Paper.) J. C.
Blake.
INDUSTRIAL CHEMISTS AND CHEMICAL ENGINEERS DIVISION
H. S. Miner, Chairman S. H. Salisbury, Secretary
I — Symposium on the Chemistry of Dyestuffs.
1. America's Progress in Dyestuff Manufacture. Louis Joseph Matos.
2. The Production of American Dyes and Coal-Tar Chemicals During
1917. Grinnell Jones.
3. The Development of the Dyestuff Industry Since 1914. J. F. Schobll-
kopf, Jr.
4. The Development and Importance of Anthraquinone Dyes. (Not
presented.) M. L. CrosslEY.
5. The Quantitative Estimation of Important Constituents of Crude
Anthracene. (Not presented.) Harry F. Lewis.
6. The Application of Dyestuffs in Cotton Dyeing. J. Mbrritt Mat-
thews.
7. Natural Dyestuffs— An Important Factor in the Dyestuff Situation.
Edward S. Chapin.
8. What is Necessary to Make the American Dyestuff Industry a Per-
manent One? (Not presented ) Herman Seydbl.
9. Manufacture, Use, and Newer Development of the Dyewood Extracts.
Charles R. Delanby.
10. Photographic Sensitizing Dyes— Their Synthetic and Absorption
Spectra. L. E. Wise and E. Q. Adams.
11. The Color Laboratory of the Bureau of Chemistry— A Brief Statement
of the Objects of Its Works and the Accomplishments to Date. H.
D. Gibbs.
ediates. E. W. Pierce.
. H. Holland.
1 Papers presented at this session appear in full in this is9uc.
12. Problems in Testing Dyes and Intern
13. Quantitative Analysis of Dyestuffs. J
n — Potash Symposium
1. Experimental Kelp Potash Plant of U. S. Department of Agriculture.
J. W. Turkhntinh.
2. American Potash. J. W. Turrentinb.
3. On the Preparation of an Active Decolorizing Carbon from Kelp. F. W.
Zerban and E. C. Ffei'.i.and (See p. 812, tins issuel.
4. The Extraction of Potash from Cement Mill and Blast Furnace Dust.
Wm II. Kr>ss.
5. The Potash Situation. A. W. Stockett.
864
THE JOURNAL OF IXIWSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
III— Papers
1. Valuations of Raw Sugars. W. D. Horne. (See p. 809, this issue.)
2. The Citric Acid Industry. Grinnell Jones and S. D. Kirkpatrick.
3. The Deoxidation of Steel by Ferromanganese. Alex. L. Feild.
4. The Cotton Oil Industry in the War. (Lantern.) David Wesson.
5. A New Illuminator for Microscopes. (Second paper.) (Lantern )
Alexander Silverman.
6. An Industrial Research Laboratory. (Lantern.) H. E. Howe.
7. Gilsonite. Robert J. Moore and Gustav Eglofp.
8. The Steam Distillation of Gasoline. Gustav Eglopp.
9. The Quantitative Estimation of the Important Constituents of Crude
Anthracene. Harry F. Lewis.
10. The Preparation and Properties of "Yttrium Mixed Metal." J. F.
G. Hicks.
11. An Investigation of Stenches and Odors for Industrial Purposes. V. C.
Allison and S. H. Katz.
12. Eckhart Method of Sugar Production. A. D. Little.
ORGANIC CHEMISTRY DIVISION
W. J. Hale, Chairman II. L. Fisher, Secretary
1. The Influence of Catalysis on the Chlorination of Hydrocarbons. V. R.
Kokatnur.
2. On the Detection of Small Quantities of Trichlorotertiarybutyl Alcohol
(Chloretone) in the Fluids and Tissues of the Body. T. B. Aldrich.
3. Studies on Derivatives of Trihalogentertiarybutyl Alcohols. II. The
Propionic and Butyric Esters of Tribromotertiarybutyl Alcohol
(Brometone). T. B. Aldrich.
4. The Identification of Acids. J. B. Rather and K. Emmet Reid.
5. The Solubility of Liquids in Liquids. N. E Gordon and E. Emmet
Rbid.
6. A New System of Nomenclature for Four-Membered Cyclic Ureas.
William J. Hals.
7. The Synthesis of 3,4-Diphenyluretidone. William J. Hale.
8. Aluminum Oxide as an Absorbent for Water in Organic Combustion.
Harry L. Fisher.
9. A Modified Form of the Inner Tube Absorption Bottle for Use in
Organic Combustion. Harry L. Fisher.
10. Methane. William Malisofp and Gustav Eglofp.
11. Ethylene. William Malisopp and Gustav Eglofp.
12. Reaction Products of Alkali-Sawdust Fusion — Formic, Acetic and
►* Oxalic Acids and Methyl Alcohol. (Lantern.) S. A. Mahood.
13. Quino-Isomerism. Oliver Kamm.
14. Misiepresentation in German Technical Literature. Oliver Kamm.
15. The Reaction Between Dimethyl Aniline and Benzene Sulfonyl Chlo-
ride. Oliver Kamm and N. W. Wroby.
PHARMACEUTICAL CHEMISTRY DIVISION
F. O. Taylor, Chairman George D. Beal, Secretary
1. The Proximate Composition of Rumex Crispus. and a Comparison of Its
Anthraquinone Content with Other Drugs of the Same Class. Ruth
E. Okey and George D. Beal.
2. An Efficient Funnel for Filtering Neutral Liquids, Especially of the
Volatile Organic Solvents. T. B. Aldrich.
3. Studies on Pepsin. I. Chemical Changes in the Purification of Pepsin.
Lewis Davis and Harvey M. Merkbr
4. Pepsin versus Rennet in Cheese Making. Harvey M. Merker.
5. Digitalis Leaves — Effect on Activity of Temperature in Drying. H. C.
Hamilton.
6. Scammony and Its Substitutes. W. L. Scovtlle.
7. Report of Committee on Analytical Methods.
8. Conference on War Time Changes in Medicinal Products, New Sub-
stances, New Methods, Etc.
PHYSICAL AND INORGANIC CHEMISTRY DIVISION
S. L. Bigelow, Chairman W. E. Henderson, Secretary
1. A Simple Interpretation of Osmotic Phenomena in Terms of the Phase
Rule. A. S. McDanibl.
2. Two Papers on Chemical Actions Produced by Radium Emanations.
(a) Part I. Combination of Hydrogen and Oxygen. (6) Part II.
Chemical Action Produced by Recoil Atoms. S. C. Lind.
3. The Isotopism of Mesothorium and Radium. R. K. Strong.
4. Solubility Curves by an Application of Floating Equilibrium. W. K
Henderson.
5. The Reduction of Tungstic Oxide. C W. DAVIS
6. Several New Forms of Apparatus, (a) A New Type of Vacuum Dis-
tillation Flask. (/') A New Type of Fractionating Column for Vacuum
Distillation, (c) A New Form of Dip Electrode for Conductivity
Measurements and Substitute for Solid Platinum Electrodes.
(Lantern.) II. C P. Wbbbr.
7. On the Separation of Germanium from Arsenic by the Distillation of
the Chloride in the Presence of a Chromatc. (Readbj title.) ritu.ir
E. Browning and Sewell E. Scott.
8. The Potential of the Thallium Electrode. Grinnell Jones and
Walter C. Schumb.
9. Ammono Nitrogen Trichloride; Probable Formation of Trichlorc-
ammonium Chloride. W. A. N'oyes and A. B. Haw
10. Crystalloluminescence and Triboluminescence. Harry B. Weiser.
! 1. The Absorption of Anions by Barium Sulfate. Harry B. Weisbr and
Jacob L. Sherrick.
12. Metallic Salts of Pyrrol, Indol and CarbazoL E. C. Franklin.
!3. Sodium Pyrogallate Solution as an Absorbent for Oxygen. G. W.
Jones and M. H. Meichan.
FERTILIZER CHEMISTRY DIVISION
J. E. Breckenridge, Chairman F. B. Carpenter, Secretary
1. Soil Acidity, the Resultant of Chemical Phenomena. (Lantern.) H.
A. NoYBS.
2. The Nature of the Recombined Potash in Cement Dust. Albert R.
Mi:rz.
3. Results of Further Cooperative Work on the Determination of Sulfur
in Pyrite, Check Sample No. 4. II. C. Moore
4. Report of Laboratory Work on the DeRoode Method for the Determina-
tion of Potish. J. E Brb;kenrid3E.
5. A Study of- the DeRoode Method for the Determination of Potash.
T E. Keitt.
6. A Study of Sources of Error Incident to the Lindo-Gladding Method
for Determining Potash. T. E. Keitt.
Conference for general discussion on interesting phases of the fertilizer
industry at the present time.
RUBBER SECTION
L. E. Weber, Chairman J. B. Tdttle, Secretary
1. The Determination of Lamp Black. A. H. Smith and S. W. Epstein.
2. Laboratory Methods for Determining the Degree of Vulcanization.
Discussion opened by D. F. Cranor.
3. The Fruit Jar Ring Situation. Discussion opened by Chas. P. Fox.
4. Vulcanization of Rubber at Constant and by a Series of Increasing
Temperatures. G. D. Kratz and Arthur H. Flower.
5. Report of the Committee on the Poisonous Nature of some Accelerators
and Precautions Regarding their Use. Discussion opened by R. D.
Earle.
6. Report of the Executive Committee. L. E Wbber, Chairman.
WATER, SEWAGE AND SANITATION DIVISION
R. S. Wbston, Chairman W. W. Skinner, Secretary
1. Purification of Cleveland's Water Supply. Joseph W. Ellms.
2. Cleveland's Sewage Projects. George B. Gascoigne.
3. The Determination of Iodide in Mineral Waters and Brines. W. F.
Baughman and W. W. Skinner.
4. A Study of Well Water. G. O. Higley.
COMMUNICATION FROM UNITED STATES SHIPPING
BOARD
Washington, D. C.
August i, 1918
American Chemical Society,
Washington, D. C.
Gentlemen:
I am going to call upon your organization for some teamwork.
The time has come for Americans everywhere to put them-
selves solidly behind American ships.
Our railroads must no longer stop at the ocean. We are
building an American merchant fleet of 25,000,000 tons — 3,000
ships. We are backing modern ships with modern port facili-
ties, establishing our bunkering stations all over the globe, and
will operate with American railroad efficiency. We will cany
American cargoes at rates corresponding to our railroad rates —
the cheapest in the world. Fast American passenger and cargo
liners will run regularly to every port in Latin America, the
Orient, Africa, Australia.
1 hiking steps to use these ships to increase your own
prosperity? Do you realize that American products of factory,
farm, and mine can be delivered to customers in foreign coun-
tries on terms which will build lasting trade?
Do you realize the possibilities for bringing back raw ma-
terials to extend your products and trade?
We must all take off our coats and work to bring these Ameri-
can ships home to the people of every American interest and
community The manufacturer must think of customers in
Latin America as being as accessible as those in the next state.
Oct., 191S
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
865
The farmer must visualize ships carrying his wheat, cotton,
breeding animals, dairy products, and fruit to new world mar-
kets. The American boy must think of ships and foreign
countries when he chooses a calling.
Has your organization appointed a live Committee on Mer-
chant Marine?
Is the chairman of this committee a man of international
vision?
Are you applying the new world vision to the interests repre-
sented in your organization and learning what ships can do toward
widening your markets?
These are your ships. It is your duty to bring them close,
regard them as new railroads, spread knowledge about them
through investigation, meetings, discussion.
Public neglect ruined our old merchant marine. Congress
was not to blame — it simply reflected the indifference of the
average American toward ships. Once more we have a real
American merchant fleet under way, backed by far-reaching
policies for efficient operation. We must dispel indifference
and keep our flag on the trade routes of the world. We are going
to take trade from no other nation. But we must serve our
own customers and help other nations in their ocean transporta-
tion problems after the war.
I want to hear personally from your organization. These
are precious days of opportunity. The nation is united for
teamwork and service. Let us "Wake Up, America!" — which
means waking up ourselves. I expect you to write me outlining
your views and making any suggestions that you think will be
helpful in our work.
With personal good wishes, I am
Yours very sincerely
Edward N. Hurley, Chairman
COMMITTEE ON ORGANIC ACCELERATORS
RUBBER SECTION, AMERICAN CHEMICAL SOCIETY
Members of the Rubber Section of the American Chemical Society:
In accordance with the resolution passed at the last meeting
of the Rubber Section of the American Chemical Society
held at Cambridge, September 12, 1917, the Committee on
Organic Accelerators respectfully submits the following report:
Owing to the increasing use of certain organic compounds as
accelerators in the vulcanizing of rubber goods, many of which
are marketed under misleading trade names, it is desirable to
call the attention of rubber manufacturers to the poisonous
properties of some of these products and to the fact that dis-
agreeable factory experience may result unless due precautions
are taken.
The more common accelerators used to-day are aniline,
hexamethylene tetramine, para-phenylene diamine, para-nitroso-
dimethyluniline, and thiocarbanilide.
symptoms of poisoning — In small amounts, pallor, vertigo,
and blueness of lips result. In large doses muscular weakness,
strangulation, and death.
antidotes — Fresh air, change of clothing, artificial respira-
tion. I'se of milk in diet is recommended. Use of alcoholic
stimulants predisposes to poisoning and is excessively injurious
after poisoning has occurred.
Hi:.\ AM ETHYLENE TETRAMINE
symptoms of poisoning — Rash and inflammation of skin
which has been in repeated contact with stock containing this
material. In severe cases, blisters tilled with water] lln"1 result.
antidote Cleanliness and care in regard to clotfa
the best preventative ( hange <>! occupation will cau e thi
rash to disappear, leaving no permanent effects.
PARA-PHENYLENE DIAMINE
symptoms of poisoning — Inhalation of the dust gives the
symptoms of a common cold with sneezing and extreme de-
pression. In larger quantities, death with symptoms similar
to those of ptomaine poisoning. This is probably the most
poisonous of all the accelerators proposed up to date. All
efforts should be made towards prevention of inhalation of dust,
by means of suction hoods over the mixing mills.
PARA-N1TROSODIMETHYLANIL1NE
symptoms OF poisoning — -This causes a severe inflammation
of the skin, increasing in severity according to the exposure.
antidote — Change of occupation.
THIOCARBANTLIDE
symptoms OF poisoning; — -This material decomposes when
heated to vulcanizing temperatures with the formation of
phenyl mustard oil, the fumes of which cause pallor, blueness
of gums and lips. Probably the least poisonous of the common
organic accelerators.
antidote — Fresh air.
recommendations
1 — Cleanliness is essential. The hands should be washed
before eating. Before leaving the factory a shower bath should
be taken and a complete change of clothing made.
2 — Mixing mills should be provided with adequate suction
hoods, in which an efficient draft is maintained.
3 — Ventilation of press rooms, especially if thiocarbanilide is
used.
4 — Immediate attention to early symptoms, and, if possible,
temporary change of occupation in the factory.
5 — Periodical medical examination of employees in mixing
and compounding departments, and an educational campaign
among employees in regard to use of alcohol and chewing to-
bacco while at work.
6 — -In the case of accelerators sold under trade names it is sug-
gested that steps be taken to ascertain the nature of the material.
Respectfully submitted
Richard B. Earle, Chairman
September 9, 1918
DIVISION OF INDUSTRIAL CHEMISTS AND CHEMICAL
ENGINEERS
MINUTES OF SESSIONS, 56TH MEETING A. C. S.
A symposium on the chemistry of dyestuffs was held on the after-
noon of Tuesday, September 10, 1918, R. NorrisShreve presiding.
All papers listed on the program were presented except those
of Messrs. Crossley, Lewis, and Seydel. Those interested in
the formation of a Dye Section were asked to leave their names
and addresses with Mr. Shreve. The meeting seemed to think
that the cooperation possible and the benefit to the industry
would be such that the Council at its next meeting should be
asked to form a Section on Dyes.
At the business meeting there were no reports from the Execu-
tive Committee or the Secretary. The Committee on Analysis
of Oils and Fats made a further report, which was accepted and
referred to Dr. Hillebrand's Supervisory Committee on Standard
Methods of Analysis, and to the Journal of Industrial and
Engineering Chemistry for publication. There were no other
reports.
The Nominating Committee, which consisted of Messrs. Paul
Rudnick, E. P. Hicks, and C. P. Long, made the following
ndations: II. S. Miner, Chairman; II. D. Bachelor,
vrman; II. U. Howe, Secretary; W. F. Hillebrand, S. W.
Parr, A. W. Smith, David Wesson, J. G. Vail, and ex officio,
Chas. H. Hcrty, Executive Committee.
i> ra on the program were pre* nted either in full or by
abstract. The Potash Symposium brought out discussion by
866
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol.
10 Xo. 10
Messrs. Grimwood, Herty, Wesson, Ashman, Jones, Cabot,
Zerban, Parr, Mabery, Field, and Stockett.
w Upon invitation, Dr. C. E. K. Mees spoke of the new work
taken up by the Eastman Kodak Company which has as its
object the supplying of chemicals needed for research which
cannot be obtained in the market and are not capable of being
made commercially by chemical firms. Large quantity pro-
duction will not be undertaken now, but the making of small
amounts of a great many compounds will be a specialty. In
this M work the cooperation of graduate students, research men,
and industrial laboratories is required. Universities which can
manufacture some of these chemicals will find a buyer in the
Eastman Kodak Company, and the research man who would
ordinarily make ioo grams will be asked to produce a kilo of any
unusual substance he may make, with the expectation that the
Company will buy, store, and later sell the material as it may
be needed. Industrial men can help by calling attention to
new materials, new sources of raw materials, etc. With our
resources it may easily be possible to entirely supersede Kahl-
baum and other foreign sources of this material.
All of this is the outcome of Dr. Roger Adams' work, and the
plea of a professor who pointed out that unless someone began
to make the unusual organic and inorganic chemicals here, we
would all be forced after the war to return to German sources.
The Division approved the resolution of the Organic Division
relative to nomenclature, and adjourned after discussing types
of meetings and Dr. Herty's remarks on improving his Journal.
H. E. Howe
Acting Secretary
Princeton. The authorities of Princeton and the Princeton
members felt constrained to withdraw their invitation, and
asked the Society to visit them at a more convenient season and
under more favorable circumstances.
The meeting was therefore held, on the dates announced,
at Atlantic City, with headquarters at the Hotel Traymore!
The meeting followed immediately after the Chemical Expo-
sition at New York, permitting advantageous combination
therewith. The Symposium on "Electrochemistry after the
War" took both Tuesday sessions.
FALL MEETING, AMERICAN ELECTROCHEMICAL
SOCIETY, SEPTEMBER 30-OCTOBER 2, 1918
The recent order of the Government (made public September
5) commandeering colleges, universities, and technical schools,
rendered it inadvisable to attempt to hold the meeting at
PROGRAM OF PAPERS
The Oscillatory Current Induction Furnace. E. F. Northrup.
Processes Within the Electrode which Accompany the Discharge of Hy-
drogen and Oxygen. D. P. Smith.
The Sign of Potential. O. P. Watts.
An Apparatus for the Separation of Radium Emanation and Its Determina-
tion Electroscopically. J. E. Underwood and H. Schlundt.
Notes on the Heterogeneous Equilibrium of Hydrogen and Oxygen Mixed
with Radium Emanation. S. C. Lind.
Hardness of Soft Iron and Copper Compared. F. C. Kelley.
Nitrogen Fixation Furnaces. E. Kilburn Scott.
Relative Volatilities of Refractory Materials. W. R. Morr.
The Discharge Characteristics of a Common Type of 2H"by 6" Dry Cell
C. A Giixingham.
Symposium on Electrochemistry After the War
The Electric Furnace After the War. F. A. J. FitzGerald.
The Future of Electric SteeL J. A. Mathew.
Electric Pig Iron After the War. R. Turnbull.
The Future of Electrolytic Chlorine. A. H. Hooker.
Commercial Uses of Chlorine. V. R. Kokatnur.
The Government and the Technical Man After the War. F. A. Lidburv
Tariff Problems in the Electrochemical Industries. Grinnell Jones.
The War and the Nitrogen Industry. W. L. Landis.
The Power Situation After the War. C. A. Winder.
Research After the War. W. D. Bancroft.
NOTL5 AND CORRESPONDENCE
PLATINUM REGULATIONS1
The following regulations are hereby promulgated under the
provisions of the Act of October 6, 1917 (40 Stat. 383), as amended
by the Act of July 1, 1918 (Public Xo. 1S1), authorizing the
Director of the Bureau of Mines, under rules and regulations
approved by the Secretary of the Interior, to limit during the
period of the war, the sale, possession, and use of platinum,
iridium, and palladium, and compounds thereof
Section I — The War Industries Board is hereby designated
under Section 21 of the Act of October 6, 191 7, and the Pres-
ident's proclamation of October 26, 191 7, as the agent of the
Director of the Bureau of Mines in the execution of the regula-
tions as hereinafter indicated.
Section II — From and after the date of these regulations un-
der the penalties prescribed by Section 19 of the Act of October
6, 191 7, 2 no person3 shall:
(A) Use any platinum or platinum scrap, iridium or iridium
scrap, palladium or palladium scrap, and, or, compounds thereof,
1 Released October 1. 1918
'Section 19 of the Act of October 6. 1917, is as follows: "That any
person violating any of the provisions of this Act. or any rules or regulations
made thereunder, shall be guilty of misdemeanor, and shall be punished by a
fine of not more than 55,000 or by imprisonment not more than one year
or by both such fine and imprisonment."
» The word "person," for the purposes of these regulations, shall be
construed in accordance with the definition contained in Section 4 of the
Act of October 6, 1917, which is as follows: "That the word 'person1
when used herein shall include States, Territories, the District of Columbia,
Alaska, and other dependencies of the United States, and municipal sub-
divisions thereof, individual citizens, firms, associations, societies, and
corporations of the United States and of other countries at peace with the
United States."
in the manufacture, alteration, or repair of any ornament or
article of jewelry.
(B) Manufacture for use in dentistry any metal, metal parts,
or alloys containing more than 20 per cent by weight of platinum,
or 40 per cent by weight of platinum, iridium, and, or, palladium
combined, or manufacture supplies therefrom.
Section III — From and after the date of these regulations,
under the penalties prescribed by Section 19 of the Act of Octo-
ber 6, 1917, no person shall without a license:
(A) Purchase, sell, barter, or deal in unmanufactured plat-
inum, iridium, or palladium, or compounds thereof (including
crude, scrap, filings, polishings, or sweeps) except that sales may
be made without a license to an authorized agent of the United
States or to a licensee authorized to purchase the same; or
possess for more than ninety days after the date of these regula-
tions one ounce Troy, or more, of such unmanufactured plat-
inum, iridium, palladium, or compounds thereof.
(B) Possess, use, sell, purchase, or barter, for purposes con-
nected with his business, platinum, iridium, palladium, or com-
pounds thereof (except that sales may be made without license
to an authorized agent of the United States, or to a licensee
authorized to purchase the same) if such person be engaged in:
1 — Producing platinum, iridium, or palladium, or compounds
thereof by mining.
2 — Producing sulfuric acid, nitric acid, or other chemical
products where platinum, iridium, palladium, or compounds
thereof are used in such production.
3 — Importing or exporting platinum, iridium, or palladium,
or compounds thereof.
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
867
4 — -Producing platinum, iridium, or palladium, or compounds
thereof, either as a primary product or as a by-product of smelt-
ing or refining.
5— Manufacturing electrical appliances and, or, parts thereof
containing platinum, iridium, or palladium or compounds thereof.
6 — Manufacturing surgical appliances and X-Ray apparatus
containing platinum, iridium, or palladium, or compounds thereof .
7 — Manufacturing chemical apparatus and reagents of all
kinds containing platinum, iridium, or palladium, or compounds
thereof.
8 — Conducting or operating chemical laboratories in which
platinum, iridium, or palladium, or compounds thereof are used.
9 — Manufacturing scientific instruments containing platinum,
iridium, or palladium, or compounds thereof.
10 — Manufacturing and, or, distributing dental supplies con-
taining platinum, iridium, or palladium, or compounds thereof.
11 — Manufacturing and, or, dealing in jewelry containing
platinum, iridium, or palladium, or compounds thereof.
12 — Manufacturing or producing any article or product not
mentioned above where such business requires more than one
ounce Troy per month of platinum, iridium, or palladium, or
compounds thereof.
Section IV — Applications for licenses shall be made under
oath to any licensing agent duly authorized under the Act of
October 6, 1917, as provided in the regulations issued under this
Act.
Section V — Every applicant for a license will be required to
submit with his application a sworn inventory of all plaLinum,
iridium, or palladium, or compounds thereof, in his possession
or control ; and every licensee will be required to submit at such
times as may be designated by the War Industries Board a sworn
inventory of his holdings of platinum, iridium, or palladium, or
compounds thereof, in whatever form they may be.
The Director of the Bureau of Mines at the request of the
War Industries Board may at any time require from any user
or possessor a detailed sworn inventory of any and all materials
held by him containing platinum, iridium, palladium, or com-
pounds thereof, and such inventory must be furnished promptly
upon receipt of such requirement.
Section VI — All licenses shall be issued in the name of the
Director of the Bureau of Mines and countersigned by the War
Industries Board, and shall be, and remain, subject to the fol-
lowing conditions:
(A) Each license shall contain such appropriate conditions as
the Bureau of Mines through the War Industries Board may
impose.
(B) The Bureau of Mines through the War Industries Board
may change the conditions of the license from time to time, as
it may deem necessary.
(C) Records shall be kept by each licensee of all his sales, pur-
chases, and other transfers of platinum, iridium, or palladium,
or compounds thereof, and of articles containing platinum, irid-
ium, or palladium, or compounds thereof, with the names and
addresses of the purchasers, sellers, and, or, transferees, and the
quantities involved, which records shall be open at all reason-
able times to the duly authorized representatives of the Director
of the Bureau of Mines.
(D) Any and all platinum, iridium, or palladium, or com-
pounds thereof, acquired under the authority of such license,
shall be used strictly for the purposes and in the manner stated
in such license.
(E) Upon request of the War Industries Board, the licensee
shall report the prices at which sales of his products containing
platinum, iridium, or palladium, or compounds thereof, are
being made, and the right to prohibit further sale of such arti-
cles at prices deemed exorbitant by it is reserved to the War
Industries Board.
Section VII — Any licenses issued hereunder may be revoked
for violation of any of these regulations, or for violation of any
of the conditions contained in such license, or if such revocation
is deemed necessary or advisable for purposes of the National
Security and Common Defense.
Section VIII — The War Industries Board will, upon request,
furnish a list of Government agents or licensees authorized to
purchase platinum, iridium, or compounds thereof. Neither the
United States nor its representatives will assume any responsi-
bility, financial or otherwise, where sales are made to licensees.
Section IX — The prices at which platinum, iridium, or pal-
ladium will be purchased by a duly authorized agent of the United
States or by such licensee as may be authorized to purchase or
sell platinum, iridium, or palladium, or compounds thereof, will
be such prices as may be determined by the proper Govern-
mental agency authorized to determine such prices.
Section X — Whenever such Government agents and such
licensees as may be authorized to purchase platinum, iridium, or
palladium, or compounds thereof, shall refuse to purchase the
same from any person who is compelled by these regulations to
sell the same, or is forbidden by these regulations to possess or
use the same then such person shall promptly notify the Plat-
inum Section, War Industries Board, Washington, D. C.
Section XI — These regulations shall not operate to relieve
any person upon whom an order requisitioning platinum, iridium,
or palladium, or compounds thereof, may have been or may
hereafter be served, from any obligation imposed upon him by
such order.
Section XII — These regulations are supplemental and amend-
atory to the regulations heretofore issued under the Explosives
Act of October 6, 191 7.
PLATINUM WANTED BY THE GOVERNMENT
Editor of the Journal of Industrial and Engineering Chemistry:
Replying to your letter of recent date I beg to advise you that
the Government is desirous of procuring platinum and will re-
ceive deposits of that metal in any form and in any amount.
Payment will be made at the rate of $105 per ounce after the
value has been determined by melt and assay and nominal charges
to cover the cost of determining the value of the deposits are
deducted.
I have designated the United States Assay Office at New York
as the Government institution to receive deposits of platinum.
Packages should be sent to the following address: The Super-
intendent, United States Assay Office, New York, N. Y.
(Signed) R. T. Baker
Director of the Mint
TWO LETTERS ON REPRODUCING BEILSTEIN'S HAND-
BUCH DER ORGANISCHEN CHEMLE
Editor of the Journal of Industrial and Engineering Chemistry:
I will be one of 1000 to pay not to exceed $50 for a copy of
Beilstein, I believe you could readily procure sufficient sub-
scribers to such an undertaking. Why ask anyone to donate
$30,000?
South Bbnd. Ind.ana S. J. McGRATH
September 12, 1918
EdiiOl "f the Journal of Industrial and Engineering Chemistry:
I have noticed with much interest yaui editorial in the last
number <>l the JOURNAL on the subject of reprinting Beilstein,
and I might say that my patriotic sentiments are not entirely
1 by your suggestion, but I would go you one better
and suggest the photographing and reprinting of I'ricdlander, or
868
THE JOURNAL OP INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No.
Schultz-Huemann, or some other complete edition of the Ger-
man chemical patents.
I happen to be one of the fortunate who have Beilstein, but I
would like another copy for laboratory use.
My company is not one of the largest ones and therefore
could not subscribe the $30,000, but wc will take one copy at
$100 instead of the Sio, which you suggest. In fact, if it came
down to the scratch you might induce us to pay twice that
amount, and we would subscribe proportionally to the reproduc-
tion of any one of the editions giving the German patent speci-
fications.
I think this is a splendid suggestion on your part. I hope
you will push it with all possible speed, and as you say, let the
Huns do the worrying about our patriotism. I do not think
that this will be very cruel, because 1 think they will have
other things to worry about which will ease the pain caused by
this slight offensive.
Peerless Color Company R. W. CornElison
Bo..nd Brook, n. J. President and General Manager
September 20. 1918 s
LIBRARY FOR EDGEWOOD ARSENAL LABORATORY
Editor of the Journal of Industrial and Engineering Chemistry:
Attached herewith is a copy of a letter which I recently
addressed to our Commanding Officer, Colonel Wm. H. Walker.
It is self-explanatory. Colonel Walker has approved my sug-
gestion that I write to you. Since writing the above we have
located a copy of Beilstein's Organische Chemie, Metallurgical
and Chemical Engineering, Transactions of the American Society
of Testing Materials, Chemical Abstracts.
The attached letter (copy) to Prof. V. H. Gottschalk, Uni-
versity of Missouri, is one which is also self-explanatory. Prof.
Gottschalk's letter as well as others which we have received are
full of splendid patriotism and scientific interest.
From what you saw here on your recent visit, you can
readily appreciate our need of any files of the well-known chem-
ical journals. Will you give us a lift? We dream of the Amer-
ican Chemical Journal, Journal of the Chemical Society, Liebig's
Annalen, the Berichte, and others.
Chemical Laboratory (Signed) Wm. LLOYD Evans
Edcewood Arsenal Major, C.W.S., U. S. A.
September 20, 1918 J
Col. Wm. H. Walker.
Commanding Officer,
Baltimore, Md.
Dear Sir:
As we arc becoming more settled in our laboratory work,
the need for the well-known handbooks and chemical journals
becomes more apparent daily. Wc are badly in need of such
works as Beilstein's Organische Chemie, Landolt-Bornstein
Tabellen, Journal of the American Chemical Society, Journal of
Industrial and Engineering Chemistry, Metallurgical and Chem-
ical Engineering, Journal of the Sanely of Chemical Industry,
Transactions of the A merit an Society of Testing Materials, Trans-
actions of the American Electrochemical Society, and many
others that readily suggest themselves. Through the kindness
of the duPont Company, of Wilmington, we have been able
b locafc thi owners of a few of these desirable works, but as
you can readily imagine they are very difficult to obtain. You
will be happy to know that l>r. Lra Remsen has offered us his
Gmelin-Kraul as a loan.
It has occurred to me that a notice placed in the Journal
of Industrial and Engineering Chemistry and also in Science, ex-
plaining the needs of this laboratory, might bring forth loans
of books we greatly desire. If the Commanding officer, Edge-
wood Arsenal, concurs in this view, might I respectfully sug-
gest that this notice be asked for, and that all communications
in reference to the same be made to the Commanding Officer,
Edgewood Arsenal?
(Signed) Wm. Lloyd Evans,
Chemical Laboratory Major, C. W. S , V. S. A.
Edgewood Arsenal
August 31, 1918
AGREEMENT
The Edgewood Arsenal acknowledges the loan by Mr V.
H. Gottschalk of the books on chemistry and related subjects,
listed below, and agrees to return them without damage at the
end of the war. In case of damage or loss involving any or all
of the books mentioned, the Edgewood Arsenal assumes liability
therefor up to 150 per cent of the original price.
It is understood that the cost of packing and shipping the
books to and from Edgewood Arsenal will be borne by the Gov-
ernment.
The following books are included in the above agreement:
Handbuch der anorganischen Chemie, Abegg, 6 Vols.
Handbuch der angewandlen physikalischen Chemie, to date
of last issue shipped to America.
Arendt's Sammlung Cltem. und Chem.-Tech. Vorlrage, Vols.
i-i5-
Moissan, Traite de Chimie Mineral.
Zeitschrift fur physikalische Chemie, Vols 42-70, Index 25-50.
Annalen der Physik (Drude), Vols. 1-36.
Winkelmann, Handbuch der Physik (Optik, Vols. 3, 4, 5, is
loaned to Prof. Dean).
(Signed) Wm. H. Walker
Chemicaj. Laboratory Colonel, C.W.S., U. S. A.
Edgewood Arsenal
August 30. 1918
ORDNANCE DEPARTMENT, SCHOOL OF EXPLOSD/ES
MANUFACTURE, COLUMBIA UNIVERSITY
The Ordnance Department of the Army, particularly in
the Production and Inspection Divisions, is in need of men with
training in the manufacture of explosives and the related raw
materials. The manufacture of explosives is developing out of
proportion to the number of men in the country who have had
training and experience in that work. To meet this condition
the War Department Committee on Education and Special
Training is establishing in the Department of Chemical Engi-
neering at Columbia University in the City of New York an
Ordnance Department School of Explosives Manufacture.
The object of this School is to give men with proper preliminary
qualifications the training necessary to fit them for use by the
Ordnance Department as commissioned officers in the super-
vision of factory operation and inspection of the finished products
in plants manufacturing explosives and raw materials for ex-
plosives.
The school will be only for enlisted men in the military service
who are detailed for instruction in the school by the Ordnance
Department. The ways in which students will be obtained are
three:
1 — Transfer of men already in the military service.
2 — Induction of men of draft age who have not yet been
called.
3 — Volunteer enlistment of men not in draft age.
The minimum requirement as to technical training for ad-
mission will be graduation from a recognized college or uni-
versity with a bachelor's degree in chemistry or chemical engi-
neering, or factory experience of equivalent character.
The course of training will be of [3 weeks' length anil will
consist of:
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
869
1 — Military drill and instruction
2 — Class room and lecture instruction
3 — Laboratory and plant work
4 — Visits to plants
In the course of study the men will be made familiar with the
methods of manufacture, of factory control, and of inspection
of explosives such as smokeless gunpowder, trinitrotoluol,
picric acid, ammonium nitrate, toluol, phenol, etc. The particu-
lar subjects on which emphasis is laid in the course will vary
from period to period with the need for men trained for work
in particular groups of plants.
While in the school each man will be rated both as to his
technical performance and personal qualities exhibited. On the
satisfactory completion of the course this rating will be made the
basis of recommendation for a commission as second lieutenant
in the Ordnance Department. The granting of commission
will depend upon the number of commissions available and the
varying needs of the Ordnance Department. While worthy
graduates are expected to be commissioned, it is understood that
commissions are not guaranteed. In any case the graduates of
the school will be utilized in technical work by the Ordnance
Department whether commissioned as officers or not.
The assignment of men for the first session has been com-
pleted. The second session will start about December 1 and
arrangements for assignments to it should be made about one
month earlier.
The general plan is to devote the morning hours to lectures
and reading, and the afternoons to laboratory practice. Dur-
ing the course considerable time will be spent in plants actually
manufacturing explosives or explosive raw materials. In
common with the enlisted men, students in the other special
army school at Columbia, students in this school will have the
military drill of the post, amounting to about an hour and a half
daily.
First and Second Weeks
9-10 a.m. each day. Lectures on the general principles
governing the manufacture of explosives and
the tests for quality.
10-11 a.m. two days a week. Lectures on military regula-
tions and relations.
1-5 p.m. Laboratory practice in testing acceptable and
unacceptable samples of explosive raw ma-
terials such as benzol, toluol, nitric acid, etc.
Third and Fourth Weeks
9-10 a.m. each day. Lectures on the methods of manu-
facture and of testing picric acid and ammo-
nium picrate and the raw materials from which
they are made.
10-1 1 a.m. two days a week. Military lectures continued.
1-5 p.m. Laboratory practice on picric acid, ammonium
picrate and related materials.
Two days of the third week to be spent at a picric acid plant
in New Jersey.
Fifth Week
9-10 a.m. each day. Lectures on the methods of manu-
facture and testing of toluol, benzol, solvent
naphtha and xylol.
10-1 1 a.m. two days a week. Military lectures continued.
I 1-5 p.m. Laboratory practice with hydrocarbons.
Two days at hydrocarbon plants in vicinity of New York City.
Sixth and Seventh Weeks
9-10 a.m. each day. Lectures on the methods of manu-
facture and of testing trinitrotoluol.
10-11 a.m. two days a week. Military lectures continued.
1-5 p.m. Laboratory practice with trinitrotoluol.
Two days spent at the TNT plant at Renville, N. J.
Eighth and Ninth Weeks
9-10 a.m. each day. Lectures on the methods of manu-
facture and testing of guncotton and smoke-
less gunpowder.
10-11 a.m. two days a week. Military lectures continued.
1-.5 p.m. Laboratory practice with guncotton and Btnolte
less gunpowder.
Two days spent at smokeless powder plant at Parlin, N. J.
Tenth Week
9-10 a.m. each day. Lectures on methods of manufacture
and testing of ammonium nitrate, ammonium
nitrate, TNT mixtures, and shell filling.
1-5 p.m. Laboratory practice with ammonium nitrate and
ammonium nitrate mixtures.
One day at shell loading plant at Perth Ainboy, N. J.
Eleventh Week
9-10 a.m. each day. Lectures on the methods of manu-
facture and testing of tetryl and tetrani-
traniline.
1-5 p.m. Laboratory practice with tetryl and tetrani-
traniline.
Two days at a tetryl or tetranitraniline plant.
Twelfth Week
9-10 a.m. each day. Lectures on the methods of manu-
facture and testing of mercury fulminate, other
detonators, and fuses.
1-5 p.m. Laboratory practice in connection with detona-
tors and fuses.
One day at plant manufacturing or using detonators, Pompton
Lakes, N. J.
It is understood that the field covered by the school will vary
from period to period as the needs of the Ordnance Department
for men trained for work in particular types of plants may vary.
CHEMISTRY FOR SOLDIERS IN TRAINING CAMPS
Editor of the Journal of Industrial and Engineering Chemistry:
It suggests itself to me that the Publicity Committee of the
American Chemical Society should extend its activities into
the training camps of the United States Army.
There is no question in anybody's mind but that the war is
primarily a chemical war. It has been stated that the man
with the most gas will win the war.
We are desirous, as a Society, to increase the influence of
chemistry and chemists in the country and the best way that
we can do it to-day is to take upon ourselves as a Society to sup-
ply elemental chemical information to the soldiers of our Army.
All the men have had at least public school training, so that by
primitive similes, it should be possible for a speaker to make
chemistry, so far as it relates to the war, at least interesting to
the men in the ranks. I feel that this is a golden opportunity
for us, which has not as yet, to my knowledge, been taken care
of. J. W. Beckman
San Francisco, Cal.
September 7, 1918
THE EMBLEM OF THE AMERICAN CHEMICAL SOCIETY
Editor of the Journal of Industrial and Engineering Chemistry:
Mr. Charles A. Doremus' letter in the August issue of This
Journal concerning the change of the emblem of the American
Chemical Society must deserve due attention from the mem-
bers of the Society. The Society's present emblem must be
changed, not because it pictures an apparatus of German in-
vention, but because the emblem does not represent chemical
science in any way. Personally, I do not see how a CO2 ab-
sorption bulb can express or convey any wide thought of chemical
science and its practice. The emblem of the American Chem-
ical Society should be of such a design that it would express
the spirit and the scope of chemical science and should have a
business-like and dignified appearance. 1 confess I do not wear
the present emblem, for it is too superficial and has no scientific,
n-rhnical, or business-like aspect Something must be done to
raise the standard of the Society's emblematical expression.
For my part, as a membei of the American Chemical
I suggest thai Mendeleeff'a p riodic law be taken as the basis
for designing a new, first class emblem,
nat.onm. Carbon company Gregory Torossian
c'r.i:vm.AND. August. .'i'. 1918
870
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 10
WASHINGTON LLTTLR
By Paul Wooton, Union Trust Building, Washington, D. C.
Only minor changes will be made in the War Minerals Bill in
conference. While the conferees have not met as yet, Rep-
resentative Foster, the Chairman of the Committee on Mines
and Mining of the House of Representatives, is willing to accept
the bill as re-written by Senator Henderson, the Chairman
of the Committee on Minos and Mining of the Senate.
The Senate committee objected strenuously to the minimum
price principle which was contained in the House bill. It
feared that conditions easily could become such as to cause the
Government to incur onerous obligations. The committee
therefore elaborated the contract principle, which also had the
approval of the House, which would lessen the Government's
liability. The appropriation was increased from $10,000,000
to $50,000,000. The sum, however, is to be a revolving fund
and probably will be returned to the Treasury when the emer-
gency has passed. In addition, the bill carries $500,000 for
administration expenses.
The Senate committee also disapproved of the licensing
feature. After hearing from a large number of well-qualified
witnesses, it appeared to be the consensus of opinion that the
legislation could be administered successfully without the
annoyance to the industries handling war minerals, which
certainly would accompany a licensing plan such as that pro-
vided in the Lever Act or in the Explosives Act.
Phosphorus is the only mineral added to the list by the
Senate. Sodium, however, was substituted for "sea salt."
Phosphorus was added because of the greatly increased demand
for its use in smoke screens. Senator Smoot made an ineffectual
effort to amend the bill so as to take from under its jurisdiction
chalk, fluorspar, fuller's earth, kaolin, and mica. Mr. Smoot
insisted that those substances need not come under control at
this time and that the bill should be restricted to the war minerals
where the need of control is evident. He declared that the
bill could be amended in a week at any time the War Industries
Boaid would show cause for adding to the list. The bill, as
passed, contains the following minerals: metallurgical products
and their chemical compounds, antimony, arsenic, ball clay,
bismuth, bromine, cerium, chalk, chromium, cobalt, corundum,
emery, fluorspar, ferrosilicon, fuller's earth, graphite, grinding
pebbles, iridium, kaolin, magnesite, manganese, mercury,
mica, molybdenum, osmium, sodium, platinum, palladium,
paper clay, phosphorus, potassium, pyrites, radium, sulfur,
thorium, tin, titanium, tungsten, uranium, vanadium and
zirconium.
The consideration of the War Minerals Bill occasioned debate
for the greater part of two sessions, but the bill was not amended
in important particulars. The committee accepted in advance
such amendments as were adopted. The President has written
Senator Henderson to assure him that he has done an important
service in securing the passage of a bill which is apparently so
workable.
Imports and exports of certain chemical materials, as reported
by the Department of Commerce for July 191 8, and the figures
for July 1917, as finally revised, are as follows:
July July
Exports 1917 1918
Acids:
Carbolic J 726,109 $ 101,883
1,943,632 1,257,864
Sulfuric 65.726 142,195
Dves and dycslufls 1,278,709 1,428.669
Given in. . 234.873 245,164
Medical preparations 637,809 979 078
Caustic soda 604,261 423.773
Soda ash 398,859 372.940
Total Cukmicals 12,777,324 12,584,853
July July
Imports 1917 1918
Arsenic $ 18.231 $ 39.833
Creosote oil 121.240 23.953
Colots or dyes 105,372 211.721
Inilifio 462.432 504,716
Total coal-tar distillates 754,220 797 101
Camphor, crude 211,440
Shellac 350,199 619,760
Nitrate of potash 228,799 71,365
Nitrate of soda 4,781.100 6,445,280
Total Chemicals 11,152,394 12,468,950
It is regarded as so essential that officials are urging industries
to take organized steps to acquaint district boards with their
needs, so that the most intelligent action can be taken. It is
pointed out that confusion is certain to result if each employer
tries to take up the matter with the draft board himself. Each
industry, it is suggested, would do well in selecting an individual
or a committee to devote entire time to this very important
matter. Experience has shown that systematic effort along
such lines has been very helpful to industries and at the same
time has made easier the task which confronts each district
board.
The Provost Marshal General has made it very clear that the
spirit of the regulations is to construe liberally the provisions
regarding the deferment of necessary employees. The working
of the new questionnaire makes possible a broader interpreta-
tion. It is quite generally understood that workmen necessary
to the operation of a plant are to be given deferred classification
but the same is not true of the administrative force, or of those
engaged in selling and purchasing for necessary industries.
The General Staff has outlined definitely what it regards as the
essential occupation, so far as operatives are concerned, in the
manufacture of sulfuric acid. That list includes: works mana-
ger; plant superintendents; chief chemist; trained chemists-
doing actual supervision of process work; chief engineer; elec-
trical engineer; mechanical engineer; burner men for mechanical
furnaces; chamber men; contact process men; power house
engineer; concentrator operators; concentrator testers doing
supervisory work; tank-car line supervisors; locomotive engi-
neers, firemen, and yard masters (included only where factory
includes an industrial standard gauge railroad); locomotive,
mono-rail, bridge, and gantry crane operators; heads of clerical
departments certified by the plant management as essential to
continuous operation; maintenance engineer; master mechanic;
foremen of skilled trades, including brick masons, boiler makers,
carpenters, electricians, iron workers, machinists, pipe fitters;
sufficient skilled men of each of above skilled trades as may be
certified by the plant management as essential to continued
operation; lead burners. Special police and truck drivers are
regarded as necessary employees whom it would be difficult to
replace by men over draft age. While the General Staff does
not make mention of the necessary employees in the offices, it is
obvious that they are to be given as careful consideration by
district boards as are workers in the plants.
After much preliminary heralding, the War Industries Board
made public on Sept. 9 its new preference list of industries.
The list was made up after extended experience in meeting
essential requirements and has met with very general approval.
While Chairman Baruch is in receipt of numerous protests from
industries which believe they should be included, the consensus
of opinion apparently is that the list could not be expanded
greatly and attain its object.
Under Class 1 are grouped those industries of exceptional
importance in carrying on the war. The requirements of the
industries in that group for fuel, electric energy, labor, and
transportation will be satisfied fully before attention is paid
to the wants of the remaining three classes. Among the other
three classes, there is to be no absolute preference. Their re-
quirements will be given preference over the industries which are
not included in the list, but it does not mean that the require-
ments of Class 2 wnll be fully satisfied before providing any
of the needs of Class 3. It may be necessary in many instances
to keep an industry in Class 4 partially supplied at the expense
of an industry in Class 2. The list does indicate, however.
that the Class 2 industry is of relatively greater importance
than a Class 3 or a Class 4 industry.
With the extension of the draft ages, the matter of industrial
exemption, ill the words of an officer in the Provost Marshal
General's office, changes from an important to a vital question.
The text of the War Department's announcement advising
of the suspension of work on the Muscle Shoals power plant is
as follows:
The Ordnance Department announces that the temporary suspension
of work on the water power development at the Muscle Shoals nitrate
plants will not in any way affect the production of nitrates at these or any
of the other plants now engaged in their production.
This action was taken upon the representation of the War Industries
Board and affects only the erection of the huge water power plant being
built on the Tennessee River, power from which was not anticipated for
4 or 5 years. The water power development was undertaken by the War
Department in line with its established policy of utilizing these nitrate
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
87i
plants for the benefit of agriculture after the war is over, when the water
power plant would be available.
Work is progressing rapidly on the Muscle Shoals plants, one of which
is about 60 per cent complete, and over 20,000 men are now employed there.
Power for their operation is obtained from a steam-electric station erected
■an the Tennessee River, and also purchased from the Alabama Power Com-
pany. This power is adequate for the operation of the nitrate plants. The
water power development was projected merely to obtain cheaper power in
future years.
The nitrate division of the Ordnance Department has taken
•over the experimental ammonia plant and laboratory which has
been conducted near Washington by the Department of Agri-
culture. The work is in charge of R. O. E. Davis and L. H.
Greathouse.
Following experiments with lenses for air pilots' glasses, the
Medical Research Board of the Division of Military Aeronautics
announces that it has been able to effect the casting of certain
substances in thin sheets which, while not glass, can be used as
such and may afford a practical substitute for it in goggles.
This substance has been on the market for some time but the
company which makes it has not up to the present been able
to cast it in the right strength and thickness suitable for goggles.
Under the direction of the Medical Research Board, thin
sheets of the material have been produced which not only are
of the proper texture and thickness but can be ground and
polished. The substance is hard and non-inflammable and in-
sures practically a non-shatterable lense for the protection of the
pilot's eyes.
By order of the Secretary of War, the Training Camp for
the Chemical Warfare Service, now under construction at
Lakehurst, N. J., is designated as "Camp Kendrick."
This new camp is named in honor of Professor (Colonel,
retired) Henry L. Kendrick, LL.D., who, after considerable
service as a commissioned officer, served as professor of chem-
istry, mineralogy, and geology at the U. S. Military Academy
from March 3, 1857, until his retirement from active service,
December 13, 1880.
Henry L. Kendrick was appointed a cadet at the Military
Academy from New Hampshire, Sept. 1, 1831; Second Brevet
Lieutenant, Infantry, July 1, 1835; Second Lieutenant, April 1,
1836; First Lieutenant, June 20, 1837; Captain, June 18, 1846;
Brevet Major of Volunteers, for gallantry and meritorious
conduct in the defense of Pueblo, October 12, 1847; Professor,
Military Academy, March 3, 1857; Brigadier General Volunteers
(declined), Sept. 23, 1862; retired as Colonel, December 13,
1880, at his own request, having served 45 years as a com-
missioned officer and being over 62 years of age.
He received the degree of LL.D., March 3, 1857. He died
in New York City May 24, 1891. He had no leave of absence
from 1863 to 1880.
PERSONAL NOTL5
Dr. Lucius P. Brown, who, following an investigation of the
health department by the Hylan administration. New York
City, was recently tried on charges of neglect of duty, acquitted,
and unanimously reinstated as Director of the Bureau of Foods
and Drugs of the New York Health Department, has now ob-
tained a leave of absence for the duration of the war to accept a
commission as captain in the food and nutrition division of the
Sanitary Corps of the Surgeon-General's office.
Dr. J. Bishop Tingle, professor of chemistry at McMaster
University, Toronto, has been elected a fellow of the Royal
Society of Canada.
Mr. George C. Bunker, in charge of water purification. Canal
Zone, has been engaged by the municipality of Lima, Peru,
to investigate the water supplies now in use and those available
for future use.
Mr. E. R. Meyer, formerly connected with the City of Toledo
Water Department as chief chemist for seven years and for the
past year connected with the Trommer Co., Fremont, O., is
now with the Diamond Match Co., Oswego, N. Y., as assistant
chemist.
Mr. Hamden Hill, research chemist of the Texas Oil Co., Bay-
onne, N. J., plant, died at St. Luke's hospital, New York City,
on September 23, 1918, astheresult of burns due to an explosion
of gasoline vapors in the laboratory.
Dr. H. K. Benson, director of the Bureau of Industrial Re-
search, University of Washington, has been commissioned
captain in the nitrate division of the Army Ordnance Depart-
ment. He will make investigations relative to the use of the
arc process in nitrogen fixation. Until his entrance into the
army, Dr. Benson acted as chief consultant for the American
Nitrogen Products Co., Seattle, which is operating a com-
mercial plant for the production of sodium nitrite at La Grande,
Washington.
Mr. M. H. Barnes, formerly chemist for the Illinois Steel
Co., Gary, Indiana, is now division inspector for the Aluminum
Company of America, Maryville, Tenn.
Miss Irene DeMatty, for several years librarian of the
Mellon Institute, Pittsburgh, and compiler of the New Publica-
tions column of This Journal, was married in Greenville, CaL,
on September 2, 1918, to Mr. Robert James Piersol.
Mr. Albert H. Carle, formerly instructor in chemistry at
Union College, Schenectady, N. Y., is now employed in the
chemical department of the Continental Can Co., Inc., Canons-
burg, Pa.
Mr. W. Jesse Brown has resigned his position as division engineer
for the l'ortland Cement Association to accept a com
as captain in the Ordnance Department, Nitrate Dim ion,
he will be stationed at U. S. Nitrate Plant No. 1, Sheffield, Ala.
Mr. Harold Ralph Wells, formerly graduate student and
teacher in chemistry at the University of Michigan, after nearly a
year's training in the Aviation Section of the Signal Reserve
Corps, has been commissioned Second Lieutenant and is stationed
at Park Field, Tenn., training fliers.
Mr. L. H. Goebel has resigned as superintendent of filtration
and chief chemist of the Water Filtration Plant of the Union
Stock Yard and Transit Co., Chicago, 111., to become associated
with the engineering staff of Wallace and Tiernan Co., manu-
facturers of chlorine control apparatus and sanitary engineering
specialties.
Dr. Earl F. Farnau, formerly assistant professor of chemistry'
at New York University, has been appointed associate professor
of organic chemistry at the University of Cincinnati.
Mr. Ross A. Baker, Chief Gas Officer, Camp Pike, Ark., has
been made officer in charge of gas training for Chief Gas Officers,
Army Gas School, Camp AA, Humphreys, Va. Mr. Baker was
formerly assistant professor in chemistry at the University of
Minnesota.
Mr. Arthur Lowenstein, a member of the Chicago Section of the
American Chemical Society, has been elected vice president of
Wilson and Company of Chicago.
Dr. Ralph E. Oesper, formerly assistant professor of chemistry <
at Smith College, has been appointed associate professor of
analytical chemistry at the University of Cincinnati.
Dr. Clifford J. Rolle and Dr. Leonora Neuffer have been
appointed instructors in chemistry at the University of Cin-
cinnati.
Professor F. P. Treadwell of Zurich, Switzerland, died sud-
denly of heart disease on June 25, 1918. Chemists generally
will feel his loss keenly as his excellent textbooks on analytical
chemistry are widely used. Treadwell, American by birth,
was born at Portsmouth, N. H., in 1857. In the early seventies
he attended school at Heidelberg, and later at the university was
lecture assistant from 1878 to 1881 under Bunsen. His subse-
quent professional service was at the Eidgenossiche Polytech-
nicum in Zurich.
Mr. J. Wilkird Hershey, who for six years has had charge of the
physics and chemistry departments at Defiance College, has
been appointed head of the chemistry department at McPherson
College, McPherson, Kansas.
Mr. F. O. Sprague, formerly with the Cattaraugus Tanning
Co. and Bcardmore & Co., is now supervising the tanneries of the
Transylvania Tanning Co., Brevard, N. C, the Toxaway Tan-
ning Co., and the Rosman Tanning Extract Co., Rosman,
N. C.
Dr. A. Ii. Coleman, formerly with the Federal DyestulT and
Chemical Corporation of Kingsport, Tenn., is now employed
as research chemist for the Ault and Wiborg Co., Cincinnati,
Ohio.
872
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 10
INDUSTRIAL NOTL5
Coal laud in West Virginia will be developed 1'-. the American
Eagle Colliery Co., Charleston, incorporated with a capital of
$600,000. The incorporators are George S. Crouch, Y. 1.
Black, L. G. Sumrnerfield, and others.
Cellulose Co., New York, financed by Yickers Co. and Nobel
Co., London, will build the $10,000,000 Cumberland, Md.,
cellulose manufacturing plant which the War I Apartment
recently announced would be commenced. Until the war is
won the cellulose products will In- taken by the Government for
airplanes; after that the Cellulose Company intends manu-
facturing acids, drugs, dyes, etc., from cellulose and other
materials.
The Mississippi Wood Products Company has been incorpo-
rated, with $500,000 capital, by W. B. Burke and P. H. Starts
of Charleston and G. E. Lamb of Clinton, Iowa. Output will
be wood alcohol and acetone manufactured from the waste of
the Lamb-Fish lumber mills.
A petition lias been presented to the Secretary of Industry
and Commerce, Mexico, for permission to develop petroleum
deposits believed to exist in Lower California.
The Atlantic Potash Corporation has been incorporated at
Dover, Del., with a capital of $1,000,000, to manufacture potash
and chemicals.
A new chemical plant will be erected at a cost of $1,000,000
at Mechanicsville, N. Y. The plant will utilize the by-products
from the West Virginia Pulp & Paper Company's plant in the
manufacture of acetone for aeroplane wings.
The Castle Chemical & Color Co., Valley Stream, N. Y„ has
been incorporated with a capital of $300,000 by H. B. Knapp,
I. J. Hartof, and E. Huneker.
The plant of the British-American Chemical Co., Ridgefield
Park, N. J., manufacturing chemicals for war use, is to be in-
creased by the erection of additions costing approximately
$1,500,000.
The U. S. Nitrate Co., Tacoma, Wash., has been incorporated
by J. E. Austin, J. E. Berkheimer, F. Campbell, and August
Stein, with a capital stock of $1,000,000.
The wood chemical plant at Lyles, Tenn., which the Bon
Air Coal and Iron Corporation of Nashville is building in ac-
cordance with contract to supply the Government with ma-
terials for explosives manufacturing, is expected to be ready
for operation by December 1. Each day the completed fac-
tory will produce from 2,000 to 3,000 gal. of wood alcohol,
40,000 lbs. of acetate of lime, and 10,000 bushels of charcoal.
All the alcohol and acetate of lime will be taken by the Govern-
ment for the purpose of manufacturing explosives, while the out-
put of charcoal will be burned in the Bon Air Coal and Iron
Company's iron furnace.
Importation of vegetable oils and material for their produc-
tion has trebled in value since the beginning of the war, and the
United States, in common with other parts of the world, has
greatly increased its consumption of food oils. With the de-
mand for animal fats for the men in the trenches, people at
home have turned to vegetable fats to take the place of the
meats, butter, cheese, and condensed milk which they are send-
ing to the battlefields. In addition to this, the war itself has
made great demands upon the vegetable oils of the world, as
a source of glycerin. A compilation by the National City
Bank of New York shows that the United States alone,
although the world's largest producers of cottonseed oil, im-
ported in 1917 approximately $75,000,000 of food oils and
material for their production, about one-fourth of this coming
from the Philippine Islands.
Witli something like 110,000 acres of castor beans now being
grown in the South under contract for the Government at a
fixed price, the war work authorities of the Government recently
took the next step in providing an adequate supply of castor
oil for the lubrication of the fleet of airships now being built.
After nearly three months of investigation, stmlv, and negotia-
tion, carried mi by cooperative efforts of the Signal Corps, the
War Industries Board, and the Bureau of Plant Industry, of the
United States Department of Agriculture, a contract has been
let for the establishment of a plant in tin- Smith at which it is
proposed to crush all the castor beans grown for the Govern-
ment in Florida and adjoining States. This plant is to
be located at Gainesville, Fla., and will be the largest castor-
oil plant in the world.
Ricketts& Company, Inc., mining, metallurgical, and chemical
1 , have opened new laboratories at Room 509, 80
Maiden Lane, New York City, where they are equipped for assay
and analytical work of all kinds, especially analyses of glycerin
and manganese.
Copper and iron products for maritime purposes will be manu-
factured by the Curtis Bay, Md., Copper and Iron Works,
incorporated with $1,000,000 capital by William F. Cochrane
of South Baltimore, Md., M. C. Whitaker of Curtis Bay, Md.,
Patrick H. Loftus of New York, and others.
The Harrison Works of E. I. du Pont de Nemours & Com-
pany have opened a new Chicago office at 1542 McCormick
Bldg., 332 S. Michigan Avenue. Under the direction of district
salesmanager, W. H. Hasse, this office will be devoted exclusively
to the sale of chemicals, pigments, and dry colors.
Messrs. A. E. S. Thompson & Company, handling large
quantities of chemicals and dyes in the Oriental market, have
established a San Francisco branch in the Merchants Exchange
Building for the convenience of their clientele in America.
The plant of the La Salle Portland Cement Co., of La Salle,
111. (known before the war as the German-American Portland
Cement Co.), has been taken over by the Alien Property Custo-
dian.
The Bureau of Markets has announced that 75,000 tons of
nitrate of soda were bought in Chile through the War Industries
Board and distributed to the farmers in this country at cost
through the Department of Agriculture.
A process for making soap out of paraffin is announced by
Dr. Bergman, at Leipzig. By the introduction of air the paraffin
is oxidized while heated to about 1300 in an iron boiler. The
result is a brown ointment-like substance which, when treated
with an alkali, produces a good lathery soap.
Phosphorus for war purposes may be manufactured at Tampa,
Fla., by the Government; 26,000 kilowatts of electric power
will be required. The War Department contemplates building
the plant and Major Wm. G. Lockwood is now investigating
as to the necessary facilities.
A $100,000 guncotton factory will be built by the Trinity-
Products Co., Dallas, Texas.
The Union Paint Co. of Manhattan has been incorporated
with a capital of Si. 000,000 by S. H. Mcintosh, C. Mayer, and
T. E- Byrnes, 120 Broadway, New York City.
The Southern Pine Tar and Oil Co., Savannah, Ga., has been
incorporated with S20o,ooo capital by Henry Henken, W. W.
Wilder, W. H. Proctor, and others. It will manufacture oil,
tar, and various other products from southern pine timber.
A number of Swedish cellulose factories have combined to
form a company for the production of alcohol from sulfite pulp.
A number of sulfite spirit factories are ready and during this
year nine new ones will be built and in 19 19 five more are
planned. Then a yearly production of 20,000,000 liters of
alcohol will be attained.
The U. S. Geological Survey estimates a record-breaking
outturn of copper for the current year. Even if the output
has increased, the demand keeps up in like proportion, so that
two records, one for consumption and another for production,
may be established during 191 8.
Members of the chemical trade in New York and vicinity,
at the suggestion of the National League for Woman's Service,
have raised $2566 to purchase and equip an ambulance to convey
wounded soldiers to the base hospitals from the vessels arriving
at Atlantic ports. This sum was made up as requested of
individual contributions not exceeding $100 each.
A mvsterious explosion occurred on August 19, 1918, at the
Strausscr Chemical Company's plant at Chauncey. N. Y . where
a big Government order for acids used in manufacturing ex-
plosives was being filled. The explosion did not occur in any
of the tanks of chemicals, but on the outside of the main build-
ing.
The Swedish dynamite industry is being seriously handicapped
by the scarcity of glycerin, and difficulties are being encountered
in providing the mining enterprises with sufficient quantities of
explosive. Recent experiments in the use of liquid air as an
explosive have resulted in several concerns procuring licenses
for using German methods for compressing air. Machinery
for these factories, which are regarded as war substitutes, has
to be imported from Germany.
Oct., 191S
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
GOVERNMENT PUBLICATIONS
By R. S. McBride, Bureau of Standards. Washington
NOTICE — Publications for which price is indicated can be
purchased from the Superintendent of Documents, Government
Printing Office, Washington, D. C. Other publications can
usually be supplied from the Bureau or Department from which
they originate. Commerce Reports are received by all large
libraries and may be consulted there, or single numbers can be
secured by application to the Bureau of Foreign and Domestic
Commerce, Department of Commerce, Washington. The regu-
lar subscription rate for these Commerce Reports mailed daily is
$2.50 per year, payable in advance, to the Superintendent of
Documents.
:
PUBLIC HEALTH SERVICE
The following foui articles make up Bulletin 112 of the
Hygienic Laboratory. 52 pp. Paper, 10 cents.
(1) Phenols as Preservatives of Antipneumococcic Serum,
Pharmacological Study (with Bibliography). Carl Voegtlin.
(2) Nature of Contaminations of Biological Products. I. A.
Bengtson.
(3) Studies in Preservatives of Biological Products, Effects
of Certain Substances on Organisms Found in Biological Prod-
ucts. M. H. Neill.
(4) Effect of Ether on Tetanus Spores and on Certain Other
Microorganisms. H. B. Corbitt.
NATIONAL ADVISORY COMMITTEE FOR AERONAUTICS
The third annual report of the National Advisory Com-
mittee for Aeronautics includes the following reports that are of
chemical interest. The full report covers 495 pages and is avail-
able from the Superintendent of Documents. Bound in paper,
$1.50.
Report 13. Meteorology and Aeronautics. Part 1, Physical
properties and dynamics of atmosphere; Part 2, Topographic and
climatic factors in relation to aeronautics; Part 3, Current
meteorology and its use. Prepared by WnxiAM R. Blair.
Submitted by Subcommittee on Relation of Atmosphere to
Aeronautics.
Report 14. Experimental Research on Air Propellers. Wil-
liam F. Durand. Part 1, Aerodynamic laboratory at Leland
Stanford Junior University and equipment installed, with
special reference to tests on air propellers; Part 2, Tests on 48
model forms of air propellers, with analysis and discussion of
results and presentation of same in graphic form; Part 3, Brief
discussion of law of similitude as affecting relation between
results derived from model forms and those to be anticipated
from full-sized forms.
Report 22. Fabrics for Aeronautic Construction, Subcom-
mittee on Standardization and Investigation of Materials.
Part 1, Cotton airplane fabrics, K. D. WhalEN; Part 2, Balloon
fabrics, contributed by Bureau of Standards, Balloon Fabric
Committee.
Report 23. Aeronautic Power Plant Investigations, Sub-
committee on Power Plants. Part 1, Performance of aeronautic
engines at high altitudes; Part 2, Radiator design; Part .< Spark
plugs, H. C. IlICKINSON.
GEOLOGICAL SURVEY
Bismuth in 1017. J. B. UmplEBY. Separate from Mineral
Resources iif the I'nited States, 1917, Part I. ,i i>i> Published
June 10
The demand for bismuth, unlike that for most other metals,
has not greatlj increa ed during the war. There continue to
be only two producers of bismuth in this country, so that the
production ma iven, bu1 it was verj littli in I
that for 1916, ami tin- wholesale price is understood l
•'bout 1, cent Pei 1 1 > lowei The bismuth produced in this
country is almost entirely a by-product obtained in the refining
of lead bullion. Market conditions have not heretofore justified
the recovery of bismuth at many plants where it could be ob-
tained from flue dust or bullion, and as the cose of mining and
delivery to these plants is charged against other constituents
of the ore, it is doubtful whether ore that is primarily valuable
for bismuth will ever command a ready market in this country
unless the use of the metal is greatly extended.
The imports of bismuth in 1917 were somewhat less than in
1 9 16, although greater than in 1915. Prior to the last decade
the supply of bismuth in this country was almost entirely im-
ported, but in recent years most of the imports have been dis-
placed by the domestic product. The industry, however, is
not a large one in this country, probably less than 250 short
tons annually being sufficient to meet the demand.
Selenium in 1917. J. B. UmplEby. Separate from Mineral
Resources of the United States, Part I. 1 p. Published June
19-
For the first time in recent years more than two companies
reported a production of selenium in 191 7, so that figures may
now be given. The output in 1917 was 39,630 pounds, valued
at $70,000.
Selenium, it is understood, was in demand in 1917, and the
principal producing company reports that its output has been
contracted for well into the future. This is in keeping with the
fact that the value of imports for consumption of selenium and
salts of selenium rose from $59 in 191 5 and $302 in 19 16 to
$2,236 in 1917.
The shortage of imported manganese suitable for the glass
industry has compelled the manufacturers of glass to seek a
substitute, and it is reported that selenium has been found to
be the most satisfactory.
Most of the selenium produced is a by-product in the electro-
lytic refining of copper. It is the opinion of metallurgists that if
market conditions warranted, the domestic production would be
greatly increased.
Prices at the refinery ranged from $1.29 to $3 per lb., but as
usual the price for small lots was much higher and ranged be-
tween wide limits, depending largely on the quantity purchased.
Tellurium in 1917. J. B. UmplEby. Separate from Mineral
Resources of the United States, 1917, Part I. 1 p. Published
June 19.
There continues to be little market for tellurium and a corre-
spondingly small production. Only two refiners, the Raritan
Copper Works and the United States Smelting, Refining &
Mining Co., reported a production in 1917.
Tellurium, like selenium, is a by-product from the electrolytic
refining of copper. Tin domestic production is capable of large
expansion if market conditions should warrant, as almost all
blister copper contains recoverable quantities of tellurium.
Much of this would be saved, if a demand existed, ^ prices ol
$1.50 to $2.50 per lb. In 1917 prices at tin- refinery averaged
about $3 per lb., but a very small additional out put would
probably have Hooded tin- market.
A Geologic Reconnaissance of the Uinta Mountains, Northern
Utah, with Special Reference to Phosphate. A. R. Sin it/.
Bulletin 690 C. Prom Contributions to Economic Geology,
,,,i,s, put I 64 pp. Published May 10 No detailed work
upon which to base ■> reliable estimate of tonnage has been
done in tins field. It is apparent, however, from tin neon
. \auuuatiou that :i large amount , ,\ pho ■ 1 > ' 1 ■ ' ■
874
I III; JOl RNAL OF INDUSTRIAL AND ENGINEERING ' HEMISTRY Vol. 10, Xo. 10
Geology and Oil Prospects of the Salinas Valley-Parkfield
Area, California. W. A. English. Bulk-tin 691-H. From
Contributions to Economic Geology, 1918, Part II. 42 pp.
1 June 18. Though by far the larger part of the area
examined has little to recommend it for wild-cat drilling, certain
areas appi ai to be well worth testing.
Oil Shale of the Uinta Basin, Northeastern Utah, and Results
of Dry Distillation of Miscellaneous Shale Samples. D. E.
Winchester. Bulletin 691-B. From Contributions to
Economic Geology, 1918. Part II. 29 pp. Published April
30. "The reconnaissance studies of the I Finta Basin have proved
the existence along its entire southern margin of a bed or beds
of oil shale of minable thickness and as rich or richer than those
mined in Scotland at the presenl time Previous examinations
by members of the Geological Survey have revealed the fact
that at practically all points along the north side of the basin,
the Green River formation (containing the oil shale) is con-
beneath younger rocks which overlie the oil-shale beds
jnconformably, so thai the ana within the Uinta Basin under-
lain by oil shale cannot be determined without extensive pros-
pecting with the drill. However, evidence at hand seems to
indicate that the oil shale may be present beneath a great part
of the basin, and it is estimated that the Utah portion of the
basin alone contains sufficient shale to produce 42,800,000,000
barrels of crude shale oil, with perhaps 500,000,000 tons of
ammonium sulfate as a by-product."
BUREAU OF FOREIGN AND DOMESTIC COMMERCE
Statistical Abstract of United States, 1917. 804 pp. Paper,
40 cents. This report presents in condensed form statements
regarding commerce, productions, industries, population, finance,
currency, indebtedness, and wealth of country, for series of
years, compiled from more important statistical data collected
by various Government departments; also condensed statement
of commerce of principal foreign countries.
Standard Specifications and Tests for Portland Cement.
Industrial Standards Serial, Publication No 1. 47 pp. Paper,
10 cents. The text of these specifications was adopted by the
American Society for Testing Materials and by the United
Stales Government. This is Revised 1917 Edition printed in
Spanish and English. It was prepared with the cooperation
01 the Bureau of Standaids.
COMMERCE REPORTS JULY, 1918
The turpentine and rosin industry of India is increasing,
thoughnol \ii abletosupplj the entire local demands. Methods
of production arc described in detail. (P. 7)
Ii Council of Ottawa has established a number of
research fellowships in science, with special emphasis on in-
dustrial applications "Studentships" of £75° per year and
fellowships of $1000 i<> Si 500 pel yeai an open i<> graduate
Students in any Canadian unh (P. 2l)
The use of cardboard containers to replace tin in England has
brought about n<>t onlj a great saving in tin, but also in steel,
of whirl: d is estimated that 60,OO0 tons are thus saved annually.
New discoveries ol tungsten ore in veins are report
Swatow, Chin 1 P
Cultivation of the castoi bean in Malaga, Spain,
encouraged to meet increased demands for castor oil for air-
plane lubrication. 1 1' [1
Great difficulty is being experienced in Norway to obtain
sufficient bark (or tanning material, to replace former imports
intent of Norwegian bark, 40,000 tons
requirei 1 The principal barks used art
oak. and willow, all cut loan hewn lues and formerly wasted.
That cut at sap time is superioi to that cul in winter. A sulfite
cellulose extract, known as" Norwi n tanning.
(P i,.-
Manganese ore containing 40 per cent of manganese is now
being shipped to th< ' P. 161,1
Peat fiber, also called "peat wool," is being used extensively
in Sweden and Denmark for the manufacture of matting, carpet,
feet soles in foo and by the addition of 30 to 40
per cent of wool, cloth can be produced I'
The output of manganese ore from Panama is increasing,
over 18,000 tons having been exported to the U. S. (P. 264)
Monazite sands discovered in Burma contain so low a per-
centage of thorium (only 0.18 per cent ThOo), as to be of no
commercial value. (P. 274)
A special scientific commission appointed to consider the
best method of making caustic soda in Brazil has recommended
the electrolytic process. (P. 292)
I i of camphor from Japan have been restricted, owing
to greatly increased domestic demands, especially for celluloid.
(P. 299)
The metal output of Mexico in 191 7, in kilos, was as follows:
Gold, 5,788,972; silver, 648,684,365; copper, 141,528,966; lead,
29,769,455; zinc, 3,888,124; antimony, 2,140,590. (P. 325)
A detailed account is given of the application in England
of the solvent extraction process for the recovery of fats, espe-
cially from "sud calce" (from the textile industry) and sewage,
sludge. The process is so successful that it now represents a
profitable undertaking as well as a conservation of fat. (Pp.
357-366)
In a recent fuel conservation order in England, total fuel,
including coal, gas, and electricity, used for heating or lighting
is restricted according to the size of the house, etc. In order to
encourage the manufacture and use of gas in those districts in
which it can be economically made (and thus increase the supply
of by-products), gas may be substituted for coal, at the rate of
only 12,000 cu. ft. of gas per ton of coal in districts unfavorable
for gas manufacture, and at the rate of 18,000 cu. ft. per ton in
favorable districts. (Pp. 369-373)
Imports of tin into the United States in 1917-18 were the
highest ever recorded. 13 per cent were imported in the form
of Bolivian ore to be smelted in this country'- (P- 412)
Large amounts of iron oxide pigment ("red oxides") ate now
exported from Malaga to the United States. The product is puri-
fied by levigation. The coloring power is not determined solely
by the FeiOj content, since the Persian Gulf oxides, with lower
Fe203 content, have higher coloring power than the Spanish
oxides. (P. 412)
Extraction of crude oil, acetic acid, ammonia, pitch, and
gum spirit from kauri peat gum swamps in New Zealand is
becoming an important industry. (P. 415)
Special Supplements Issued in July
Spain— 15a Chin*
Mexico — 32b British South Africa — 66a
is ro tin: United States
Vkra Cruz (P. 390)
Indigo
Jalap root
Hides
Rubber
Silver
Alum
Chicle
Saffron
Vanilla
Lead
Mica
Aniseed oil
Mercury
Chile tP. 408)
l ore
Copper rcgulus
Glue
Hides
Mercury
Sodium nitrate
OillU.lY ''■
Silver
Tartar
Thymol
Essential oils
Almond oil
xide pigment
Mexico — Sup 32b
Calcium citrate
Copra
Oil of In
calco
Lead ore
Silver ore
Zinc ore
1 tURBAN, So. AjFRICA-
Sup G
i e bark
Wattle I'ark
Gum copal
Hides
Mica
Corundum
Antimony
Albumen
Camphor
C. nulla rides
Aniline dyes
Indigo
Call nuts
Musk
Rhubarb
Sodium benzoate
Copper
Peanuts
le tallow
Hides
Bean oil
Castor oil
Cottonseed oil
Peanut oil
Rape oil
Wood oil
Oct., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
875
NEW PUBLICATIONS
By Clara M. Guppy, Librarian, Mellon Institute of Industrial Research, Pittsburgh
Alcohol: Its Composition and Preparation. Central Control Board of
England. 133 pp. Price, $0.60. Longmans, Green & Co., New York.
Analysis: Aids to the Analysis of Food and Drugs. C. G. Moor and W.
Partridge. 4th Ed. 12mo. Price, 4s. Bailliere, London.
Chemical Analysis of Iron. A.A.Blair. 8th Ed. 8vo. 318 pp. Price,
$5.00. J. B. Lippincott, Philadelphia.
Chemistry: Essentials of Modern Chemistry. C. E. Dull. 12mo.
458 pp. Price, SI. 40. Henry Holt & Co., New York.
Chemistry: An Intermediate Textbook of Physiological Chemistry. C.
J. V. Pettibone. 8vo. 328 pp. Price, $2.50. C. V. Mosby Co.,
St. Louis.
Chemistry: Principles of Chemistry. J. H. Hildebrand. 12mo. 313
pp. Price, SI. 75. The Macmillan Co., New York.
Chemistry: Textbook of Physical Chemistry. A. T. Lincoln. 12mo.
547 pp. Price, $3.50. D. C. Heath & Co., New York.
Chemistry for Engineers and Manufacturers. B. Blount and A. G.
Bloxam. 2nd Ed. 8vo. 404 pp. Price, 14s. Chas. Griffin & Co.,
London.
Chemistry of Essential Oils and Artificial Perfumers. Vol. 1. E. J.
Parry. 3rd Ed. 8vo. 532 pp. Price, 25s. Scott, Greenwood &
Co, London.
Concrete Stone Manufacture. H. M. Whipple. 2nd Ed. 12mo. 318
pp. Price, SI. 50. Concrete-Cement Age Pub., Detroit, Mich.
Food: Its Composition and Preparation. M. T. Dowd and J. D. Jameson.
12mo. 173 pp. Price. SI. 25. John Wiley & Sons, Inc., New York.
Hindu Achievements in Exact Science. A Study in the History of Scientific
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Longmans, Green & Co., New York,
Hydraulic and Placer Mining. E. B. Wilson. 3rd Ed. 12mo. 425 pp.
Price, $3.00. John Wiley & Sons, Inc., New York.
International Mining Law. T. F. Van Wagenen. 12mo. 342 pp. Price,
S3. 50 McGraw-Hill Co., New York.
Minerals, Prospecting for. S. H. Cox. 7th Ed. 8vo. 271 pp. Price,
5s. Charles Griffin & Co., London.
Mining Geology: A Textbook of Mining Geology. James Park. 8vo.
354 pp. Price, 9s. Charles Griffin & Co., London.
Popular Oil Geology. Victor Ziegler. 12mo. 149 pp. Price, $2.50.
John Wiley & Sons, Inc., New York.
Soap Makers Directory, 1918. 21st Ed. 8vo. 97 pp. Price, 2s. 6d.
Simpkin. Marshall & Co., London.
Stoichiometry. Sydney Youno. 2nd Ed. 8vo. 363 pp. Price, $3.75.
Longmans, Green & Co., New York.
Studies on Solution in Its Relation to Light-Absorption, Conductivity,
Viscosity, and Hydrolysis. P. B. Davis and Others. 8vo. 144 pp.
Price, $2.00. Carnegie Institute of Washington, Washington, D. C.
Water Rights Determination from an Engineering Standpoint. J. M.
Whithav. 8vo. 204 pp. Price, $2.50. John Wiley & Sons, Inc.,
New York.
RECENT JOURNAL ARTICLES
Aluminum and Its Light Alloys. P. D. Merica. Chemical and Metallurgi-
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Analysis of Ferrozirconium and Zirconium in Steel. J. D. Ferguson.
Engineering and Mining Journal, Vol. 106 (1918), No. 8, p. 356.
Bisulfite Liquor and Its Constituents. James Beveridge. Paper, Vol.
22 (1918), No. 23, pp. 11-15.
Carbocoal Fuel Process Perfected. C. T. Malcomson. Iron Trade Re-
view. Vol. 63 (1918). No. 9, pp. 496-497.
Chromite. J. C. Williams. Mining and Scientific Press, Vol. 117 (1918),
No 9, pp. 281-282.
Coal: Aspects of the Low Temperature Carbonization of Coal. E. C.
Evans. Journal of the Society of Chemical Industry, Vol. 37 (1918), No.
14, pp. 212(-219(.
Coal: Danger to Equipment from Impure Coal. W. S.~ GOTO.D. h •on
Trade Review, Vol. 63 I 1918), No. 9, p. 501.
Coke: Some Characteristics of American Coke in By-Product Coking
Practice. I". W. Spkrr. Jr. Journal of the Franklin Institute, Vol. 186
(1918), No. 2. pp. 133-164.
Coke: The Wastage of Coke By-Products. Frederick McCoy. Engi-
neering and Mining Journal, Vol 106 (1918), No. 6, pp. 254-255.
Colloidal Chemistry in Papcrmaking. W. M. Bovard. Pulp and Paper
Magazine. Vol 16 (1
Combustion Train for Carbon Determination; Apparatus Giving Results in
Six Minutes and Meeting Color Test Inaccuracies Arising from Varying
Heat Treatment of Samples. J. It. Stetsek and R, II. NorTi
Age. Vol 102 (1918), No 8. pp I H-445.
Concrete: Failures in Reinforced Concrete. H, J. CRBIOHTON. Pulfi
and P&per Magazine Vol 16 (1918), No 35, pp T 7 1-77.1.
Cutting Steel Ingots with Oxy-Hydrogen. W. B, PBKOua. Iron Trade
Review, Vol. 63 (19
Development of Electric Melting Furnaces. H. W. Gn.LETT and A. E\
Rhoads. The Metal Industry, Vol. 16 (1918), No. 8, pp. 355-358.
Die Blocks: Correct Heat Treatment of Die Blocks. Gustaf Plterson.
The American Drop Forger, Vol. 4 (1918), No. 8, pp. 295-297.
Dyestuffs. L. J. MaTOS. Journal of the Franklin Institute, Vol. 186
(1918), No. 2, pp. 187-210.
Fertilizer: The General Fertilizer Situation. C. G. Wilson. The
American Fertilizer, Vol. 49 (1918), No. 3, pp. 128-138.
Filtered Water for Industrial Use. Large Savings are Effected by the
Purification of Water Used for Steam Generation and Cooling Purposes.
H. C. Stevens. Iron Trade Review, Vol. 63 (1918), No. 9, pp. 491-494
Forging: Fuel Analysis of a Drop Forge Plant. Part 2. B. K. Read.
American Drop Forger, Vol. 4 (1918), No. 8, pp. 307-312.
Forging: Possibilities of the Forging Machine. E. R. Hagen. American
Drop Forger, Vol. 4 (1918), No. 8, pp. 304-305.
Fuel: Application of Efficiency Principles in Burning Fuel Under Boilers.
Joseph Harrington. Journal of the Cleveland Engineering Society.
Vol. 11 (1918), No. 1, pp. 45-56.
Fuel: Maximum Fuel Production with Minimum Fuel Waste. D. M.
Myers. Industrial Management, Vol. 56 (1918), No. 2. p. 104.
Galvanizing: Modern Practice in Galvanizing Sheets. Methods of Con-
structing and Operating Galvanizing Pots. C. F. Poppleton. Iron
Age, Vol. 102 (1918), No. 8, pp. 433-436.
Gasoline-Driven Diamond-Drill Outfit. J. M. LongyEar. Engineering
and Mining Journal, Vol. 106 (1918), No. 8. pp. 343-345.
Hammer Foundations: Question of Correct Hammer Foundations.
Terrel Croft. American Drop Forger, Vol. 4 (1918), No. 8, pp. 300-
304.
Industrial Research: Developments in Industrial Research. C. L.
REESE. Chemical and Metallurgical Engineering, Vol. 19 (1918), No.
4, pp 197-199.
Japanese Steel: Future of the Japanese Steel Industry. J. P. Suzuki.
Iron Trade Review, Vol. 63 (1918). No. 7, pp. 389-390.
Liquid Crystals: Studies in Liquid Crystals. T. C. Chaudhari. Chemical
News, Vol. 117 (1918), No. 3054, pp. 269-272.
Lubrication: Methods of Conducting Tests of Lubricants on Internal
Combustion Engines. S. F. Lentz. Lubrication, Vol. 5 (1918), No. 9,
pp. 4-9.
Magnetic Permeability of Steel. F. P. Fahy. Chemical and Metallurgical
Engineering, Vol. 19 (1918), No. 5, pp. 247-250.
Manufacture of Ferro- Alloys in Colorado. R. M. Keeney. Engineering
and Mining Journal. Vol. 106 (1918), No. 9, pp. 405-409.
Manufacture of Tin and Lead Foil. L. J. Krom. Metal Industry, Vol. 16
(1918). No. 8, pp. 352-354.
Metallurgical Treatment of Radium Ores. R. B. Moore. Engineering
Mining Journal, Vol. 106 (1918). No. 9, pp. 410-412.
Mining in the Telluride District of Colorado. H. J. Wolf. Engineering
and Mining Journal, Vol. 106 (1918), No. 9, pp. 395-399.
Molybdenite Operations at Climax, Colorado. D. F. Haley. Engineering
and Mining Journal, Vol. 106 (1918), No. 9, p. 394.
Nitrate Deposits of Southeastern Oregon. I. A. Williams. Mining and
Scientific Press, Vol. 117 (1918), No. 9, pp. 285-289.
Potash: The Recovery of Potash as a By-Product in the Manufacture of
Portland Cement. J. J. Porter. Chemical Engineer, Vol. 26 (1918),
No. 8, pp. 289-290.
Radium Ore Deposits. R. B. MoorB. Engineering and Mining Journal,
Vol. 106 (1918), No 9, pp. 392-393.
Refrigeration and Ice Making. C. I.. Hubbard. Industrial Management,
Vol. 56 (1918), X.. 2, pp. 105-109.
Remelting of Aluminum Pig in the Electric Furnace. D D Miller.
Chemical and Metallurgical Engineering, Vol. 19 (1918), No. 5, pp. 251-
254.
Roaster: The New American Spirtlet Roaster. F. J Harlow. Engi-
neering and Mining Journal. Vol 106 (1918), No. 7, pp. 293-299.
Roasting of Sulfotelluride Ores for Amalgamating and Cyaniding. A. L.
: 1 1. and 1 M Trott. Engineering and Mining Journal, Vol.
106 (191! PI 100-404.
Soap and Its Textile Use. \V EC. Buti.br. Textile World Journal, Vol.
9, p. 33.
Sulfite Coal. R. W StEBhlBNSRT. Pulp and \ "I 16
(1918). "--710.
Sulfito Pulp Manufacture, Chemistry of the Process and Details of the
Various Operations. I VoJ 22 (1918), No. 25,
pp 11-13.
Sulfur and Pyrites Situation in Relation to the Fertilizer Industry. A. D.
/ .rlilizer. Vol 49 (1918). No. 3, pp. 113-123.
Sulfur in Natural Gas. J. P. Phii.lii" Monthly, 1918, No.
' 1
Sulfuric Acid: The Production of Sulfuric Acid. W. 1
r. Vol. 49 (1918), No. 3, pp. 123-125.
876
MARKET REPORT-SEPTEMBER, 1918
WHOLESALE PRICES PREVAILING IN THE NEW YORK MARKET ON SEPTEMBER 19, I918
INORGANIC CHEMICALS
Acetate of Lime 100 Lbs.
Alum, ammonia, lump 100 Lbs.
Aluminum Sulfate, (iron free) Lb.
Ammonium Carbonate, domestic Lb.
Ammonium Chloride, white Lb.
Aqua Ammonia, 26°, drums
Arsenic, white
Barium Chloride
Barium Nitrate
Barytes, prime white, foreign
Bleaching Powder, 35 per cent
Blue Vitriol
Borax, crystals, in bags
Boric Acid, powdered crystals
Brimstone, crude, domestic Long
Bromine, technical, bulk
Calcium Chloride, lump, 70 to 75% fused
Caustic Soda, 76 per cent 100
Chalk, light precipitated
China Clay, imported
Feldspar
Fuller's Earth, foreign, powdered
Fuller's Earth, domestic
Glauber's Salt, in bbl» 100
Green Vitriol, bulk 100
Hydrochloric Add, commercial
Iodine, resublimed
Lead Acetate, white crystals
Lead Nitrate
Litharge, American
Lithium Carbonate
Magnesium Carbonate, U. S. P
Magnesite, "Calcined"
Nitric Aoid, 40°
Nitric Acid, 42*
Phosphoric Acid, 48/50%
Phosphorus, yellow
Plaster of Paris
Potassium Bichromate
Potassium Bromide, granular
Potassium Carbonate, calcined, 80 @ 85%.. .
Potassium Chlorate, crystals, spot
Potassium Cyanide, bulk, 98-99 per cent
Potassium Hydroxide, 88 @ 92%
Potassium Iodide, bulk
Potassium Nitrate
Potassium Permanganate, bulk.U. S. P
Quicksilver, flask 75
Red Lead, American, dry 100
Salt Cake, glass makers'
Silver Nitrate
Soapstone, in bags
Soda Ash. 58%, in bags 100
Sodium Acetate, broken lump Lb. 20
Sodium Bicarbonate, domestic 100 Lbs. 3>
Sodium Bichromate Lb. 23
Sodium Chlorate Lb. 25
Sodium Cyanide Lb. 32
Sodium Fluoride, commercial Lb. 17
Sodium Hyposulfite 100 Lbs. 2.60
Sodium Nitrate, 95 per cent, spot 100 Lbs. 4 4."
Sodium Silicate, liquid, 40" Be 2'
Sodium Sulfldc, 60%, fused in bbls Lb.
Sodium Bisulfite, powdered 12
Strontium Nitrate Lb. 25
Sulfur 100 Lbs. 2.25
Sulfuric Acid, chamber 66° Be Ton
Sulfuric Acid, oleum (fuming) Ton
Talc, American white Ton
Terra Alba, American, No. 1 100 Lbs.
Tin Bichloride, 50° Lb.
Tin Oxide Lb.
White Lead, American, dry Lb.
Zinc Carbonate Lb.
Zinc Chloride, commercial Lb.
nominal
Lb.
nominal
Lb.
9'/« @
17
Ton
75.00 @
90.00
Lb.
12 @
14
Ton
30.00 @
35.00
Lb.
4'/l @
5
Lb.
9V4 @
9V.
Lb.
7 'A @
IOV4
Lb.
7«A @
8«/«
Ton
nominal
Lb.
75 @
Ton
20.00 @
22.00
Lbs.
4*25 @
4.50
Lb.
4V< @
5
Ton
20.00 @
30.00
Ton
8.00 @
15.00
Ton
nominal
Ton
20.00 @
30.00
Lbs.
200 @
3.00
Lbs.
2.00 @
2.25
Lb.
C. P. nonn
nal
Lb.
4.25 @
4.30
Lb.
17 &
18
Lb.
C. P. 85
Lb.
14 @
15
Lb.
1.50
Lb.
20 &
30
Ton
60.00 @
65.00
Lb.
T/i
Lb.
8>/s
Lb.
7 '/J @
9
Lb.
1.10 @
1.15
Bbl.
2.00 @
2.50
nominal
Lb.
3.75
a
4.00
Lb.
27
a
30
Lb.
1 .85
a
2.00
Lbs.
130.00
a
135.00
Lbs.
11.25
a
11 .50
Ton
22 00
a
25.00
Ox.
63Vi
@
65
Ton
10.00
a
12.50
Lbs.
2.50
a
2.60
3 60
5.00
18.00
32.00
15.00
1.17V.
15 a
1 .00
10'/.
ORGANIC CHEMICALS
Acetanilid, C. P., in bbls Lb. 70
Acetic Acid, 56 per cent, in bbls Lb. 1 0 . 76
Acetic Acid, glacial, 99'/.% Lb. 19.50
Acetone, drums Lb. 25 '
Alcohol, denatured, 180 proof Gal. 68
Alcohol, sugar cane, 188 proof
Alcohol, wood, 95 per cent, refined
Amyl Acetute
Aniline Oil, drums extra
Benzoic Acid, ex-toluol
Benzol, pure
Camphor, refined in bulk, bbls
Carbolic Acid, U. S. P., crystals, drums
Carbon Bisulfide
Carbon Tetrachloride, drums, 100 gals
Chloroform
Citric Acid, domestic, crystals
Creosote, beech wood
Cresol. U. S. P
Dextrine, corn (carloads, bags)
Dextrine, imported potato
Ether, U.S. P. 1900
Formaldehyde, 40 per cent
Glycerine, dynamite, drums extra
Oxalic Acid, in casks
Pyrogallic Acid, resublimed, bulk
Salicylic Acid, U. S. P
Starch, corn (carloads, bags) pearl 100
Starch, potato, Japanese
Starch, rice
Starch, sago flour
Starch, wheat
Tannic Acid, commercial
Tartaric Acid, crystals
OILS, WAXES, ETC.
Beeswax, pure, white Lb.
Black Mineral Oil, 29 gravity Gal.
Castor Oil, No. 3 Lb.
Ceresin, yellow Lb.
Corn Oil. crude 100 Lbs.
Cottonseed Oil, crude, f. o. b. mill Lb.
Cottonseed Oil, p. s. y 100 Lbs.
Menhaden Oil, crude (southern) Gal.
Neat's-foot Oil. 20° Gal.
Paraffin, crude, 118 to 120 m. p Lb.
Paraffin Oil, high viscosity Gal.
Rosin, "F" Grade, 280 lbs Bbl.
Rosin Oil, first run Gal.
Shellac. T. N Lb.
Spermaceti, cake Lb.
Sperm Oil, bleached winter, 38° Gal.
Spindle Oil. No. 200 Gal.
Stearic Acid, double-pressed Lb.
Tallow, acidle&s Gal.
Tar Oil, distilled Gal.
Turpentine, spirits of Gal.
METALS
Aluminum, No. 1, ingots Lb.
Antimony, ordinary Lb.
Bismuth, N. Y Lb.
Copper, electrolytic Lb.
Copper, lake Lb.
Lead, N. Y Lb.
Gal.
4.90
•
Gal.
91V.
a
Gal.
5.30
a
Lb.
28'/.
a
Lb.
2.65
a
Gal.
23
a
Lb.
1 -24; .
a
Lb.
42
a
Lb.
9
a
Lb.
ominal
Lb.
70
a
Lb.
82
a
Lb.
2.00
a
Lb.
20
a
Lb.
8
a
Lb.
nominal
Lb.
27
a
Lb.
16V.
a
Lb.
60
a
Lb.
41
a
Lb.
3.25
a
Lb.
85
a
Lbs.
6.00
a
Lb.
13
a
Lb.
12 V.
a
Lb.
9V«
a
Lb.
nominal
Lb.
65
a
Lb.
82
a
Nickel,
Piatinu
ctrolytic Lb.
refined, soft Or.
63
a
*5
24
m
25
30
g
32
17
a
IB
17.75
■
18.00
17 V.
a
—
21.00
w
22.00
1.15
a
1.25
3.45
a
3.55
a
76
a
70
a
33
a
2.25
a
40
a
25
^
1.60
10.77
19.70
Tin, Straits Lb.
Tungsten (WOi) Per Unit
Zinc, N. Y
FERTILIZER MATERIALS
Ammonium Sulfate 100 Lbs.
Blood, dried, f . o. b. Chicago Unit
Bone. 3 and 50. ground, raw Ton
Calcium Cyanamide Unit of Ammonia
Calcium Nitrate, Norwegian 1 00 Lbs.
Castor Meal Unit
Fish Scrap, domestic, dried, f. o b. works Unit
Phosphate, acid, 16 per cent Ton
Phosphate rock, f. o. b. mine: Ton
Florida land pebble, 68 per cent Ton
Tennessee, 78-80 per cent Ton
Potassium "muriate,** basis 80 per cent Ton
Pyrites, furnace size, imported Unit
Tankage, high-grade, f . o. b. Chicago Unit
3.<
a
34
ia
. a
14
3
so
:6
55
1
a
a
a
8.05
■
nominal
oi 7,
lominal
3
65
56
:o
00
a
'4
00
9
40
a
')
60
38.00 a 40.00
nominal
/ 25 and XV
(g> 1 7 50
nominal
5.00 a 6-00
7.00 a 8.00
290.00 @ 300.00
nominal
■A 6.80
The Journal of Industrial
and Engineering Chemistry
Published by THE AMERICAN CHEMICAL SOCIETY
AT SA9TON. PA.
Volume X
NOVEMBER 1, 1918
Nc
Editor: CHARLES H. HERTY
Assistant Editor: Grace MacLeod
Advertising Manager: G. W. Nott
ADVISORY BOARD
H. E. Barnard H. K. Benson F. K. Cameron B. C. Hesse A. D. Little A. V. H. Mory
Published monthly. Subscription price to non-members of the American Chemical Society, $6.00 yearly; single copy, 60 cents
Price per single copy to American Chemical Society members, 50 cents. Foreign postage, seventy-five cents, Canada, Cuba and Mexico excepted
Entered as Second-class Matter December 19, 1908, at the Post-Office at Easton. Pa., under the Act of March 3, 1879
Acceptance for mailing at special rate of postage provided for in Section 1 103. Act of October 3. 1917. authorised July 13. 1918.
All communications should be sent to The Journal of Industrial and Engineering Chemistry.
Telephone: Vanderbilt 1930 35 East 41st Street, New York City
Subscriptions and claims for lost copies should be referred to Charles L. Parsons, Box 505, Washington, D. C.
acb Printing Cosi
TABLE OF CONTENTS
Editorials:
Preparation for After the War 878
Developments in Ceramics 878
Commissions for Baseball Players 879
A Record of Achievement 879
Conservation Begins at Home 879
Another Idol Shattered 880
Pernicious Activity 880
Our Preparation for After the War. Bemhard C.
Hesse 881
Chemical Markets in the Union of South Africa.' O.
P. Hopkins 887
Original Papers:
Examination of Organic Developing Agents. H. T.
Clarke 891
A Summary of the Literature on the Solubility of Sys-
tems Related to Xiter Cake. H. W. Foote 896
The Recrystallization of Niter Cake. Blair Saxton. . . 897
The Formation nf Aromatic Hydrocarbons from Natural
Gas Condensate. J. G. Davidson 901
Laboratory and Plant:
Methods of Analysis Used in the Coal-Tar Industry.
Ill — Heavy and Middle Oils. J. M. Weiss 91 1
The Polariscope Situation and the Need of an Inter-
national Saccharimetric Scale. C. A. Browne 916
Addresses .
The Potash Situation. A. W. Stockett .918
Russia's Production of Platinum. Albert R. Merz 920
The Preparation of Several Useful Substances from Corn
Cobs !•' B. LaForge and C. S. Hudson
Statistics of Garbage Collection and Garbage Grease
Recovery in American Cities. Raymond Pearl
Cotton I Ml Industry in the War. David Wesson 930
The Bureau OP FOREIGN and DOMESTIC CoMMERCl
Relations n, American Chemical Industry:
Government Trade-Building Information, C l>
Snow 93 1
Our Publications and Then Bearing on tin Chemical
Industi v 0 1' Hopkins
The Method of Preparation ol the C< n u of ( hi n
Imports. E. R. Pickrell
Current Industrial News:
Analysis of White Metal; Lubricating <iil, Venezuelan
Tradi Inquii i< Pot 1 1 1 i 1 « - . New C<
Mixer; Combustion of Coal; Batik |)\<
Lamp Tests, New Radio- Active Element R.I
Seed Oil; The Schoop Metal-Spray Process; Catalytic
Processes in Germany; Cadmium in Brass; Acid Re-
sisting Ferro-Silicons; New Norwegian Industries;
Newfoundland Cod Liver Oil; National Metal and
Chemical Bank; Discoloration of White Paint; Gas
in Glass Industry; Heating in a Liquid; Sources of
lire; Bolivian W'olfram Industry; Gas and Petrol
Engines; Antifriction Metals; Hydrosulfites: Metallic
Liquids; Starting Rheostats; Air Raid Signals; Oxida-
tion of Ammonia; Synthetic Rubber; Corrosion of
Brass Tubes; Tool Steels; Compression Strength of
Glass and Quartz ; Fats and Oils in Germany ; Damas-
cene Steel; Chinese Pencil Factory; Japanese-Chilean
Nitrate Enterprise; Drying Ovens; Riveting Re-
corder; Platinum Substitute; New South-African
Industries; Aeroplane Construction; New Steam
Motor; A New Plastic Compound; Iron and Steel
Trade of Aden 937
Scientific Societies:
Resolution Concerning Organic Nomenclature; Fall
Meeting, American Electrochemical Society —
Atlantic City. September 30 to October J. 1918; The
Milwaukee Meeting of the American Institute of
Mining Engineers; Report of the Committee on Re-
search and Analytical Methods. Fertilizer Division,
American Chemical Society 944
Notes ami CORRESPONDENCE:
Tin- Census .if Chemists; Deferred Classification and
Furloughs for Government and State Chemists;
Chemical Industry in the Netherlands; Portrait of
| harles M. Hall for the Chemists' Club; Codpera
lion 1 the Alien Property Custodian
An Aliiuinent Chart tin the Evaluation of Coal —
Correction; Personnel, Research Division, Chemical
Wai I I tion 946
kin Letter 948
1 v ts 949
Industrial Notes 951
Government Publications 954
Book Re\ IBWS
Sulfuric Acid Handbook; Treatisi on ! deal
Chemi I ise. An 1 lutlini "i the Chemisti \
. .1 tin Stl net 111 1] E li men! s ol I 1. lilts Tile Chi
■ .'I French; fhe Science an. I
I'li-i i Photography; The American Feftilizei
Hand ] I's ( hemical
Annual; Sir Wm i ,, Scientist and Man
New Publications 96 ,
Market R bpi '>• 1
878
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. n
EDITORIALS
PREPARATION FOR AFTER THE WAR
The beginning of the end is at hand. A hitter four-
year struggle has sufficed to indicate clearly the pi al
of potency of that great military machine which was
shot through with the conviction that might must
triumph. Little did the leaders of the Teutonic hordes
realize what possibilities of resistance lay in the spirit
of free men. Strengthened now with the ever in-
creasing impetuous hosts of Americans the armies
of the Entente Allies are steadily driving back the
enemy, giving no time for recovery of strength, no
opportunity for such concentration of forces as might
prove an effective resistance. Filled with the con-
viction that only "Unconditional Surrender" will
satisfy those who have been eye-witnesses of the many
crimes against humanity, our men are hastening their
steps toward Berlin. Doubtless many obstacles will
be thrown in the path of that mighty advance; it may
be retarded from time to time but it cannot be stopped.
How long this final stage will last no one can predict,
but no one doubts its finality.
With the advent of peace new adjustments of our
present abnormal life will be immediately required.
Especially will this be true for chemists whose entire
activities have been so directly centered on war prob-
lems. During this war period chemistry has come
into its own in this country, and the responsibilities
are thereby increased as to the wise solution of those
large problems which will confront us during the early
days of the peace period.
With characteristic foresightedness Dr. B. C. Hesse,
a member of the Committee Advisory to the President
and a councilor-at-large, prepared an address on this
subject which was to have been delivered before the
Philadelphia Section. Unfortunately the ravages of
the prevailing epidemic have made impossible the
holding of the meeting at which the address was to
have been read. We are glad to be able to print the
address as the special feature of this issue, and would
urge its careful and thoughtful reading by every
member of the American Chemical Society.
In this address Dr. Hesse has dared "to think out
loud," regardless of whether or not his thoughts may
be sound, an example well worthy of imitation if
progress is to be made. Without seeking to divert
in the slightest the minds of chemists from those
problems directly connected with the winning of the
war, he points out that
In the tense industrial, commercial, and financial world-wide
struggle that is bound to ensue directly after the close of
hostilities, success will in all probability fall in a greater measure
to those who have, in advance, prepared a comprehensive
workable plan adapted for immediate development and opera-
tion, and sufficiently elastic to allow of effective adaptation to
changing or unforeseen conditions, than to those who have not
so prepared themselves.
In I lie preparation of such a plan it is urged that the
councilors in consultation with the members of their
respective local sections prepare lists of suggestions
for future activities and comment in a spirit of con-
structive criticism upon the suggestions made by
others. Often during the past few months members
have commented upon the difficulty in securing
speakers for the meetings of the coming winter. Might
it not be well to vary these programs and occasionally
to do without speakers, devoting the time instead to
informal discussion of after-war problems?
The councilors of the Philadelphia Section were so
much impressed by the spirit of Dr. Hesse's address
that they have already started action. A letter from
Dr. J. Howard Graham, the Secretary of that Section,
informs us that the following plan has been adopted:
That a letter be printed and sent to all chairmen and secre-
taries of the 54 sections, calling attention to preprints mailed
under separate cover, and especial attention to pages 3 and 14
of the same, and urging that the preprints be sent immediately
to all councilors, and that suggestions for plans for "Prepara-
tion for After the War," be sent through the secretaries to me
so that our council might boil them down, eliminate duplicates,
and forward them in bound form to the general council for their
consideration. A personal and typewritten letter is also to be
sent to the 54 secretaries urging their cooperation to the ut-
most of their time, and calling attention to the fact that the
Philadelphia Section, realizing the importance of the move-
ment, has simply agreed to act as a clearing-house for the many
suggestions that we believe it possible to make.
This action of the Philadelphia Section provides the
machinery for a thorough interchange of opinion, and
for a compilation of suggestions which should prove of
inestimable value to those who may be charged, per-
haps suddenly, with the responsibility of presenting
the views of chemists upon after-war problems, and of
formulating those measures which will lead truly to
greater usefulness of our science to our country, a
peace service just as obligatory upon us as is the
splendid war service now being given.
In no whit, however, is it intended that these dis-
cussions of after-war problems should interfere with
that concentrated effort needed to furnish an abun-
dance of those products of the chemist's skill which,
at the least sacrifice of the lives of our men, will wring
from the enemy the only words which will satisfy our
people — "Unconditional Surrender!"
DEVELOPMENTS IN CERAMICS
The clothes became too small for the growing body,
hence the American Ceramic Society decided to dis-
card the annual volume of "Transactions" with which
it formerly was content and to issue instead a monthly
periodical. The Journal of the American Cera'
ciety.
The editor is Dr. George H. Brown of Rutgers Col-
ew Brunswick, N. J., and associated with him
is the Committee on Publications: Drs. L. E. Bar-
ringer, chairman. A. V. Bleininger, H. Ries, and E. \\ .
Tillotson.
In spite of 'ions placed upon the ceramic
industry by the Fuel Administrator, abundant signs
exist of unusual activities in this field which give rich
promise for its future. Outward evidences of this
activity arc noted in the creation of the School of
Nov., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
879
Ceramics, with its special building, at the University
of Illinois, under the leadership of Dr. E. W. Wash-
burn; the segregation of the ceramics exhibits
at the recent Exposition; the resignation of Dr.
Arthur L. Da}' from the directorship of the Geo-
physical Laboratory in order to undertake research for
one of the great glass companies, already markedly
successful in its efforts to render America independent
in glassware.
The mention of the names of Drs. Day and Wash-
burn in connection with this industry emphasizes again
the increasing call of the industries for physical chem-
ists in industrial research, and this in turn brings us
back to the responsibility resting upon universities to
lay stress upon physical chemistry in the curriculum
for the chemists of the future.
COMMISSIONS FOR BASEBALL PLAYERS
Many letters have been received containing unfa-
vorable comments on the appointment of well known
baseball players to commissioned offices in the Chem-
ical Warfare Service. Complaint is made that this
tends to lower the dignity of the chemical profession
and to work an injustice to men who have spent years
in chemical training, yet who still rank as privates or
non-commissioned officers.
We must confess to an inability to sympathize with
these criticisms, and do not believe that this is in any
wise due to a natural predilection for baseball players.
The Service in question is not a Chemical Service, but
a Chemical Warfare Service. Its personnel numbers
approximately thirty thousand. As there are only
some sixteen thousand chemists recorded in the
country, and as many of these are still connected with
the industries, it is evident that a considerable major-
ity of the members of the Chemical Warfare Service
are not chemists.
Furthermore, while the work of the chemist is the
all-important foundation of this division of the War
Department, there is also the important function of
applying the results of the chemists' work most force-
fully to the enemy in the offensive and to our own
soldiers in the defensive. For this work natural lead-
ers are desired, men of proved personality, of fine
physique and undoubted personal courage.
In the light of the requirements we congratulate the
Chemical Warfare Service on the appointments, con-
fident that these officers will command the respect of
the men in the field, will hold their nerve at every
critical moment, and will contribute their full measure
of terror to the enemy as he increases his backward pace
through the liberated lands of France and Belgium.
No, let's not worry about that matter. A much
larger and far more important problem remains un-
solved, namely, the most efficient utilization of the
service (we mean service and are not thinking about
the matter of commissions) of the chemists already in
uniform. We met one last week, known to us for
years, who is doing mere clerical work which could be
done by any man of average intelligence without the
slightest knowledge of chemistry; two others were un-
loading box cars at a well-known arsenal. Still other
men, of marked attainments, while nominally engaged
in chemical work, are really put at tasks which the tyro
could perform just as well.
It has been stated that the government require-
ments for next year call for two thousand additional
chemists. A systematic search for these should begin
within the ranks of all branches of the service. We
believe that a good "shaking down" would reveal many
such men qualified for the work in mind, now engaged
in less important tasks. We have preached efficiency;
we must practice it.
A RECORD OF ACHIEVEMENT
The dyestuff census compiled for the Bureau of
Foreign and Domestic Commerce by Dr. Thomas H.
Norton in 19 16 gave for the first time, and with reason-
able accuracy, an itemized statement of our importa-
tion of coal-tar dyes. It was a sketch in detail of our
dependency, and has proved a valuable guide in the
development of the new American industry.
The "Census of Dyes and Coal-Tar Chemicals, 1917,"
just issued by the U. S. Tariff Commission as Tariff
Information Series — No. 6, is a record of achievement
during the intervening time, of which all Americans
may be proud.
In planning for the future of the industry, opinion
may be replaced by facts, carefully collected
and clearly presented in this new census. The for-
midable list of one hundred and ninety manufacturers
shows how widespread is the activity in this line.
Every chemist, whether or not connected with the in-
dustry, will find interest in Part II, a concise and accu-
rate twelve-page "History of the Dye Industry in the
United States Since the Beginning of the European
War."
While we are waiting to learn the character of the
report the Tariff Commission will make to the Ways
and Means Committee as a result of this study, will
not someone inform us as to what is a "dyestuff,"
particularly as differentiated from a dye? We
confess to very loose practice in the indiscriminate use
of the two words, chiefly because we have been unable
to find two authorities who agree.
CONSERVATION BEGINS AT HOME
The little girl had been almost worrying the life out
of us to secure every particle of tin foil in the cigarette
boxes. The enthusiasm of the six-year-old conserva-
tionist was due to the fact that "the Government
wanted tin and asked everybody to save it." The two-
fold source of the request changed the worry into
pleasure and we reached the office feeling just a bit
a better citizen. There on the desk was a pile of edi-
torial preprints, three pages each, and held together at
one corner by an effective though scarcely visible tin-
coated clip. On the other side of the desk was the
morning mail, the top letter of which was a three-page
communication, a form letter, from a government
bureau in Washington. Almost dazzling to the eye
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. n
was the huge tin-coated fastener which held the three
sheets together. It was a complicated affair, but we
were interested not so mu ingenuity and com-
plexity as in the unusual and unneci ary bulk. The
of the laboratory returned, and the I
ed, with the following result:
Weight of preprint clip = 0.02
Weight of government bureau clip 6 6435 grams
To make sure, the matter was followed a sup further
and the lit lie clip and a portion of the huge one were
each dissolved in hydrochloric acid (it was good to get
hold of a test tube again), and the solution:
qualitatively for tin. The one showed a slight amount,
the other an abundance. Quai ests were not
necessary as the preprint clip was round, the other
flat, therefore the 300 per cent ratio was sure to be
increased, and it was bad enough as it was. The only
way we could help the situation immediately was to
buy another package of cigarettes nil save the tin
foil for the little girl, but we did gather a clearer idea
of what a friend meant when he said: "I don't care
how much they tax me for carrying on this war, if
the funds are applied efficiently toward winning the
war."
ANOTHER IDOL SHATTERED
The fetish of Teutonic superrhemistry is re-
ceiving some hard blows nowadays. In laboratories
and in plants results are being achieved which will act
as pincers, forcing German retirement just as truly
and as effectively as the successive blows of our armed
forces are to-day by a similar process bringing near tin-
day of complete victory.
'I'lir debt of Germany to other countries for the basic
ideas on which its chemical industry is founded is
being constantly illuminated by many recently pub-
lished articles. Someone familiar with all the facts
should write an article on Germany's debt to the
American chemical industry, legally and illegally in-
curred, as a result of the tour of German chemists
through the plants of this country immediately after
the Eighth International Congress oi Applied Chem-
ist ry in New Y< irk City in 191
While waiting for that story i1 may be well to record
in the chemical literature another in ance oi German
inspiration drawn from A merican environment and
example. In 1914 the L'. S. Foreign and
tic Commerce published a monograph.
Agents Series Xo. 78, entitled "Commercial Oi
tions in Germany," by Archibald J. Wolfe. From
page 50 of that publication the following is repr »
alics being ours:
Verbin 7a k Wahrung Dbr Interessen Dbr Chbmischen
Industrie Deutschlands The chemical industry 1- one of
tlie best organized in Germany. Tin- interests of all the
chemical trades are served i>\ this oik- central organiza-
tion, wjth headquarters at Berlin, Closely allied 1,. n
are tlu- Association of Fertilizer Manufacturers, at Ham
burg; tlu- Syndicate of Soda Manufacturers, .it Bern-
burg and iii' \ ociation of Lead Paint Manufacturers,
1 1 ologne. It has 290 active members (manufacture
cerns) and 138 personal members, who an- heads of maim
facturing establishments, 'flu- annua] income of tlu- associa
tiou is about 60,000 in nk-. ($14,280 . ol which 1 1.000 marks
! on the official organ of the organization,
mische Industrie, and 24,000 mark-, ss.jior on the
administration. Its official organ is one of the high-grade,
well edited German trade publications.
The impetus to the formation of this association was given
nl the Philadelphia Exposition [1876] when several representa-
tives of tin: German chemical industry met at Ike banquet
given by the AMBRit an Chemical Society to their foreign col-
li was decided at that informal meeting to form an
hi for the protection of the common interests of the
chemical industry in customs and taxation matters The
scientific interests of the industry had been well served up to
that time by the German Chemical Society, but it was only in
1 that the German chemists effected a closer alliance
between the scientific laboratory and the manufacturing estab-
lishment A convention of all manufacturers and scientists
interested in the chemical industry was called at Frankfort-
on-the-Main in 1S77, in order to found an association for the
protection of the interests of that industry, particularly as at
that time the entire economic legislation of Germany was under-
going a change. This association has been active, and success-
fully so, in representing the interests of the chemical industry
in the matter of customs tariffs, taxation of industries, negotia-
tion of commercial treaties, classification of chemicals for freight
rates, patent and trade-mark laws, and in labor legislation and
labor difficulties. The organization is remarkable for the
liberal treatment extended to foreigners. Foreign scientists
and other foreigners having an interest in the technical phases
of the chemical industry are admitted as members, and may
attend tin session of the Association, but have no right to vote.
Permanent commissions for matters requiring special study are
organized under the auspices of the society, among them com-
missions for patents and trade-marks, for customs tariffs, for
the investigation of complaints of individual manufacturers
against acts of local authorities, etc.
The membership fee in the association has been increased
from time to time, and is based on the annual pay roll of each
concern. The minimum is 25 marks $5 95 I and the maximum
500 marks (Si 19) per annum. It has organized an important
employees' insurance association for the chemical trade. Its
statistical bureau tabulates in the most detailed manner not
only the production in the chemical industry, but also the wage
scales. It publishes an accurate directory of the chemical
industry.
An American Chemical Society banquet is capable
of producing almost anything, but we did not know
that it was in such a genial and at that time friendly
atmosphere that the "Yerem zur Wahrung. etc.." had
its birth.
Even at that date, the initial year of existence of
the Ami rican C he mica l Society, the Manufacturing
Chemists' Association of the United States had already
passed some eight or ten years of useful life.
Travel is a great educator!
PERNICIOUS ACTD7ITY
In the midst of these strenuous abnormal times even
our printer's devil had to run amuck. After we had
approvi rig of the heading to the Expo-
sition section of the October issue he slipped one over
on us, too late for correction, and made the heading
read "Fourth National Exposition of Chemical Engi-
neers."
That none of our readers have called attention
to the slip we take as an evidence of good-will, or per-
haps as an indication that chemists, unlike newspaper
readers in . : 1 ention to headlines.
ttle imp may have had the serious
of upsetting convention and giving credit to
those to whom credit is due. for it was only through
the work of chemical engineers that the Exposition was
possible.
Nov., IQlJ
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
OUR PREPARATION FOR AFTLR THE WAR
Address prepared by Bernhard C. Hesse for the Philadelphia Sec
of the American Chemical Society, October 17, 1918
The American Chemical Society has long since
completed its preparations for active assistance in
our war; its participation is in full swing and opera-
tion and is capable of all needful expansion. The
real business now in hand is for each of us to contribute
all that we can to every effort to bring the war quickly to
a successful issue.
However, all the belligerent countries, including
our own, have been engaged for some time past, and
in more or less official manner, in tentatively consid-
ering after-the-war conditions and how best to pro-
vide for them. Some of these tentative conclusions
have found their way into print. Due to this neces-
sary tentativeness all these discussions leave a feeling
of confusion on a great many points, yet in them there
clearly stands forth the unanimous decision that here-
after each nation must be as independent of all other
nations as its resources in men, minds, and ma-
terials will enable it to become.
Our own Government has not yet, so far as I am
aware, given out any statement as to what it may or
may not be thinking of for after the war. In view
of the greatly increased public appreciation of and
wholesome interest in chemical endeavor as a factor in
our national life.it seems highly improbable that the
chemical requirements of our nation will not be
thoroughly considered in any such plans. Further,
it is not inconceivable that the American Chemical
Society with its more than 12,000 members, meeting
in 54 local sections in 33 states of the union, may
be called upon for assistance, not only in the making
of such plans, but also in their execution.
Whether so called upon or not, it is clear that in
consequence of the very great changes and gigantic
readjustments that will then surely take place in the
economic life of practically the entire world, the
American Chemical Society and all its members
will find ready to hand many problems of varying
scope that must be solved by us, and solved right and
fairly promptly, and which are not connected with
Government functions in any way, if we wish to live
up to the proper and just demands of loyal citizen-
ship and of professional responsibility. No doubt
there will be many who will then believe in close
affiliation with or even in actual control by the Federal
Government of many matters which others will re-
gard and have heretofore regarded as belonging to
non-governmental agencies solely.
In the tense industrial, commercial, and financial
world-wide struggle that is bound to ensn
after the close of hostilities, success will in all proba-
bility fall in a greater measure to those who havi
advance, prepared a comprehensive workable plan
adapted for immediate development and oper;
and sufficiently elastic to allow oi adaptation
to changing or unfoi ditions, than to
who have m red 1 hemselves.
When that time . omes, neither the Am (ui v. Chi u
ical Society nor the American chemical profession
should be found among the unprepared. But it would
be an entirely mistaken policy for us to become so
intent upon after-the-war preparedness that we were
thereby and in any way to neglect, overlook, or omit
even a single win-the-war activity. I am convinced
that there is much of such preparation that we can
do without taking any of our attention from the
paramount business before us. Necessarily, some of
these preparations are now in nebulous outline only,
but they can undoubtedly be made sufficiently con-
crete for effective treatment if we seriously take coun-
sel among ourselves betimes.
responsibility reciprocal
It is clear that when time comes for action on behalf
of the American Chemical Society such action will
have to be determined and taken, and perhaps taken
promptly, by a relatively small number of persons;
they can act the more intelligently for the Society
the better informed they are of the thought of our
members on such subjects. There is therefore a
reciprocal responsibility. Our Society officers must
get the views of the members and the members must
get their views to their officers. What individuals
will have to act for the Society at such time is now
unknown. Hence, members should proceed now or
with as little delay as possible to formulate as well
as they can what they want done and get it in such
shape that it can be revised from time to time and
promptly handed over in as concrete shape as possi-
ble to those who will have to carry the burden, when
that time comes.
To do this calls in the first instance, at least, for
no new machinery nor committees nor appointments.
Our splendid Society organization is admirably adapted
to take on that load. Our Council is an advisory body
to our Directors and to our executive officers. Each
of our local sections has a councilor for every ioo of
its members or fraction of ioo members. In addi-
tion, we have 12 councilors-at-large. This machinery
ought to enable us to get something concrete together
in a relatively short'space of time.
proposed geneeai plan of action
As I see it, if the councilors of each Local Section
will get the views of the members of their respective
sections and will put them into one document with a
separate and consecutively numbered paragraph for
each recommendation, these 54 documents can then
rown into one document of numbered para-
graphs, and this single can go back to the
local councilors for additions, if need be. In that way
we will have compressed into a sm he ideas
oi ill our individual members and make them
iromptly available for comprehensive analysis
anient. Even so, we must not look for a com-
plete 1- 1 -;1 and wlnle v<
should be taken at this first attempt yet the work
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. n
should not be held up merely because it is not a pol-
ished job in all respects. Before a job like this is
finished there will have to be a lot of "ironing out"
of rough places. Yet it can be done. It has been
done, but of course on a much smaller scale, by the
New York Section in respect of the three symposiums
held by it on the relations between universities and
the industries.1 That resume does not pretend to
offer a complete solution but it nevertheless is an ac-
curate and workable summary of the papers there
treated. This is the same kind of a job, only very
much larger. With such a document before them our
executive or other officers acting for us at that time
can proceed with greater confidence, than they other-
wise could, that they are acting in reasonable accord
with the best obtainable judgment of our members
and our members could then look forward to such
action, assured that their proposals had all been
given consideration.
With me personally this is not wholly an academic
or supposititious matter. If the time for action comes
before January I, 1920, I, as a member of the Ad-
visory Committee to the President of the American
Chemical Society, will, no doubt, have to bear my
proper share of responsibility for decisions reached
and actions taken on behalf of our Society. There
is ample room for errors both of commission and omis-
sion. Whenever I consider the large number of new
and strange problems that may come up at such a
time I confess I become somewhat uneasy. On some
subjects I have very definite convictions, on others
I am less certain of myself, and on still others I have
neither information nor opinion. Withal there is
the uncertainty arising from the question that applies
to each problem: "What do the members think about
this?" And, again, there is the vexing question:
"Have I overlooked anything vital?" With a docu-
ment obtained as above outlined before me there is
no doubt in my mind that I could and would act,
with far greater confidence than otherwise, that I
was properly considering the best judgment of the
membership and that I was acting in the light of the
best and most comprehensive information and help
obtainable from our members. Beyond question
such a document would be of great help to me per-
sonally and I cannot imagine that it could fail to be
so for all those who will have to act in a similar capacity,
although I am in no wise speaking for them nor any
of them but myself.
MEMBERS INDIVIDUALLY RESPONSIBLE
These are extraordinary times and call for extraor-
dinary measures. The membership must take ex-
traordinary steps to get its views on these topics
before those upon whom the burden of wise decision
and effective execution must fall. Any member who
has ideas on these subjects and fails to get them be-
fore his councilors is not "toting fair." Each of us
must regard himself as a Committee of One to do
this job and do it promptly. Wo owe this to our coun-
try, to our profession, and to ourselves.
I am making this suggestion to the membership
> This Journal, 8 (1916), 658.
as a whole, because I am thoroughly convinced that
if I did not do so I would fall far short of dealing fair
with the members who have honored me with their
confidence by placing me among the councilors-at-large
and upon the Advisory Committee to our Society's
president.
When time for action comes we will be standing
upon the threshold of a new order of things. We
must leave nothing undone that can be done to make
sure that those who are to carry our burdens for us
have then been given every help that it is within
our power to give. Cooperative effort the world over
will take on new impetus and we must not fall behind
the new standards of efficiency and cooperation that
the world will then begin to set. Our aim should be
to lead in this effort and not to trail after anyone.
We cannot then afford to experiment very much;
we should get things right the very first time.
Of course, those who will have to make the deci-
sion will have the advantage of being guided by events
as they then stand, whereas any attempt now to reach
a decision as to desirable or needful policies will be
disadvantaged by the absence of the event. Never-
theless, there must be certain fundamental policies
that will have to be settled regardless of the specific
event and as to which there is legitimate present
difference of opinion. These we should decide as far
in advance as possible so that we will have much of
our talking out of the way and permit our getting
down to action along these predetermined lines and
to meeting new problems as they arise.
In order to visualize and to make as concrete as I
now can what in general and in part is in my mind
I will proceed to illustrate, with as little detail as may
be, some of the problems that have presented them-
selves to me.
Broadly, these divide themselves into two classes:
internal and external, and under each are the two sub-
heads, with or without co-action with our Government,
Federal or otherwise; some are of a mixed nature. I
shall not now attempt to arrange this material in any
rigidly logical or connected order for I regard that at
present more a hindrance than a help.
DIRECTED GROWTH OF CHEMICAL KNOWLEDGE
Our Society was organized in 1876 for the "advance-
ment of chemistry and the promotion of chemical
research." Through its general meetings, the meet-
ings of its Local Sections, and the publication of three
separate journals, much has been done toward dis-
seminating chemical knowledge among American
chemists and providing efficient vehicles of scientific
record and communication. This is no small accom-
plishment. But that is now out of the way and is
running itself. Can we not now do something new
that is just as necessary as the above was in 1876. and
just as nebulous and difficult as the problems then
tackled? Shall we continue merely to be a recording
agency and a means of communication? Can we not
take an active and effective part in determining, at
least in some degree, how and in what directions and
to what extent chemistry shall advance and chemical
research shall be promoted? Are we to-day engaged
Nov., 1018
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
in the kind of pioneer work that the founders of our
Society did in 1876? I am inclined to think that the
answer must be "No!" that is. we are not breaking
new ground, although we are very effectively cultiva-
ting old ground. Ought we not do more? I think
the present war has taught us that we should and must.
Certainly, the creative part of research, in its truest
sense, we cannot expect to control or guide. Never-
theless, it is of importance to the country and to our
science, once a general reaction or property has been
discovered, say, by Mr. A, that the full details and
scope thereof shall become known and recorded with
the least delay. Why should not Mr. A (or Miss A,
for that matter) be placed in a position where, through
the cooperation of others, those details can be promptly
worked out carefully and under good supervision?
There is no insuperable obstacle to giving A credit
for the reaction and B, C, D, and so on, credit for the
details that they may determine and fix, but it is not
an easy thing to do. If that could be done it would
relieve those who do not have a sufficient number of
cooperating students to enable them rapidly to work
out the large amount of requisite detail, from such de-
tail work, and would permit them freely and without
the restraining thought of not having completed that
other work, to engage in new work in which they
could use their creative and constructive ability to
better advantage.
POOLING MEN, MINDS, AND MATERIALS
But, to take this subject out of the field of clashing
priority and similar claims, let us consider another
phase. There are gaps a-plenty in our knowledge of
theoretically foreseeable preparations, inorganic and
organic alike. Why not have these gaps charted and
the work of filling them in by our colleges and univer-
sities coordinated, directed, and, if need be, supported
by our Society? To be sure, we would have to feel
our way very carefully at first, but the fact that it has
not been done is, in this case, no reason why it should
not be attempted. Not the smallest good from such
a work would be closer acquaintance between our
various instructional and investigational laboratories
and encouragement to investigation by students, but
fields abandoned by their original workers would be
kept in mind and further developed when oppor-
tunity offered; continued and balanced growth of our
store of fact-knowledge would result. Further, there
must be any number of reactions for identification and
differentiation, modes of separation, and the like,
which are awaiting discovery and recording. Can it
be that it is impracticable for the laboratories of this
country to "pool" their resources in students, instruc-
tors, and facilities, and systematically to work out
these fact-details? I am convinced that it can be
done and I believe that our Society is the proper
agency to effect such "mobilizing," to use a war-time
expression, of our country's resources in men, minds,
and materials. It will not do to say, "it can't be done."
It is proportionately not as difficult as the job tin-
founders of our Society tackled in 1876. I am con
vinced that the American Chemical Society has be-
come so strong and so large that it is under obliga-
tion to the country to do everything that can be done
once and for all for the benefit of all the chemists of
the country. This particular job of getting a line on
the unworked and abandoned chemical fields, lining
up our country's resources in institutions and personnel,
distributing the work to be accomplished, publishing
the results, attending to it that the "moppers-up"
follow as close on the heels of investigators as circum-
stances will permit, and keeping the whole work in
proper alinement is peculiarly one that our Society
should undertake.
government control of chemical research
If we do not do it, it is not unreasonable to expect
that our Federal Government will, so'oner or later;
perhaps that may be a good thing, but I am inclined
to think not. If we chemists cannot efficiently direct
the new growth of chemical knowledge, the Federal
Government also probably cannot; if we will not
then our Government would be perfectly justified in
taking a hand, an event already foreshadowed in pro-
posed legislation of the Sixty-fourth Congress. We
must be prepared to find that hereafter those govern-
ments that are spending large sums on chemical re-
search are going to view the field as a whole and are
going to determine in large measure what is to be in-
vestigated and to what extent and, further, that they
will not be over-communicative on such matters as
may affect national interests, external or internal. In
that event, our country will be disadvantaged. On the
other hand, if we so order our affairs that our resources
are "pooled" or "integrated," as the latest stylish legal
expression has it, and our efforts are directed as a
unit and the other countries do not, we will not be
at any disadvantage at any rate. The choice, there-
fore, as I see it is: if we do we will surely not be hurt;
if we do not, we may be hurt. The answer is not in
doubt: The Boards of Editors of our "Journal," of our
"Chemical Abstracts," and of our "Journal of Indus-
trial and Engineering Chemistry," will serve as an ex-
cellent starting point. The final answer lies with us,
as members, and with no one else.
AMERICAN HANDBOOKS ESSENTIAL
In 1 80 1 seven of the European languages were
spoken by 161,800,000 people. Arranged in the order
of the size of their percentage participation, these
languages are:
French 19.4
Russian 19.0
German r 18.7
Spanish 16.2
English 12.7
Italian 9.3
PortuRuese 4.7
In ion, 585,000,000 people spoke these seven
languages; arranged in the order of their percentage
participation they are:
English 27.3
German 22.2
Russian 17.1
French 11.9
Italian 8.6
Spanish 8.6
Portuguese 4.3
If now we divide the 1911 percentages by the i^'oi
percentages, we will gel the "growth-rate" for tach
of these seven European languages; the result is
884 THE JOURNAL OF INDUSTRIAL AXD ENGINEERING CHEMISTRY Vol. 10, No. n
EnR|ish Pe2"nt simply cannot be that we chemists cannot do equally
German 119 well by the fact-material of pure and applied chemis-
Russian 90 . . rr
Prcnch 61 try , inorganic, organic, physical, and theoretical. The
Spanish!!!!!!;!;!!;!!;!;!;;;!;;;;;;;!!;;!'.!!!! 54 procedure involved in effecting these proposals is not
ortiisuese 91 at a,j ngw £or ^js country; the only novel feature is
That is, English and German were the only Ian- the materials upon which it is proposed to operate;
guages that really grew and English grew 181 per the critical, painstaking research and sifting insepara-
cent as fast as German. ble from the Pharmacopoeia would not be so prominent
To-day our Society publishes three chemical jour- a part of these proposals where close reading and full,
nals, each in its field the equal of anything published accurate recording, based upon systems already in
in any language; this was not true 50 years ago nor existence or to be created, are the prime essentials,
even 30 years ago. This progress is highly gratifying Other like successful cooperative American efforts
and augurs well for the future. arei no doubt, known to each of you.
But how about those storehouses of the sum total If we undertake the work now under discussion there
of our chemical fact-knowledge and references to the wil! still be gaps between revisions during which it
original sources which are the indispensable tools for might be desirable or even necessary to publish sup-
research? Has not the time come when for very good plemental volumes or independent systematic records
and practical reasons, we should have our own hand- of interim progress like one or the other of the year-
books? Why should we be compelled to go to Beil- books that have been published abroad in the past, or
stein for fundamental information in organic chem- on the general plan of the annual progress reports
istry, to Gmelin-Kraut for inorganic, and to Stohmann which, for a short time, our Society published, or of
and Kerl for industrial information? Or to Morely those published by the American Pharmaceutical As-
and Muir of England or Thorpe of England? Or to sociation for so many years.
Wurtz of France or Fremy of France? We have made OUR JorRNALS AND orR G0VE]lNMENX
ourselves independent of the Centralblatt; why can ^, . , , , , .
__ „„+ „ tU , , , ., -, wu , ,, . , , , , There is probably no government that is so lavish
we not go the whole length? Why should not the lead- . ...... , , - , ,
;„„ „,.ki;„ +;~ ,. e *t.- 1 • a u • .u ui 1 j- ,n publishing, in good readable form, matter from all
ing publications of this kind be in the world s leading ' , , , , , , <■ .
nr,A ™~o+ *-„„\A\ : 1 •,,,., f parts of the world for the benefit of its citizens as the
and most rapidly growing language? It is clear from *; TT
■p„-nr.-.„ „. ,>,;«,„„„ ♦!,„*. n, 1 .. 1 ... Government of the Lnited States. It is probably
European experience that the only way to keep pubh- , , ,* }
„-,+;~„o „f +1,-- „ *■ *j*-u iil true that there is no people that is so indifferent to
cations of this sort up to date is by putting them un- , . . _ y K ,. ,
Aa*. +i^Q ™„t,-„i „<■ „ ■ +• i-i c • i_- u the efforts of its Government to enlighten it as the
der the control of organizations like our Society, which , ,,„.,„ , . , ,
„:j_ .■ _ j-. .. , , .. ., people of the L nited States an- that includes us chem-
provide continuous editorship and can expand it if . y . . ,. .
„^^a k„ 1 „,„ „n 1 u j ™ , ists. Apart from a very limitid number of our trade
need be, and we all know such need. These are only . . , . , ,
a few of the things that can be done once and for all Publications, our chemical journals have not made
for the benefit of all American chemists and I earnestly any sustalned or systematic effort to go through the
„,„„„,.„ +u„+ tu„ * ,,„ r^ €• j valuable material so made accessible, dieest it for
propose that the American Chemical Society do B
tj,„~ r\( ,.„ .„ 4. u . j ti .1 ., • their respective readers so that we could with any
them. (Jt course, we cannot hope to do all these things , , , . ,
~- <,,,k,.+:+,.+„,. f +u * u j. -r 1- degree of confidence go to the volume for any one year
or substitutes for them at once, but if we members ,,.•.<■ f - / ,
will set down in black and white all the things we are and find' f°r examPIe' the important features of the
convinced our Society should do and keep that list of world's and 0ur 0Wn develoPment alo"g lines of chemical
"Wants" up to date, our responsible officers can plan lndustry and lts sPe«fic trends and Part.cularly the
more wisely than they otherwise could, what things eXtent and nature °f 0Ur dePendence uPon fore'8n
shall be undertaken, and how and to what extent. co"ntrles ln thls reSard-
The initiative lies with us as members and not else- £ t0ok thlS War to Wake US up t0 thlS matter and
where. Without a complete picture of the enter- OUr Dlrectors have recently set aside a fund to enable
prises to be undertaken our officers cannot as safely T'n' J°"r"al "f Ind»*trial *»* Engineering Chemistry
'proceed as they otherwise could. t0 try t0 supply that feature- and our first
Tf r,nr <?r.n,ot,r „,;n ,.„^i„-t 1 *u ■ efforts in that direction are to be found in its
It our bociety will undertake these new enterprises . _ .
nr como ^f tv.o™ tv,„„ ...„ „.n u u j ■ i. • September 1018 issue. To be sure, this is a new
or some ot them, then we will be advancing chemis- h , , ,
try and promoting chemical research" more nearly in venture and !t WOuld be ""reasonable to expect that
the sense our founders had in mind in 1876, than if We had SCOred a bul1 S'eye- ^U> are d°mg the beSt
we refrain from so doing. we can ln this' t0 us' new hcld; we are feeling our way ;
you may want to call it ''groping" and perhaps you
it has been done before are right. If any of our members have suggestions for
The physicians, the medical societies, and the medical betterment they can rest assured that those sugges-
colleges of this country about too years ago and after tions will be welcomed by those who have charge of
almost 3 years of cooperative labor published the that field. This work is couched in modes of expression
first U. S. Pharmacopoeia (which has been revised and proceeds from points of view that are unfamiliar
decennially ever since and latterly in cooperation with to most of us; to grasp its message in all its bearings
pharmacists, pharmaceutical colleges and societies and we will be compelled, in effect, to acquire a new lan-
several of the United States Government services) and guage and a new mode of thought. But that is our job.
have produced a work which for decades has been the If and when we get our bearings in this branch of
premier publication pf its kind m t h. world. li Government publications, we will try to extend our
Nov., 1918
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
work to other suitable branches. It is not too much
to hope that in the course of a few years we will have
developed this work to such an extent that This
Journal will annually contain a bird's-eye view of
international trade and production, by countries, of
chemicals, chemical products, and materials of and
for chemical industry practically the world over.
There is so very much room for varied elucidative pre-
sentation and treatment of matters of this kind that
it is earnestly to be hoped that other chemical publica-
tions in this country will enter this field each with an
eye to the main requirements and viewpoints of its
own readers. The more angles we can get from which
to view these matters the better for our country and
our profession. Among the benefits of this work
that I look forward to is not only that of giving us of
the present day a bird's-eye view of the chemical indus-
try of the world and more particularly of this country,
that is, a view of the thing as a whole, but further, the
opportunity it will afford for the oncoming chemists
of to-morrow gradually to absorb this viewpoint by
specific instruction or otherwise on their way through
college or other courses of learning with the result that
when they take their places in our profession and our
business, comprehensive view and understanding of
their function in the industrial and economic fabric as a
whole will come almost as second nature to them.
The proposals I have so far made call primarily
for no extraordinary! help from our Federal Govern-
ment, though it is no doubt true that as we progress
in those fields we will be able to make practical and
practicable suggestions for betterment or expansion
of such Governmental publications and activities.
OUR CHEMICAL DEPENDENCE
There are, however, matters in which special Gov-
ernmental work is necessary. As an example, take
the matter of the nature and extent of our dependence
on foreign countries for chemicals, chemical products,
and materials of and for chemical industry. The
material published prior to 19 14 was not adapted to
giving effective answer to that question. There was
not enough detail. The first step in this direction was
taken when the Bureau of Foreign and Domestic
Commerce late in 1916, under the direction of Dr.
Thomas H. Norton, published what has since come to
be known in general usage as the "Norton Dye
Census." Early in 191 7, as the direct result of a
suggestion made by Dr. Norton in This Journal,
arrangements were initiated by our Society with the
Bureau of Foreign and Domestic Commerce for similar
treatment of imports in 1913-14 of all chemicals, chem-
ical products, and products of and for chemical indus-
try other than dyes, and along the general an
posite lines followed in a number of foreign countries
an,d our own country. It took consider;! M\
year to get all those details straightened out and then
it took several months to locate a chemist to su]
the work and then some considerable time to get the
necessary invoices and working staff to
all that, happily, is now behind us and we can look
forward to a list of about 4000 items for which the
Bureau of Foreign and Domestic Commerce will give
us the amounts and values of each item and the coun-
tries of origin of our imports for that period, the last
peace-year before the war. Now that we are prac-
tically "out of the woods" on this phase of the work, it
seems incredible that we should have had to spend so
much time getting where we now are. The reason is
not Government "red-tape" — not by any means. Very
little of that was encountered. The answer is not sim-
ple: in the first place it took a long time to analyze
the problem into its elements because we chemists
did not know exactly what we wanted and of course
the Government officials could not guess what we
wanted. I haunted many offices in Washington and
in New York trying to find out what we needed and to
get it into workable shape. In the second place, when
we got things boiled down the only available way looked
to be such a tremendously rocky road that we spent
quite some time looking for "short-cuts" but to no
use. There was nothing for it but to arrange with
the Treasury Department to have each of the ap-
proximately 100 ports of entry segregate from a total
of over 500,000 invoices those invoices containing the
desired material. To pick out this material from
Table 9 of the Bureau of Foreign and Domestic Com-
merce did not take long, once I had made up my mind
that I could not get any substantial help in that direc-
tion from the membership-at-large of our Society,
although certain few Sections did give me great help.
I am perfectly fair when I say that the greatest single
cause of delay was due to my attempts to hear from our
membership, an effort of great magnitude consuming
practically eight months. The reason behind that
is no doubt our own inexperience in these matters, and
I am very sure that it was not due to unwillingness in any
degree. However, that is behind us. When that publi-
cation appears, as I hope it may in February 1919, I
am sure that the Committee on Import Statistics of
our Society appointed last month at our Cleveland
meeting will have the benefit of every constructive
criticism our membership can make. It is too much
to expect that our first effort is perfect, but we do hope
for "better luck" next time.
This publication, then, in connection with the Nor-
ton Dye Census, will be the best information we can
get as to the nature, extent, and scope of our chemical
dependence upon foreign countries in 1914. Except-
ing dyes for the moment, which seem to need no further
help from our Society, and turning to the other ma-
terials, there is one thing that can be done once and
for all for American chemists and which should be
done and is being done by the American Cii
Society; that is, to translate all manufactured and
semi-manufactured products into needful raw materials
and their amounts and to classify these as of mineral,
animal, or vegetable origin as well as that can 1>
Unless present tentative plans go wrong the Geo-
Survey and the Department of Agriculture will
tell us in suitable publications where those raw ma-
terials come from and which of them can
haps those which ultimately shall be) obtained in the
States, the object of 1
more speedily and more certainly than otherwise to
886
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. n
give full force and effect to our Declaration of Chemical
Independence towards which we now have such
magnificent results to our credit, and whose advan-
tages we should never relinquish but, on the contrary,
should unremittingly protect and energetically de-
velop. I hope that when we similarly record the im-
ports for the first peace-year there will be only 2000
items of imports with big reductions each succeeding
year until we have brought our chemical dependence
to its irreducible minimum. In order that this result
may be further hastened the Tariff Commission may
tell us in a suitable publication about the industrial
uses of each of these entries.
PROMPT SPECIFIC RESPONSE ESSENTIAL
I have dwelt upon this particular enterprise of our
Society at this length not only because it is important
as such but also because it shows to what extent a
cooperative effort can be blocked through oversight.
If more of our Sections than did had notified me
promptly that they could not be of service, the work
would have been pushed ahead faster in some other
direction; but, without seeming arbitrary or high-
handed, I could not, in fairness, do otherwise than I
did, and I therefore hope that in all future coopera-
tive efforts Sections will understand, and act accord-
ingly, that time limits set must be observed and that
before the expiration of that time limit they will
definitely express themselves either by giving help or
by stating that they need not be waited for, as one
Section did to my great comfort. Then those who
have to do our work know where they stand and can
act accordingly.
With this piece of work, the result of cooperation
between at least six Government Bureaus, Depart-
ments, or Commissions and our Society, completed,
it is not too much to expect that in the future when we
will have time to look more closely into the status and
possibilities for development of our industries or the
betterment of our national research, educational, or
other facilities, ways and means of further effective
cooperation with Government agencies, Federal or
otherwise, will readily be found.
Dl CY-FREE CHEMICALS AM) APPARATUS
If the reports, spread both by word of mouth and
through the press, to the effect that our college and
other chemical laboratories have been greatly ham-
pered since the beginning of the war for lack of certain
supplies, both apparatus and chemicals, which formerly
came to us from abroad have actual foundation in
herald we not carefully study that question,
come to our conclusion as to the remedy, if any, and
forcefully present it in such quarters as may be need-
ful to prevent recurrence? Have we not been too com-
plaisant, both in college and out, as to this dependence
upon foreign supply sources? Have we not perhaps
too actively helped along the idea that foreign labora-
tory chemicals, foreign filter paper, foreign test tubes,
foreign microscopes, foreign porcelain, foreign glass-
ware, and foreign-almost-everything were the real
and only things to use? Have we really encouraged
domestic makers of related materials to supply these
things from domestic sources and manufacture?
What percentage of our laboratories in 191 3 were of all-
American equipment? Have not our colleges contrib-
uted a great deal to that state of affairs by using
foreign-made goods so extensively in their equipment
of those laboratories where most of us received our
introduction to materials of this kind? I presume
we will all agree that it is of vital national importance
that our colleges, universities, and the like be kept at
all times at top-notch ability and that measures should
be taken to prevent their being crippled at any time.
Would it help matters any to abolish our practice of
many years' standing; namely, duty-free importation
of materials of these kinds for scientific, philosophical,
and educational purposes? Perhaps not, but should
we not know what our opinion on that point is and
should we not now and thoroughly go into it again
with the events of the past four years clearly in mind?
I will not attempt to give a categorical answer, but
will merely ask: If it be proper to tax dyes to the end
that we may have a domestic dye industry for the ulti-
mate purpose that large domestic dependent industrial
interests may never again be placed in jeopardy,
may it not also be proper to tax foreign-made educa-
tional and scientific materials to the end that these be
made here and for the ultimate purpose that our edu-
cational and scientific undertakings dependent thereon
may never again be placed in jeopardy? This is a
question that requires a great deal of thought and one
that cannot be settled off-hand; furthermore, it is a
question that may require Federal legislative or other
action.
CHEMICAL COMMERCIAL AGENTS
If chemistry and chemical industry be really so
essential to national welfare as they are now quite
generally accepted as being, should there not be more
and effective chemical talent embraced in our foreign
consular and similar services than there has been?
Should not the American Chemical Society get at
the facts, form an opinion, and be prepared to express
and follow up that opinion? This may involve added
Federal administrative action.
These problems are some of the very many that
have been in my mind in a more or less general way
and are probably fairly typical of all the rest. But
there is just one other big and very handsome
thing I should like to see done, and I believe
the American Chemical Society really ought to do
it. It is not truly a war measure, although its
utilitarian side was made more readily discernible by
the war. It has considerable utilitarian or senti-
mental possibilities, as you prefer, through the en-
couragement the beginner or even an "old timer" in
chemistry can get from it when things look very "blue"
and the world is "all wrong." quite apart from the new
hat it may help engender.
AMERICA'S contribution to chemistry
What I have in mind is that the contribution of
Americans chemists to the science and industry of
chemistry is not as well known as it should be nor is it
a matter that could be readily ascertained, at any rate
Nov., 191 8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
887
not before 19 14. Professor Edgar F. Smith, by his
books "Chemistry in America" (published in 1914) and
"The Life of Robert Hare" (published in 191 7) has most
auspiciously inaugurated the work of worthily pre-
senting the labors and triumphs of America's chemists.
Could the Fiftieth Anniversary of the American Chem-
ical Society, which comes in 1926, be more fittingly
marked and celebrated than by a Jubilee Volume,
which contains as compact and complete an account'
as could then be made of what American chemists
have done? From 1768, the date of the earliest known
American chemical research, to 1926 makes a span
of 158 years. Just think of the tradition, concrete
and tangible, crammed to the bursting point with the
triumphs and trials of Americans, that would be con-
tained in such a volume. Could any one appraise in
dollars and cents or otherwise the value of the stimula-
tion to and the enthusiasm for more and better work on
the part of America's then chemists, from beginner to
old-timer, that such a volume would create? Could
we give the Nation abetter or more dependable means
of appraising the value of chemistry in its affairs?
Incorrect knowledge of national achievements and
capabilities is a national weakness; correct knowledge
is a national strength.
I know that our Society has many burdens to face
in the near future, but could wc not find time and op-
portunity for this work also?
OUR MEMBERS IN THE SERVICE
It may safely be taken for granted that those of our
members in Service, both at home and abroad, are
acquiring new points of view as to what the future
course of action of America's chemists should be
and that they are formulating more or less definite
lines of action for the American Chemical Society.
When they come triumphantly home they will expect
to find our Society prepared to receive, consider, and to
act upon their suggestions. No doubt, at meetings
of our newest Section, "for the entire territory of
France," this subject will be threshed out more or
less formally and conclusively. Should we not then
be able to match their plans with something we have
planned so that we can compare the two programs and
act upon the result with the least delay? Would
any other course be fair to them?
conclusion
I am fully aware that in proposing pre-peace pre-
paredness a task of very great dimensions is being
opened up. But can we, in good conscience, do less?
Our faces are set toward a future filled with perplexing
problems; much effort will have to be put forth, not all
of it can succeed. Many or even all of my suggestions
may be impracticable or impractical, my present view
to the contrary notwithstanding; that is something we
must each and all individually be prepared to face;
that should not and must not, in these extraordinary
times, deter any of us from making all suggestions that
to us seem proper. An imperfect suggestion may well
contain the germ of a valuable plan. Neither personal
pride nor fear of chagrin must in these times make us
shrink from contributing whatever we can; fear of
personal failure must resolutely be put to one side. We
must accustom ourselves to "thinking out loud;" not
all thoughts bear fruit, but that is no reason whatever
why we should not now "think out loud."
25 Broad Street
New York City
CHLMICAL MARKLT5 IN THL UNION OF 50UTH AFRICA
By O. P. Hopkins,
The Union of South Africa is a self-governing British
dominion comprising the Cape, Natal, Orange Free
State, and Transvaal provinces, the total area of which
is 473,075 sq. mi. with a population of 5,973,394,
of which 1,276,242 are whites. Mining and agricul-
ture are the chief industries, but the output of gold
and diamonds easily exceeds in value all other products.
The principal mineral products in 1914 were gold,
$173,560,000; diamonds, $26,703,000; coal, $10,847,-
000; copper, $3,369,000; tin, $1,515,000.
Manufacturing is still in a backward state despite
the war stimulation and recent earnest discussion of
plans for promoting industrial development. The
manufacture of wattle-bark extract for export, in
place of the bark formerly taken largely by Germany,
is a war industry, and there has also been a marked
increase in sugar production. The diamond and
feather industries, on the other hand, have bei
adversely affected by the war. As a whole, t he Union
has had its share of war prosperity, the fly in the oint-
ment being the high prices of necessities, which, as in
other countries, have counteracted to a large extent
the high wages received by the poorer classes.
The pi luchascs of heavy and fine chemicals
Washington, D. C.
are high, so that the Union is a more attractive field
for the sale of such products than many of the more
thickly settled countries that receive more attention
from our manufacturers. The principal difficulty
lies in the fact that the mother country does the bulk
of the business and in all likelihood will continue to
do so. American products are well and favorably
known, however, and a steady expansion of the busi-
ness should be possible, especially in view of the fact
that there are certain German lines to replace, although
it should be recognized at the start that this is one of
the markets that Teuton chemical products did not
domin
An idea of the extent of the market for cle
and allied materials and products can be gained from
table, which shows imports by principal
classes for the calendar years 1914, 1916 and 191 7.
It should be borne in mind that there was a disloca-
tion of trade during the latter part of 1914, where-
fore that year should not be considered normal. The
total imports of all classes of goods into the Union in
1914 fell about 20 per cent below the total for 1913; in
value, the imports for 1916 correspond very nearly to
normal.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. n
Summary op Imports op Chemicals and Allied Lines
Classes 1914 1916 1917
Chemicals $6,226,000 $7. 566. 000 $7,392,000
Drugs, medicines, perfumery . etc . . 2. 089. 000 2,760.000 2.595.OO0
Dyes and tanning materials 28,000 132.000 137.000
Explosives 1,189.000 1.646,000 1,201.000
Fertilizers 880.000 617.000 219,000
Oils. fats, and waxes 5,215,000 8,216,000 9.614.000
Paints,.varnishes, etc 831,000 1,304.000 951,000
Metals and miscellaneous ma-
terials 1.527,000 3,041.000 2.260,000
Miscellaneous products 5,264,000 6,754,000 6,169,000
Total 23.249,000 32,036,000 30,538,000
An idea of the relative importance of the principal
chemicals and allied products that enter the import
trade may be gained from the following arrangement, in
which the articles are divided into two convenient
classes and arranged according to their importance
in 19 1 7, only such lines being included as exceeded
$400,000 in value during one or more of the three
years considered. It will be seen that the three most
important items under the heading "Chemicals, drugs,
etc." have to do with mining, the principal industry
ofj the country; that is, they are materials for the
manufacture of explosives for breaking rock, or ma-
terials for the reduction of the ore. Large quanti-
ties of explosives, however, are now being manufac-
tured for war purposes. These classes are followed
by the finer chemicals included under the headings
perfumery, medicines, and pharmaceutical supplies,
the per capita consumption of which, considering the
limited white population, is rather high. The only
important item imported for agricultural purposes
is superphosphates, the last on the list. The most im-
posing totals for the allied products are mineral oils, in
which the United States has a large share, paper,
paraffin wax, and vegetable oils.
Relative Importance op Various Lines Imported
Articles 1914 1916 1917
i, Drvcs, Etc.:
Glycerin $2,101,000 $1,826,000 $1,910,000
Industrial nitrates 1.073.000 1.357.000 1,829.000
Sodium cvanide 1.812.000 2.167.000 1.703.000
Perfumery 398.000 668,000 677,000
Medicinal preparations 514.000 648.000 595,000
Pharmaceutical supplies 722.000 620.000 375,000
Superphosphates 429,000 437.000 148.000
Allied Materials and Products:
Mincr.il oil 3.196.000 4.105,000 5.565.000
Paper 1.267,000 3,031.000 2,595,000
Paraffin wax 626.000 1.461.000 1,812,000
Vegetable oil 872,000 1,608,000 1,295.000
Zinc 683,000 1,898,000 1,191,000
903,000 1,651.000 974.000
Sugar 1,315.000 245.000 821.000
Fuse 463.000 888,000 752.000
Detonators 201.000 568.000 302,000
Mil MICALS
The following table shows the extent to which the
various articles that may be classed as chemicals are
imported into the Union of South Africa and the ex-
tent to which the principal competing countries
share in the market. The glycerin is imported chiefly
from the mother country, but there has recently been
an acute shortage and great efforts are being made to
stimulate the domestic output and at the same time
to produce mine explosives that do not require glyc-
erin.
The sodium cyanide was supplied by Great Britain
and Germany before the war and now comes exclu-
sively from the former country. The United States
has no share in the trade. The sodium nitrate is
imported directly from Chile.
Articles
Acids:
Acetic
United Kingdom.
United States....
Nitric
United Kingdom.
United States
Sulfuric
United Kingdom.
United States... .
Tannic
Germany
United Kingdom.
United States
Tartaric
Germany
Italy
United Kingdom.
United States
Ammonia:
For ice-making
Australia
United Kingdom.
United States
Carbonate
United Kingdom..
United States
Nitrate
Belgium
Germany
Norwa\
United States
Borax
United Kingdom
United States
Calcium carbide
Canada
Imports op Chemicals
1914
34.431
14.800
6.536
11.879
No
60,850
60,019
550
256.065
111.161
105.273
12,994
6.833
4,794
1,187
1 1 . 290
226.560
213.464
4.531
United States
Carbonic acid gas
Germany
United kingdom
United States
Chloride of lime
United Kingdom
United States
Creosote
United Kingdom
United States
Disinfectants and germicides
United Kingdom
United States
Glvcerin, industrial:
Crude 2.100.927
United Kingdom 1,177,173
United States 258
Other (0)
United Kingdom
I'nited States
Nitrates for manufacturing purposes.. 1.073,117
Chile 1.0+4.682
United States
Potash:
Cyanide 9.184
United Kingdom 3 , 299
United States
Saltpeter 6.575
United Kingdom 3.991
United States
Compounds of. n. o. dl
United Kingdom
Germany
United States
Sheep and cattle dip
United Kingdom
United States
Soda:
Carbonate
United Kingdom
United States
Caustic 107.005
United Kingdom 101.778
United States 4.701
Cvanide 1.812.431
Germany 739.990
1 "iiited Kingdom 1 .064, 153
United States
Compounds of. n. o. d1 69,815
United Kingdom 63.157
United States 5
Sulfur:
Roclc. including iron pyrites
55.883
Japan
Spain
I'nited States
Flowers of
Italy
Japan
United Kingdom
United States
69.815
16.878
16.328
633
215.250
102.252
1S.2S4
2.414
38.874
22.639
1916
5.086
3.854
895
2.866
2.253
613
3.489
2.711
779
3.708
25.190
12.818
706
10.628
25.856
10,701
7,680
7,266
3.460
3.460
42.923
120.553
120.081
443
257.564
149.071
64.924
14.590
5.646
34
4.375
54
31.625
28.552
2.068
8.444
8,424
20
393,948
363.659
20.220
1.340,205
2.930
1.356.980
1.348.751
92
15
117.195
85,271
1.849
S.123
264.684
56.851
15
546.476
76.896
2.167.287
2,159,739
78.935
70.730
6,994
80.755
44,836
146.701
124.S07
1917
2.370
1.630
419
2,837
2.453
384
3.815
2.793
1.022
2,331
297
3,236
41.794
24 . 284
14.634
934
31.439
10.692
9.227
11,519
7.583
7.568
15
42,923
18,396
17.841
268
43.638
15,461
16,478
11,699
8,186
8.186
574
15
140.326
111.477
14.809
2.304
4,989
4,989
19,675
18.566
258
2.384
2.384
396 . 090
363,216
24.464
711
1 . 3 1 1 , 1 28
1.255,465
19.282
1.829.357
1.746.626
15.860
14.463
1,397
67.411
46.188
11.281
259.414
1S6.718
62.685
45.896
42.480
1.976
248.817
160.045
124.743
.703.241
49 . 239
46.013
1.796
89.787
37.229
152.025
43.677
7.597
10.166
745
25.160
13.582 15.9
1 . 436 5.5
(a) No classification of glycerin attempted in 1914.
' Not otherwise distinguished.
Sheep and cattle dips, germicides, and disinfec-
tants together form a considerable total, of which
Great Britain has almost a monopoly. According
to the Weekly Bulletin of the Canadian Department
Nov., 1018
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
of Trade and Commerce, there will be a steadily in-
creasing demand for ammonia for ice-making, as
the refrigerating industry is bound to grow.
To those who have pondered the German success
in other countries, the insignificant part that German
chemicals have played in this market, as shown in
the preceding table, will come as a surprise.
DRUGS, MEDICINES, PHARMACEUTICAL SUPPLIES
In medicinal supplies and perfumeries the United
States has a very fair share of the South African trade,
the United Kingdom alone having a larger business,
and Germany being nowhere. In pharmaceutical
supplies English goods predominate, although Amer-
ican lines are sold in some quantity. German manu-
facturers did twice as much business as their Ameri-
can competitors in this line in 1914. In estimating
the effect the war has had on the trade, the rise in
prices should be kept in mind when comparing the
import values for the different years. The South
African market for drugs, medicines, etc., can be
estimated from the following table:
Imports op Drugs, Medicines, Etc.
Articles 1914 1916 1917
Bacteriological products, including vaccine
virus, etc $22,765 $17,9.18 $14,400
United Kingdom ,. 14,390 10.390 5,373
United States 7,154 6,780 8,522
Bromine, litharge, and manganese dioxide. . . 25,992 65.051 24,338
United Kingdom 23,534 62,588 19,228
United States 1,061 822 73
Magnesium sulfate 10,147 29,133 19,043
United Kingdom 9,617 23.982 16,449
United States 243 1,484
Medicinal preparations:
Spirituous 70,827 127,108 108,596
United Kingdom 39,837 82,804 68,477
United States 25,832 41,584 36,416
Non-spirituous 442,897 520,721 486,456
United Kingdom 339.380 417,707 362,326
United States 77,023 83,724 98,070
Opium 2,934 6,818 7,660
Turkish Empire 2,389 3,353 560
United States
Perfumery and perfumed spirits:
Perfumery 311,442 527,178 517,411
United Kingdom 149,873 237.733 227,815
United States 111.204 205,298 232,118
Perfumed spirits 84,001 140,476 159,538
Germany 26,231
United Kingdom 46,310 123,712 147,304
United States 988 1.981 3,076
Pharmaceutical supplies 721.541 620,216 375,256
Germany 98,498 759 73
United Kingdom 515,966 460,955 266.762
United States 42,304 61,337 42,188
Saccharine 910 3,319 1,518
United Kingdom 857 3,314 1,056
United States 53 5 24
Spirits, non-potable:
Alcohol 117 526 229
Methylated 224 117 5
Other plain spirits ... ... 555
Tartar, cream of 36,100 49,088 48,105
France 22.225 28,698 32,683
Germany 7,947
United Kingdom 5,792 3,051 7,354
United States 12,594 4,102
Tinctures 1,475 3,908 1,178
United Kingdom 1,012 3,076 535
United States 297 822 642
All other' 358,613 648.501 831,568
Germany 73.991 1,382 1.126
United Kingdom 233,565 517.718 576,748
United States 23.758 73.032 109,462
1 Includes all other drugs, chemicals, and pharmaceutical products.
DYES AND TANNING MATERIALS
The items included under this head in the follow-
ing table are those shown in the official statistics.
The only articles of any importance are evidently
included under the "All other" head, which itself is
comparatively insignificant:
Imports op Dyes and Tanning Materials
Articles 1914 1916 1917
Bark $ 107 $9,179 $3,275
Cutch 307 944 1,981
Gambier 866 886 1,236
Logwood 170 788 3,854
Myrobalans 331 7,057 4,536
Sumac 428 1.178 5,169
All other, n. o. d 25,394 111,477 116,981
United Kingdom 10,273 60,121 57,338
United States 5,359 42,971 46,403
FERTILIZERS
The only important fertilizer imported into the
Union of South Africa is superphosphate, the bulk
of which came from the Netherlands before the war.
In 1016 England was the most important source of
supply, with Japan, a newcomer, second. In 1917
Japan had the field to herself, although unable to
satisfy demands. Details of the fertilizer trade are
shown in the following table:
Imports op Fertilizers
Articles 1914 1916 1917
Ammonium sulfate $11,719 $3,859 $3,903
Basic slag 67,090 100.318 12,191
United Kingdom 29,374 100,318 12,191
United States
Bone manures 89.023 4,404 10,069
India 24,498 ... 8,527
United Kingdom 25,691 4,205 297
United States 5
Guano 24.171 448 7,140
Nitrate of soda 1.105 73
Phosphates, raw 5 , 767
Potash 30,080
Superphosphates 428,753 437,133 148,063
Japan 139,352 130,914
Netherlands 290,633
United Kingdom 87,986 289,187 17,135
United States 8,595 15
All other 222,604 70,584 38,013
Netherlands 78,341
United Kingdom 138,510 60,077 12,395
United States 3,509 17,953
COLORS, PAINTS, AND PAINTERS' GOODS
In this line the United States has a monopoly of
the trade in turpentine and a goodly share of the
business in water paints, distempers, and ocher.
The mother country dominates the important "All
other" class. Details of the trade are as follows:
Imports op Paints, Colors, and Painters' Goods
Articles 1914 1916 1917
Ocher $35,998 $47,897 $44,909
United Kingdom 35,852 47,858 44.826
United States
Turpentine and substitutes 71.654 93,632 88,225
United States 69,498 87,627 83,281
Varnish 107,535 184,811 128,787
United Kingdom 93,569 163,758 110,664
United States 9.412 17,792 15,817
Water paints and distempers 59,673 81.582 57,065
United Kingdom 24,756 30,927 23,753
United States 33,963 48,147 31,481
All other kinds 556,075 895.601 632,193
United Kingdom 484,689 819.922 495,770
United States 43.005 45,127 95,287
EXPLOSIVES
A glance at the next table will show that the mining
industry has not depended upon foreign manufac-
turers to any great extent for explosives, although
reliance seems to be placed upon outside sources
for such accessories as fuses and detonators. As al-
ready mentioned, the shortage of glycerin has worked
a hardship on the domestic explosive industry, but
the manufacturers have been producing an explosive
called sengite to take the place of gelignite, the new
preparation not calling for glycerin. Nevertheless
the Chairman of the Scientific and Technical Com-
mittee, in a report published by the Department of
Mines and Industries and dated January 1918, states:
The mining industry is dependent upon an adequate supply of
explosives, in the manufacture of which glycerin forms an
890
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. n
essential ingredient, and, unless the requisite quantity of this
latter chemical is obtained, the supply of gold to the United
Kingdom, the revenue of the Union, the livelihood of many
persons directly or indirectly dependent upon the mining in-
dustry, and the market for South African produce, must be
seriously curtailed.
Imports op Explosi
Articles 1914 1916 1917
Blasting compounds:
Collodion and guncotton $245,247 $ ... $ ...
Germany 65,173
United Kingdom 180.074
United States
Dynamite and other compounds 58.739 7.587
United Kingdom 58,695 7,582
United States ....
Caps, percussion 633 336 638
Cartridges, loaded 183,560 155.208 125.045
Germany 26.508 83
United Kingdom 144.501 102.499 62.111
United States 6,303 52.339 62.311
Detonators 200.670 568.212 301.621
United Kingdom 195,580 279.849 243.510
United States 288.365 58.111
Fuse 463.116 887.981 752,346
Germany 75,495
United Kingdom 379.772 570.121 718.695
United States 1.956 308,074 33,409
Gunpowder, including powder contained in
cartridges 37,263 26.956 21.052
United Kingdom 30.250 21.549 13.870
United States 676 5,183 6,419
OILS, FATS, AND WAXES
Mineral oils form by far the largest item in this
group of imports, and the United States dominates
the trade, especially in lubricating and illuminating
oils. The Dutch East Indies are a formidable com-
petitor in the trade in the lighter distillates. Amer-
ican producers have some share in the edible-oil trade,
but considering the vegetable-oil business as a whole
the United States is not an important factor. Amer-
ican exporters had about half the business in paraffin
wax before the war, but are second now to the ex-
porters of India, although sales have increased greatly
in value. The imports of "anti-friction grease"
were divided rather evenly between Great Britain
and the United States before the war, but our ex-
porters have increased their share since hostilities
started. Details of the imports of these lines are
shown in the table that follows:
Imports of Oils, Fats, and Waxes
Articles 1914 1916
Oils, animal:
Fish S 2.005 $ 9,154
Lard 4.950 9,825
Whale 38.655 131
Other animal 2.205 3.796
Oils, mineral:
Lubricating 726.637 926,343
United States 627,667 844.937
Motor spirit, including benzene and
naphtha 1,164.301 1,760.413
Dutch East India Islands 557.837 869.507
United Stales 600.872 884.613
Paraffin' 1.2X4.581 1,225.629
United States 1,283.170 1,225.369
Other mineral 20,902 192,831
Oils, vegetable:
Castor 80,808 130,364
India 26,572 39.268
United Kingdom 48.787 86.921
United States 774 190
Cocoa butter 10,843 8.838
United Kingdom 5.276 5,154
United States 3,679
Coconut 165,991
Australia 29,068
India 25,253 27.078
Mauritius 16,576 58,366
Zanzibar 29,31 1
United States
Colza and rape 4.755 15.023
Cottonseed, industrial 99,462 105,146
China 11,824 77.I.S4
United Kingdom 77,986 19,505
United Stat. 2. 136 6,696
Linseed 189,8
United Kingdom 189,161 320,722
United States 2.136 6,696
1 Kerosene.
Imports op Oils, Fats, and Waxes (Concluded)
2.661,328
1,055.807
1.601.566
1.485,383
1,485.383
308.123
205.541
106.820
96.858
200
'.. 122
4,759
1,178
145.285
38.353
24 . 703
43 . 1 1 2
5.558
13.310
90.833
81.655
117
Articles
Oils, vegetable {concluded):
Palm and palm kernel
British West Africa
Nigeria
United States
Salad:
Cottonseed
United States
Other salad oils
India
United Kingdom
United States
Other vegetable
Anti- friction grease
United Kingdom
United States
Margarine and other butter substitutes
Netherlands
United Kingdom
United States
Wax:
Beeswax
Paraffin
India
United Kingdom
United States
1914
1916
Ste
United Kingdom...,
United States
Oil-bearing materials:
Copra
Zanzibar
United States
Palm kernels
British West Africa.
United States
All other
$ 76,755
$ 431.284
$ 125.546
13,128
347,167
297
62,393
76,030
120.787
149.606
150,501
83.719
123,819
133,927
79.708
126,738
261.385
315,675
3.037
75.056
137.566
43.745
66,448
77.032
48,865
82.658
51,298
50.077
16.313
54.715
214.953
331.764
315.992
113.005
132.890
124.539
97.427
198,529
191,186
107.521
152,268
32.980
52,592
65.820
5.159
50.378
84.069
22.259
1,509
652
2,623
1.976
7.193
10,030
626.163
1,461.118
1.811,671
148.404
259.531
914.547
122,310
66.326
517.608
1.113.922
770.620
148,219
118.227
145.266
61 ,970
110.454
134.340
9,052
7.626
10.925
253.903
299.937
196.938
230,176
78,575 118.952
MISCELLANEOUS PRODUCTS
The United States has never enjoyed the lion's
share of the trade in any of the articles included in
this group except baking powder, yet a study of the
following table should reveal possibilities for future
opportunities that will be well worth while. The
demand for some of these lines will grow steadily
once the war is over and it is unlikely that certain of
the old sources of supply will be relied upon again for
some years to come.
Imports of Miscellaneous Products
Articles 1914 1916 1917
Baking powder $228,726 $243,174 $409,803
United Kingdom 14.429 31,914 15.632
United States 211.372 211.051 394,152
Blacking and shoe polish 241,129 254.941 240.275
United Kingdom 234.872 241,968 226.132
United States 3.796 12.886 13.758
Blue 63,864 70.043 114.636
United Kingdom 63,494 68,550 114,582
United States 151 24
Candles 22.858 10.774 4.628
United Kingdom 19.982 10.186 4.531
United States 433 10 7S
Extracts and essences:
Food 123.576 130,086 68.219
United Kingdom 120.782 125,623 62.520
United States 618 2.526 4.370
Flavoring, spirituous 83.879 110.971 89,145
France 14.829 26.708 28.061
United Kingdom 67.124 83.130 60.627
United States 185 779 268
Flavoring, non-spirituous 9,942 12,556 5.918
United Kingdom 7.889 8.162 2.132
United States 219 419 355
Glass:
Bottles and jars 499,848 894.356 509.703
Germany 78.443 13,456 1.304
Japan 63.469 61.907
Sweden 75.022 J45.656
United Kingdom 267.4r>S 261.351
United States 46.860 236,288
Plate 115,682 1S2.464 137,245
Belgium 32,523 4.069 151
Canada SO. 891 J.S47
United Kingdom 160.195 133.966
United States 15 15.364 3.05r.
Window 97.287 206,057 142,827
Belgium 44.573 10.7"- 1".I74
United Kingdom 44.388 98.912 90.814
United Si. ins 44 S5.456 26.275
Glassware n o d 190,719 368,302 183,964
Belgium 46,870 m.,"04 18,658
Germany 900 209
Japan "20 76 . S03 59 . 503
United Kincdom 56.106 t.2.729 48.816
United States 12.994 83.437 40.548
Glue... 19,155 50.616
United Kingdom 12.984 33.559 »'.648
United States 1.343 2,861 1.436
Matches 17.048 8.609 3.981
Sweden 15.714 S.098 3.830
United States 5
Nov., 1 918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Imports of Miscellaneous Products
Articles 1914
aper:
Printing $ 960,346
Canada.
Germany
Norway
United Kingdon
United States. .
Wrapping
iiii.-1-i
Germany
Norway
Sweden
United Kingdom
United States
Photographic material1..
Germany
United Kingdom
United States
Soap:
Common, brown, etc..
Australia
United Kingdom. . . .
United States
Toilet
United Kingdom. . . .
United States
Extracts and powders.
United Kingdom. . . .
United States
Sugar, molasses, etc.:
288,394
73,295
30,133
110.898
439.567
45 . 235
306,765
2,540
35,117
57,070
110,898
80,847
5,290
240,177
15.418
132,491
87,845
184,467
150,862
7,539
28,455
155,101
102,757
39,905
11,996
11,315
428
58,899
54,627
312,750
312,493
(Concluded)
1916
11,903,503
312,634
895
116,675
224,044
996.095
213.654
1,127,320
288.365
209
177,175
348,101
288.282
79.752
292.569
122
GIu
United States
Golden sirup
United Kingdom...
United States
Molasses and treacle 3 . 650
Saccharum 1 , 197
Sugar 1,314.889
Mauritius 588,384
Portuguese Hast Africa 586 , 1 70
United States 7,898
' Sensitized goods not stated separately.
172,002
77,013
30.211
63.834
263,000
174.284
85.203
26.333
25,895
389
69,012
67,771
107,443
106,937
165
3,158
1.523
245.495
14. 999
186,056
34,523
113,200
382.346
606,142
225.095
840.634
168.113
50.514
251.866
278.627,
50.646
295.353
130,208
82,293
23.924
19.432
207.011
151 .597
50.495
21.408
21,198
107
111.930
100,664
27.968
24,990
1,645
808
545
821,339
43,608
724,052
49 , 843
MISCELLANEOUS MATERIALS
Zinc is the only item of outstanding importance in
this group and it is now imported almost exclusively
from the United States. Previous to the war Ger-
many was a serious rival. The extent to which the
various items are imported is shown in the following
table:
Imports of Miscellaneous Materials
Articles 1914 1916 1918
Metals:
Copper, bar. ingot, rod $ 24,747 $ 39,959 $ 23,126
Iron, pig and ingot 20,770 36,903 56,617
Lead, bar, pig, and sheet 80,419 119,190 58,734
Quicksilver 134,817 192,003 188,664
Tin, bar, block, ingot 50,096 81,616 170,688
Zinc, unmanufactured 683,251 1,898,485 1,191,217
Belgium 68,112
Germany 245,086 92 24
United States 340,052 1,810,684 1,079,818
Other Materials:
Asphalt and bitumen 1 7 , 729
Cement 340, 169
Emery
India rubber ;
Lime
id gutta-percha.
Mica
Pitch
Plumbago
Plaster
Resin and rosin
Tar and substitutes
(o) Not stated separately
12,195
(8)
12,502
2.097
8,210
3,528
5.305
45.132
14.230
227.475
25.185
105.720
9,519
2,900
3,314
6,152
11.422
129,206
137,887
20,863
105.389
23.987
141,840
1,479
2,599
4,015
4.730
8,098
115.653
142,224
ORIGINAL PAPERS
EXAMINATION OF ORGANIC DEVELOPING AGENTS
By H. T. Clarke
Received July 20, 1918
From the time that the European war cut off the
supply of foreign organic chemicals to this country,
two distinct activities have been apparent in the photo-
graphic developing agent trade; on the one hand, the
efforts of manufacturing concerns to produce the most
necessary substances, like hydroquinone and salts
of />-aminophenol, and, on the other, the less commend-
able manipulations of the purveyors of bogus and
adulterated developing agents. For the control of
both of these activities chemists are necessary — to
check the purity of the genuine products and expose
the composition of the false. Moreover, in many
cases developing agents are submitted under fancy
names and it is necessary to identify the substances
they contain.
The work of the analyst thus falls into three classes:
the separation and identification of genuine developing
agents; the quantitative determination of such sub-
stances; and the identification of the materials em-
ployed for adulteration or substitution.
The following scheme for the identification of the
commoner developing agents is drawn up to meet
the first; a few suggestions for quantitative work fol-
low; but owing to the enormous number and variety
of adulterants, no attempt can be made to indicate
all of the methods employed for their detection and
estimation, which in any case are subject to the meth-
ods of routine analysis.
QUALITATIVE METHODS
GROUP TESTS
Taking o. 1 g. of sample:
I — Insoluble in 5 cc. of cold water:
/>-Hydroxylphenyl glycine
II — Soluble in 5 cc. of ether:
Hydroquinone
Chlorohydroquinone
Catechol
Pyrogallol
III — Soluble in 5 cc. of alcohol:
p-Aminophenol base
/>-Aminophenol hydrochloride
5-Amino-2-cresol hydrochloride
2,4-Diaminophenol hydrochloride
^-Dimethylaminophenol oxalate
Ilia — Insoluble in alcohol :
p-Aminophenol sulfate
5-Amino-2-cresol sulfate
/>-MethylaminophenoI sulfate
/>-Dimethylaminophenol sulfate
o-Methylaminophenol sulfate
^-Phenylenediainine hydrochloride
DISTINGUISHING TESTS
(A) Test aqueous solutions with litmus: Neutral
or only faintly acid with Group II; Groups III and
Ilia give markedly acid solutions (with the exception
of pure />-aminophenol base). Test aqueous solu-
tions for chlorides, sulfate, oxalate, and other com-
mon anions.
(B) Treat o.i g. in i cc. hot water with one or
two drops of 10 per cent sodium carbonate solution,
and let mixtu minutes to cool.
892
THE JOURNAL OF INDUSTRIAL AXD ENGINEERING CHEMISTRY Vol. 10, Xo. 11
group i. p-Hydroxyphenylglycine — Dissolves with effer-
vescence; very little change on standing.
group 11. Hydroquinone, Chlorohydroquinone, and Catechol —
No effervescence; solution darkens slowly on standing.
Pyrogallol — No effervescence, solution darkens rapidly on
standing.
GROUPS in and ma — AH cause effervescence except pure
p-aminophenol base.
Crystalline precipitates formed on cooling: Salts of p-amino-
phenol, s-amino-2-cresol and o-methylaminophenol.
No precipitate on cooling: Salts of 2,4-diaminophenol,
p-methylaminophenol, p-dimethylaminophenol, and p-pkenylene-
diamine.
(C) To 0.1 g. of sample in 2 cc. of water add a
few drops of 10 per cent ferric chloride solution.
group \— p-Hydroxyphenylglycine gives no color reaction in
the cold; odor of quinonc on boiling.
group 11 — Hydroquinonc gives dark greenish precipitate of
quinhydrone in the cold; strong odor of quinone on boiling.
Chlorohydroquinone gives reddish brown coloration in the
cold, odor resembling that of quinonc on boiling.
Catechol gives a green coloration with one drop of ferric chlor-
ide; with excess a nearly black precipitate is formed; no odor
is produced on boiling.
Pyrogallol gives intense reddish brown coloration in the cold;
no odor on boiling.
groups ill and ma — Salts of p-aminophenol and 5-amino-2-
cresol give purple colorations in the cold; odors of quinones on
boiling; the purple colors are not destroyed.
p-Methylaminophenol sulfate behaves similarly, except that
the purple coloration is developed more slowly.
Salts of p-dimethylaminophenol give no color in the cold; the
solution darkens on boiling, with formation of quinone odor.
With 2,4-diaminophenol hydrochloride an intense red color is
developed in the cold; no odor is produced on boiling.
With o-methylaminophenol sulfate a dark purple color is pro-
duced, turning to red-brown on standing or more rapidly on
warming. No odor is produced on boiling.
With p-phcnylenediamine hydrochloride a deep green color is
developed, followed immediately by a dull purple; on boiling,
the color changes to a dull reddish brown, and the odor of quinone
is produced.
(D) To 0.1 g. of sample in 1 cc. of water add 2
cc. of s per cent silver nitrate solution.
group 1 — p-Hydroxyphenylglycine in suspension causes a
black deposit in the cold which, on boiling, instantly becomes
light brown, while the liquid rapidly acquires a purple color.
group 11 — Hydroquinone gives a silky white precipitate in
the cold; the odor of quinone is developed on boiling.
Chlorohydroquinone scarcely reduces silver nitrate in the cold,
but rapidly on boiling.
Catechol slowly reduces the reagent in the cold; no character-
istic color or odor developed in boiling.
Pyrogallol causes instant reduction in the cold, giving a brown
precipitate; no odor produced on boiling.
GROUPS m and ma — Salts of p-aminophenol, p-methylamino-
phenol and 5-amino-2-cresol give purple colorations, with
quinonc-likc odors on boiling.
Sails of p-dimethylaminophenol give no color in the cold; on
boiling, a brownish red color and the odor of quinone are de-
veloped.
2,4-Diaminophenol hydrochloride yields an intense red color;
no odor on boiling.
o-Methylaminophenol sulfate gives a yellowish brown color in
the cold, becoming reddish brown on heating; no odor developed
on boiling.
p-Phenylenediamine hydrochloride yields in the cold a transi-
tory pale green color, followed instantly by a deep purple; no
color change and no odor on boiling.
SPECIFIC TESTS
Two reactions which should be performed with
every developing agent are acetylation and benzoyla-
tion.
In acetylation the substance is mixed with about
three times its weight of acetic anhydride, together,
if the developing agent be a salt of a base, with an
equal weight of anhydrous sodium acetate, and the
mixture gently boiled for a few instants over a flame.
After the mass has cooled, about ten volumes of
water are added and the separated solid filtered off
and recrystallized from alcohol or similar solvent.
In benzoylation (Schotten-Baumann process) the
substance is mixed with about four times its weight
of benzoyl chloride, and an excess of 10 per cent
caustic soda solution added, whereupon the mixture
is vigorously shaken in a stoppered tube, cooling if
necessary, and occasionally releasing any excess
pressure by opening the stopper. Shaking must be
continued until the irritating odor of the benzoyl
chloride has disappeared. Care must be taken that
an excess of alkali is present at the end of the reac-
tion. The separated solid is then filtered off. washed
with water, and recrystallized from acetone or other
suitable solvent.
The derivatives thus produced possess character-
istic melting points, so that any identification can be
definitely established by their aid.
group 1 — p-Hydroxyphenylglycine dissolves readily in dilute
sodium carbonate, sodium hydroxide, sodium sulfite, or am-
monia; also in dilute mineral acids, but not in dilute acetic
acid. When pure it crystallizes in colorless leaflets, melting in-
distinctly with decomposition above 200 °.
group 11 — -The four substances described in this group all
form bright yellow, water-soluble compounds with sulfurous
acid (or sodium bisulfite and dilute acid).
Hydroquinone crystallizes readily from water in colorless
needles melting at 169 °. It boils at 285 °. The vapor is almost
odorless. It is insoluble in benzene. Quinhydrone, precipi-
tated by a cold acid solution of ferric chloride, or of potassium
bichromate, melts at 171 °. Quinone, formed by the action of an
excess of acid bichromate, melts at 116°. The diacetyl deriva-
tive melts at 1230; the dibenzoyl derivative melts at 199°.
Chlorohydroquinone is too soluble in water to crystallize from
aqueous solution. It dissolves readily in warm benzene. It
melts at 1060 and boils at 263°. The vapor has a distinct
phenolic odor. The diacetyl derivative melts at 99 °. Chloro-
quinonc, produced by oxidizing with acid bichromate, melts
at 57 °.
Catechol forms feathery needles which melt at 1040 and boil
at 245 ° and are extremely soluble in water. It is readily solu-
ble in hot benzene, sparingly in cold. It possesses an odor re-
sembling that of pyrogallol. On treatment with bromine in
carbon tetrachloride solution, hydrogen bromide is evolved,
and a tetrabromo derivative melting at 192 ° is produced. The
diacetyl derivative melts at 63°; the dibenzoyl derivative melts
at 84 °.
Pyrogallol is extremely soluble in water. It is slightly solu-
ble in hot benzene, almost insoluble in cold. It melts at ijjB
and boils at 293°. It possesses a peculiar and characteristic
odor. Its aqueous solution gives a blue precipitate with ferrous
Nov., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
893
sulfate. The triacetyl derivative melts at 161 °; the tribenzoyl
derivative melts at 89 °.
groups in and ma. p-Aminophenol and Its Salts — The free
base crystallizes from water in leaflets, melting with decomposi-
tion at 184 °, -soluble in about 100 parts of cold water. It is
moderately soluble in hot alcohol, sparingly in ether. The
hydrochloride crystallizes in prisms, and is sparingly soluble in
concentrated hydrochloric acid. The sulfate, crystallizing in
fine needles, is less soluble in cold water than the hydrochloride,
but the hydrochloride is precipitated from an aqueous solution
of the sulfate on adding concentrated hydrochloric acid. On '
adding to a cold, slightly acid solution an excess of sodium
acetate and then a few drops of benzaldehyde, the pale yellow
benzylidene derivative is soon precipitated, which crystallizes
from methyl alcohol in needles melting at 183 °. The diacetyl
derivative melts at 1500; the dibenzoyl derivative melts at 234 °.
S-Amino-2-cresol and its salts resemble £>-aminophenol and
its corresponding salts very closely in solubility and chemical
behavior. The free base crystallizes from water in flat needles
melting with decomposition at 176°. The hydrochloride crys-
tallizes either in needles, or, less frequently, in leaflets. The
sulfate crystallizes in fine needles. On oxidation with acid
bichromate it yields toluquinone melting at 68 °. The benzyli-
dene derivative is markedly less soluble than benzyliden;-^-
aminophenol in methyl alcohol, from which it crystallizes in
leaflets melting at 208 °. The diacetyl derivative melts at 103°;
on gentle hydrolysis with alkali it yields the monoacetyl deriva-
tive melting at 179°. The dibenzoyl derivative melts at 1940.
2, 4-Diamino phenol is met with only as the hydrochloride.
The free base is not precipitated from solution on addition of
sodium carbonate; the neutralized solution darkens very rapidly
in air. The hydrochloride is sparingly soluble in concentrated
hydrochloric acid. Attempts to prepare a benzylidene de-
rivative led to a smeary yellow product. The triacetyl de-
rivative melts at 1800; the tribenzoyl derivative melts at 231 °.
p-Methylaminophenol is met with only as the sulfate, which
crystallizes in fine needles. The free base is fairly readily solu-
ble in cold water, but is precipitated on neutralizing a cold
saturated solution of the sulfate with sodium carbonate; it
melts at 85 ° and is extremely soluble in ether. On allowing a
solution in an excess of sodium hydroxide to stand in air, a dark
color rapidly develops, accompanied by a characteristic odor
not unlike that of a trace of pyridine. On adding sodium ni-
trite solution in slight excess to a solution acidified with sul-
furic acid, the sparingly soluble nitroso derivative separates in
colorless needles melting at 1360. The perfectly pure mono-
methyl compound yields no benzylidene derivative on treat-
ment with sodium acetate and benzaldehyde, but technical
samples are rarely entirely free from salts of p-aminophenol,
which is converted by benzaldehyde into the insoluble benzyli-
dene £-aminophenol. A good technical sample should be com-
pletely soluble in three parts of concentrated hydrochloric
acid. The diacetyl derivative is insoluble in cold water and
melts at 97 ° ; on gentle hydrolysis by warming with dilute alkali
this is converted in the monoacetyl compound (soluble in alkali
and precipitated by acid) which melts at 2400. The dibenzoyl
derivative melts at 173°.
p-Dimethylaminophenol — The sulfate crystallizes in hexagonal
tablets which are extremely soluble in water. The oxalate is
moderately soluble in water and alcohol; it melts at 187° to
191 °. The free base is fairly readily soluble in cold water; it
melts at 75° and is extremely soluble in ether. On allowing a
solution in sodium hydroxide to stand in air, the same dark
color and pyridine-like odor are developed as with the mono-
methyl compound. On adding sodium nitrite to a solution in
dilute acid, a reddish brown coloration is formed, with evolu-
tion of gas. On adding a saturated solution of potassium ferro-
cyanide to a fairly concentrated solution in dilute sulfuric acid,
a white crystalline precipitate of the acid ferrocyanide soon
separates. It forms an acetyl derivative melting at 78 °, and a
benzoyl derivative (soluble in dilute acid) which melts at 158 °.
o-Methylaminophenol — The sulfate crystallizes in stout needles
which are extremely soluble in water; the free base, which is
slightly soluble in cold water but readily so in hot water, crys-
tallizes in leaflets melting at 96 °. It dissolves in alkali, forming
a solution which slowly darkens to a dull green color on standing
in air, giving a pyridine-like odor, but more slowly than the para
compound. The free base and its sulfate are completely solu-
ble in three parts of concentrated hydrochloric acid. On add-
ing sodium nitrite to a solution in dilute acid, the nitrous com-
pound is precipitated in colorless leaflets which melt with de-
composition about 1 300 after darkening from 1200 onwards
(the melting point is rather indistinct and depends upon the
rapidity with which the bath is heated). The derivative ob-
tained on acetylation is a liquid which dissolves in cold water;
on gentle hydrolysis by warming with dilute alkali it yields the
monoacetyl compound (soluble in alkali and precipitated by
acid) which melts at 1500. The dibenzoyl derivative melts
at 113°.
p-Phenylenediamine — The hydrochloride crystallizes in leaflets
which are readily soluble in water. The free base, melting at
140°, is moderately soluble in cold water and sparingly in ether.
On adding to a cold dilute solution an excess of sodium acetate
and then a few drops of benzaldehyde, the pale yellow dibenzyli-
dene derivative is precipitated; this crystallizes from methyl
alcohol, in which it forms a bright yellow solution, in thin leaflets,
melting at 138 ". Both the diacetyl and dibenzoyl derivatives
melt at temperatures too high for convenient measurement.
QUANTITATIVE METHODS
It frequently happens that photographic developers
placed upon the market consist of mixtures of develop-
ing agents or of impure simple substances, so that it
may be necessary to separate and estimate the con-
stituents of a mixture or to determine the purity of a
sample of a single substance.
group 1 — No direct method for determining the purity of a
sample of £-hydroxyphenylglycine is available. An ash de-
termination should be made, and the amount of matter insolu-
ble in dilute sodium carbonate estimated. If a sulfite be present
the sulfurous acid liberated by mineral acid should be deter-
mined by the method indicated below.
group II — -All the substances in this group should leave no
ash on ignition; if there be any, it should be estimated. Like-
wise, all should dissolve in water and, in ether without residue,
and should leave no considerable residue when the main con-
stituent is volatilized under atmospheric or reduced pressure.
The melting point forms a fairly satisfactory criterion of the
purity when the sample is found to be completely soluble in
ether.
The proportion of hydroquinone in a sample of chlorohydro-
quinone may be estimated by isolating and weighing the matter
insoluble in wurm benzene.
groups in and iim — Water-insoluble material and ash should
be estimated; in Group III the amount of matter insoluble in
alcohol should also be determined. The proportion of chloride,
sulfate, sulfite, etc., should be determined; and in certain cases
it may be well to estimate the total nitrogen by the Kjeldahl
method, making certain, of course, thai free ammonium salts
are absent
It is important in all cases to determine the amount
of salts of />-aminophenol or aminocresol present, both
in samples consisting principally of one of these com-
pounds and in samples of methylated derivatives.
The procedure is as follows:
THE JOURNAL Of INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. u
Ten grams of the sample are dissolved in about 150
cc. of cold water (or, in the case of the free base, dilute
hydrochloric acid). Heating must be avoided, since
this may cause impurities to enter into solution which
do not again separate on cooling. A slight excess of
sodium acetate is then added, and to the cold solu-
tion about 10 cc. of benzaldehyde are run in. When
the sample contains a relatively small proportion
of aminophenol, as in samples of />-methylamino-
phenol sulfate, the amount of benzaldehyde should
be considerably reduced. After standing over night
the mixture, which should still contain excess of
benzaldehyde, is filtered by suction, the solid well
washed with water, dried in the steam oven, and
weighed. A Gooch crucible answers satisfactorily.
The following factors are applied for expressing
the result:
As />-amioopbenol hydrochloride 0 . 738
As <>-aminophenol sulfate 0.802
As />-aminophenol base 0 . 554
As 5-amino-2-cresol hydrochloride 0.756
As .5-amino-2-cresol sulfate 0.815
As 5-amino-2-cresol base 0.584
For the remaining substances in this group the
simple though non-specific total nitrogen content
must be determined and the assumption made that
all the nitrogen is in the form of the pure substance.
inorganic radicles — When an ash has been found
and shown to consist of a salt of an alkali metal, a
weighed sample of the substance should be ignited
in a platinum crucible and the residue repeatedly
evaporated to dryness and heated to redness after
adding a few drops of 20 per cent sulfuric acid; in
this way the metal is completely converted into the
sulfate.
Chlorides and bromides should be determined by
the Volhard method. Direct estimation of alkali
carbonate is difficult or even impossible in some in-
stances, and may have to be effected by difference.
Sulfites are best estimated by distilling an acidified
solution of the sample into alkali and titrating the
distillate against standard iodine solution, running
the sulfite into the iodine. A regular Kjeldahl dis-
tillation apparatus answers well for the purpose.
TYPICAL ANALYSES
For obvious reasons the sources of the material
used for these typical analyses are not indicated;
"they represent a selection from a very large number
performed in the years 1916-101 8.
"mq" developer tube (april 1916) — The total
weight of material in the compartment containing
the developing agent was 0.6276 g. This was placed
on a filter and well washed with ether; the ethereal
solution, on evaporation, left pure hydroquinone;
the insoluble residue, when dried at 100°, weighed
o. 1 241 g. and was found to consist of pure />-methyl-
aminophenol sulfate. The hydroquinone was not
weighed, but estimated by difference.
"mq" developer tube (april 1916) — A similar
analysis on another tube showed total weight 0.5713
g.; ether-soluble material consisted of pure hydro-
quinone; ether-insoluble material weighed 0.1120 g.
and consisted of technically pure ^-aminophenol
hydrochloride.
developing agent (march 1916) — The material
was a light brown powder of rather moist appearance.
It contained no substance soluble in ether, but dis-
solved partially in alcohol, the alcoholic extract de-
positing /i-aminophenol hydrochloride o'n evapora-
tion. 2.000 g. were boiled with alcohol and filtered
on a weighed Gooch crucible. The insoluble residue
was well washed with hot alcohol and dried to con-
stant weight in vacuo over sulfuric acid. It weighed
0.728 g. and consisted of pure starch. The filtrate
was evaporated to dryness and the residue dried at
115°; it weighed 0.998 g. Another 2.000 g. sample
were heated in the oven at n 5 ° to constant weight;
it lost 0.308 g.
The material thus consisted of
Per cent
^-Aminophenol hydrochloride 49.9
Starch 36.4
Moisture 15.4
101.7
"jietol" (april 19 18) — This consisted of tech-
nical /"-aminophenol hydrochloride, without a trace
of methylated product.
"metol" (april 1918)- — The label claimed the
contents to be "Hydrochloride of methyl-/>-amino-
»»-cresol guaranteed 96.3 per cent pure." The ma-
terial consisted entirely of 5-amino-2-cresol hydro-
chloride, without a trace of methylated product.
"metol substitute" (april 1916) — The material
was first extracted with ether, and the filtrate found
to contain only pure hydroquinone. 2.7654 g. gave
0.5122 g. of hydroquinone, or 18.5 per cent. The
residue showed the presence of sulfite and sulfate as
the only acid radicles; on ignition, a residue consisting
of sodium salts was left. />-Methylaminophenol was
found by the usual methods, and the behavior of the
material led to the suspicion that cane sugar was
present. This was confirmed by boiling with strong
hydrochloric acid, when the characteristic brown color
and odor of caramel were developed. Further ex-
amination failed to show the presence of other sub-
stances.
The portion insoluble in ether was dissolved in
water and diluted to 50 cc. ; this solution in a 20 cm.
tube gave a rotation of 2.900, using mercury green
light, corresponding to 0.932 g. cane sugar in the
sample, or 33.7 per cent.
Another portion of the original sample was ignited
in a platinum crucible and the residue converted into
sodium sulfate; 1.3604 g. gave 0.5319 g. of sodium
sulfate, corresponding to 34.7 per cent of sodium
sulfite. (The sulfurous acid content was not deter-
mined as a check.)
For estimating the />-methylaminophenol sulfate, a
portion was digested with sulfuric acid and the nitro-
gen determined by the Kjeldahl process; 1.4SS0 g.
required 8.6 cc. of N/10 acid, corresponding to o. 14S g.
/>-methylaminophenol sulfate, or 10 per cent.
The material thus contained:
Per cent
Hydroquinone 18.5
Cane sugar 33.7
Sodium sulfite 34.7
f-Methylaminophenol sulfate '0.0
96.9
Nov., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
895
"metol substitute" (june 1016) — The material
on treatment with ether yielded a soluble constituent
which was identified as pyrogallol; the residue, which
contained no nitrogenous matter, consisted entirely
of sodium sulfite; the ethereal extract from 5.1215 g.
gave, on evaporation, 1.3050 g. of pyrogallol or 25.5
per cent; the residue was acidified and the sulfurous
acid distilled into alkali, which was then diluted to
200 cc. Of this solution 15.9 cc. were required by
60 cc. of standard iodine solution, equivalent to 50.0
g. sodium sulfite per liter, corresponding to a total
of 3-773 g- sodium sulfite, or 73.8 per cent. An-
other sample was ignited with sulfuric acid: 1.2730 g.
gave 1.0455 g. sodium sulfate, corresponding to
0.9280 g. sodium sulfite or 72.9 per cent.
The material thus consisted of:
Per cent
Pyrogallol 25.5
Sodium sulfite 73 . 4
Iodine estimation: 0.8996 g. gave 0.0613 g- Agl.
Expressed as potassium iodide, 0.0487 g., or 5.4
per cent.
Sulfite estimation: 1.2140 g. required 36.0 cc. of
standard iodine solution (1 liter corresponding to
50.0 g. of anhydrous sodium sulfite) corresponding
to o. 179 g. or 14. 7 per cent sodium sulfite.
Alkali metals: o. 2135 g. gave 0.0512 g. mixed sodium
and potassium sulfates. This corresponds to 5.4
per cent potassium iodide plus 14.7 per cent sodium
sulfite plus 3.7 per cent sodium carbonate.
Nitrogen estimation (Kjeldahl): 0.6030 g. required
11. 5 cc. of N/10 acid, corresponding to 0.198 g., or
32.8 per cent of p-methylaminophenol sulfate.
Composition:
Hydroquinone
f>-MethylaminophenoI sulfate.
Sodium sulfite
Potassium iodide
Sodium carbonate
Per cent
52
0
32
fl
14
7
5
4
3
7
developing agent (july 1916) — Ether dissolved
out a small amount of dark smeary material, which
was not further investigated. The residue, on further
examination, was found to consist of impure ^-amino-
phenol hydrochloride mixed with lead chloride and a
small amount of lead sulfate. The lead was deter-
mined by ignition with sulfuric acid: 1.7130 g. gave
1. 1270 g. of lead sulfate, or 0.429 equivalent of lead
per 100 g. of sample. In another sample chlorine
and nitrogen were determined by collecting in alkali
the gases evolved on heating with sulfuric acid in
the Kjeldahl process: 1.6070 g. were heated with 25
cc. of sulfuric acid, the gases evolved during the early
stages of digestion being absorbed in 25 cc. of 10 per
cent alkali. This was diluted to 100 cc. 10 cc. of
the solution required 22.6 cc. of N/20 silver nitrate
after deducting the blank test, corresponding to
0.710 equivalent of chlorine per 100 g. of sample.
The ammonia required 46.4 cc. of N/10 acid, corre-
sponding to 0.289 equivalent per 100 g. of sample.
Deducting, this leaves 0.421 equivalent of chlorine
combined as lead chloride; again deducting, there re-
mains 0.008 equivalent of lead sulfate.
Composition of 100 g. of sample:
Per cent
Impure />-aminophenol hydrochloride 0. 289 equivalent or 42.1
Lead chloride 0.421 equivalent or 58.5
Lead sulfate 0 . 008 equivalent or 1.2
101.8
The above analysis is of course accurate only to
about i or 2 per cent, especially in the figure for
^-aminophenol since all nitrogenous matter has been
calculated as />-aminophenol hydrochloride.
developing agent (September 1916) — This ma-
terial was stated by its label to be "Identical to Metol."
On treatment with ether a considerable quantity en-
tered into solution; the ethereal extract, on evapora-
tion, left hydroquinone: 1.2140 g. gave 0.6300 g.
or 52.0 per cent of hydroquinone. The insoluble
portion was found to contain sulfite, sulfate, car-
bonate, iodide, sodium, potassium, and a salt of
p-methylaminophcnol.
metol substitute (june 1918) — The material
was extracted with ether, which, on evaporation, left
no residue. Methyl alcohol dissolved a considerable
proportion; the filtrate, on evaporation, left a residue
consisting of pure ammonium />-toluenesulfonate,
which was identified by the preparation of the corre-
sponding sulfonic chloride and sulfonamide, both of
which had the correct melting points. Further ex-
amination showed the presence of a salt of ^-methyl-
aminophenol and a small amount of some sodium
salt. Sulfate was found to be present.
As ammonium ^-toluene sulfonate has no developing
action, the principal interest lay in the proportion of
/>-methylaminophenol present. A weighed quantity
was accordingly dissolved in water and heated to
boiling. To the boiling solution an excess of sodium
carbonate solution containing a small amount of
sodium sulfite was added, and the mixture boiled until
every trace of ammonia was expelled. The residue
was then immediately acidified with dilute sulfuric
acid, and the nitrogen determined by the Kjeldahl
method: o. 1200 g. required 8.5 cc. of N/10 acid corre-
sponding to 0.146 g., or 12.0 per cent of methyl-
aminophenol sulfate. The material thus contained
12.0 per cent />-methylaminophenol sulfate, the re-
mainder consisting of ammonium ^-toluenesulfonate
together with a small proportion of sodium salts.
adulterants — These are of such diverse nature
that it is impossible to suggest any general lines of
examination. Among the adulterants and useless
substitutes the following have been encountered:
Starch
Cane BtJ
Citric acid
Sodium formate
Potassium oxalate
Koch.ll.
Potassium bromide Sodium carbonate
Potassium iodide Ammonium chloride
Potassium nitrate Ammonium sulfate
Sodium chloride Calcium sulfate
Sodium sulfate Magnesium sulfate
m sulfite Lend chloride
Potassium ferrocyanidc Sodium bisulfite
Iioracic acid Sodium sulfide
Borax Sodium hydrosjda
Rkskakcii Laboratory
Eastman Kodak Company
RoCIIHHTHH, N. V.
Lead sulfate
8o6
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. n
A SUMMARY OF THE LITERATURE ON THE SOLUBILITY
OF SYSTEMS RELATED TO NITER CAKE1
By H. W. Foots
Received July 24. 1918
In a recent article1 Johnston has pointed out that
"the best mode of using a solution of niter cake for any
particular purpose could be ascertained from the ap-
propriate solubility data." He has called attention, in
particular, to the importance of such data for the
three-component system Xa2S04-H2S04-H20, and of
four-component systems like Xa2S04-FcSO.r-H2S04-
H20. No system of the latter type has been investi-
gated. There are 4 three-component systems which
lead up to it of which only the following three have
any importance:
(1) Na2S04-H2S04-H20
(2) Na2S04-RS04-H20
(3) RS04-H2S04-H20
Another system which may prove to be of some im-
portance in connection with the utilization of niter cake
is that consisting of Na2S04-(NH4)2S04rH20.
I propose to review briefly the literature relating to
the solubility of these systems, omitting older data
obtained before the solubility relations in three-com-
ponent systems were well understood. In some of
the very recent publications, I have not been able to
consult the original articles and in these cases the
reference to Chemical Abstracts has been added.
Na2S04-H2S04-H20
This system has been investigated by D'Ans3 and
very recently by Pascal.4 A few data are also given
by Herz.6 The results obtained by D'Ans were chiefly
at 25°. The writer has recently repeated a number
of his determinations and in general obtained excellent
agreement. Pascal investigated the system under a
wide range of temperature but only a summary of his
results, expressed in a diagram without numerical data,
has been published up to the present. The diagram
is inaccurate in at least one respect, as it represents the
solubility of the salt Xa;S04. ioH20 far above its
transition temperature, where it can no longer exist.
The results at 25 ° taken from his diagram do not agree
closely with those of D'An
This system is not as simple as it might appear, for
besides the decahydrate and the anhydrous salt, a
series of four acid sulfates was found by D'Ans, each
salt existing in contact with solutions of varying acid
concentration between limits set by the formation of
other solid phases. A transition temperature exists
at 16.67°, at which temperature the three solid phases
Na2S04.hoH20, NasS04, and Xa3H(S04)2. H20 exist in
equilibrium with solution and vapor. Below this tem-
perature, the anhydrous salt cannot exist in stable
equilibrium with acid solutions, and with increasing
acidity the decahydrate is followed directly by an acid
salt.
1 Published at the request of the Division of Chemistry nnd Chem-
ical Technology of the National Research Council.
' Tuts Journal, 10 (1918), 468.
I Ber., 39 (1906), 1534; Z. anorg. Chtm., 49 (1906). 356; 61 (1909), 91.
< Comfit, rend., 164 (1917), 628.
• Z. anorg. Chem.. 73 (1912). 274.
The solubility results in this system are important
on account of the possibility of separating niter cake
into its components by direct crystallization or leach-
ing. This possibility is considered in detail by Saxton
in the following article and no further mention is
necessary here.
Xa2S04-RS04-H20
The first system of this type to be thoroughly in-
vestigated was that with magnesium sulfate.1 Later,
similar systems were investigated by KoppelJ for
R = Cu, Fe", Co, Ni, Zn, Cd. Mn. Very recently,
Schreinemaker and Prooye3 have again investigated
the system containing manganese as the bivalent metal,
Massink4 that containing copper, and LeChatelier and
Bogitch5 that with ferrous iron. Cameron and Sei-
dell9 have determined the solubility at 25° of calcium
sulfate in solutions of sodium sulfate and in connec-
tion with the formation of salt deposits, van't HofP
and others have investigated the same system. It is
evident, therefore, that systems of this type have been
investigated thoroughly. In many cases, the data are
given for a considerable range of temperature. Ex-
cepting calcium sulfate, all the systems form double
salts of the 1:1 type with either 2 or 4 molecules of
water. Unlike most double salts, they are formed
from the single salts by raising the temperature. The
transition temperatures, at which the two single salts,
double salt, solution, and vapor are in equilibrium,
were determined in all systems investigated by Koppel.
They all fall between the limits 8.7° and 22°. Below
the transition temperature only the single salts crys-
tallize. Beginning at temperatures slightly above the
transition points, the double salts can be recrystallized
from water without decomposition.
RS04-H2S04-H20
The following systems of this type have been in-
vestigated, usually at 25°: R = Fe',8 R = Cu,»
R = Ba,10 R = Ca,11 R = Be.12 Very incomplete data
for R = Zn are given by Hoffman13 who describes an
acid sulfate.
For copper and ferrous sulfates, and probably for
all similar sulfates, the type of solubility with increas-
ing concentration of sulfuric acid, is similar, the con-
centration of the sulfate decreasing with increasing
acidity. Ferrous sulfate and zinc sulfate form acid
salts from strongly acid solutions, while copper sulfate
does not, giving ultimately the anhydrous sulfate.
' Van't Hoff and van Deventer, Z. fihysik. Chem.. 1 (1887), 170; Roose-
boom, Ibid., 2 (1888). 513.
'Ibid., 42 (1902), 1; 52. (1905), 385.
« Proc. Akad. Welenschofifien, 16, 1326; Chem. Abs., 8, 1068.
■ Z. fihysik. Chem., 92 (1917), 351; Chem. Abs., 11, 3184.
« Rev. UetaU., 12 (1915). 949; Chem. Abs., 10, 2460.
• J. Phys. Chem., 6 (190H. 649.
' A summary of this work is found in Z. anorg. Chem.. 47 (1905). 244.
• Kenwick. J. Phys. Chim.. 12 (1908). 693; Wirth, Z. anorg. Chem., T»
(1913), 360. Data are also given for ferric and aluminum sulfates.
Florentin. Bull. Soc. Chim., IS (1913). 362.
» Bell and Taber. J. Phys. Chem., 12 (1908). 171; Foote, J. Am. Chtm.
Soc, 37 (1915), 288.
» Volkhonskii, J. Russ. Phys.-Ckem. Soc, 41, 1763; Chtm. Abs., •
(1911), 617.
» Cameron and Breazeale. J. Phys. Chem.. 7 (1903). 571.
» Wirth, Z. anorg. Chem., 79 (1913). 357.
» Z. angn: Chem.. 23 (1910), 1672.
No/., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
897
Barium sulfate becomes more soluble in strong sul-
furic acid, as is well known, and an acid sulfate forms
from strongly acid solutions.
Na2S04-(NH4)2S04-H20
This system has recently been well investigated by
Matignon and Meyer1 through a considerable range of
temperature. The work is of importance at present
because of the possibility of using niter cake to absorb
ammonia and produce ammonium sulfate. The at-
tempts which have been made to do this have been
summarized by Johnston.2 They appear not to have
been very successful thus far and the results obtained
have been irregular. With the data which have now
been published, it is possible to calculate exactly what
can be done in this direction.
A double salt, Na2S04. (NH4)2S04. 2H20, forms, with
a transition temperature at 59°. Above this temper-
ature, only the single salts are deposited from solution.
Na2S04-RS04-H2S04-H20
No four-component system of this type has been
thoroughly investigated. D'Ans has given a few data
for solutions containing calcium sulfate. An investi-
gation is in progress in this laboratory on such a
system containing copper sulfate. It is to be hoped
that investigators elsewhere may work out the data
for other sulfates. The problem is an interesting one
from a scientific standpoint as well as pointing out
possible uses for niter cake.
Sheffield Chemical Laboratory
Yale University
New Haven, Connecticut
THE RECRYSTALLIZATION OF NITER CAKE3
By Blair Saxton
Received July 24, 1918
In this paper the solubility data of D'Ans* for 25 °
and of Pascal2 for o° will be used to calculate in some
detail the extent of the separation of niter cake into
its constituents which can be effected by leaching or
crystallizing at these temperatures. The data of D'Ans
are very good. Unfortunately Pascal has expressed
his results in a triangular diagram only and data scaled
from this are not reliable. Calculations have been
made for 0°, however, and they are valuable in show-
ing that the separation can be made more efficiently
at that temperature than at 25°. Solubility deter-
minations for temperatures lower than 25 ° are in
progress in this laboratory and then the possibilities
at these temperatures will be considered. Calcula-
tions somewhat similar to these which follow have
recently been made by Hildebrand5 and Blasdale.'
CRYSTALLIZATION AT 25°
At this temperature we may crystallize the following
solids: Na2S04.ioH20, Na2S04, Na3H(S04)2. H20,
Na,H(S04)2, NaHS04.H20, NaHS04, NaH,(SO«),.-
■ Compt. rend., 165 (1917), 787; 166 (1918J, 115.
3 Loc. cil.
' Published at the request of the Division of Chemistry and Chem-
ical Technology of the National Research Council,
* Loc. cit., preceding article.
■ This Journal, 10 (1918), 96.
•Ibid., 10 (1918), 347.
i.5H20, and NaH3(SOj)2. Of these we may discard
the last three, since their removal from solution takes
out too much sulfuric acid. Further, Na3H(S04)2. H20
need not be considered since it rarely forms. The data
of D'Ans, expressed in per cent of solution by weight,
are given in Table I together with the composition of
each solid phase considered.
Table I
Solubility at 25°
-Solution — .
NajSO.
21.90
32.07
Solid Phases HiSO.
NaiSO.JOHiO 0.00
NajSOt. 1 0H:O .^_>. Na2SO< 8.67
NajS04^I^.Na3H(SO.)a 16.34
Na)H(SO1)!^Z^lNaHS04.H20.... 30.60
NaHSOi.Hs0^j^.NaHS04 56.49
Composition of Salts
NaiSClOHiO 0.00
NaiH(SO.)s 18. 70
NaHSOi.HsO 35.50
NaHSO. 40.83
34.64
30.05(a>
6.68
44.10
81.30
51.46
59. 17
HjO
78.10
59.26
49.02
39.35
36.83
55.90
0.00
13.04
0.00
(a) Determined by H. W. Foote. D'Ans gives 26.30.
These solubility data are also plotted in the figure.
Straight lines have been drawn between the points
representing the univariant systems and the calcula-
tions are based on this approximation. Here also are
shown lines radiating from the origin representing the
composition of niter cakes of 20, 25, 30, and 35 per
cent sulfuric acid, also similar lines for the two acid
H2bQa in t>olu
sulfates, Na3H(S04)2 and NaHS04.H20. The inter-
section of one of these lines with the solubility curve
gives the composition of solution which will first be-
come saturated with the solid phase represented by
that branch of the curve intersected. This of course
tells what solid will form first on crystallizing at 250.
For instance, it shows that a niter cake which is 25
per cent sulfuric acid is never saturated with the
decahydrate; hence it never forms on crystallizing.1
Considering the lines of the diagram as straight and
letting a: and y represent the concentrations of sodium
sulfate and sulfuric acid, respectively, in saturated solu-
tion, il [uations for these lines become as follows:
AB, x = 21 . 90 + 1 . 173 y
• = 29.17 + 0.335 y
CD, j = 39.90 — 0.322 y
DE, x = 57. 67 — o. 903 y
1 The point of saturation can also be calculated by solving two simul-
taneous equations: one, the equation for a branch of the solubility curve;
the other, the equation for the line showing the composition of the niter
cake or solute. The line AH in the diagram is represented by the equation
x — 21.90 + 1.173 y. A 20 per cent acid niter cake is represented by the
equation x - 4 y. On solving these we obtain x - 7.75 and y - 31.00.
TUE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No, n
Given these equations and the composition of the sol-
ute before crystallization, it is possible to calculate the
weight of the solid separating and the composition of
the residual solution. For instance, let us consider
the solid crystallizing to be Na2SOj. If we represent
the weights of sodium sulfate and sulfuric acid in
solution before crystallization as n and s, respectively,
and the amount of Na2S04 separating from solution
as z, then at any point along BC the following relation
must exist:
w — 2 _ x = 29.17 + 0-335?
s y y
and, solving for z, z = n — s (0.335 + )>
or if we are dealing with a niter cake whose weight is
c and which is 5 per cent sulfuric acid, this becomes:
= 87.3
(•■
0133S +
2 q i 7 \
y 1
If the solid separating is Na3H(S04)2, the value of 2
is calculated by means of a similar equation, i.e., ~
n — 0.8132 _ 39. 90 — 0.322 y
s — o. 187 2 y
Hence we are able to calculate how much of any solid
will separate if we know the composition of the niter
cake or the solution from it, and the per cent of sulfate
acid in solution after crystallization.
Further, we can calculate the weight of water. in
the solution after crystallizing, or, which amounts to
the same thing, the amount of water to be added to
the solid niter cake in leaching at 25° in order to leave
2 grams of one of the solid phases. If we are evapo-
rating the solution instead of leaching the solid, this
weight of water added to c, the weight of the cake,
will give the weight to which the solution must be
evaporated, except when the solid separating is a
hydrate, in which case the total weight is the sum of
the weight of the solution — sodium sulfate, acid,
water, and z. The extent to which the evaporation
must be carried can also be very easily controlled by
testing the acid concentration of the solution. Again
considering the solid separating to be Na2SOi, w, the
weight of water may be calculated as follows:
w _ 100 ■ (.v + y) 70. 8j 1 .335 y
s y v
-(
7Q- 83
335).
or if < is t]i< cake or solute and 5
-l concentration.
(0.70&3
\ v
0.01335
Similarly, general calculations can be made for each
of the other solid phases. The results for those phases
which are here considered are assembled in Table II.
The equations are much simplified for any given
value of j. For instance, if we take a solution of 100
g. of a 35 per cent acid niter cake which deposits
t,H(S04)i first on crystallizing at 25°, we
35 and c = 100,
(35.0 — 0.1872) (
.678)
744.8
0.8732 y — 7-461
'60. 10
y
If we know the value of both * and y for the solu-
tion in equilibrium with a given solid, we may avoid
using these general equations. Again, starting with
1 00 g. of 3 5 per cent acid niter cake, we may calculate the
maximum amount of Na3H(SC>4)2 that can separate by
using the data for the point D in the diagram. This-
gives us
65.00 — 0.8132 30.05
= --= 0.982,
35.00 — 0.1872 30.00
from which 2 becomes 48.66. Then the weight of
sulfuric acid left in solution, 35.00 — o. 187 2, becomes
25.90. This is the type of calculation which has been
used mostly in this paper, since it tells us the most we
can do in separating any one solid phase. Hence in
speaking of crystallizing Na2SC>4.ioH20, Na»SO«,
Na,H(S04)2, or NaHS04.H20, we refer to crystallizing
each to the points B, C, D, and E, respectively. If,
however, a specific use of niter-cake solution requires
a certain acid concentration, one can tell from the
figure what will first crystallize, and calculate how
much will separate, and how much sodium sulfate and
sulfuric acid will be left in solution by using the general
equations.
In separating niter cake into its constituents either
by leaching or crystallizing at 25° we have the follow-
ing possible processes which may be used separately
or combined:
(A) Remove Na2SC>4.ioH20 from solution. This
may be done by evaporating the solution to a calcu-
lated weight, or just to an acid content of 8.67 per
cent, or by leaching completely with the calculated
amount of water. The solute (sodium sulfate + sul-
furic acid) will then be 21.28 per cent acid. Of the
niter cakes here considered only the one which is 20
per cent acid can deposit this salt at 25 °.
(B) Remove Na2S04 from solution. This can be
done exactly as A. The acid content of the solution
at crystallization, however, will be 16.34 per cent.
The solute will be 32.05 per cent sulfuric acid.
(C) Remove Na3H(S04)2 from solution by processes
similar to A and B. The concentration of sulfuric acid
in the final solution should be 30.60 per cent, and in
the solute, 50.45 per cent.
(D) Recrystallize the Na»H(SO0i from C by first
removing Na2SC>4 by process B and then crystallizing
Na3H(S04)2 from the filtrate. 100 g. Na3H(SC>4)j
when thus treated will give 41.66 g. Xa2S04 by evap-
orating to 156. 1 g. or leaching with 56.1 g. of water.
The filtrate will then deposit 33.81 g. Na3H(.SC>4)i
when evaporated to 74.2 g. The solution will then
contain 12.15 S- of sodium sulfate and 12.3S g. of
acid. The end result in concentration is the same as
C, but 12.38 g. of sulfuric acid have been recovered in
solution which otherwise would be in solid NajH(SC>4)j.
The result of recrystallizing any amount of Xa3H(SC>4)t
in this way can be calculated from these data.
Nov., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
899
Table II
Solid Phase Expression for s
Na-SO. c — cs (o.01335 + °i£L7\
Na,H(SO,). c ( 1.145 — 0.007765s + 8 S44 ~
\ 0.8732 y
19 90s — (0.322 s + n)y
7.461 — 0 8732 y
NaHSC.HsO e f 1.197 — 0.001165s 4- 245' ~ ° 6'
V 0 8351y
SPRESSION
1.7083
0
57.67 s— (0.903 s + n)y
c = the weight of niter cake or solute.
s = the per cent of sulfuric acid in the niter cake or solute.
3 = the weight of solid separating.
20.47 — 0.8351 y
(E) Remove NaHS04.H20 from solution by the
methods given for A, B, and C. In this case the con-
centration of acid in the solute will be 89.43 Per cent
and in the solution, 56.49 per cent. The only advan-
tage in crystallizing this acid sulfate is to raise the
concentration of acid. By doing this, much of the
acid is removed from solution. Some of this could be
recovered by recrystallizing, first separating Na3H(S04)2
and then NaHS04.H20. In order to make a good
recovery of acid, this would involve too many opera-
tions to be practical. NaHS04.H20 is 35.50 per cent
sulfuric acid, 51.46 per cent sodium sulfate, and 13.04
per cent water and corresponds to a 40.83 per cent acid
niter cake. Its saturated solution may contain as
much as 56.49 per cent of acid. Uses may be found
for its solution without further treatment.
Finally these processes may be combined to consid-
erable advantage. In Table III will be found such
combinations as BCD. This means that Na2S04 has
been removed from the solution of a niter cake, then
Na3H(S04)2 has been crystallized from the filtrate, and,
finally, this acid salt has been recrystallized and the
residual solutions, having the same concentration,
have been combined. In making calculations for these
combined processes the writer found it convenient to
work out the results which could be obtained with
100 g. of solute for each case and from that data to
make the calculations desired. After completing pro-
cess B, for example, the solutions will always have the
same composition independent of the composition of
the original niter cake. The same is true for process
C. The data for these two solutions are as follows:
After Na2S04 has been removed from solution, 100
g. of the solute in the filtrate will contain 32.05 g. of
acid and 67.95 g. of sodium sulfate. This filtrate, on
evaporation to 127.27 g., will give 57.96 g. of
Na3H(S04)2 and a solution which contains 20.83 g. of
sodium sulfate and 21.21 g. of sulfuric acid.
After Na3H(S04)2 has been crystallized from solu-
tion, 100 g. of the solute in the filtrate will contain
50.45 g. of acid and 49. 55 g. of sodium sulfate. When
this filtrate is evaporated to 123.5 g. it will deposit
92.21 g. of NaHS04.H20 and leave a solution which
contains 17. 71 g. of acid and 2. 10 g. of sodium sulfate.
In Table III are the results of such treatments as
have been outlined on 100 g. of niter cake of 20, 25,
30, and 35 per cent acid. In column four is given the
= the weight of sodiurr.
= the per cent of sulfui
= the weight of water i
■Or*--)
is __ 0.187 =,(6A1
(«_35.5.)(°-^
(s — 0.355 s) ( *^H _ o.C
sulfate in the niter cake or solute.
c acid in solution after crystallizatii
solution after crystallization.
— 0.000973
weight at final crystallization in any series of processes.
If the combined process is BC the weight for C is
given, the weight for B having previously been given.
If the final process is D, two weights are given, the
first being the weight at which Na2S04 separates, the
latter that at which Na3H(S04)2 is removed in the
recrystallization of Na3H(S04)2.
Table III
H3S0.
H:SC»4 re
HiSOj
HiSUi covered
NaiSO,
Weight
in solu-
in solu-
left in
Number
at final
tion
solute
solid
Per
Treat-
of opera-
crystalli-
Per
Per
Per
Per
cent
ment
tions
zation
cent
cent
cent
cent
20.0
A
1
244.3
8.67
21.28
100.0
7.5
B
1
160.0
16.34
32.05
100.0
47.0
BC
79.4
30.60
50.45
66.2
83.8
BCD
4
56.5, 26.8
30.60
50.45
88.5
78.3
BCDD
6
19.1, 9.1
30.60
50.45
96.1
76.4
C>
1
102.6
30.60
50.45
10.3
97.5
CD
3
149.7, 71.2
30.60
50.45
69.7
82.9
BCE
3
32.4
56.49
89.43
23.2
99.3
BCDDE
7
33.8
56.49
89.43
33.8
99.0
25.0
B
1
175.0
16.34
32.05
100.0
29.3
BC
99.3
30.60
50.45
66.2
78.3
BCD
4
70.6, 33.6
30.60
50.45
88.5
71.0
c>
1
112.9
30.60
50.45
40.0
86.9
CD
3
125.1, 59.5
30.60
50.45
79.7
73.9
ODD
42.3, 20.1
30.60
50.45
93.1
69.5
BCE
3
40.5
56.49
89.43
23.2
99.1
30.0
B
t
190.0
16.34
32.05
100.0
9.1
BC
119.3
30.60
50.45
66.2
72.1
BCD
4
83.7,40.3
30.60
50.45
88.5
62 . 7
C>
1
123.1
30.60
50.45
59.9
74.5
CD
3
100.5, 47.8
10.60
50.45
86.4
63.6
BCE
3
65.1
56.49
89.43
23.2
98.8
35.0
C
1
133.3
30.60
50.45
74.0
60.9
CD
3
76.0, 36.1
30.60
50.45
91.2
48.2
CE
2
63.4
56.49
89.43
26.0
98.3
CDE
4
78.2
56.49
89.43
32.0
98.0
• This can be
done from the original solution by evaporating to the
sight given and allowing to stand at 25°.
All NaiSOUOHjO and Na*SO.
It is evident from these figures that the way to proceed
with a niter cake of less than 25 per cent acid in order
to produce a solute and solution which are 50.45 per
cent and 30.60 per cent acid, respectively, is to remove
Na2S04 and Na3H(S04)2 consecutively from solution,
recrystallize the acid sulfate, and combine the solu-
tions (process BCD). This involves four operations
and leaves 88.5 per cent of the acid in solution and
over 70 per cent of the sodium sulfate in the solid.
The recrystallization of the acid sulfate could be re-
peated, thus recovering 96. 1 per cent of the acid but
it would mean six operations and hence is hardly prac-
tical. If the niter cake is over 25 per cent acid,
Na3H(SO«)2 can be efficiently separated from the
original solution, recrystallized, and the solutions com-
bined. This takes only three operations. If the niter
cake is 25 to 32 per cent acid, the recovery of sulfuric
acid «ill be from 80 to 85 per cent. If the niter cake
is 32 to 50 per cenl acid, 91 a per cenl of the latter
900
THE JOURNAL OF INDUSTRIAL AND ENGINEERING ' HEMISTRY Vol. 10, Xo. u
will be recovered in solution. At 250 no method for
concentrating the acid in solution as far as the point
E in the diagram (a solution of 56.4 per cent, and a
solute of 89.43 per cent acid) is possible without
removing 70 to 80 per cent of the acid. Of course
NaHSO<.H20 can be removed so that the solution
will have any desired concentration represented along
the line DE. Proceeding for short distances along
DE would not sacrifice an unreasonable amount of
acid.
In order to test the practicability of these calcula-
tions, experiments were made on the removal of
Na2S04 and Na3H(SO)2 from solutions of 100 g. of 30
per cent acid niter cake. The solutions were made by
warming 158.7 g. of recrystallized Glauber's salt with
31.6 g. of 95 per cent sulfuric acid in Erlenmeyer flasks.
A small amount of anhydrous sodium sulfate remained
undissolved.
One sample of such a solution, since it weighed 190.3
g., was cooled without further evaporation, corked,
and immersed in a thermostat at 25° for 48 hrs. The
Na2S04 was filtered through a small suction filter and
washed free from mother liquor with the solution
recommended by D'Ans, consisting of 50 cc. of water,
10 cc. of concentrated sulfuric acid, and 75 cc. of
alcohol. After removing the mother liquor, the salt was
washed with alcohol and then with ether. When dry
it weighed 7.0 g., while the amount calculated for
the point C is 6.4 g. A little Na3H(S04)2 no doubt
separated since the solution analyzed 16.42 per cent
sulfuric acid and D'Ans found 16.34 per cent for the
univariant point C.
A second sample of the solution was evaporated to
124 g. and treated in the same way. The calculated
weight of the solution at crystallization is 123. 1 g. but
the last stages of evaporation offered some difficulties
since the solution practically solidified. The acid sul-
fate was washed and dried in the same way as was the
Na2S04. When dry it weighed 68.5 g., while the cal-
culated weight is 64.4 g. Here again the univariant
point was reached, since the solution analyzed 30.61
per cent acid, while D'Ans found 30.60 per cent.
The salt on analysis for sulfuric acid proved to be pure
Na3H(S0.i)2. Considering the roughness of these ex-
ats, both of them can be considered as satis-
.factory checks on the calculations.
RECRYSTALLIZATION AT 0°
The data of Pascal have been scaled from his dia-
gram and are given in Table IV and plotted in the
figure. They are expressed in per cent by weight of
solution.
Table IV
. — Solution .
Solid 1 HiSO. NaiSOi HjO
NaiSO«.10H.<> 0.00 3.68 96.26
NaiSO«.10HiO ~^^_ NuH(SOi)i.... 28.14 23.93 47.86
N«»H(SO«)i ^^ NaHSCHiO 46.81 5.26 47.60
NaHSOi.HiO ^Z^. NaHSOl 61.28 1 84 36.29
These data are inaccurate as has been pointed out,
but they are valuable, as the following calculations
will show. These calculations have not been carried
out in as great detail as those for 25° because of the
data on which they are based.
At o° we have four solids which can reasonably be
separated: Xa2S04. ioH20, Xa3H(S04)2, XaHSO^.HjO,
and XaHSO<. Solutions of niter cake of the range of
compositions considered in this paper will first be
saturated with Glauber's salt at o°. The removal of
this alone is very effective. It will leave all the acid
in solution and the concentration of acid in the solu-
tion and solute will be 28.14 and 54.04 Per cent,
respectively. If Xa3H(S04)} is then crystallized from
the solution, 82.6 per cent of the acid will be recov-
ered, the solution will be 46.81 per cent acid, while
the concentration of acid in the solute will be 89.90
per cent. Recrystallizing the acid sulfate, by remov-
ing Xa2S04.ioH20 and Xa3H(S04)2, successively, from
its solution, and then combining the solutions will not
change the composition of the solution or solute, but
will recover in solution 97.0 per cent of the acid. 100
g. of Xa3H(S04)2 recrystallized in this way at 0° will
give 148.3 g. of Xa2S04.ioH20 when treated with
114. 7 g. of water or its solution evaporated to 214. 7 g.
The solution will then separate 17.43 g- of Xa3H(S04)j
when evaporated to 50.3 g. The final solution will
contain 1 . 73 g. of sodium sulfate and 15.44 g. of
sulfuric acid.
If higher concentration of acid is desired this may
be accomplished by evaporation and removal of
NaHS04.H20. This also can be done efficiently as
can be seen from a glance at Table V. By removing
Glauber's salt, Xa3H(S04)2, and XaHS04.HsO, suc-
cessively, from solution we are able to recover 77.7
per cent of the acid and obtain, as the result of these
three operations, a solute and solution of 97.10 and
61.28 per cent sulfuric acid, respectively. From 98.7
to 99.4 per cent of the sodium sulfate in the cake is
left in the solid. Any further desired concentration
can be effected from this point since there is little
sodium sulfate left in solution and very little if any
of the acid salts can separate and hence little sulfuric
acid can be removed. In other words, the solution
now behaves like a solution of sulfuric acid only.
The results obtained with 100 g. of niter cake of
several compositions are given in Table V. The mean-
ing of the letters in column two is the same as in Table
III.
Table V
H:SO.
niter Weight
cake Number at final
Per Treat- of opera- crystalli-
cent ment tions zation
JO .0 A 1 213.9
AC 2 53.8
ACD 4 40.0. 9.4
ACE 3 27.9
25.0 A 1 210.6
AC 2 67 . 2
ACD 4 50.0. 11.7
ACE 3 34.9
30.0 A 1 207.4
AC 2 80.7
HiSO. re-
H:SO« H1SO1 covered NasSO.
in solu- in in solu- left in
tion solute tion solid
Per Per Per Per
cent cent cent cent
28.14 54.04 100.0 78.7
46.81 89.90 82.6 97.7
46.81 89.90 97.0 97.3
61.28 97.10 77.7 99.4
28.14 54.04 100.0 71.6
46.81 89.90 82.6 97.1
46.81 89.90 97.0 96.4
61.28 97.10 77.7 99.2
28.14 54.04 100.0 63.6
46.81 89.90 82.6 96.0
ACD 4 60.0, 14.0 46.81 89.90 97.0 95.3
ACE 3 41.9 61.28 97.10 77.7 99.0
35.0 A 1 204.2 28.14 54.04 100.0 45.8
AC 2 94.1 46.81 89.90 82.6 95.0
ACD 4 70.0. 16.4 46.81 89.90 97.0 99.1
ACE 3 48.9 61.28 97.10 77.7 98.1
It is evident that crystallization or leaching at o°
is much more effective than at 250 in that greater
concentration and recovery of acid can be effected with
fewer operations at the lower temperature. It is inter-
Nov., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
esting to note in this connection that Wood1 has used
a system of cold water percolation in order to concen-
trate acid in the solution from niter cake, and that
this treatment has been recommended by Prideaux.2
Unfortunately, at the present time the data are not
available for temperatures between the two given. It
may be possible that it is unnecessary to use a tem-
perature as low as o° in order to obtain a satisfactory
separation. Solubility determinations for this system
at 12° are being carried out in this laboratory by Pro-,
fessor Foote, who suggested this paper to the writer.
In the preceding paper reference has been made to
the work of Matignon and Meyer on the solubility
relations in the system Na2S04-(NH4)2S04-H20. The
writer proposes to treat this system as he has treated
the system discussed in the present paper.
SUMMARY
General equations have been developed for the sys-
tem Na2S04-H2S04-H20, at 25 °, by means of which
we can calculate how much of any one solid phase will
separate from a solution if we know the composition
of the original solute and the acid concentration of the
solution after crystallization.
General equations have also been developed for this
system at 25° by means of which we may calculate the
weight of water in the solution after crystallization, or
the weight of water to be added to the solid niter cake
in order to leave a calculated weight of one of the
solid phases.
A very simple type of calculation has been applied
to niter cake of several compositions, by which the max-
imum amount of each solid phase which can be removed
from solution at 25 ° and at 0° has been calculated.
Leaching or crystallizing processes have been sug-
gested by which sulfuric acid may be concentrated in
the solution and sodium sulfate in the solid, at the two
temperatures mentioned.
It was found that this separation can be done much
more efficiently at the lower temperature.
Sheffield Chemical Laboratory
Yale University
New Haven, Connecticut
THE FORMATION OF AROMATIC HYDROCARBONS
, FROM NATURAL GAS CONDENSATE3
By J. G. Davidson
Received May 23, 1918
INTRODUCTION
In several papers which have appeared recently
Zanetti4 has shown that it is possible to produce aro-
' J. Soc. Chem. Ind.. 36 (1917), 1216A.
sIbid., 36 (1917), 1216B.
' This paper is condensed from a dissertation submitted in partial
fulfillment of the requirements for the degree of Doctor of Philosophy in the
Faculty of Pure Science of Columbia University.
The work was begun under the directiou of Dr. J. E. Zanetti and is,
in part, a continuation of his work. After the summer of 1917, when Dr.
Zanetti entered the Chemical Warfare Service, the work was carried on
more or less independently although I am glad to thank Dr. Nelson, Dr.
Freas, and Dr. Fisher for their many invaluable suggestions, and without
whose help the work could not have been finished.
* "The Thermal Decomposition of the Propane-Butane Fraction from
Natural Gas Condensate," This Journal, 8 (1916), 674; "The Thermal
Decomposition of the Hthanc-Propane Fraction from Natural Gas Con-
densate," Ibid., 8 (1916), 777; "Aromatic Hydrocarbons from the Thermal
Decomposition of Natural Gas Condensate," Ibid., 9 (1917), 474.
matic hydrocarbons by the thermal decomposition
of straight-chain hydrocarbons of low molecular
weight.
Previous to this, Bone and Coward1 had passed
ethane, ethylene, and acetylene through porcelain
tubes at various temperatures from 500 ° to 10000 C.
and had noted that the decomposition of ethylene
gave a black, viscous tar. The quantity of tar was too
minute to admit of analysis but they mentioned the
fact that a few crystals of naphthalene were noticed
also. They hold aromatic formation to be produced
by the breaking down of ethylene to acetylene from
which the aromatic hydrocarbons are produced by
polymerization.
Pring and Fairlie2 found that acetylene at high tem-
peratures and in the presence of hydrogen produces
methane for the most part, although some ethane
was formed also. When ethylene and hydrogen were
heated together no acetylene was produced even at
very high temperatures. Methane, however, was
produced in large quantities.
Jones3 studied the formation of aromatic com-
pounds in coal tar and is of the opinion that acetylene
plays an unimportant part in the reaction, inclining
more to the belief that the ring bodies are formed
directly from olefines with the splitting out of hydro-
gen.
Previous work in this laboratory pointed to con-
clusions which were similar to Jones', and in an effort
to get a further insight into the reaction the following
work was undertaken :
It was decided to divide the work into several
parts and investigate each as fully as time allowed,
for it was quite evident from the beginning that any
one of the separate fields was capable of large expan-
sion with possible loss of the original aim.
The divisions of the work are as follows: (1) The
effect of catalyzers on the decomposition of straight-
chain hydrocarbons of low molecular weight. (2)
The influence of temperature and of pressure on the
production of aromatic hydrocarbons. (3) The for-
mulation of the reaction,
Straight-chain hydrocarbons — >•
Aromatic hydrocarbons
EXPERIMENTAL
material — The material used was the ethane-propane
fraction of natural gas condensate, supplied in steel
tanks under high pressure. The tanks are built on
the siphon system, a pipe reaching almost to the
bottom, so the composition of the delivered gas re-
mains almost constant. Analysis of the gas showed
it to be composed almost entirely of the two hydro-
carbons, although some butane, and possibly some
was also present. No other gases were
in the original material, although tests were
or oxygen, carbon dioxide, olefines, and hydro-
gen.
1 "Thermal Decomposition of Hydrocarbons," J. Chcm. Soc, 98
(1908), 1197.
* "Synthesis of Hydrocarbons at High Temperatures," Ibid., 99
(1911), 1796.
' "Aromatic Formation," J. Soc. Chem. Ind., 36 (1917), 3.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. ;o, Noi u
Aspirator G-as
Sampler
Tar InducTion HeaTing A ppa raTus
D rym q
rieTer
appamius — The arrangement of the apparatus
will be understood from Fig. i. The gas was led
through the referee meter, capable of being read to
one-thousandth part of a cubic foot, then through the
calcium chloride towers to the cracking chamber.
The cracking chamber was a silica tube one inch in
diameter about 2 ft. long and could be heated by the
resistance furnace shown. The temperature could
be controlled within a few degrees by the adjustable
rheostat, while its actual value was read by means
of the pyrometer. After the gas had been cracked it
was quickly cooled in the metal condenser and passed
into the precipitator. (At first a small copper plate
and a fine iron wire were kept charged at opposite
sides of the bottle. This did not work satisfactorily
and the inlet tube was then surrounded with wire
gauze as shown in the figure. This worked well for
a time, as the gas had to pass through the charged
wire meshes to escape, and deposition therefore was
easy. After some time the meshes of the gauze be-
came stopped up and required frequent renewal. The
form of precipitator was then changed to that shown
in Fig. 2, which was very satisfactory.) From
the tar precipitator the gas was allowed to escape,
as shown by the light arrow, or by-passed in
the direction of the heavy arrow when a sample was
being collected. This arrangement was necessary to
prevent a change in the rate of flow through the crack-
ing chamber, which was caused when trying to take a
sample direct from the tar precipitator.
After a sample of sufficient volume had collected
in the gas sampler the gas was allowed to pass in the
same direction for a half hour longer in order that
all parts of the apparatus might be in equilibrium.
Failure to do this produced results that could not be
checked. After a half hour had elapsed the stop-
cocks \\. so the gas followed the light arrow
again and the collected sample of gas was forced out
into a gas collecting bottle by way of the dotted arrow.
The apparatus for the analysis of the cracked gas
was a modification of Burrell's gas apparatus.1 Noth-
ing new is claimed for this apparatus except its greater
accessibility and ease of manipulation. It is shown
in Fig. 3. Babb pipettes with an extra stopcock blown
in the bend, as shown, were substituted for the Ost-
wald pipette in Burrell's apparatus. This extra stop-
cock facilitates refilling and cleaning the pipettes
without the necessity of disconnecting from the main
part of the apparatus. Beyond this the form of the
Babb pipette lends itself admirably to rapid and com-
plete absorption.
The slow combustion pipette (B) was made of trans-
parent quartz rather than glass in order to reduce
breakage. When using the ordinary glass pipette
for slow combustions the oxygen would sometimes
catch fire and burn at the point where the capillary
opens out into the pipette. This would always re-
sult in a fracture at that point; furthermore, it was
necessary after a combustion to wait almost 5 min.
before the glass was cool enough to allow the mer-
cury, which always had some drops of water on the
surface, to be raised. After considerable trouble
from both of these causes it was decided to have the
pipette made of silica. The pipette as described gives
the best of satisfaction.
Copper oxide was used to determine the hydrogen.
The copper oxide was also enclosed in a tube of trans-
parent silica, in preference to glass, which will break
if drops of condensed water are drawn into the hot
part of the tube. Use of a silica tube was suggested
for this purpose by Suydam,- but it was found best
1 "New Forms of Gas Analysis Apparatus," This Journal, i (1912),
296.
I "A New Model of the Burrell and Oberfell Apparatus for the Analysis
of LUuminatiog Gas," This Journal. 9 (1917), 972.
Nov., 101S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
9°3
to make the tube hori-
zontal rather than
vertical as he advises.
This position prevents
stoppages, which hap-
pen after a time with
the vertical form.
procedure — The
gas was led through
the cracking chamber
at the rate of 0.5 cu.
ft. per hr., the rate of
flow being frequently
checked with a stop-
watch. The temper-
ature of the silica tube
was rapidly raised to
the desired point and
kept there by adjust-
ing the rheostat.
When the tempera-
ture had become con-
stant and the gas
had passed through
the tube and tar pre-
cipitator for sufficient
time to sweep out all
traces of gas from
a preceding run, a
sample was taken, as
described before, and
the temperature of the
tube raised for the
next determination. While equilibrium was being
reached again the first sample of gas was analyzed.
When catalyzers were used in the form of foil or
gauze, pieces of uniform size were cut, rolled up to
fit the tube snugly, and pushed in so the entire heated
zone was filled with catalyzer. When small pieces of
material had to be used for catalyzer the cracking
tube was packed with loose material, which was held in
place with a plug of copper gauze, preliminary work
having shown that copper has no decided effect as
catalyzer.
gas analysis — All capillary errors and the larger
error due to gas left in the copper oxide tube have been
carefully determined and allowed for in the reports
of analysis. As preliminary work showed no other
gases to be present, unsaturated hydrocarbons, hy-
drogen, and saturated hydrocarbons were the only
ones determined.
Pipettes 1 and 2 (Fig. 3) contained 30 per cent
potassium hydroxide. Pipette 3 contained saturated
bromine water.
The unsaturated hydrocarbons were determined bj
absorption in Pipette ?, one passage of tin
sufficient if the olefine content of tin
17 per cent. When the unsaturated hyd
existed in greater amounts it wa neo ry to pass
the gas through this pipette twice. Completi lb
sorption is definitely shown by the
vapor above tli layer, Bi !,ing
the amount of absorption it was necessary to pass the
gas through Pipettes 1 and 2 to remove all traces of
bromine vapor. Otherwise, the bromine causes a
heavy sludge of mercuric bromide to form in the
measuring pipette. This sludge clings to the sides
of the tube and makes further work impossible.
It was necessary to use bromine water for the ab-
sorption of defines, because sulfuric acid, either fum-
ing or concentrated, was found to absorb some of the
, saturated hydrocarbons left in the gas which had been
cracked at low temperatures. Above 7500 C. the
residual saturated hydrocarbons consisted solely of
methane, so either sulfuric acid or bromine water could
be used for gas cracked above this temperature.
After the contraction due to the absorption of the
unsaturated hydrocarbons was measured, the gas
was slowly passed through the copper oxide tube to
the slow combustion pipette and back, until no further
contraction occurred. The shrinkage was calculated
as hydrogen. The temperature of the copper oxide
tube was kept at 3100 C. by means of a nichrome re-
sistance heater controlled by a rheostat. This tem-
perature was found to give rapid absorption of hy-
drogen, without noticeably attacking the saturated
hydrocarbons still present.
The residue was then passed into the silica slow-com-
bustion pipette, the wire brought to low whiteness,
and the oxygen passed in. In samples taken above
600° C. the residue consisted solely of methane and
ethane, and above 750° C. only methane survived.
go4 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. n
550° C 600' C. 650° C. 700° C. 750° C. 800° C. 850° C. 900° C. 950° C.
Catalyzhr Unsat. H Unsat. H. Unsat. H Unsat. H Unsat. H Unsat. H Unsat. H Unsat. H Unsat. H
Non„i 40 09 8.0 4.8* 18.0 10.9 24.6 13.3 27.2 19.8 17.6 28.9 8.9 39.6 5.3 50.7
p\?mice' (Coarse)'2' ''' ' 5 3 4 9* 12.3 2.3 23.7 4.8* 28.4 19.8 21.8 30.5 19.5 32.5* 9.0 43.4 2.7 560* 1.5 63.5*
Pumec Fine)' 28 2 5 5.8 3.9 21.7 13.8 29.6 16.6* 24.2 27.0 19.8 33.5 8.5 45.7 1.9 55.4 1.7 63.0
nra^s 7r,S( 26 4 0* 4.2 3.2 12.2 7.3 24.8 10.1* 27.7 19.4* 15.5 26.2 12.1 36.5 6.9 44.9 3.7 53.6*
Nickel <C,auze)i ' 33 42 9.3 10.3 3.6 61.0* 1.7 69.7 1.8 68.2 0.5 82.0 0.5 80.5 0.3 84.5
Iron (GauS 36 6 1 10.9 7.1 21.5 11.9 26.9 21.2* 7.1 54.5* 1.9 62.8 1.5 66.8
Iron St'rio'sH 20 3 5 11.0 5.9* 22.8 11.2 16.3 37.8* 5.6 56.0 1.5 64.2 .. 0.8 60.3 0.0 70.5
Chromium (Lumps)'"' 46 2 1* 7.9 2.1* 18.4 6.9* 28.3 13.7 28.8 22.8 22.5 27.7 16.9 33.6* 8.9 44.4 3.9 54.7
SJSkoS'. 12 4.4* 8.7 6.2* 22.4 12.5 23.1 26.1 21.4 33.4 19.9 35.1 13.1 40.4 3.2 53.7*
Cacium Carbide™ 2 2 4 3.8 4.4 11.9 8.3* 24.4 20.1 24.2 25.5* 16.1 41.2* 9.9 46.8 4.2 57.3 0.6 64.3
M oM.de num (Wire)"" 0.0 1.0 8.8 3.3* 23.6 9.0 30.1 15.2* 23.5 25.3* 17.3 30.2 9.8 39.7 3.1 49.2 1.6 54.7
T i£ „ ,?m . mos) ' 2 4 2 6* 7.0 2.9 10.5 8.6 28.1 14.9 23.7 25.1 23.5 26.3 11.5 36.1 4.4.50.0*
C.lcium (Turnings)"" K8 o!o 7.8 3.4 28.4 9.3 30.2 15.8 26.7 22.9 15.2 34.9 Calcium melts above 800° C.
SinconVumosI 8 0 8.9 8.0 2.4 17.0 6.9* 28.1 11.5 25.7 18.8 18.0 27.2 9.6 34.3 2.2 50.9*
CobaTt (Strips)" 2 1 1.8 9.4 3.2 22.3 8.2 29.7 13.0 27.9 18.9* 14.8 43.2* 2.7 56.5* 1.0 60.8*
Tungsten (Rods) 6.2 2.1 14.9 4.8* 22.4 8.4 29.8 13.4* 27.6 18.3* 17.1 28.5 10.0 35.0 1.8 53.2*
Pl.tin.itn Mil""" 22 05 12.3 5.7* 23.1 8.9 30.2 14.6 30.7 17.6 17.9 25.3 9.4 36.8 6.5 42.1* 2.2 57.8
Coin (Foil) 16 3 7* 9.6 3.8 25.2 8.8 31.0 16.0* 25.2 20.8 20.7 23.4* 11.8 34.2* 5.2 46.3
Silver (Foil).'..''. '.'■ 9^4 2.5 13.0 3.4 20.6 9.8 29.8 14.0 27.4 19.7 21.4 26.6* 10.5 37.1 5.8 43.7*
* For purposes of reference the observations are all grouped under nine temperatures. Where the actual observed temperature varied more than 5*
from that which heads the column, an • marks the fact. The exact temperature may be found by consulting the curves.
1 Light fog appeared at 610° C. Fog became heavy and brown at 800° C. and almost black at 900° C. Solid material was deposited at this higher
1 Light fog appeared at 785°' C. but soon disappeared. No tar was found in the precipitator, but a very small amount was found in the cool end of the
condenser Naphthalene crystals were found in the cool end of the cracking tube. Pumice was stained black through all the pores and had gained 2 g.
in weight, but this could not be removed by heating in air.
1 Traces of fog visible at times, other conditions similar to (2).
* No carbon on gauze at 650° C. Fog began at 740° C. Gauze examined again at 800° C. Surface was tarnished but no free carbon present. Heavy
fog above 800° C Heavy deposit of tar and naphthalene in the tar precipitator.
» Gauze changed after each determination as the carbon deposited in one run was sufficient to plug up the tube. No fog visible at any time and no-
tar.
« Remarks for nickel apply heref6).
' Heavy fog above 750° C. Considerable tar deposited. No free carbon. The chromium was seemingly unaffected.
1 Yield of tar small. Some free carbon in cracking tube. The lumps of manganese which were made by the Goldschmidt process crumbled into pieces.
• No visible fog at' any time. No tar deposited. At the end of run the pieces of calcium carbide were found cemented together by pieces of bard
.° Heavy fog above 750° C. Good tar deposit. A few hard lumps of coke were found adhering to the wire after two or three runs.
l' Heavy fog but not much tar. Large amount of carbon in the form of soft lampblack in the cracking tube.
12 Heavy fog and good tar yield. Platinum was tarnished at end of run but was easily cleaned. No free carbon deposited.
This was checked up so many times that finally this Straight-chain hydrocarbons — >
last determination was not carried out above 7500 C. Aromatic hydrocarbons + Hydrogen + Methane
The composition of the olefines will be taken up in a R may als0 be pointed out here that many of the
later part of this paper. decompositions observed when a substance was "passed
In no case where tar was formed during a run did through a red.hot iron tube" may have been due to
it deposit in noticeable amounts before a tempera- the specific catalytic action of the ir0n pipe. particu-
ture of 7000 to 750° C. was reached. Slight bluish lafly [q thoge caseg where ,arge amounts of free car.
fogs were sometimes observed earlier, but in no case bon wgre produced
was tar recovered from them. The carbon deposited in these experiments varied
The tabulated results are shown above. See also ffom h&rd coke_like> and closely adherent material
Figs. 4 to 7 inclusive. t0 soft> velvety lampblack (this latter when the three
discussion of results anticatalysts were used) that did not adhere to the
tube. Bone and Coward1 hold that the decomposi-
In accordance with former work it is observed that tion of methane gives the hard variety, while ethylene
a tar is produced by heating straight-chain hydrocar- gives the soft materiai. Our work seems to confirm
bons of low molecular weight to a temperature of th[s^ for in those cases where soft carbon was deposited
7000 C. and above. This tar has been shown1 to the amount of methane in the gas was small,
consist of a mixture of simple aromatic compounds,
such as benzene, with more complex ones, such as ™e influence of temperature and of pressure on
phenanthrene. With the exception of nickel, iron, and the production of aromatic hydro-
cobalt, metals do not seem to have any great catalytic
effect upon the reaction, nor does variation in the In this part of the experimental work it was first
surface exposed seem to influence the reaction. It is attempted to ascertain at what temperature the
to be noted in this connection that Bone and Coward2 maximum yield of tar was obtained, and definitely
found that the decomposition of methane was a sur- establish whether any of the catalysts previously
face effect, but the decomposition of ethane and of used promoted the formation of tar.
ethylene was not. The same apparatus was used, with the exception
The metals nickel, iron, and cobalt act as anticata- that an improved form of precipitator was used. This
lysts, so far as the production of tar is concerned. is shown in Fig. 2 and is simply a 2 in. tube drawn
Their presence causes the main reaction to be of the down on one end to a point which is fitted with a rub-
order ber tube and pinchcock. A cylinder of gauze which
Straight-chain hydrocarbons — *• Carbon + Hydrogen fits the tube tight was one electrode, the other was sim-
_. , i*,i + „„,+„;„ ply a fine iron wire insulated by a glass tube. This
The above reaction always takes place to a certain Y . . t 1 • <•,„_
., .. , ■ -,.- f tl,„ u„jr, insulation was necessary to prevent sparking trom
extent in the thermal decomposition of the hydro- ^ Ti. -o ™» » in
, . . , .. . . -, • v the center electrode to the gauze. The same a in.
carbons, but in most of the cases examined it is much ... , , «. A n,.
. . .. .. .. spark coil was used as a source of current and tne
less important than the reaction H, . . . . f.^,;„„ „,;»
whole precipitator was immersed in a freezing mix-
' Zanctti. I.oc. Cll.
» Loc. cil. ' Loc- "'•
Nov., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
90s
.-,;
— l/nsat
S~~
Hydroqen
,y>
' /
-^^5<
//''
'';;.:-"-
::.."' 1
^0£
w
Temperature
Fig. 4
ture. This precipitator worked so well that it was
possible to pass the gas through the cracking tube
at a rate of 3 to 4 cu. ft. per hr. and still have complete
precipitation of the tar.
procedure — The furnace was brought up to the de-
sired temperature and the gas admitted at the rate
of approximately 1 cu. ft. per hr. The precipitator
was started and the apparatus left to itself. At in-
tervals, the temperature and the rate of flow were
checked up, and while it was found possible to regulate
the temperature within a few degrees, it was not always
possible to regulate the rate of flow closer than 5 or
10 per cent of the rate desired. This was chiefly due
to the gradual choking of the delivery pipe with naph-
thalene. At the end of a run the time was noted, the
tar run out of the precipitator, its volume measured,
and its specific gravity taken at 20 ° C. No analysis
of the tar was attempted. The precipitator and tube
were cleaned and a new run made the next day.
A few of the catalyzers which seemed most promising
were introduced into the cracking tube, as before,
and the yields determined after the most favorable
temperature for the formation of tar had been worked
out.
No records were made below 7500 C, as the yields
of tar were negligible.
The results are shown in both tabular and graphic
form (Fig. 8).
Temp.
Deg. C.
750
800
850
900(a)
850
Vol. of
Gas Length
Used of Run
Cu. Ft. Hours
8.2 7.7
7.6 8.1
7.9 8.2
Vol. of
Tar
Obtained
Cc.
16.3
25.5
42.0
Rate
Cu. Ft.
Per Hr.
1.06
0.94
0.96
7.2 1.2 1.01
Copper as Catalyzer
7.2 53.4 1.18
Chromium as Catalyzer
5.4 41.0 1.32
Silicon as Catalyzer
6.1 49.0 1.04
Tungstcn'as Catalyzer
7.0 45.4 1.23
Yield
per
Cu. Ft.
2.24
3.33
5.30
0.16
10) In the run at 900° C. a large i
nt of naphthalene
Sp. Gr.
0.9819
1.0040
1.0600
0.999
1.002
1.016
1.038
produced.
d on the electrodes in such
It deposited on the sides of the precipitator
way that its volume could not be measured
It is evident from the above that a temperature of
850° C, or thereabouts, is the best for tar formation.
The increasing specific gravity of the tar with higher
temperatures shows a decreasing content of the lighter
aromatic hydrocarbons such as benzene, and also in-
dicates the formation of more complex substances such
as naphthalene and phenanthrene. Other work, which
is not yet completed, "confirms this point.
The use of catalysts seems to give a slightly better
yield of tar, but this may be due to the more advan-
tageous transfer of heat to the gas when the packing
tube is packed. The specific gravity and the general
appearance of the tar resulting from the use of cata-
lysts are also approximately the same as of the tar pro-
duced at the same temperature, but without the use
of a catalyst.
It seems, therefore, that catalysts have no marked
beneficial effect on tar formation from straight-chain
hydrocarbons.
In order to gain an insight into the reactions taking
place during tar formation it was thought worth
while to investigate the effect of pressure on the gaseous
products and on the yield of tar.
The effect of diminished pressure as well as increased
pressure was studied. For diminished pressure the
apparatus already described worked very well, after
a few alterations had been made. A manometer for
measuring the pressures had to be fitted and a slightly
different method of by-passing the gas, when samples
were collected, was necessary. The silica tube was
entirely unsuited for the pressure work, however, and
it was found impossible to heat a copper tube to the
required temperatures in the electric furnaces at
hand. It was therefore decided to build a furnace
using the cracking tube as a core. An iron tube was
inadmissible, of course, because of its anticatalytic
effect, so copper, although rather soft and of low
melting point, was decided upon. It has no cata-
lytic effect and may be readily obtained in any size.
no too
The construction of the furnace is simple, but a
few words of explanation may not be out of place.
The tube itself was extra heavy copper pipe, i in. in
diameter and 3 ft. long. It was found impossible to
oo6
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. n
cut good threads on the ends, so 6-in. sections of heavy
brass pipe were brazed on and silver soldered to make
a tight joint. These brass ends were threaded and
fitted with hydraulic iron fittings and valves. All
joints were made tight with litharge-glycerin cement.
Twenty-inch strips of 'A in. asbestos board were first
wired around the pipe, and the nichrome wire wound
in two sections on the strips. The ends of the wires
were brought out to l/S w- asbestos board heads.
The furnace would heat up to 9000 C. in 20 min.
Beyond that temperature we did not think it advisable
to venture.
procedure — The procedure was about the same
as before. The furnace was brought up to tempera-
ture, the rate of flow adjusted, and the pressure regu-
lated. Vacuum was obtained by a motor-driven
Nelson pump, and arrangement was made for altering
the strength of vacuum by introducing a valve that
could be opened to the atmosphere.
Silicon
Copper
|
Chromium
Tungsten
•
Showing Yield of
Different Contact
Tar mth
Agents
\
Pressure was obtained by connecting the furnace
directly to the tank of compressed gas through a pres-
sure reduction valve that could be adjusted within a
pound or two. An escape valve in the far end of the
furnace provided another adjustment. The same
runs were made as before and the cracked gas analyzed
as described in Part I.
The work of high pressure was taken up first. After
the furnace had been brought up to temperature, gas
was run through it at atmospheric pressure, a sample
taken, and the pressure raised to 25 lbs. While
equilibrium was being reached in the furnace the first
sample was analyzed. In the same way the pressure
was raised to 50, 75, and 100 lbs., the tempera-
ture being held constant meanwhile. This usually
constituted a day's work. The next day the work
was repeated at the next higher temperature until
the whole range of temperatures had been recovered.
The results may be observed in the following graphs
(Fig. 9).
From the results of the work it seems that two en-
tirely different reactions take place in the cracking,
and they may be divided into those that take place
below 700° C. and those that take place above 700° C.
Up to 7000 C. increase of pressure causes increase
of unsaturated hydrocarbons and hydrogen in the
cracked gas. At 700 ° C however, a sharp change is
noted, and from that point on increase of pressure de-
creases the amounts of unsaturated hydrocarbons and
Temperature
Nov., 1018 TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
got
Temperature
Fig. 10
hydrogen in the cracked gas. There is no doubt
that many complex reactions are taking place in the
heated tube, but below 700° C. decrease of volume
is unquestionably taking place. Above that tempera-
ture we have supposed that condensation to aromatic
hydrocarbons takes place. This point is well sus-
tained by other writers, but, at the same time, large
quantities of hydrogen are split off and much methane
is liberated, so the sum total of the reaction is an in-
crease of volume. Pressure therefore should inhibit
the reaction.
This view is confirmed by the fact that in all the
runs above 7000 C. at atmospheric pressure the vapor
in the tar precipitator is brown with tar, and tar is
deposited as usual. As soon as pressure is applied,
however, the vapors become colorless and no more
tar is deposited. The first increment of 25 lbs. pressure
was sufficient to prevent the formation of tar, in all
cases but the last (8500 C), where a slight fog per-
sisted until a pressure of 50 lbs. was reached.
The curves (Figs. 10 and 11) in which percentage
composition of the gas is plotted against tempera-
ture, the pressure being constant, show great simi-
larity among themselves and with the simple curves
representing runs at atmospheric pressure.
In the diminished pressure work, the procedure was
the same as above except that the samples had to be
taken in a slightly different way, that need not be
described here. The temperature was held constant
while readings at atmospheric pressure, at 61, 46, 31,
and at 16 cm. of mercury were taken. The exact
degree of diminished pressure was rather difficult to
maintain, but by careful adjustment of a stopcock
which permitted access to the atmosphere at one end
of a T-tube, the other end being connected to the tar
precipitator, this was finally accomplished.
The results (Fig. 12) bear out in detail those ob-
tained with increased pressure. As the pressure be-
comes less, the content of unsaturated hydrocarbons
and of hydrogen in the cracked gas becomes less at
all temperatures up to 7000 C. This time 750° seems
to be the transition point, the percentage of hydrogen
falling slightly while the percentage of olefines in-
creases somewhat. Thereafter the percentage of
hydrogen decreases rapidly with diminished pressure
Temperature
Fig. 1!
while the percentage of unsaturated hydrocarbons in-
creases correspondingly.
Tar made its appearance at 750° C, but diminished
with the pressure. Very little tar was deposited at
any temperature under diminished pressure, which
may be due to two things. Under conditions of di-
minished pressure the gas is not exposed to the effect
of heat as long as it is under atmospheric pressure.
On the other hand, the formation of tar is a condensa-
tion, and as such would be impeded by diminished
pressure. The point brought out is that the forma-
tion of tar takes place in two stages.
The first one involves splitting of the saturated
bodies into unsaturated bodies, with the splitting out
of hydrogen and consequent increase of volume.
Diminished pressure accelerates this stage and in one
case the percentage of unsaturated hydrocarbons rises
as high as 39 per cent, which is considerably more
than attained at any other time. The next step, how-
ever, requires the condensation of these unsaturated
bodies into aromatic bodies, and pressures should
favor this. It is true that hydrogen may split out
also at this point, but, even so, condensation is diffi-
cult to effect under diminished pressure.
The curves in which percentage composition is
plotted against temperature, while the pressure is
held constant, show a constantly increasing maximum
for the unsaturated bodies and also show that this
maximum is reached at a higher temperature as the
pressure becomes less.
In short, the pressure experiments definitely show
that the main reaction concerned in the formation of
aromatic hydrocarbons from straight-chain hydrocar-
bons of low molecular weight begins at a tempera-
ture around 7000 C, and is a reaction that proceeds
with increase of volume despite the fact that it is a
condensation.
They show, furthermore, that the reaction proceeds
in two steps, the first of which is impeded by pressure,
the second of which is impeded by diminished pressure.
Diminished pressure, however, largely increases the
yield of unsaturated hydrocarbons, and as these will
later be shown to be valuable substances, a new way
is opened for the produi odies in large
amounts.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. n
" (ompoithon of -
THE REACTION
SIMPLE STRAIGHT-CHAIN HYDROCARBONS >
AROMATIC HYDROCARBONS
There are two views held concerning the formation
of aromatic bodies from the straight-chain series. The
theory claiming the largest number of adherents is the
decomposition of the saturated hydrocarbons step
by step to acetylene, which then polymerizes to ben-
zene.1
The other view holds that aromatic bodies can be
formed from olefine bodies directly without going
through the acetylene stage.2 It must be admitted
that little experimental evidence has been produced to
substantiate this latter view, the chief reliance being
placed in the fact that it has been impossible to detect
acetylene at any stage of the reaction. It was de-
cided to investigate the reaction concerned in this
work, with the hope that we could fit it to one or the
other of these views.
The evidence of the polymerization of acetylene to
benzene is incontrovertible, so this work was not re-
peated. The work was therefore begun by mixing
known amounts of acetylene with the gas used in
our previous work. This was accomplished by passing
a definite amount of acetylene through the referee
meter into an empty gas holder, following this by the
addition of sufficient natural gas condensate to make
up a mixed gas of desired acetylene content. The
-mixture was allowed to stand a day before being used,
that thorough mixture might take place. It was then
run through the cracking tube in the original appara-
tus and the cracked gas allowed to bubble through
ammoniacal silver nitrate, followed by ammoniacal
cuprous chloride.
The following mixtures were experimented with:
Per cent
Natural Gas Condensate 99 . 0
Natural Gas Condensate 99.5
Natural Gas Condensate 99.0
Natural Gas Condensate 97.5
Natural Gas Condensate 95.0
Natural Gas Condensate 90.0
Acetylene.
Acetylene.
Acetylene.
Acetylene.
Acetylene.
Per cent
0.1
0.5
1.0
2.5
5.0
Acetylene 10.0
As the mixed gas was led through the cracking tube,
the temperature was raised from an initial tempera-
' Ucrthelot. Aim. Mm.. [■» ] 9, 469.
1 D. T. Jones, "The Thermal Decomposition o( Hydrogcnated Hydro-
carbons," J. Chem. Soc.,101 (1915), IS82,and "The Thermal Decomposition
of Low Temperature Coal Tar," J. Soc. Chem. Ind., 36 (1917), 3.
ture of 550° C. to one of gs°° C., by steps of 500. In
every case the test for acetylene was positive. In
the 0.1 per cent and 0.5 per cent mixtures the test
was less pronounced at higher temperatures than at
lower ones, but this was to be expected, as acetylene
in the presence of large amounts of hydrogen passes
partly to ethylene or ethane, and partly breaks up
into carbon and hydrogen.1
The point to be noted here is that sufficient acetylene
remains even in a 0.1 per cent mixture, which has been
passed through a tube slowly (0.5 cu. ft. per hr.)
and cracked at a temperature up to 050° C, to give
a decided test for a triple bonded component.
We must conclude, therefore, that acetylene, if
formed in appreciable amounts in the thermal decom-
position of natural gas condensate, would not entirely
decompose again. In any event, enough would re-
main to give a reaction with silver nitrate or cuprous
chloride. Although the absence of acetylene has been
reported in this connection, we repeated the tests,
using clean gas, and could find no trace of acetylene.
Examination of the bromides formed by passing
the cracked gas through bromine under water and
cooled with ice and salt showed no tetrabromacetylene.
The absence of acetylene or other triple bonded
hydrocarbons seems to establish the fact that aromatic
formation is not in this case dependent upon their
formation.
In order to study the unsaturated bodies more
thoroughly, about 500 g. of mixed bromides were pre-
pared as described above.
It has been pointed out before that methane was the
only hydrocarbon remaining when the gas was cracked
at a temperature of 7500 C, or above, so simple
bromides of ethane or propane need not be looked for.
In order to make certain that substitution was not
taking place in the methane, however, a preliminary
experiment was run in which the bromine was used
dissolved in carbon tetrachloride. Hydrobromic acid
is given off from such a solution when substitution
takes place as opposed to addition. The gases, after
passing through the bromine solution, were cooled
to — 200 C, and then passed through glass wool at
the same temperature to catch any volatilized bromine
vapor. They were then allowed to bubble through
standard potassium hydroxide. Back titration showed
that almost no acid had come over, and therefore that
substitution was not taking place to any appreciable
extent.
The 500 g. of mixed bromides prepared above were
distilled under 4 cm. vacuum with the following results:
Sp. Gr.
1.46
1.89
2.13
1st drop at 29° C
29°-50i 6.5
50">-60° 35.0
W-to* 45.0
Residue 10.0
Loss 3.5
100.0
Xo trouble was experienced in the distillation, as
decomposition of the bromides did not take place.
The liquid distillates were then mixed and redistilled
at atmospheric pressure with the following results:
1 Bone and Coward, Loc. tit.
Nov., 101S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
909
Volume
Temperature Per cent
1st drop at 89° C
89°-125° 10.3
125°-133° 44.7 Ethylene Bromide
Fraction
133°-137° 12.8 Propylene Bromide
Fraction
Residue 29.4
Loss 2.8
100.0
The residue from the vacuum distillation was almost
entirely tetrabrombutane, while a large amount of
this same material was extracted from the thick liquid
that remained in the distillation flask above. It is
evident that the bromides are, as reported by Zanetti,1
a mixture of ethylene bromide, a smaller amount of
propylene bromide, and from 10 per cent to 20 per
cent tetrabrombutane (butadien tetrabromide). Small
amounts of other bromides are also present, but no
acetylene tetrabromide (b. p. 137° C, sp. gr. 2.9)
was found. The bromine content of the ethylene
and propylene bromides was checked up by analysis
and found to be correct within 0.5 per cent. The
melting point of the tetrabrombutane was found to
be 1170 C. (correct value = 1180 C.) and its bromine
content corresponded to the formula dr^Br.!.
The source of the tetrabrombutane needs inquiry.
But very little butane exists in the original gas, which,
as remarked before, consists of almost nothing but
ethane and propane. The butane content is not large,
and accounts in no way for the large yield of tetra-
brombutane. A building-up process must therefore
be responsible for the greatest part of the yield. It is
a known fact that butadien yields tetrabrombutane
on bromination and, since the presence of this com-
pound was suspected, experiments were carried out
to isolate it.
In order' to prove this point, the gases, after cracking
at 8500 C, and after all the tar was removed by the
precipitator, were cooled down in three stages. The
cleaned gas was slowly led through three wide test
tubes placed in thermos bottles containing cooling
liquids. In Tube 1, the gas was cooled to — 30 C.
Any benzene still present was frozen out in this tube.
Tube 2 was kept at a temperature of — 90 ° C. by
means of a mixture of alcohol and liquid air, while
Tube 3 was placed in liquid air direct. The tem-
perature of the gas in this last tube was about
— 1 700 C.
The boiling points of some of the substances we
are dealing with are given as follows:
Methane — 164°
Ethane — 89°
Propane — 39°
Butane + 0.6"
Ethylene —103"
Propylene — 50°
Butylene — 5"
Butadien — 5°
Hydrogen —256°
Benzene, f. p + 5°
Ethane, propane, and butane can be ruled out at
once, as methane is the only saturated hydrocarbon
remaining in the gas at this temperature. Assuming
all the rest of the gases to be present, it is
that only benzene will be deposited in 'lube r. Pro-
pylene, butylene, and butadien will condense in Tube
a, while ethylene and some methane will condense in
1 Loc. cit.
Tube 3. Hydrogen mixed with a large amount of
the vapor of methane will pass on uncondensed.
Some solid did appear in Tube i, showirg that the
precipitator does not remove all the benzene; Tubes
2 and 3 contained liquid condensates. These con-
densates were very mobile, almost colorless liquids
with pronounced odors.
In Tube 2 we are concerned with the presence of
butadien, so after 20 to 30 cc. of liquid had collected,
the tube was disconnected and allowed to warm up
slowly to — 20 ° C. The propylene all boiled off in
the process and the volume shrunk to less than one-
half. Keeping the tube in the cooling mixture,
pure bromine was dropped into the liquid which still
remained. A reaction of almost explosive violence
took place and the liquid began to boil rapidly.
Addition of bromine was continued until the liquid
remained slightly red, then a little liquid from Tube 3
was added to combine with the excess bromine. About
half the liquid remaining, after the propylene had
boiled off, was lost in the bromination process which
had generated enough heat to keep the bromides
formed liquid for some time, even though the bath
was still at a temperature of — 20 ° C. Shortly after-
ward, however, the whole residue in the test tube
solidified. The tube was withdrawn, a portion of the
crystals recrystallized from alcohol, and the melting
point determined. M. p. = 117* C. No butane
dibromide, which would result from the presence of
butene, was observed.
This experiment was repeated, but this time after
30 to 40 cc. of liquid had collected in Tube 2, it was
disconnected and closed with a stopper and delivery
tube, whose end was beneath bromine covered with
water and cooled with a mixture of ice and salt. The
gases evolved as Tube 2 warmed up to — 200 C.
were allowed to bubble through the bromine until the
temperature of — 200 C. was reached. Another tube
containing bromine was then substituted for the first
one and Tube 2, containing the condensed gas, was
removed from the thermos bottle and allowed to come
to room temperature, the evolved gases passing through
the bromine as before. All the liquid in the tube
had vanished before a temperature of — 2° C. was
reached.
By distillation, propylene bromide was rpadily ob-
tainable from the first tube of bromine as a heavy,
almost colorless liquid, with a pronounced and rather
-lor, b. p. = 139. 8° C, sp. gr. = 1 . 942 at 17° C.
The liquid in the second tube solidified and was identi-
fied by its in al as tetrabrombu
Tube 3 -was now disconnected from the apparatus
and transfers aining a mix-
ture of liquid air and alcohol at a temperature of
— 115° C. \ 'ition took place as it warmed
up to this temperature, and methane (b. p. = - — 1640 C.)
boiled off. A clear liquid remained which was prac-
tically all ethylene. It ■ d by brominating
a small portion of it and taking the melting point
(m. p. - +90 C).
The experiment was repeated once more, but this
time, after the propylene] had boile ,,• 2 and
01 ' >
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. n
the methane off Tube 3, the remaining material as it
volatilized was led in each case to a small gasometer.
The gas so obtained represented a mixture of approxi-
mately 30 per cent butadien and 70 per cent ethylene.
This mixed gas was passed through the original
apparatus and cracked at a temperature of 850° C.
A small amount of tar similar in all respects to the
original tar was obtained. Its specific gravity was
1. 010. Further analysis was not attempted, owing
to the small amount formed. The cracked gas was
then analyzed and shown to be 50 per cent unsaturated,
20 per cent methane, and 30 per cent hydrogen. The
cracked gas, when cooled down as before, gave a large
amount of ethylene in Tube 3 along with some ethane.
Tube 2 had only a trace of condensate, showing that
all the butadien had combined.1
CONCLUSIONS
The presence of butadien in large quantities in the
cracked gas can be explained only by the combination
of two molecules of ethylene, with the splitting off
of hydrogen, thus
II ,c =s CH2 + H2C = CH; — ■*■
H2C = CH — HC = CHo + H2
If now we presume that another molecule of ethylene
can unite with the butadien, we have all the necessary
steps for the formation of benzene. D. T. Jones2
finds that cyclohexane on heating to 5oo°C. passes to
cyclohexene which then decomposes in two ways,
yielding benzene on one hand and butadien with ethyl-
ene on the other.
CH2
H2C/NCH2
CH2
CH2
HjCi^C H
HjC^CH;
CH2
+ H,
H2C = CH— HC = CH2 + H2C = CH,
yf CH
HCffVH
HCX ACH
CH
+ 3H2
The present work merely requires the union of the
ethylene and butadien of this equation to form cyclo-
hexane which most likely has no separate existence,
breaking down at once into benzene and hydrogen.
This reaction involves an increase of volume and would
therefore be inhibited by increase of pressure, a fact
which has already been proved true above*.
In support of these views we have the work of
Jones,1 win. inclines to the belief that defines condense
to aromatic bodies. He states, "It is highly probable
that a necessary transient stage is the formation and
condensation of the stable conjugated double linking,
' CH = CH — CH = CH — ." The presence of this
1 Kor references on the preparation and properties of butadien sec
/. Cktm. Soc, 27 (1874), 406: J. Chem. Soc, 49 (1886), 80; and Am 308
(1899), 333.
' Loc. cit.
linkage in its simplest form, butadien, has been demon-
strated above.
Staudinger,1 starting with isoprene, showed that
45 to 55 per cent of this material was converted into
a tar by passing it through a tube at 7500 C. This tar
contained aromatic hydrocarbons similar to those
Zanetti found in his tar. Staudinger also cracked
butadien alone and obtained from it a tar that con-
tained about 25 per cent benzene.
It seems to be established, therefore, that diolefines>
on cracking, pass in large part to closed chain bodies.
It has been demonstrated in this work that simple ole-
fines and diolefines are produced by the cracking of
the ethane-propane fraction of natural gas condensate.
The aromatic bodies found in the tar comes from the
condensation of the diolefines and this therefore gives
us all the necessary steps in the formation of aromatic
bodies from straight-chain hydrocarbons of less than
four carbon atoms, and without the necessity of passing
through the stage of acetylene.
SIM MARY
I — It has been shown that most metals are without
action on the reaction
Paraffin hydrocarbons — *■ Aromatic hydrocarbons.
The metals nickel, iron, and cobalt are anticatalysts
for the above reaction, but promote to a marked de-
gree the reaction
Paraffin hydrocarbons — >• Carbon + Hydrogen.
II — The effect of temperature and pressure on the
production of aromatic hydrocarbons has been studied.
It has been pointed out that a temperature of 8500 C.
is most favorable for the formation of liquid tar and
that the formation of complex aromatic bodies in-
creases with the temperature.
Ill — Increase of pressure inhibits the formation of
tar while diminished pressure increases the yield of
unsaturated bodies but also decreases the actual yield
of tar.
IV — Butadien has been isolated in fairly large
amounts from the unsaturated bodies produced in the
thermal decomposition of natural gas condensate.
V — Acetylene has been shown to be without action
in the formation of the aromatic compounds.
VI — Tar containing aromatic bodies has been pro-
duced from the cracking of a mixture of butadien and
ethylene.
VII — The most probable reaction for the formation
of aromatic bodies from natural gas condensate is
Saturated straight- Simple
chain hydrocarbons olefines
(Ethane) (Ethylene)
Higher olefines Aromatic
with conjugated bonds hydrocarbons
(Butadien) (Benzene)
Department of Cub
Columbia Ukiversi
New York City
' Btr., 46 (1913), 2466
Nov., 101S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
LABORATORY AND PLANT
METHODS OF ANALYSIS USED IN THE COAL-TAR
INDUSTRY. HI— HEAVY AND MIDDLE OILS
By J. M. Weiss
Received September 9, 1918
HEAVY OIL TESTS
TEST H2 WATER1
apparatus — Same as given under B2 (see Fig.
II, Paper I, This Journal, 10 (1918), 735).
method — 200 cc. of oil shall be measured in a grad-
uated cylinder, and poured into a copper still,
allowing the cylinder to drain into the still for
several minutes. Attach lid and then the clamp,
using a paper gasket slightly wet with oil, around
the flange of the still. Heat shall be applied by means
of the ring burner, which shall be placed just above
the level of the oil in the still at the beginning of the
test, and gradually lowered when most of the water
has distilled over. The distillation shall be continued
until the vapor temperature, indicated by the ther-
mometer with the bulb opposite the off-take of the
connecting tube, reaches 205 ° C, the distillate being
collected in the separatory funnel. When the distilla-
tion is completed, and a clear separation of water and
oil in the funnel has taken place, the water shall be
read by volume and drawn off; and any light oil dis-
tilled over with the water shall be returned to the oil
in the still after it has cooled sufficiently. The de-
hydrated oil from the still shall be used for the dis-
tillation and other tests.
TEST H3 SPECIFIC GRAVITY (SPINDLE)1
apparatus — Hydrometer and cylinder (See Fig.
II, Paper I, This Journal, 10 (191S), 735). Two
hydrometers with ranges 1.00 to 1.0S and 1.07 to
1.15 will suffice. These shall be calibrated at 15.5°
C. (6o° F.).
method — The oil shall be brought to a tempera-
ture of 380 C. (100° F.) and the determination shall
be made at that temperature unless the oil is not en-
tirely liquid at 38 ° C. The cylinder shall be filled .
with dry oil, the latter stirred, and the tempera-
ture noted. The hydrometer shall be inserted and
the reading taken. In case the oil requires to be
brought to a higher temperature than 38 ° C. in order
to render it completely fluid, it shall be tested at the
lowest temperature at which it is completely fluid,
and a correction made by adding 0.00075 to the ob-
served specific gravity for each degree Centigrade
above 38 °, at which the test is made.
precautions — Before taking the specific gravity
the oil in the cylinder should be stirred thoroughly with
a glass rod, and this rod when withdrawn from the
liquid should show no solid particles at the instant
of withdrawal. Care should be taken that the hydrom-
eter does not touch the sides 01 botl of the cylin-
der when the reading is taken, and that the oil sur-
face is free from froth and bubbles.
1 See A. S. T. M. Method D-38-17, A. S. T. M. Standards adopted in
ACCURACY o. 002.
note — The correction factor, 0.00075, does not
apply with equal accuracy to all oils, but serious error
due to its use will be avoided if the precaution
of avoiding unnecessarily high temperature is ob-
served.
The factor 0.00075 and its method of use are ap-
proximations.
TEST H4 SPECIFIC GRAVITY (WESTPHAL)
apparatus — Westphal balance. 25 cc. glass cylin-
der.
method — The balance shall be set up and adjusted
so that the plummet when suspended to swing freely
in air exactly balances the beam. A reading shall
then be taken in water at 15. 5 ° C. and if the balance
is properly made and adjusted, this will be unity. A
second reading in oil at 15. 5 ° C. gives the specific
gravity directly.
precautions — If the reading in water at 15. 5 ° C.
is not unity when the balance is adjusted in air so
that the plummet balances the beam, the balance
shall not be adjusted in water, but the oil reading
divided by the water reading shall be taken as the
specific gravity.
Boiled distilled water shall be used. Care shall be
taken to see that the wire from which the plummet is
suspended is immersed in both oil and water to the
same point when the instrument is in balance. Care
must be taken to see that the plummet is clean and
dry before immersion.
note — If the specific gravity is to be taken at a
temperature above 15. 50 C, a reading must be taken
in water at the same temperature and the specific
gravity at t/t° C. obtained. This may be con-
verted into specific gravity at l°/is. 5° C. by multiply-
ing by the density of water at /°/i5-5° C. These
density figures for water may be found in reference
books such as Van Nostrand's Chemical Annual. To
calculate from 38c/38° to 38°/i5.5° C. the factor is
0.99385. From the foregoing it will be readily seen that
it is incorrect to calculate the specific gravity at
38V15.50 by dividing the reading in oil at 38° by the
reading in water at 15. 5 ° C. as is occasionally done.
test 115 — insoluble in benzol1
All matter as to apparatus, method, notes, and pre-
cautions as given under B72 apply to this test on these
materials.
accuracy — 0.2 per cent.
note — At least 10 g. of oil shall be taken for the test.
test h6 — retort distillation1
apparatus — Retort: This shall be a tubulated
glass retort of the form and approximate dimensions
shown in Fig. XII with a capacity of 250 to 290 cc.
The capacity shall be measured by placing the retort
1 See A. S. T. M. Method D-38-17, A. S. T. M. Standards adopted in
1917.
' Tins Journal, 10 (1918), 736.
912
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. n
with the bottom of the bulb and the end of the off-
take in the same horizontal plane, and pouring water
into the bulb through the tubulature until it overflows
the off-take. The amount remaining in the bulb shall
be considered its capacity.
Condenser tube: This shall be a suitable form of
tapered glass tubing of the following dimensions:
Diameter of small end, 12.5 mm.; permissible variation, 1.5 mm.
Diameter of large end, 28.5 mm.; permissible variation, 3.0 mm.
Length, 360.0 mm.; permissible variation, 4.0 mm.
Shield: An asbestos shield of the form and approxi-
mate dimensions shown in Fig. XII shall be used to
protect the retort from air currents and to prevent
radiation. This may be covered with galvanized
iron, as such an arrangement is more convenient
and more permanent.
Receivers: Erlenmeyer flasks of 50 to 100 cc.
capacity are the most convenient form.
Thermometer: This shall conform to specification
as given under C7.
Assembly: The retort shall be supported on a
tripod or on rings over two sheets of 20-mesh gauze, 6 in.
square, as shown in Fig. XII. It shall be connected
to the condenser tube by a tight cork and the ther-
mometer inserted in a tight cork in the tubulature,
with the bottom of the bulb l/s in. from the surface
of the oil in the retort. The exact location of the
thermometer bulb shall be determined by placing a
vertical rule graduated in divisions not exceeding Vie
in. back of the retort when the latter is in position for
the test, and sighting the level of the liquid and the
point for the bottom of the thermometer bulb. The
distance from the bulb of the thermometer to the out-
let end of the condenser tube shall be not more than
24 nor less than 20 in. The burner shall be protected
from draughts by a suitable shield or chimney (see
Fig. XII).
EytiMitt*
Fio. XII — Assembly op Distillation Test for Heavy Oil
A. S. T. M. D-38-17
METHOD — Exactly 100 g. of oil shall be weighed into
the retort, the apparatus assembled, and heat ap-
plied. The distillation shall be conducted at the rate
of at least one drop and not more than two drops
per second, and the distillate collected in weighed re-
ceivers. The condenser tube shall be warmed when-
ever necessary to prevent accumulation of solid dis-
tillates. Fractions shall be collected at the following
points: 210°, 2350, 2700, 3150, and 355° C. The
receivers shall be changed as the mercury passes the
dividing temperature for each fraction. When the
temperature reaches 355 °, the flame shall be removed
from the retort, and any oil which has condensed in
the off-take shall be drained into the 355 ° fraction.
notes — The residue shall remain in the retort with
the cork and the thermometer in position until no
vapors are visible; it shall then be weighed. If the
residue is to be further tested, it shall then be poured
directly into the brass collar used in the float test or
into a tin box and covered and allowed to cool to air
temperature. Care must be taken not to pour at a
temperature high enough to cause loss of oil vapors.
If the residue becomes so cool that it cannot be poured
readily from the retort, it shall be re-heated and com-
pletely melted by holding the bulb of the retort in hot
water or steam and not by the application of a flame.
For weighing the receivers and fractions, a balance
accurate to at least 0.05 g. shall be used.
During the progress of the distillation the thermom-
eter shall remain in its original position. No correc-
tion shall be made for the emergent stem of the ther-
mometer.
When any measurable amount of water is present
in the distillate it shall be separated as nearly as possi-
ble and reported separately, all results being calculated
on the basis of dry oil. When more than 2 per cent of
water is present, water-free oil shall be obtained by
separately distilling a larger quantity of oil, return-
ing to the oil any oil carried over with the water, and
using dried oil for the final distillation (see H2).
TEST H; SPECIFIC GRAVITY FRACTIONS (WESTPHAL)1
apparatus — A special type of Westphal balance is
obtainable, designed for testing very small quantities.
However, the ordinary type of Westphal balance can
be adapted to testing small fractions by the use of a
special plummet. The plummet can readily be made
in the laboratory from a piece of ordinary glass tubing
7 mm. outside diameter, sealed at the end, and melt-
ing into the glass, where sealed, a short platinum
wire. After cooling place 9 to 10 g. of mercury in
the tube, making a column 35 to 40 mm. high. Seal
off the tube within 20 mm. of the top of the mercury
column with blowpipe flame. The plummet shall
have a length of about 55 to 60 mm. over all and shall
weigh between 10 and 12 g.
method — The weights necessary to balance the
plummet in air and in water of the required tempera-
ture shall be noted and similarly the weight necessary
to balance the plummet in oil at the same tempera-
ture.
If a = weight to balance in air
b = weight to balance in water to *°
c «= weight to balance in oil at 1°
c — a
Specific gravity t°/l° »
b — a
precautions — When using the small plummet,
special care is needed that the adjustment of the
balance be accurately made.
note — For corrections from i°/t° C. to '°/i5-5° C.,
see note under H4.
1 See paper by J. M. Weiss, This Journal. 7 (1915). 21,
Method D-38-17, A. S. T. M. Standards adopted in 1917.
nd A. S. T. M.
Nov., 1018
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
913
This method is adapted to fractions which are liquid
•under 60° C. and may usually be applied to the 23 5 °
to 3 1 5 ° fraction.
test h§ specific gravity fractions (platinum
pan)1
All matter under B62 applies to this test on this
material.
note — This method is adapted to solid and semi-
solid fractions such as are usually obtained from
315° to 3550 C.
TEST HQ FLOAT TEST ON RESIDUE3
All matter as to apparatus, method, precautions
and notes, as given under C8, applies to this test on
these materials.
TEST H9 FLOAT TEST ON RESIDUE MATERIAL3
All matter as to apparatus, method, precautions
and notes as given under C8 applies to this test on
these materials.
-coke4
shown
Fig.
glass bulbs
shall be warmed slightly to
apparatus — Hard
XII shall be used.
method — The bulb
drive out all moisture, cooled in a desiccator, and
weighed. Then the bulb shall be heated again by placing
it momentarily in an open Bunsen flame, the tubular
placed underneath the surface of the oil to be tested,
and the bulb allowed to cool until sufficient oil is sucked
in to fill the bulb about two-thirds full.
Any globules of oil sticking to the inside of the
tubular shall be drawn into the bulb by shaking, or
expelled by slowly heating it. The outer surface shall
be carefully wiped off and the bulb reweighed. This
procedure will give about 1 gram of oil.
A strip of thin asbestos paper about 1/t in. wide and
about 1 in. long shall be placed around the neck of the
bulb and the two free ends caught close up to the neck
with a pair of crucible tongs. The oil shall then be
distilled off as in making ordinary oil distillation,
starting with a very low flame and conducting the
distillation as fast as can be maintained without
foaming.
When oil ceases to come over, the heat shall be in-
creased until the highest temperature of the Bunsen
flame is attained, the whole bulb being heated red-hot
until the evolution of gas ceases, and any carbon stick-
ing to the outside of the tubular is completely burned
off. The bulb shall then be cooled in a desiccator,
weighed, and the percentage of coke residue calculated
on water-free oil.
precautions — Be careful to heat the oil slowly at
the start to avoid spurting. If the oil contains over
2 per cent of water it should be dried before testing.
The oil must be thoroughly liquefied and uniform
throughout.
' See paper by J. M. Weiss, Tins Journal. 7 (1915), 21, and A. S.T. M.
Method D-38-17, A. S. T. M. Standards adoptedso 1917.
' Tins Joi rnal, 10 (1918), 736.
• See standard method of the Am. Wood Prcs. Assoc, adopted in 1916
and A. S. T. M., D-38-17. tentative method, A. S. T. M. Proceedings 1917,
Part I , p. 826.
' Ibid., p. 828.
u
\M
notes — A large diameter cork with a cup-shaped
hole cut in the center forms a convenient holder in
which to weigh the bulb. When a stock of bulbs is
received, one or more
should be given a heat test
to determine hardness.
Occasionally bulbs have
been found too soft, there-
fore melting below the
temperature required to
coke the oil and thus pro-
ducing low results.
TEST HI I TAR ACIDS (CON-
TRACTION method)
apparatd s — Tar-acid
separatory funnel, type i
(see Fig. XIII). Tar-acid
separatory funnel, type 2
(see Fig. XIV). Distilla-
tion apparatus.
method — 100 cc. of oil
shall be placed in a distilling
apparatus such as is used
under test F5 and distilled
until at least 93 per cent
of distillate has been ob-
tained or until the vapor
temperature has reached
400° C. The entire dis-
tillate shall be transferred
to a tar-acid separatory
funnel — type 1 designed for
oils which have 25 per
cent tar acids or over, or ^cp
type 2 for oils containing .
less than this amount. The
funnel with the oil shall be
placed in a water bath and
kept at a constant tem-
perature of 60° C. until no
change in volume takes
place. It shall then be ex-
tracted with successive por-
tions of 50 cc. each of 10
per cent caustic soda solu-
tion until no further diminu-
tion in volume occurs.
The soda shall be added to »)|vS
the oil, the whole thor-
oughly shaken, then re-
turned to the bath at 6o° C.
and allowed to settle com-
pletely. After settling is
complete, the soda layer
shall be drawn off and the
volume of residual oil
noted. When the point of
no further contraction is rea diminution in
volume of the oil shall be considered as tar acids.
I s — In some cases (such as creosote tar solu-
containing small i, there will
efficient material to bring the oil up into the
Fir.. XIII— Dbtail of Tar-Acid
Sbparatory Funnbl, Typb I
A — Ground glass stopper
B — Capacity given from stop-
cock up
C — Ground glass stopcock
914
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No. n
er*-<r
Id
Fio. XIV — Sbparatoky Punnbl fok
Acid Distkrmination, Tvim: 2
\ — Ground glitss stopper
13 — •/• in. drilled hole
> — Ground glass stopcock
graduated section of
type 2 separatory fun-
nel. In such cases, suffi-
i ii hi tar-acid-free, clean,
naphtha may be
added to dilute the oil
and 1 prin.L; it within the
:cd portion. If
this is done, the ex-
d oil cannot be
<>r subsequent dry
salt tests but an addi-
tional portion must be
extracted for this pur-
pose.
This test is recom-
mended for all general
work in oil specifica-
tions and general com-
parative tests, but gives
results slightly higher
than the true tar-acid
content of the oil. The
reason for this is that
soda withdraws from
creosote oil certain com-
pounds which are not
subsequently liberated
from the soda solution
in the form of an oil.
These substances are
evidently acid in nature
but not phenolic bodies.
test hi2 tar acids
(liberation method)
apparatus — Same as
used under Hi i. Water
and tarseparatoryfunnel
(see Fig. II, Article I,
This Journal, io
(1918), 735-
METHOD IOO CC. Of
oil shall be distilled as
prescribed under Hn.
(Where the content of
tar acids is very low, a
distillation may be made
on 200 cc. so as to ob-
tain a more accurate
test.) The oil shall be
1 in a separatory
funnel with successive
50 cc. portions of 10 per
cent caustic soda or until
no more tar acids are re-
moved. The well-settled
rbolate shall
Ik- acidified in a sm3ll
beaker with 40 per cent
sulfuric acid, taking care
p t he mixture cool
at all times. (If the content of tar acids is under
5 per cent, use the water in tar separatory funnel and
measure carefully into it 10 cc. of "Hiflash" naphtha.
The liberated tar acids and sulfate solution are then
poured through this layer of naphtha several times,
drawing the material off at the bottom of the funnel
into the original beaker and pouring it back into the top
of the funnel. This washes out the beaker and al-
lows all the tar acids to be absorbed by the naphtha.)
Tin- funnel shall then be allowed to stand until the ■
layers separate perfectly clearly when the sulfate
solution shall be drawn off and the increase in volume
of the naphtha taken as the dry tar acids present.
When the content of acids is over 5 per cent, the same
procedure can be used, measuring 65 cc. of "Hiflash"
naphtha into the tar-acid separatory funnel, type 2.
precaution — All results must be figured on the
basis of dry oil.
notes — In distilling 200 cc. of oil, it is necessary
to use a distilling bulb of about 500 cc. capacity.
"Hiflash" naphtha may be obtained from The Barrett
Company Chemical Department.
This method gives approximately the amount of
tar acids that can be recovered from an oil in practice.
Results by this method are usually about 90 per
cent of the results obtained by the method as given
under Hn.
TEST HI3 HEMPEL DISTILLATION1
apparatus — Forest Service Hempel flask.2 Con-
denser tube (see Fig. II, Article I, This Journal,
10 (1918), 735). Thermometer, graduated from 0° to
4000; specifications as under C9. Glass beads. As-
bestos shield.
The apparatus assembly is shown in Fig. XV.
method — The empty flask shall be tared, 250 g. of
melted, well-shaken oil introduced, and a second weight
taken. The flask shall be supported on an asbestos
board with a slightly irregular opening of very nearly
the largest diameter of the flask, and the apparatus
assembled as in Fig. XV. The distillation shall be
run at the rate of 1 drop per sec, and fractions col-
lected in weighed flasks between the following tempera-
tures: Up to 1700, 170° to 2050, 2050 to 225°, 225°
to 2350, 235° to 245°, 245° to 255°, 255° to 285°, 285°
to 295°, 295° to 305°, 305° to 320°, and if feasible,
320° to 360°.
The character of the fractions and their weights
shall be recorded.
precautions — Drafts on the distilling apparatus
must be avoided.
note — In noting the character of the fractions, the
operator should observe the apparent amount of
salts separating at room temperatures and roughly
approximate the nature of the fraction, c. g., solid,
half solid, liquid, etc.
test H14 — index of refraction of fractions
apparatus — Zeiss- Abbe refract ometer.
METHOD— Water at 60° C. shall be circulated
through the water jacket which surrounds the main
' Adapted from Forest Service Circular Hi, V. S. Dept. Agriculture.
> A. H. T. 28220. IS. & A. 3072.
Nov., 101S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
9i5
prisms. After the temperature of the water in the
jacket has been brought to this point, the prisms shall
be separated and a few drops of the oil to be tested
placed between them. They are then brought to-
gether and locked in position. The prisms shall now
be rotated until the field of view consists of a light and
dark portion. The telescope is provided with a recti-
cule which can be brought into exact coincidence with
the observed border line between the light and dark
field. The compensator prisms are rotated until a
sharp line of demarcation is produced. The index
of refraction shall be read on the scale through the
eye piece on the left side of the refractometer.
Fie. XV — Assembly of Hempbl Distillation Test for He
Forest Service Method
precautions — The temperature must be kept at
60 ° C. throughout the test. The lenses and prisms
should be kept perfectly clean. Special lens paper
should be used for this purpose so as to avoid scratch-
ing or damaging the surfaces.
Take care that the reflector does not show the line
of a window sash which may be mistaken for the border
line. Such a reflection can be detected by moving
the mirror, when the true line does not move.
notes — The light is regulated by the reflector
beneath the prisms until suitable illumination is ob-
tained.
If the line cannot be produced, either there is in-
sufficient oil between the prisms or the index of re-
fraction of the material lies outside the range of the
instrument.
With each refractometer is supplied a soli
of known refractive index for use in checking the
original adjustment of the instrument. Directions
for its use accompany the instrument.
TEST HI 5 SULFONATION RESIDUE1
apparatus — Milk bottles, A. H. T. 33,964, E. & A.
4,45°-
Centrifuge: Any milk bottle centrifuge will do;
there are many types; refer to any apparatus catalog.
A convenient type where only few tests are run is
A. H. T. 33,936, E. & A. 1,883. Where many tests are
being handled, A. H. T. 33,940, E. & A. 1,978 is better.
method — Ten grams of the fraction of oil to be
tested shall be weighed into a Babcock milk bottle.
To this shall be added 40 cc. of 37 N sulfuric acid (total
S03, 80.07 per cent), 10 cc. at a time. The bottle
with its contents shall be shaken for 2 min. after each
addition of 10 cc. of acid. After all the acid has been
added the bottle shall be kept at a constant tempera-
ture of from 98 ° to 100° C. for one hour, during which
time it shall be shaken vigorously every 10 min. At
the end of an hour the bottle shall be removed, cooled,
filled to the top of the graduation with ordinary sul-
furic acid, and then whirled for 5 min. in a Babcock
separator. The unsulfonated residue shall then be
read off from the graduations. The graduated por-
tion of the bottles measures 2 cc. and is divided into
10 major graduations. These major graduations
are subdivided into either 5 or 10 smaller divisions.
The reading, expressed in terms of major divisions,
multiplied by 2, gives per cent directly.
precautions — The unsulfonated residue should be a
clear transparent oil. If there is an apparent residue
of dark or gummy appearance, the sulfonation is
probably incomplete and the test should be repeated.
The addition of the acid should be regulated so
tha,t the mixture ceases to heat up on shaking, before
another portion is added. If acid is added too quickly,
foaming results.
Sometimes the material will start to foam on re-
moval from the hot bath. Immersion in cold water
will usually stop the foam. Proper strength of sul-
furic acid is essential.
acciracv — 0.1 per cent of amount taken, that is,
0.01 cc, unless the per cent residue exceeds 5, when
0.5 per cent variation is allowable.
notes — Occasionally a solid residue of white paraffin
is obtained. In this case the bottle should be warmed
sufficiently to melt the paraffin and re-whizzed. The
reading may be taken while the material is liquid.
This method differs from the original Forest Service
method in that the oil is weighed and not measured.
On solid fractions an accurate measurement is impossi-
ble. Therefore, we have specified weight and our per
cent result really represents cc. per 100 g. If a real
per cent by volume is required the result should be
multiplied by the determined specific gravity of the
oil fraction and the result reported as per cent by
volume (calculated).
The 37 N acid should contain So. 07 per cent total
S0». It is made by mixing analyzed ordinary con-
.1 sulfuric acid with analyzed fuming sulfuric
a' i<l m the proper proportions. It is best to run a
best on the mixture to insure the fact that the
1 >rrect.
' Adopted from Forest Servict Circular 191, U. S. Dept. Anricu!ture.
916
THE JOURNAL OF INDUSTRIAL AND ENGINEER/ N(, I II I.MISTRY Vol. 10, Xo. n
TEST Hl6 TAR BASES
This test shall be carried out exactly as described un-
der Hi i, using 20 per cent sulfuric acid instead of 10
per cent caustic soda. As there are rarely more than
5 per cent of bases in any coal-tar oil, the tar-acid
funnel, type 2, should be used for this purpose.
TEST HI7 DEY SALTS AT 4.5° C. (40 ° F.)
apparatus — Copper beaker, 500 cc, A. H. T.
21,812, E. & A. 750. Buchner funnel (a suitable type
is A. H. T. 28,616, E. & A. .3,254). Filter flask (a
suitable type is A. H. T. 28,248, E. & A. 3,090). Let-
ter press. Vacuum pump.
method — The whole sample of oil after the extrac-
tion of tar acids as in Hn or Hi 2 shall be used. (Note
that this represents 100 cc. of the original oil.) It
shall be placed in the copper beaker and cooled with
stirring to 4. 5° C. (400 F.) in a suitable bath and held
at that temperature for 15 min. The contents of
the beaker shall then be quickly filtered off on the
Buchner funnel and the oil removed from the solids
as quickly as possible. The solid cake shall then be
removed from the filter and pressed repeatedly in a
letter press between strips of blotting paper or filter
paper until only a trace of oil is given up to the paper.
The solids shall then be weighed. Their weight in
grams divided by the specific gravity of the oil gives
the per cent by weight of dry solids.
precautions — To quicken the filtering, a spatula
should be used to press the solids down in the funnel
and avoid channeling.
accuracy — =*= 1 per cent.
TEST Hl8 LIMPID POINT
apparatus — Test tube, 5 in. long by 1 in. inside
diameter. Thermometer reading from 0° to 80 ° as
used in D6. Distillation apparatus.
\n riiorj — Fifty cc. of dry oil shall be taken in a clean
distilling apparatus such as used for naphthas and
light oils and distilled to dryness, no thermometer
being used. The condenser water shall be kept hot
to avoid solidification of the distillate.
The distillate shall be well mixed and 30 cc. trans-
ferred to the test tube. This shall then be cooled,
using a freezing mixture (3 parts of shaved ice to 1 part
of salt) if necessary. During cooling the oil shall be
kept agitated by stirring with the thermometer and
cooling continued until a strong separation of crystals
iken place. The tube shall now be removed
from the cold bath and warmed at the rate of 2° C.
per minute, continually stirrin;;, until all crystals
disappear. The temperature registered by the ther-
mometer at this moment shall be recorded as the
limpid point.
precai riONS If free water should be present in
the oil, this might be mistaken for crystals, hence
dry oil must be u
i ■ -*2° C,
S — The best method to maintain the rise at
20 C. per min. is to place the tube in a beaker of water
or brine 3 ° to 5° C. above the oil temperature and warm
the bath, at about the 20 C. rate.
For oils with limpid points below o° C. a special
thermometer graduated from — 30 ° to 50° C. may be
used. The lowest temperature obtainable by the
above freezing mixtures is about ■ — 20 ° C. If no
crystals separate at this temperature a very small
amount of powdered naphthalene may be added to
seed out the solids. If no separation can be obtained
in this manner, report should be made "no separa-
tion obtainable."
MIDDLE OIL TESTS
The usual tests made are water, specific gravity,
distillation, tar acids, dry salts, tar bases, and limpid
point, and these are made in the same manner as the
corresponding tests given above under heavy oil.
The Barrett Company
17 Battery Place, New York City
THE POLARISCOPE SITUATION AND THE NEED OF AN
INTERNATIONAL SACCHAR1METRIC SCALE
By C. A. Browne
Received August 5, 1918
Among the many claims which are being made upon
industry as a result of the present war there are proba-
bly none more pressing than the demand for certain
kinds of scientific apparatus.
In the sugar industry alone there is a most serious
shortage of polariscopes, refractometers, and colorim-
eters, and with the inability to obtain certain re-
pairs the number of such instruments available for
technical control is constantly growing less.
Seventy years ago practically all of the sugar test-
ing apparatus used in the United States came from
France, and although most excellent saccharimetric
instruments have always been obtainable from that
country, nearly all of the polariscopes used in the
sugar and food laboratories of the United States at
the present time were manufactured in Qermany or
Austro-Hungary. There are several explanations for
this preference for instruments of German manufac-
ture: (i) Since the time of Liebig the technical
schools and universities of Germany have been most
frequented by American students, the result being a
greater familiarity on the part of scientists in this
country with instruments of German origin. (2) At
the time when many of our industries were established
German emigrants were the most available for certain
positions and German methods and apparatus were
thus naturally introduced. (3) German manufac-
turers have been much more active than their French
competitors in bringing their instruments" to the at-
tention of the American public.
With the entrance of the United States into the
present war the importation of scientific apparatus
from Germany and Austria came to an end. Those
who needed polariscopes were thus obliged, as 70
years ago, to turn to France, the birthplace and original
home of this instrument. The optical establishments of
France were so taxed, however, with the manufac-
ture of periscopes, field glasses, gun sights, etc., that
no time could be spared for manufacturing other
apparatus, although the instrument-makers of France
Nov., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
expressed their willingness to supply the needs of
foreign customers as soon as conditions permitted.
In a recent letter upon this subject, addressed to
the writer, the head of one of the oldest establish-
ments in Paris stated that he was most anxious to
bring his polariscopes and other apparatus to the
attention of the American public. He expressed him-
self as even willing to modify the types of his appa-
ratus to satisfy individual preferences, but with one
very important exception, viz., that he should not be
asked to copy or imitate German instruments. This
exception happens, however, in the case of polari-
scopes, to be a very important one, for nearly all in-
struments used at present in the United States are
provided with the so-called Ventzke or German sugar
scale, which requires a normal weight of 26 g. In
this connection the French manufacturer just men-
tioned writes as follows:
II y a de plus la question de la charge type 26 gr. qui parait
adoptee aux Etats-Unis.
M. Pellet, qui s'est servi de 26.04S gr., puis de 26 gr., aussi
bien que de 16.29 gr-. m'assure que 20 gr. est beaucoup plus
commode et que c'est 20 gr. la charge type internationale.
II n'y a pas plus de difficulte pour moi a faire 26 gr. que 20
gr. ou 16.29 &r. — toutes basees sur le meme pouvoir rotatoire du
sucre.
Je suis neanmoins oblige de dire que je n'aimerais pas faire 26
gr., car j'aurais l'air de copier les Allemands. Or ce sont les
Allemands qui en realite n'ont fait que nous copier, car les in-
struments a lumiere blanche aussi bien que les instruments a
lumiere jaune ont ete etudies et construits pour la primiere
fois dans ma maison.
The feelings of national and local pride, which this
manufacturer expresses so openly, are in every re-
spect praiseworthy. The discoveries of Arago, Biot,
Soleil, Laurent, and Duboscq have, without ques-
tion, placed the contributions of France to the science
of polarimetry above those of other nations. Sub-
tract from the sum total of our knowledge in this field
the part which France has contributed and the re-
mainder is pitifully small. In certain particulars,
however, English and German physicists have made
important contributions and nothing is more certain
than that the true scientist in the choice of his instru-
ments will always be guided by expediency and not
by prejudice or feeling. If the user of a polariscope
desires his instrument to be equipped with a Jellet,
or a Laurent, or a Lippich polarizing system, manufac-
turers should meet this wish irrespective of their own
feelings of national or personal preference.
But apart from all this the question raised by the
French manufacturer of substituting an international
scale for the present German standard has at the pres-
ent time a new and more far-reaching importance in
view of the increasing consolidation of interests among
the different allied nations. Leaving aside the fact
that the Ventzke sugar scale is a German invention,
there is much to be said in favor of the United States
and all the other allied nations adopting a standard
which was proposed as long ago as 1896 and which
is known as the international sugar scale.
In 1896, at the Second International Congress of
Applied Chemistry, Sidersky and Pellet advocated
the adoption of a new international sugar scale, the
normal weight of which should be 20 g. Among the
advantages suggested for its adoption are the follow-
ing: (1) The 20 g. scale being a compromise be-
tween the French 16. 29 g. scale and the German 26 g.
scale is free from all national bias. (2) The results
obtained with the 20 g. normal weight are easily con-
verted into percentages by multiplying by 5, while
the results obtained by the French or German normal
weights are not thus easily transformed. (3) Aliquot
portions of 50, 25, 20, 10, and 5 cc. of the 100 cc.
international scale normal solution represent even
gram quantities (10, 5, 4, 2 and 1 g., respectively)
which is not the case with the French or German
standards. (4) The specific rotation of sucrose at a
concentration of 20 g. in 100 cc. (18.62 per cent) is
about the maximum, while it is perceptibly lower at
concentrations above or below this amount. (5) A
20 g. normal weight is always available as a one-
piece unit in the analytical set. The French and Ger-
man normal weights are not always available as one-
piece units and to make up the quantity from an
analytical set of weights is inconvenient as well as
open to error.
No immediate action was taken by the Second In-
ternational Congress upon the proposition of Sidersky
and Pellet, but the matter was again brought up at
the third, fourth, and fifth meetings of this Congress,
more especially by Dupont, who emphasized the state-
ment made by Sidersky in 1896 "that without revolu-
tionizing or disturbing the sugar industry the adop-
tion of the proposed international scale would mark a
decided step in advance. It would remove all the un-
certainties which exist in saccharimetric standards
as well as all the inconveniences and mistakes which
result therefrom, since it would put in the hands of
industrial and commercial sugar chemists analytical
apparatus, whose graduation, being upon an identical
basis, would furnish results that were everywhere
alike."
While the various Congresses mentioned realized
the numerous advantages of the proposed interna-
tional sugar scale the influence of established usage
was too strong to permit its displacing the national
standards then in vogue. The representatives of the
Teutonic nations were particularly opposed to the
replacement of the German normal weight by the new
international standard.
In 191 2, at the seventh meeting of the International
Congress in New York, Bates reported that investiga-
tions conducted at the U. S. Bureau of Standards
showed the present German standard to be inaccurate
inasmuch as 26 g. of pure sucrose would not polarize
100 upon saccharimeters provided with the Ventzke
scale under the prescribed conditions of analysis. A
committee was appointed to investigate the question
and make a report in 1913, but the outbreak of the
war put an end to all further proceedings.
In view of the uncertainty regarding the accuracy
of the present German scale and in consideration ol
the numerous advantages of the proposed interna-
tional scale, the present would seem to be a fitting
time for the adoption of a saccharimetric normal
weight of 20 g. by all the allied nations. The increas-
ing shipment of sugar from
Till: JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. u
o England, Prance, and Italy makes a concerted
of this kind especially necessary just at pres-
ent, and it is all the more desirable in view of the
probability of an economic league in the near future
between the various allied countries. If this could
be done our sugar and food chemists would have at
their disposal a convenient, rational, accurate standard,
while our confreres in France, relieved from the em-
barrassment of having to copy a German scale, would
be free to supply the demand for polariscopes, the in-
creasing shortage of which is becoming at present a
serious detriment in many industries.
An objection which has been urged against a change
in the present sugar scale is that all polariscopes now in
use would be rendered valueless. This objection,
however, as Dupont pointed out at the Fifth Inter-
national Congress of Applied Chemistry, is not a
serious one. Polariscopes can be equipped with the
new scales at little cost and without changing the
optical construction of the instruments. If the ad-
justment of the new scale could be performed by our
National Bureau of Standards the various polari-
scopes of the country would for the first time be placed
upon a strictly uniform basis of comparison. Differ-
ences of as much as o. 3 have been noticed by the author
between the 100° point of different German saccharim-
eters supplied to the American trade.
Preliminary to the adoption of the proposed inter-
national sugar scale a committee of scientists from
the different allied countries should agree upon a con-
stant for the angular rotation of a normal quartz con-
trol plate which shall read 100 ° upon a saccharimeter
whose 100 ° point has been established by polarizing
20 g. of dry, chemically pure sucrose under the pre-
scribed conditions of analysis. When this rotation
value of the normal 100° quartz plate has been estab-
lished for sodium, mercury, or other monochromatic
light, instrument-makers and users of polariscopes
will have an infallible means of verifying the accuracy
of their scales.
If instrument-makers will then show a disposition
to meet the wishes of their patrons in minor matters
of construction there is no reason why the manufac-
turers of the allied nations cannot win for them-
selves a share of the market which heretofore has be-
longed almost exclusively to the Central Powers.
The manufacturers of the United States could find
no better time than the present in which to make
plans for the manufacture of polariscopes, saccharim-
eters, refractometers and other instruments that
were formerly imported from Germany and Austria.
Before entering this field, however, they should make
it their aim to adopt only those standards and types
which are most convenient in the opinion of the
chemists who use them. Heretofore chemists have
been obliged to take what the manufacturer was con-
tent to offer. It is time to reverse this illogical method
of procedure. Let the chemists outline their specifi-
cations and give their orders to the manufacturer who
is most ready to meet them. The writer is already in
consultation with sugar chemists upon specifications
for saccharimeters.
As it will probably be many years before commercial
and scientific relations are resumed with the Central
Powers, it would be the height of folly to wait for the
resumption of such relations before restoring our de-
pleted stocks of apparatus. It is time that we made
ourselves independent of the Central Powers in this
respect as in all others.
Uniformity of standards will make it much easier
for one allied nation to supply the wants of another
and will greatly help towards preserving that spirit
of united action which a common enemy has brought
about. The same intimate cooperation which exists
between the Allies at the battle front will be neces-
sary in the great work of reconstruction that is to
follow. In the recent words of Mr. Lloyd-George.
"Let us not make the mistake of dissolving the partner-
ship the moment the fighting is over."
New York Sugar Trade Laboratory
80 South Street. Xew York City
ADDRL55L5
THE POTASH SITUATION1
w. Stockbtt
In the last year or two potash has been very prominently
before the public, and so much information and misinformation
□ published that it is very difficult 1.. present any new
facts on the subject. As over ninety per cent of all the potash
used before the war was in the manufacture of fertilizer, the read-
ing of this paper before the American Chemical Society
hi somewhat inappropriate.
( inr dependence before the war on foreign sources for an im-
portant element in our food supply may be shown by the ac-
companying diagram.
The writer would Ik- prepared to go even further than the
nd for tin- present have our labor also dependent on a
\irce in the form of interned German prisoners of war.
Tin- prospect of becoming independent of these foreign sources
after the war is promising. Winn tin' nitrogen fixation plants
1 fa held by the Division
of Industrii I Chemical Engineers M the 56th Meeting of the
American Chcmi leveland, September I.1, 1918.
now being erected by the Government are in full working order,
there should be a sufficiency of nitrogen. The development of
our pyrite supply and the establishment of sulfuric acid plants
should insure a supply at reasonable prices. The potash supply-
is the only weak link in the fertilizer chain, and the writer is of the
opinion that it is possible to develop a domestic potash industry.
Food
Fertilizer
Labor
Nitrogen
Phosphorus
Potash
Chilean Nitrates Acid Phosphate German
Potash Salts
Spanish Pyrites
It is well known to every one that before the war the entire
world was dependent on Germany for its potash supply, and
this country was importing annually about 1,000,000 tons of
potash salts of various grades, containing approximately '40,000
tons of K.i '
Nov., 1018
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
919
The enactment of the "Potash Law" by Germany in 1910,
which at one time threatened to become a serious diplomatic
question, first drew attention to our entire dependence on
Germany for a very important element of plant food, and in
191 1 Congress made an appropriation for investigating our
own sources of supply. It was not, however, until Germany
put an embargo on the exportation of potash salts in January
1915, that the question became acute, and a serious attempt
was made to develop our domestic sources.
The year 1915 may bz said to have marked the beginning
of the American potash industry, as in that year a little over
1,000 tons of K:0 were produced. This was increased to 9,720
tons in 1916, to over 32,000 tons in 191 7, and it is probable
that the production for the present year will reach 60,000 tons
of K2O.
At the present time over 60 per cent of the total is being ob-
tained from natural brines, principally Searles Lake, California,
and the lakes of Western Nebraska. The Desert Basin and
Death Valley have long been names that appealed to the general
public as probable locations of immense deposits of potash.
These districts have been carefully examined by the U. S. Geo-
logical Survey, and as a result it may be stated that Searles
Lake is the most promising individual source of potash at pres-
ent known in this country. The extent of this has not been
definitely determined, but it has been estimated to contain
from 10,000,000 to nearly 20,000,000 tons of K;0, which would
be sufficient to meet the entire requirements of this country
for from 20 to 40 years. Two companies are operating here
and one of them, the American Trona Corporation, is said to
be the largest individual producer of potash in this country.
The eventual capacity of this plant may reach 75,000 to 100,000
tons of K2O per year. The brine from the lake is treated by
evaporation at Trona, on the edge of the lake, and it is intended
to ship the crude salts thus obtained to the refinery at San Pedro
on the coast. The brine is of a somewhat complex composi-
tion, and the successful treatment of it commercially was an
interesting problem for our chemists. Borax and soda, and
possibly salt as well, will be produced, and this should assist in
enabling this plant to continue operations at a profit when the
price of potash becomes normal. The geographical location
of Searles Lake is very unfortunate, as more than 90 per cent
6f the pre-war supply of potash was used east of the Mississippi
River. A low ocean freight rate via the Panama Canal would
be an important factor in competing with foreign supplies.
The Nebraska lakes are at present supplying nearly half of
the total amount of potash produced. These comprise a num-
ber of lakes, usually of small extent, located in the sand-hill
region of the State They usually consist of a shallow lake of
brine, with a bottom of muck and hardpan, underlain by a sand
impregnated with brine similar in composition to the lake
waters. This is the principal source of the potash. It has not
been found possible to make an estimate of the total potash
content of these lakes, but it has been stated by the Director
of the Nebraska Conservation and Soil Survey that with the
plants now producing and building, the stores of high-testing
brines would be greatly reduced within four years. One of the
lakes that had been pumped dry has since filled up again, and
it is claimed that there was no decrease in the grade of the brine.
It may be. therefore, that the life of these lakes "ill be consid-
erably prolonged and this is very much to Ik- desired, as this
source of potasli has so far been the foundation of the domestic
supply. The district is handicapped by its geographical loca-
tion, entailing high freight rates to the point-, of demand. It is
probable that eventually a central refining plant will 1"
and by producing a very high-grade product, fn
unit of K20 could be reduced by one-half
The giant kelps of the Pacific Coast ranked set 1 1
of supply in 1917, having produced 11 per cent of the total lor
that year. As tin. source is being described by Mr. Turren-
tine it will not be further dealt with here, except to point out
that it would be almost impossible to locate a source that is
further from the principal centers of demand, as the Pacific
Coastal states, including Hawaii, use less than 2 per cent of the
normal supply of potash.
A little over 2,400 tons of K20 were produced from the alunite
deposits near Marysvale, Utah. This was mostly in the form
of a high-grade sulfate 97 per cent pure. The alunite is crushed
to about >/s in. mesh, and roasted in a rotary kiln, using pul-
verized coal as fuel. The calcined material is leached with
' hot water in a closed tank at a temperature equivalent to 60
lbs. steam pressure, which takes the potassium sulfate into solu-
tion. The solution is filtered in a Kelly filter press, and the
clear filtrate is then evaporated in Swenson triple-effect evapora-
tors, and the resulting crystals centrifuged and sacked for ship-
ment. No estimate of the cost of production is available, but
unless it is possible to utilize the alumina in the residue, which
is not being done at present, it does not seem that potash can
be produced from this source at a profit at normal prices. In
Bulletin 451, published by the Bureau of Soils, entitled "The
Recovery of Potash from Alunite," by Messrs. Waggaman and
Cullen, the possibilities of obtaining both alumina and sulfuric
acid, as well as potash, is discussed, and it was estimated that
this should be very profitable at present prices, and possibly
at normal prices also. Calcined alunite, containing 15 per
cent of KoO, has also been marketed in small quantities for use
in fertilizers, a^ it has been found by experiment that this is as
effective per unit of K2O as the soluble sulfate and chloride
salts. If a deposit of alunite could be discovered in the East
near the centers of demand for fertilizers, it is probable that
this calcined product could be produced at a profit at normal
prices, but with the location of the present known deposits, the
high freight rate per unit of KoO will be prohibitive.
In the opinion of the writer, the dust from the cement kilns
is probably the most promising source of a permanent domestic
potash supply. As the result of a careful investigation by the
Bureau of Soils, it has been estimated that the maximum amount
of potash that might be recovered from all the cement works
in the country would be 100,000 tons of K>0.
It is not probable that this figure will ever be reached, as some
plants do not have sufficient potash in the raw mix to make
its recovery profitable, and others for various reasons would
not find it advisable to install plants. It does not, however,
seem unreasonable to expect that the amount from this source
should reach 50,000 tons of K2O per year, which is 20 per cent
of our normal requirements. The geographical position of the
cement industry is exceptionally fortunate, as approximately
70 per cent of the total amount of cement manufactured is pro-
duced east of the Mississippi, and this region consumes approxi-
mately 90 per cent of the normal supply of potash. The first
cement plant to recover potash from this kiln dust was the
Riverside Portland Cement Company, of California Owing
to litigation with the fruit growers in the vicinity, who claimed
that the line dust escaping from the kilns was causing damage
to the fruit trees, tin company was compelled to take steps to
abate the dust nuisance. A Cottrell electrical precipitation plant
was installed, and when the dust thus collected wis analyzed,
it was found to contain about [O per cent of KsO, o that at present
prices of potash this is a very profitable part of tin- plant, The
installation was completed early in mi.!, anil has been in con-
tinuous anil successful operation eva since, so that ti"" > no
1 uiv question about the practicability of this method
By the end of tins \e;u there will be about a dozen cement
plants recovering potash from the kiln dust, with a probable pro-
luctioo ] • to 13,000 tons of K-i 1 pel \ eat 1 to
of tin maximum amount of potash and its concentration from
tie 'in, dust involved some very interi sting chemical problems,
which appeal to havi been luccessfully solved. P
figures show that potash can be produced profitably from this
•920
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. n
source for 50 cents per unit of KjO, which should insure the
permanence of this source of supply under any conditions.
Another source which has even greater possibilities than the
cement plants, although up to the present but very little has
been done, is the dust from the blast furnaces manufacturing
pig iron. Mr. R. J. Wysor made some investigations and ex-
periments at the plant of the Bethlehem Steel Company, and
it was found that with the Cottrcll electric precipitation, prac-
tically all the dust and fume entering the treater could be pre-
cipitated successfully. In many cases the iron ore used in
manufacturing the pig iron contains sufficient potash to make its
recovery profitable, with the additional great advantage of
cleaner-gas for use in the stoves and boilers. .The amount of
potash available from this source has not been definitely esti-
mated, but it is probable that it would be from 200,000 to 300,000
tons of K2O per year.
As far as the writer has been able to learn, there is at present
only one plant being installed at any of the blast furnaces for
the recovery of potash. All of the manufacturers are at present
so intent on producing the maximum amount of pig iron that
there is very little possibility of getting them to realize the im-
portance of developing a domestic potash industry.
Another source which promises a small but permanent sup-
ply is the waste from distilleries where molasses is used to pro-
duce alcohol. This source ranked third in 191 7, with a produc-
tion of 2,800 tons of K2O. Recent improvements in methods
are claimed to have reduced costs and increased' the potash ex-
traction, and as this is practically a by-product it is probable
that potash can be produced at a profit after the war.
There are some thirty or forty small producers of potash
from wood ashes, mostly in Michigan and Wisconsin, but the
total amount from this source is only about 400 tons of K2O
per year, and it is not probable that they will be able to continue
operations under normal prices.
The greatest potential sources of potash are the potash-rich
silicate rocks, and of these the most promising are the green-
sands or glauconite of New Jersey, the Cartersville slates of
Georgia, and the leucite rocks of Wyoming. Any one of these
sources would be capable of supplying our entire requirements
for many centuries. Many patents have been issued in the
last fifty years for methods of extracting potash from these
silicates, but no general commercial process has yet been de-
veloped. Several companies have been experimenting on the
greensands on what may be called a commercial demonstration
scale, and claim that under normal conditions they will be able
to produce potash at less than $1 per unit of KjO.
Another company is operating on a small scale on the Carters-
ville slates, and producing a material containing 4 per cent of
water-soluble KjO, which is being used locally as a fertilizer.
Experiments have also been carried out on the leucite rocks,
which give promise of being successful.
There are several million tons of tailings from the gold mines
in the Cripple Creek district of Colorado, averaging about 10
per cent of K5O. These are already finely ground and are close
to transportation and supplies. Experiments have also been
made with these, but so far without success.
The development of a commercially successful process of
treating the silicate rocks would solve the potash question
permanently, and this problem should not be beyond the skill
of our chemists and metallurgists.
In conclusion, the writer is of the opinion that the sources of
potash already discovered are sufficient to supply the require-
ments of this country, if sufficiently developed. He also thinks
the prospects of this development are favorable, but it will proba-
bly require some kind of assistance by the Government. This
might perhaps best be done by subsidizing the domestic industry
to a suitable degree. In this way, the cost to the Government
would be moderate and the expense would be distributed, and
it would thus be possible to break the German monopoly with-
out placing a hardship on any particular class.
U. S. Bureau op Mines
Washington. D. C.
RUSSIA'S PRODUCTION OF PLATINUM1
By Albert R. Merz
Received September 23, 1918
Russia became the chief center of the production of platinum
soon after its identification as a product of the Urals in 1823.
Exploitation began in 1824. Previous to this time Colombia,
then having an annual production of approximately 16,000
ounces, had been the only purveyor of platinum to the world's
market. For a few years the production of Russian platinum
was in quite small quantities and obtained as a by-product in
the washing of gold-bearing sands, but as acquaintance with
its value grew and sale was found for it, the output gradually
increased.
In 1827 the Russian Minister of Finance, Count Egor Frantso-
vich Kankrin, wishing to increase the yield of platinum and to
furnish the government with an important source of income,
proposed the coinage of platinum. This was approved by the
Czar and coinage was instituted in 1828. Simultaneously
with the introduction of platinum money the government pro-
hibited the export of platinum abroad and also imposed a tax
of 10 to 15 per cent on its production. This tax which was in
kind was not, however, burdensome to the Russian platinum
producers for they used the labor of serfs in working the mines
and in consequence the cost of securing the platinum was very
little. The price paid by the government to the producers was
fixed at S4.21 an ounce.2
The first year after the realization of the measure providing
for the coinage of platinum the output rose to over 50,000
ounces and in 1843 it reached 112,571 ounces. In 1S45 the
coinage of platinum money and the purchase of the metal by
the treasury were discontinued and the restrictions on its use
for other purposes were removed.
In all, for the 18 years (1828-1845) there were coined 453.014
ounces of platinum. After the discontinuance of coinage in
1845 the government began gradually to withdraw from cir-
culation the money which had been issued and secured about
So per cent of it. The Russian platinum industry left thus
upon its own resources was for a time benumbed and the annual
production dropped to less than 1,000 ounces.
With the end of the fifties the production of platinum began
to develop anew and in 1S62 the output reached 75,060 ounces.
In 1859 the mint had accumulated a stock of platinum amounting
to 472 706 ounces, of which 234,412 ounces was in coin. Sales
of the metal had been made in small quantities to the Parisian
manufacturer, Quennesen, and to others, but in 1862 the en-
tire quantity remaining in the treasury was sold to the London
firm of Johnson, Matthey & Co., refiners to the Bank of Eng-
land, after which the tax in kind was revoked. The consump-
tion of platinum meanwhile continued to grow with each year
and parallel with this increasing consumption the quantity of
platinum secured in the Urals also increased so that in the
closing years of the 19th century it attained to 130,000 to 190,000
ounces annually, approximately 90 per cent of the world's
total annual output. Simultaneously with this growth in pro-
duction there arose among the big foreign platinum dealers a
desire to seize control of the platinum industry, and companies
were formed abroad who monopolized the Russian industry and
fixed according to their own whim the price of the metal. The
price from this time on began to be subject to violent fluctua-
tions though the average gradually increased. The complete
> Prepared as a part of the work on platinum in the course in chemical
economics and statistics at George Washington University.
« On the basis of 1 ruble equivalent to 77 cents. The value of the
Russian ruble was changed from 77 to 51 cents by a law promulgated on
September 10 August 29 of the year 1897.
Nov., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
lack of stability in price and the uncertainty of sale placed the
independent Russian producers in a most irksome position and
deprived them of the possibility of making expenditures for ex-
plorations and for the development of technical improvements in
the working of their deposits. As a result, the production of
platinum by the independent and smaller producers has been
greatly reduced. The yield of platinum since the beginning of
the present century has consequently had a downward tend-
ency.
The platinum beds of Russia which have a commercial im-
portance are not only all located in the Ural Mountains, but they
are concentrated in a very limited territory. These beds are
alluvial in character and consist of placers formed from the de-
struction of the mother-rock containing the platinum. These
placers are likewise auriferous and are associated with certain
olivine rocks called dunite.
At the time of the outbreak of the war in 1914 the greatest
proportions of the platinum output in the Urals were secured in
the Nizhne Tagil and Isov districts. The beds of the first
district are found, for the most part, on the west slope of the
Urals, while those of the second are distributed along its eastern
slope and can in turn be divided into two districts, the Goro-
blagodat and the Bisersk. Besides these there has been in
comparatively recent years a development of production in
the northern Urals in the Nikolae-Pavdinsk and the Rastes
districts, and also in the mines of the Sysertsk mining dis-
trict.
In the Isov district the production of platinum is concen-
trated in the rivers and channels composing the system of the
River Is. To the north of this region, towards the borders of
the Rastes and Nikolae-Pavdinsk districts, platinum is furnished
by the Sosnovki, Kytlymi, and Mala Kos'va Rivers. Platinum
is obtained together with gold still farther to the north on the
left tributary of the Vagran and on the system comprising
the rivers Lobva, Nias'ma, Lialia, Aktai, Emekh, Talits, and
others; here the platinum is met with in subordinate quantities
with gold and it is similarly obtained on the Mala Kos'va; more
to the east of the above- designated districts it is secured in the
placers of the Ivdevl River.
To the south of the Isov area in the region of the Baranchinsk,
Verkhne-Turin, and Nizhne-Turin works, platinum mines are
worked on the tributaries of the Tagil River and on the Imiann
and Tura Rivers, as well as on the tributaries of the Salda
River.
In the boundaries of the Nizhne-Tagil district the richest
placers are found in the valleys of the Visim, Mart'ian, Sisim,
Chaush, Cherna Rivers, and others. Farther to the south there
is observed a disappearance of the reliable platinum beds and
they are met with after that, together with gold, in the placers
of the Nev'ian, Verkhne-Iset, Bilimbaev, Alapaev, Sysert,
Kyshtym, and Mias areas and also on the Tanalyk, Sakmar,
and Urtazym Rivers. In many placers of the southern Urals
platinum is replaced by other metals of the platinum group,
principally osmiridium.
The placer deposits of platinum cannot be distinguished in
any way by their manner of occurrence from those of gold and,
besides, in many cases the placers contain both precious metals
simultaneously. As a consequence of their mode of occurrence
the platinum placer mines are worked by methods differing
but little from those employed in the exploitation of the gold
placers.
As has already been indicated, the world's requirements for
platinum have been almost entirely supplied by Russia from
early times, and in 1914 that country furnished all but 7 per
cent of the world's production for the year. In Table I there
is given the annual production of platinum in Russia from the
first year of the exploitation of the platinum (1824) to the year
1915:
Year
1824
Table I — Production at Crude Platinum in Russia
Troy ounces
1,066
1826
7,120
'
1827
13,571
1828
50,111
1929
41,457
1830
56,088
168
34 7
1831
56,891
1832
61,394
1833
61,749
1834
54,561
1835
55,509
290
104
1836
61,973
1837
62,520
1838
64,291
1839(a)
49.500
1840
49,360
287
644
1841
57,398
1842
64,106
1843
112.57.1
1844
52,128
1845
24,878
311
081
1846
619
1847
632
1848
1,053
1849
4,964
1850
5,079
12
54:
1851
6,135
1852
8,677
1853
32,402
1854
355
1855
513
48
082
1856
757
1857
4,065
1858
5,444
1859
29,413
1860
32,380
72
059
1861
55,454
1862
75,060
1863
16,084
1864
12,770
1865
73,123
232
491
1866
56,129
1867
57,399
1868
64,560
1869
75,310
1870
62,649
XIA
Year
Troy
ounces
1871
65,918
1872
48,974
1873
50,688
1874
64,770
1875
49,603
279
953-
1876
50,670
1877
55,504
1878
66,529
1879
72,809
1880
94,744
340
256
1881
95,982
1882
131,293
1883
113,666
1884
71,952
1885
83,316
496
209
1886
138.785
1887
141,721
1888
87,361
1889
84,746
1890
91,461
544
074
1891
136,204
1892
147,032
1893
163,963
1894
167,481
1895
141,936
756
616
1896
158,522
1897
180,105
1898
193,452
1899
191,701
1900
163,624
887
404
1901
204,850
1902
197,267
1903
193,225
1904
161,270
1905
168,416
925
028
1906
185,756
1907
173,587
1908
157,787
1909
164,594
1910
176,331
858
055
1911
185,617
1912
177,467
1913
157,731
1914
157,178
1915
119,789
797
782
7,630
761
The actual production for the first half of 1839, ac-
quire du Journal des Mines de Russie, was 26,047 oz.
nn gives 1,505 kg., equivalent to 48,387 oz., as the entire production
of platinum in Russia in 1839, but the writer has been unable to find his
authority for this figure.
The figures for this table were obtained from official statistics
of the Russian government with the exception of the value for
the year 1915, which was secured from "Mineral Industry,"
and this value is stated to have been taken in its turn from
official figures.
The total yield of crude platinum according to these values
from 1824 to 1915, inclusive, amounted to 7,630,761 Troy ounces.
This aggregate yield, however, should really be increased to
approximately 9,500,000 ounces, for the official data fail to give
the total production at the mines because a portion of the actual
output was stolen by the miners and another portion was con-
cealed by the producers to avoid the payment of tax upon it.
Estimates of the amount thus not officially accounted for vary
considerably and by some it has been placed as high as 60
per cent of the production officially announced. The value
usually quoted is 25 per cent.
The values for production given in Table I are shown graph-
ically in Fig. 1.
The most salient characteristics of this curve together with
their probable causes may be mentioned. First, there is to be
noted a sudden rise of the production curve in 1828, the year in
which coinage was commended. The curve continues high until
1843, when it reaches a pronounced peak which is accentuated
by the sudden drop through the years 1844 and 1845 to the
minimum of 1846. In 1843 the question arose whether the
coinage of platinum should be suspended. Before making a
definite decision on this question it was determined to continue
the coinage of platinum two years, but only in such quantity
as to take the output obtained by the platinum producers up
THE JOURNAL OF IS DUST RIAL AND ENGINEERING CHEMISTRY Vol. ro, Xo. n
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to April i, 1S44. The producers were also informed that the
platinum obtained after that date could not be accepted by the
government. In 1^45 complete suspension of the coinage of
platinum was brought about by an imperial ukase of date
June 22. The platinum industry now fell into such a state of
decline that whereas there had been an annual production of
50,000 ounces or more the yield of the metal was reduced to
that obtained as a by-product of gold mining.
The slow rise in production from the minimum for 1846 was
again brought to an abrupt end in 1853 with the commence-
ment of the Crimean War. During the years of this struggle
which continued till 1856, the annual production became less
than at any period in the history of the Russian industry. The
extent to which the platinum industry had become dependent
upon French and English purchasers is very forcibly brought to
view. Other mining industries of Russia not thus dependent
failed to show any such decrease in production for these years.
Thus the yields of gold, silver, and copper for the years 1852
to 1857 were as follows:
Gold
Silver
Copper
Yi;ak
Ounces
Ounces
Short tons
1852
719,796
559,892
7,413
1853
770,828
539,130
7,143
1854
840,886
555,495
7,056
1855
868,627
549,281
6,836
1856
871,853
545.818
6,848
1857
912,984
557,273
6,102
The year 1859 marks the commencement of a rapid rise in
the production of platinum. Two causes apparently had an
influence in bringing about this upward turn. First, there was
an increased demand for the metal due to the introduction of
Deville and Debray's process in the manufacture of platinum
vessels and other ware which considerably lowered the cost of
production of such manufactured ware Second, there was the
effect of the appointment of a commission by the Crown in [859
for the purpose of considering the advisability of again coining
platinum. This commission in [862 recommended that coinage
be again instituted. It is to be noted that the emancipation
of the serfs, which in 1862 had a very depressing influence upon
practically all the mining industries of Russia, had apparently
no effect upon the production of platinum.
The chasm-like gap in the curve which appears for the years
1863 and isii) snius to have had a numbei "I causes. The
intention to again coin platinum was definitely abandoned in
1863 There was also a lessened demand for platinum in for-
eign countries brought about bj pool trade conditions and war,
Production of Crude Platinum in Russia, 1824-1915
and an accumulation of unsold and unpurified metal in the hands
of the producers.
The minima for the years 1866 and 1S75 were probably the
consequences of the financial panics in England during those
two years.
In 1877 Johnson, Matthey & Co , who had up to this lime
controlled the greater part of the platinum trade, increased the
price which they had been paying for the crude metal and the
effect of this advance in price is seen in another upward shoot
of the curve. Demands on the supply of platinum for use in
the manufacture of incandescent lights and for other electrical
appliances now began to have a marked influence on the plat-
inum market.
The decreased production for the years 1S83 to 1885 was the
result of the exhaustion of some rich deposits of the metal by
intensified working in 1882
The diminished production for the years 1888 to 1890 has been
attributed to the drafting of employees in the Urals by the
Russian government for the building of the Trans-Siberian Rail-
way. This is claimed to have depleted the mines of laborers
and made it difficult to keep up the usual output. Unfortu-
nately the writer has been unable to secure official figures of
the number of workers engaged during the years 1885 to 1887
in producing platinum for comparison with the number of
those similarly engaged during the years in question. A com-
parison of the number of persons employed 111 the recovery of
platinum during the years 1882 to 18S4 with the number thus
engaged for the years 1888 to 1890 does not tend to confirm this
claim. The numbers of employees for the years compared are as
follows:
Year Workers Vicar
1882
1883
1884
Workers
4.959
( Mlicully the decrease in output for these years was assigned
to a diminution in the number of active mines in the Goro-
blagodat mining district where there were but 69 mines ill 1888
against 83 in [887. The quantity of sand washed was smaller
in consequence and the content of platinum in the sand had
also decreased. The main cause of the fall in output appears
to have been the diminution in richness of the platinum sands
washed for the first two years and of the quantity of sands
washed for 1890.
Nov., 1018
THE JOURNAL OF INDUSTRIAL AXD ENGINEERING CHEMISTRY
023
It is stated that in 1S95 long-continued rains did not permit
washing through the whole season and production was there-
fore reduced. Certainly a lower content of platinum in the
sands washed contributed to the decrease in the yield.
The year 1898 was an important one for the Russian platinum
industry, as it was marked by the establishment of the "Societe
Anonyme d'Industrie du Platine" in Paris, which began to
purchase mines, to lease others, and to enter into long-term
contracts with the proprietors of the largest placers, whose
mines it was unable to buy for the purchase of their entire
output. It thus gradually secured control of the greater part
of the platinum industry. The production of platinum as
well as the refining of the metal now fell almost entirely into the
control of foreigners.
Floods in 1900 are said to have caused the decrease in output
for that year. The following year is distinguished by the max-
imum yield for any year of the industry in Russia.
The richness of the platinum deposits continued to decrease
and in order to secure a given quantity of platinum, greater
quantities of the lower grade sands had to be washed. In the
early years of the 20th century dredges were introduced in the
valley of the River Is, where the most productive placer deposits
occurred. There were, however, but few of these used and hand
washing continued to be the main method of working the sands.
In 1909, it is said, four dredges delivered about 13 per cent of
the total production and the next year about 20 per cent of the
entire output was recovered by dredges or other mechanical
excavators. In 1914 about one-third of the platinum produced
was secured by modern methods of working.
The Russo-Japanese war in 1 904-1 905 is claimed by a num-
ber of writers to have caused a curtailment of production on
account of the drafting of many of the Ural miners. Also the
internal disturbances which arose in Russia immediately after-
wards are claimed to have had a like influence. A study of the
official figures relating to the period in question does not bear
out such statements. The chief factor influencing the varia-
tions in annual output from the commencement of the 20th
century through 1906 seems to be the content of platinum in
the sands washed. Thus, in spite of the two causes above
claimed as responsible for the drop in 1 904-1 905, the number
of mines, the number of miners employed in producing platinum
alone, and the number of tons of sands washed, all had upward
tendencies.
In Table II are contained statistics of the number of deposits
worked, the number of miners employed, the number of tons
of sand washed, and the yield of platinum per ton of sand, so
far as^they could be obtained.
Table II — Statistics of the Platinum Industry of Russia
Sand Washed Wt. of Platii
Year
1864
1865
1881
1882
1883
1884
1885
1886
1887
1888
1889
1890
1891
1892
1893
1894
1895
1896
1897
1898
1899
1900
1901
1902
1903
1904
1905
1906
1907
1908
1909
1910
4,95')
5.461
5,853
'. , 1 20
8,061
7,234
5,546
5,628
B,0S0
8,034
9,197
1,763
2.025
1,803
2.699
3,066
3,292
787
555
864
1,587
Tods
16.445
112. 530
271.514
363,437
276,164
352, 138
313,974
415,951
1.115,409
1 ,062,746
1,213,122
854.688
1 ,588,665
1,723,084
1,729,247
1.904,032
J. 67 1 ,242
3.148.221
749,657
776.71.'
644,942
1.084.18'.
I ,805,462
238,682
W5.9I4
289,776
999,176
Grains per Ton
From 1906 on the number of miners and the quantity of sand
washed is given for only those mines where platinum alone is
produced.
As has been previously stated, the refining of platinum has
been almost entirely in foreign hands and consequently the
crude platinum with the exception of a very small quantity
has been exported from Russia to be refined in other countries.
The small amount refined in Russia was that required for local
consumption. The largest platinum refining works was formerly
that of Johnson, Matthey & Co., in London, but Heraeus &
Co., of Hanau, Germany, early in the eighties, took the lead
from that company and maintained it into the 20th century.
Since the establishment of the Societe Anonyme d'Industrie
du Platine, its platinum refinery in Paris has refined most of
the crude platinum produced in Russia. As a result of foreign
control, the prices of crude platinum were subject to much specu-
lation which had a very unfavorable reaction upon the condition
of the Russian platinum industry. In view of this a law pro-
posed by the Ministry of Trade and Industry was enacted, of
date Dec. 20, 1913, which placed a prohibition on the exporta-
tion of crude platinum and provided for the establishment of a
refinery' in Russia. All the platinum in the country was sub-
ject to strict registration which made impossible the secret
sale of the metal to foreign buyers. As a result of this, the
position of many platinum producers became extremely em-
barrassing since they were unable to realize on their stocks of
platinum in view of the limited consumption of the metal within
the country^. The State Bank in order to relieve the distress
of these producers issued loans to them on the platinum that
they held.
The prohibition of export was found to be in conflict with
certain international treaties and it was then determined to
place an export tax of 30 per" cent ad valorem on platinum from
July 1915, the price of the crude metal to be fixed by the Coun-
cil of Ministers.
Year
1861
1X1, j
1863
186+
1865
1866
1874
1875
1876
1878
1880
1881
1882
1883
1884
1885
1886
1887
1888
1889
1890
1891
1892
1893
1K'*S
1896
1897
1898
IK' I' I
1900
1901
10
1904
190J
1908
1909
1910
iwi 1
19J I
1914
I'M !
Table III — Exports of Pl
Great
Britain France Germany
9.840
6,596
20,025
22,304
33,310
36,905
10,533
17 ,37'i
23,699
13,693
18,433
from Russia to
Austria-
Hungary
31 .941
99.299
76,891
76,364
30,545
14.746
14.74'.
26, J32
26.859
20.539
6,846
[2 09
9,480
61 .'.IK
10,533
10,006
1 ,053
1 ,580
1 ,053
7,373
527
11 . 599
125.869
...
127.44'!
135,875
I 10,61 S
1 01
27,386
54 . 245
137.455
124,815
1 38 . 509
113,756
102.17(1
99,536
71,097
..mi
!6,859
■■..,
86, 170
12,640
13,705
4X.'I7X
14.74'.
53, 19
101 , 1 16
51 ,612
50,558
58.458
13 , 693
Total
30,546
25.806
6.464
30,019
6.596
22,383
22,304
65,251
136,204
87,424
94,796
154,834
34,759
43.185
24,752
31,072
48.978
57,931
68.991
152,728
152.201
164,841
120,602
134,295
109,016
99,536
117.443
71,097
57,404
I 19,568
151,148
144,302
1 10,069
17,399
40,552
61.618
61,618
156. '141
175,900
80 050
924
THE JOURNAL OF INDUSTRIAL AXD ENGINEERING CHEMISTRY Vol. 10, No. n
In Table III is given the quantity of platinum exported from
Russia and the countries to which it was sent for those years
for which statistics were obtainable.
A study of this table yields some interesting and even sur-
prising information in view of the fact that the literature is
everywhere permeated with statements indicating that first
Johnson, Matthey & Co. and then the French "Compagnie
Industrielle du Platine" monopolized the refining of Russian
platinum and were absolute masters of the market. A summa-
tion of the exports of platinum from Russia to France, England,
and Germany for the years 1863 to 19 15 (data for 7 years miss-
ing) shows that France received 1,245,392 ounces, England
1,448,384 ounces, and Germany 2,279,280 ounces. The total
exports for four of the seven years for which detailed informa-
tion is lacking are less than 150,000 ounces and those for the
remaining three years are certainly not more than 250,000
ounces. Therefore, and since Germany undoubtedly secured
a large share of this platinum also, the above sums would not
be vitally affected by the missing data. We find, then, that
the Germans actually received more platinum than the French
and English monopolists.
Dividing the period 1863-1915 into five subperiods, we have
the exports for each of these given below:
France
England
Germany
Years
Ounces
Ounces
Ounces
1863-
-1880
3
555
512
005
212
717
IKK1
-1890
0
167
999
792
079
1891
-1900
14
220
437
645
649
356
1901
-1910
676
217
259
111
446
1)94
1911
-1915
551
400
71
624
178
534
1,245.392 1,448.384 2,279,280
It is seen from these figures that Germany received more plat-
inum from Russia than England did during each of these periods,
except the first, and though its importations for the last two
periods were exceeded by those of France that it nevertheless
secured over 28 per cent of the total exports even then.
As already stated, the literature contains numerous refer-
ences to the "monopolies" of the English and of the French
and it is interesting to note in this connection that even the
official Russian publication prepared for the World's Columbian
Exposition at Chicago has, in an apparent endeavor to foster
this impression, reversed the exports to England and Germany
for the years 1885 to 1890 in its table of exports for the years
1884 to 1890.
A
1
""" -4 \
*4 ^
it
ft
I -, I ~\ t
'— ll J fc^ 3 L ,
* B3 J M V t I
t-?- I JH C A I
- t t t L_n
Xt- A ^V
^A-^'' ^
^HT
Fig. 2— Exports of Platinum from Russia, 1861-1915
The annual exports of Russia are shown graphically in Fig. 2.
It is to be noted that the curve is subject to quite pronounced
fluctuations and therefore it is necessary to take a more or less
long period of time for the determination of the relation of
export to production of platinum.
Taking the period from 1882 to 1914 for this purpose, we find
that the quantity of platinum exported amounted to 83 .4
per cent of the production. It must be considered also that
official statistics on the export of platinum abroad for the period
in question gave figures considerably lower than the actual
export as part of the platinum was sent abroad by mail and
baggage and thus escaped registration.
Making a more detailed study of the production of platinum
in the Urals, we find that the output for the 5 years 1910-1914
was divided as follows:
District 1910 1911 1912 1913 1914
South Verkhotur 111.070 121,314 118.048 102.552 106.528
Perm 46.068 46.885 38.709 36.878 38,050
North Verkhotur 11,862 11,362 13.166 11.376 7.426
Cherdyn 6,359 5,016 6.162 6.109 4.753
South Ekaterinburg 972 1.040 1.382 816 421
176.331 185,617 177,467 157.731 157.178
We see from an inspection of the above table that for the
year 1914 the South Verkhotur district produced 67.8 per cent
of the total production, the Perm district 24.2 per cent, the
Xorth Verkhotur 4.7 per cent, and the remaining 3.3 per cent
were obtained in the Cherdyn and the South Ekaterinburg
districts.
In the South Verkhotur and Perm districts there are great
enterprises which use dredges in working the platinum placers.
These are able to work the placers with a low content of plat-
inum. The working of the majority of the small and medium-
sized mines, however, is carried on by very primitive means,
especially by the help of "starateli" or tributers.
The Iuzhno (South)-Verkhotur district takes first place in
the production of platinum. The greatest quantity of platinum
is obtained here on the Xizhne-Turin, Verkhne-Turin, Kushvin,
Baranchin, and Znamen areas of the crown lands where in 1913
there were 136 mines yielding 55,772 ounces of platinum. Next
comes the areas of the Xizhne-Tagil possessional district be-
longing to the heirs of P. P. Demidov, where 6 mines gave a
yield of 42,409 ounces. Finally, on the lands of the peasant
proprietors, 89 mines in the Visimo-Shaitan, Cherno-Istochin,
Xizhne-Turin, and Verkhne-Turin areas furnished 4,371 ounces.
The decrease of yield in this district in 1913, in comparison
with 1912, is explained by (a) a curtailment of the production
of the Demidov mines by about 3,500 ounces in conjunction
with the unfavorable condition of the platinum market, (6)
a decrease in yield of the mines situated on the peasant owner
lands by approximately 500 ounces, and (c) a fall in production
of the mines of the crown lands, chiefly those of the Societe
Anonyme dTndustries du Platine, by about 11,500 ounces.
About one-third of the platinum produced in the district is
secured by dredging while the remainder is obtained by hand
labor, partly by the work of starateli.
In 191 4 the yield of platinum in this district again rose and
reached 106,528 ounces, which is explained by an increase in
the number and the production of the mines on the peasant
lands. The number of mines increased from 89 to 134 and their
output from 4,371 ounces to 15,786 ounces. In spite of an in-
crease in the number of mines on the crown lands their produc-
tion decreased by 7,557 ounces. Altogether there were 296
mines worked in this district in 1914, 65 more than in 1913.
The Perm district takes second place in respect to the quantity
of platinum produced. The precious metal is obtained here in
the Krestovozdvizhen ("Erection of the Cross") mines belong-
ing to the company "Lys'venskii Mining District of the Heirs
of Count P. P. Shuvalov." Notwithstanding that some of the
mines were worked by means of dredges, endless chain elevators,
Archimedean screws, and other improved apparatus, almost
80 per cent of the platinum was secured in 191 4 by hand work-
ing, and one-third of the production was secured by starateli.
In the five-year period, 1909-1913, the output of the Kres-
tovozdvizhen mines fell continually. The growth in output
for 1914 was caused by an increase in the production of three
dredges and the introduction of steam shovels. Of the entire
quantity of platinum acquired in 1914 (38,050 ounces), 8,150
ounces were gotten by the help of dredges and 29,900 ounces
by hand labor.
In the Sievero-Verkhotur (Xorth Verkhotur) district platinum
was produced in only 9 mines; in the Xikolae-Pavdinsk district,
Nov, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
925
"Versts
Map op the Mining Region op ths Urals (Copied fr
Russian Map)
Borders of governments — Rivers
Railroads Platinum mines —
in 3 mines; in the Iuzhno-Zaozer district in 1 mine; in the Lialia
crown area in 1 mine; in the Znamen crown area in 3 mines;
and there was 1 mine on the land of the peasant owners. The
decrease of output for 1913 and 1914 for this district was caused
by the curtailment of work by the starateli since they have been,
in the places formerly worked by them, gradually replaced by
dredges. ' Thus the yield of platinum diminished by 3,950
ounces in 1914. This decrease fell entirely on the mines of the
Nikolae-Pavdinsk district, where in the beginning of operations
for 1914 the work of starateli was stopped altogether. These had
formerly produced most of the platinum obtained. Dredges ob-
tained 2,370 ounces of the platinum output in this district in 1914.
In the Cherdyn district are located the mines of Prince Aba-
melek-Lazarev, which are situated on the Mala and Bolshaia
Kos'va rivers (Little and Big Kos'va) and the Tylai, as well
as the mines of four "possessors," Count Stroganov, Count
Balashev, Prince Golitzen, and Prince Abamelek-Lazarev,
located in the Verkh-Iaiven area. The output of the district
decreased from 191 2 to 1914, though the same mines were
worked in 1913 and 1914. The decrease of yield was shown
by all the mines except the Mala-Kos'vin belonging to Abamelek-
Lazarev.
In the Iuzhno (South) -Ekaterinburg district the output of
platinum is very small. Besides that recovered in this district
there was also an insignificant quantity of platinum (3 . 7 ounces)
secured in the Sievero-Ekaterinburg district as a by-product
in working the gold mines.
REFERENCES
1. Annuaire du Journal des Mines de Russie, St. Petersburg, 1840-5.
2. "The Industries of Russia. Manufactures and Trade," World's
Columbian Exposition at Chicago, 1893.
3. Freidrich Matthai. "Die Industrie Russlands," Leipzig, 1873.
4. Gornozavoiskaia promyshlennosl, Rossiia, St. Petersburg.
5. Bernhard Neumann, "Die Metalle," Halle a/S, 1904.
6. The Mineral Industry, New York, 1892-1916.
7. Obshchii obzor glavnykh otraslei gornoi i goraozavodskoi promy-
shennosti, Petrograd, 1915.
I 8. Obzor vnieshnei lorgovli Rossii, St. Petersburg (Petrograd),
1865-1915.
9. Maurice Verstraete, "La Russie industrielle," Paris, 1897.
10. The Russian Year Book, London, 1911-5.
11, Sbornik slalislicheskikh sviedenii po gornoi chasli, St. Petersburg,
1864-7.
i- 12. Stalisticheskiia lablilsy po gornoi promyshlennosli Rossii, St.
Petersburg, 1879.
13. P. von Winkler, Gornyi Zhurnal, 1893, pp. 578-611.
Bureau of Soils
Department of Agriculture
Washington. D. C.
THE PREPARATION OF SEVERAL USEFUL SUBSTANCES
FROM CORN COBS1
By F.^B. LaForge and C. S. Hudson
It has been shown by Hudson and Harding2 that corn cobs
yield about 12 per cent crystalline xylose through acid hydrolysis.
The strength of acid employed was 7 per cent sulfuric and the
hydrolysis was carried out by several hours' boiling. We under-
took to determine whether this acidity could not be decreased
considerably by carrying out the hydrolysis at a higher tem-
perature in an autoclave. This proves to be possible with an
acidity as low as i3/* Per cent at a temperature of 1300,
and there is thereby opened up a way for the preparation of
crystalline xylose on a commercial basis. It was noticed that a
volatile acid is produced in noteworthy amount along with the
xylose during the hydrolysis of the corn cobs, and the identifica-
. tion of this acid as acetic indicates that it may be a valuable by-
product in the preparation of xylose from corn cobs. A strength
of 1 to 2 per cent sulfuric acid appears to be necessary in order
to obtain a good yield of xylose. If the acidity is lower there
is little sugar produced, although a considerable quantity of
the corn cobs passes into solution. Indeed, there may be ex-
tracted from corn cobs by water alone, at the somewhat higher
temperature of 1400 to 1600, a water-soluble gum which is proba-
bly a form of xylan. However, its hydrolysis by acids yields
xylose in only moderate proportions, accompanied by a sirupy
mother liquor which does not crystallize. It was therefore
sought to remove this gum from the corn cobs by water diges-
tion in order that the subsequent acid hydrolysis of the residue
might yield xylose with a smaller proportion of uncrystallizable
sirup. This has proved possible and in addition it has been
found that the gum has excellent properties as an adhesive
which render it a useful product. The solid residue that re-
mains from the corn cobs after acid hydrolysis consists prin-
cipally of cellulose. It is very absorbent and might be used as an
ingredient in molasses, stock feeds, possibly aiso as an absorbent
for nitroglycerin in the manufacture of dynamite, and for other
such purposes. It has been found that it is readily gelatinized by
70 to 75 per cent sulfuric acid and may then be hydrolyzed to
glucose after dilution with water, according to well-known
methods. The glucose so produced crystallizes well and could
doubtless be used in the same ways that crystalline glucose
from starch is employed. The manufacture of alcohol by the
fermentation of corn-cob glucose appears possible provided
sulfuric acid is obtainable cheaply.
Direct uses for xylose, as such, seem difficult to find. Its
possible food value needs investigation because it is probably
1 Contents of Address presented before the New York Section of the
n 1 hemic*] Society, May 10, 1918, by P. B LaForge.
' J. Am. Chem. Soc, 39 (1917), 1038.
926
////. mi R \ I/. Of INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. n
oxidized to some extent, especially by herbivorous animals,
bul the limit of tolerance is not known. Xylose is about half as
sweet as cane sugar. Its after-taste is not bitter, as is that of
mannose, for instance, and if uses for xylose as human food could
be established its taste is in its favor. It is well known that
xylose may be converted by the cyanhydriii synthesis to gulonic
lactone. We would call attention to the suggestion that
Mich lactones of the sugar group may furnish an excellent ma-
terial for use as a crystalline acid ingredient in baking powders.
Gulonic lactone stands out prominently as suitable for such
uses, because of its ease of crystallization and the fact that it
can be produced fairly cheaply from xylose. We have made
experiments with mixtures of gulonic lactone and bicarbonate
of soda and find that a very satisfactory baking powder may be
so prepared. The preparation of gulonic lactone from xylose
has been made by a method that is more satisfactory' than that
usually employed. It will be described in a separate paper by
one of us (L-).
We will now describe in detail the preparation from corn cobs
of the various useful substances that have been mentioned.
PREPARATION OF ADHESIVE GUM
The coarsely broken cobs are placed in an autoclave with
sufficient water to cover them. The contents are then heated
to 140°, and the temperature then raised to 160 ° during
one hour. After cooling below the boiling point of water
the autoclave is opened and the contents removed. The liquid
in the autoclave is almost fully absorbed by the dry cobs in the
process of heating. The pext step consists in the extraction of
the solution from the solid residue in which it is absorbed;
this is accomplished by subjecting the wet material to strong
pressure. The solution thus obtained is evaporated in an
open kettle to the consistency of a thick sirup, which consti-
tutes the adhesive gum. It is ready for use without further
treatment, and is recommended as a cheap adhesive in the fiber
board and paper-box industry, in bill posting, labeling, etc. The
use of this substance in place of starch, dextrine, and flour paste
would make possible an enormous saving of these foodstuffs.
The solid residue which is left in the press serves for the
preparation of other products which are described below.
PREPARATION OF XYLOSE AND ACETIC ACID
For the preparation of the sugar, xylose, and of acetic acid the
residue from the preparation of the adhesive gum is treated as
follows:
An autoclave, such as was used in the preparation of the ad-
hesive, is filled to about three-fourths of its capacity with
the solid residue from the pressing operation above referred
to. A solution of sulfuric acid containing about one and three-
quarters per cent of acid is added in sufficient quantity to cover
the solid material in the container. Heat is then applied and
the temperature of the contents of the apparatus raised to
1300 C. where it is maintained for one hour This treatment
causes the liberation and solution of xylose and acetic acid. After
cooling, the contents of the autoclave are removed and sub-
jected to pressure to expel the solution from the undissolved
solid material. This solution is then heated in contact with
a second charge as before and thus a solution containing ap-
proximately double the amounts of xylose and acetic acid in a
given volume 1-- obtained. To isolate the acetic acid from this
solution some of the steam from the heated autoclave is allowed
to escape through a condenser ami tin distillate collected. This
weak solution of acetic acid may be built up or fortified by caus-
ing it to pass through several such operations as just described,
using the weal oration instead of water as in the
lust instance. In this manner mem- and more acetic acid is
accumulated in a given volume until the desired strength of
acid is reached. This concentration may lie made to attain
5 or t> pel cent.
The xylose solution remaining in the autoclave alter the
second heating operation is separated by pressure from the solid
residue in which it is absorbed and from this solution the sugar
is obtained. To accomplish the isolation of the xylose the solu-
tion referred to is evaporated under diminished pressure to
a thick sirup which is seeded with xylose and left for itself for
about 12 hours. In order to obtain crystals of sufficient size
to separate from the mother liquor by means of a centrifuge the
following conditions must be observed: First, the solution
should be concentrated without undue delay; second, the
proper consistency, which is about that of ordinary commercial
molasses, should be attained; third, crystallization should take
place at a temperature not lower than 20° nor higher than 55'
C; fourth, after crystallization has been induced by seeding, no
more sirup should be added to the magma.
The solid residue from the pressing operations above referred
to, which consists chiefly of crude cellulose, may be used in the
preparation of stock feed.
For this purpose the press cake is coarsely ground, mixed
with a small amount of lime or soda to neutralize the slight
amount of sulfuric acid which it contains, and in this state is
mixed with any desired amount of molasses or other sirup and
dried by any suitable means. Such a mixture, if fed in connec-
tion with seed press-cake meal, may constitute cheap and good
feed for cattle or other animals.
A second use to which the crude cellulose residue may possi-
bly be put is that of an absorbent for nitroglycerin in the manu-
facture of dynamite. For this purpose the material must be
purified by washing with dilute caustic soda to remove a brown
material present as an impurity. The excess of the reagent must
be removed from the cellulose by washing with water.
The cellulose may also be of use in the manufacture of
artificial silk, leather substitutes, filaments, and plastics, by
any of the processes now in common use. Other uses to which
the impure cellulose residue may be put are the manufacture of
glucose and of alcohol.
PREPARATION OF GLUCOSE FROM CRUDE CORN-COB CELLULOSE
The residue of impure cellulose above referred to, from which
gum and xylose have been removed as already described, is
ground to a rather fine powder and intimately mixed with about
an equal weight of sulfuric acid of about 75 per cent strength.
In determining the strength of acid to be used allowance should
be made for the small amount of moisture left in the cake after
the pressing operation. The resulting mixture is a stiff dough
which is black in color. After the "dough" has been allowed
to stand at room temperature for about 6 hrs , it is mixed
with a convenient amount of water (5 to 8 parts), and the
mixture is boiled for about one hour, after which the undissolved
solid residue is removed from the very slightly colored solution
by means of a filter press. Slaked lime which has been sifted
free from lumps and suspended in water is added to the filtrate
in quantity sufficient to very nearly neutralize the free acid in the
solution. The calcium sulfate which separates out on this
treatment is removed by means of a centrifuge or filter press.
The solid residue of calcium sulfate is washed with water and
the washings are added to the filtrate. The resulting liquid is a
dilute solution of glucose. This solution is added to a second
portion of ground press cake which has been treated with sul-
furic acid as above described and the subsequent operations of
boiling, filtering, etc., repeated as before. This process may be
again repeated until the sugar content of the solution has been
increased to the desired degree.
In order to isolate the glucose in the crystalline state the final
solution is exactly neutralized with lime, filtered, and concen-
trated to a thick sirup. This sirup soon crystallizes to a solid
mass. Glucose prepared after this manner has a slight brown
color but is free from any objectionable taste and can be used
directly as an ingredient of stock feed
Nov., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
927
In case the product were to be used for human food, very
pure sulfuric acid and lime would have to be used in this prepara-
tion and decolorizing carbon or bone char would doubtless have
to be employed.
The glucose solution above referred to is very rapidly and
completely fermented by yeast and hence could be used for the
production of alcohol.
By the process above described, about 50 per cent of the weight
of the crude corn-cob cellulose is converted into glucose.
The solid residue from the first treatment of the material
which was removed by the filter press, may again be subjected
to digestion with 75 per cent sulfuric acid, as was the original
material, and again a yield of 50 per cent of its weight of glucose
may be obtained by the above process, making the total yield
75 per cent, or 37 .5 per cent of the weight of the corn cob.
From two tons of sulfuric acid of the above-mentioned strength
one ton of glucose could be prepared. In order to compete
with glucose or molasses from other sources for the manufac-
ture of alcohol, sulfuric acid of 75 per cent strength would have
to be obtained at a price not much greater than $8 .00 per ton.
CONCLUSION
While the methods for obtaining these principal products
from corn cobs have not as yet been tested out on a large fac-
tory scale, they can be said to be already out of the laboratory
stage, since the work has been carried on by means of auto-
claves, powerful presses, vacuum stills, centrifuges, etc.
The yields of the various products constitute approximately
the following percentages of the weight of the dry corn cobs:
Product Per cent
Adhesive Gum 30
Crystalline Xylose 5
Acetic Acid 2 . 5 to 3
Crystalline Glucose 37
The United States is the world's greatest producer of corn.
Our annual crop ranges from 2 1/2 to 3 billion bushels, and repre-
sents nearly 75 per cent of the world's production. Other coun-
tries which rank as great corn producers are Austria-Hungary,
Mexico, Argentine, and Italy. For every bushel of corn there
is approximately a bushel of cobs which, however, weigh only
one-fourth as much as the grain. Corn cobs are not utilized
to any great extent. They have a certain value as fuel and
also have been used as an ingredient of stock feeds. They con-
tain, however, little or nothing that is directly available for
animal nutrition. They are one of the great waste products
of our agriculture. We believe, however, that the methods
of utilizing them which have been described in this article may
eventually render them a valuable source of raw material for
manufacturing.
Carbohydrate Laboratory, Bureau of Chemistry
Department of Agriculture
Washington. D. C.
STATISTICS OF GARBAGE COLLECTION AND GARBAGE
GREASE RECOVERY IN AMERICAN CITIES
By Raymond Peari.
Received August 28, 1918
In July 1917, the writer inaugurated in the Statistical Division
of the United States Food Administration a system of volun-
tary statistical returns from the leading cities in the country, re-
garding the amount of garbage collected monthly and, where
possible, the amount of grease recovered from the gail
lected. The purpose underlying the plan was to obtain infoi ma
tion which would serve the officials of tin Pood Admini
as ;ui index of the effectiveness of their propaganda campaign
urging the people to avoid waste in the preparation and '■
food. In view of the somewhat novel cl
material which has been collected in this work, it m di ITS
ble to give it permanent record by publishing it where it will
be available to public health officials and others who may be
interested. Accordingly there is presented here the records
of two complete years, from May 1916 to April 1918, inclusive.
The statistical material was obtained through the voluntary
cooperation of municipal officials. In the first instance the
mayors of all the larger cities in the country were asked if they
would not arrange to have the proper official in their munici-
palities make a monthly report to the Food Administration on
the amount, in tons, of garbage collected each month in the
current year and the corresponding month of the previous
year, beginning with May 191 7. The response was very
gratifying, particularly in regard to the willingness, not to say
eagerness, to cooperate, of those asked. In a rather considera-
ble number of cases it developed, apparently quite as much to
the astonishment of the city officials as to ours, that the city
had no record, nor any ready method of finding out how much
garbage was collected in that city in a given interval of time.
Finally, however, we were able to get 96 cities, with an estimated
aggregate population of over 26,000,000 reporting regularly and
for each month in the 2 years from May 1916 to May 1918.
These cities include roughly about one-fourth of all the people
living in this country. The numbers are sufficiently large to
give considerable trustworthiness to the data as indicative of
urban conditions in the country in general. The statistics are
certainly much more comprehensive in their scope than any
garbage statistics for the United States that have hitherto been
brought together, so far as the writer is aware.
At the end of the year a tabulation of all the monthly returns
which had been made was returned to the reporting city official
for verification or correction. In this way it is believed that the
figures here given are accurate so far as concerns the reporting
of the municipal records. The original records themselves in
some cases obviously do not include the whole of the garbage
produced. In a few they are grotesquely far from the mark.
//
^
^//
» >
,'
^N 1
\-
y
y
s
■».
\
<?
*~<z
Fig. I— The Seasonal Curve op Garbage Production, Based on
Average Returns prom 9ft Largest Cities
It is, for example, inconceivable that the hundred odd thousand
people who live in Nashville, Term., produce only about 400 tons
of garbage in a year, while about an equal number, say 10,000
fewer, of people living in Norfolk, Va., produce in the neighbor-
hood of 30,000 tons in a year. The fact is that the figures given
in tin, paper refer to tonnage of garbage officially collected either
by or under the official control of the municipality so that the
amount is a matter of city record. Only in cities where by
forbidden to disposi oi gai b igi in any a\
di livery to the organized official collecting agency of
the city can the statistics hen given be regarded as representing
the total am. unit produi 1 •'<
928
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. n
2,497
416
674
36
220
124
155
750
Total Garbage Collections,
May 1917-April 1918 and May
City
Akron, Ohio
AUentown, Pa
Atlanta, Ga
Atlantic City, N. J
Augusta, Ga
Aurora, 111
Baltimore, Md
Berkeley, Cal
Boston, Mass
Bridgeport, Conn
Brockton, Mass
Buffalo, N. Y
Cambridge, Mass
Cedar Rapids, Iowa. . .
Charleston, S. C
Charlotte, N. C
Chelsea, Mass
Chicago, IU
Cincinnati, Ohio
Cleveland, Ohio
Colorado Springs, Col..
Columbus, Ohio
Dallas, Texas....'.
Dayton, Ohio
Detroit. Mich
East Orange. N. J
El Paso, Texas
Erie, Pa
Everett, Mass
Fort Wayne, Ind
Galveston, Texas
Grand Rapids, Mich...
Hartford, Conn
Haverhill, Mass
Holyokc, Mass
Houston, Texas
Indianapolis, Ind
Jacksonville, Fla
Jersey City, N. J
Joliet, 111
Kansas City, Mo
Lexington, Ky
Los Angeles. Cal
Lowell, Mass
Lynn, Mass
Manchester. N. II
Memphis, Tenn
Milwaukee. Wis
Minneapolis, Minn....
Mobile, Ala
Nashville, Tenn
New Bedford, Mass. . .
New Orleans. La
Newport, Ky
New York City. N. Y..
Niagara Falls, N. Y.. .
Norfolk, Va
Oakland, Cal
Oklahoma City, Okla..
Pasadena. Cal
Passaic. N. J
Paterson, N. J
Philadelphia, Pa
Pittsburgh, Pa
Pittsfield, Mass
Portland, Maine
Portland, Oregon
Quincy, Mass
Racine, Wis
Reading, Pa
Richmond. Va
Roanoke, Va
Roehester, N. Y
Sacramento, Cal
St. Louis, Mo
St. Paul, Minn
Salem, Mass
San Diego, Cal
San Francisco, Cal. . . .
San Jose, Cal
Savannah, Ga..
Schenectady, N. Y
Scranton, Pa
Somerville, Mass
Springfield, 111
Springfield, Mass
Syracuse, N. Y
Tampa, Fla
Terra Haute. Ind
Toledo. Ohio
Trenton. N. J
Washington, I>. C
Wheeling, W. Vn
Wilmington, Del
Worcester, Mass
Youngstown, Ohio
Table I
by Tons, from 96 Cities for the 2 Years
1916-April 1917
Relative
figure
Tons Collected 1917-18
138
1,709
579
lation
000(a)
000(a)
1)00(0)
660
040
022
0001 a)
i ,i)
628(a)
113(a)
449
558
981
667(d)
041 6)
000(a)
0001,,)
722
300(d)
073
000(a)
000(a)
537
000(a)
000
852
222(a)
000(a)
000(a)
057(a)
000(M
000(a)
OOO(o)
870(a)
50 1 if,)
192(a)
758
000(a)
889(4)
000(a)
847
097(c)
000
978(a)
425
000(a)
995
000(a)
000(a)
060
057
158
000(a)
000
456(a)
000(a)
159(b)
604
943
500(a)
000(a)
443
518
090
607(a)
867
000(a)
5 ,i)
000(a)
561(c)
ooo
574
000(a)
500(a)
650(a)
000(a)
994
000(a)
000(a)
000
805
000
811
500(a)
000(a)
942
624
886
083
.<
593(i:)
000(o)
s;
265
000(a)
000(a)
May
1917-
April
1918
591
412
373
480
509
68 5
874
335
166
117
38 2
138
.'8 2
900
4 10
746
235
L03
466
B32
295
220
677
270
740
948
927
750
862
954
339
829
541
708
203
929
654
846
232
730
985
345
935
591
477
231
008
041
145
410
774
459
')(>(,
257
900
251
610
658
727
987
159
160
612
418
012
674
506
May
1916- 191617
April taken
529 118.2
340 102.0
798 94.7
792 81.8
338 96.2
805 83.6
915 91.5
726 91.2
650 88.0
897 91.3
794 71.1
70.5
93.9
102.3
83.8
109.4
71.1
74.9
83.8
92.9
96.4
84.8
82.4
94.3
94.1
99.9
83.9
88.6
77.1
58.6
84.6
94.4
91.9
92.1
84.6
57.0
90.3
97 4
100.9
91.3
101.2
86.5
96.5
93.1
146.2
105.0
98.0
112.3
71 . 1
90.5
80.7
87.9
73.8
84.6
75.4
84.2
70.7
86.8
85.3
90.7
67.3
87.5
91.4
80.4
93.0
81 .8
Total 26,034,685
(a) Population in 1918
(c) Population in 1916.
2.388.932 2,609,134 90.1
(a) Population in 1917.
(<f) Population in 1915.
The fact that the figures are for collection rather than produc-
tion (lues not invalidate relative comparisons of one year with
another, provided of course that the scope of official collection
did not change in the period. Pains have been taken to make
sure by correspondence that no such changes in the plan of col-
lection came in in the cities dealt with during the period covered.
The basic statistics are contained in Table I, in which the 96
cities covered are listed alphabetically. The data given
population, (6) gross tonnage of garbage collected in 1917-18,
(c) gross tonnage of garbage collected in 1916-17, fiscal year
ending April 30 being taken in both cases, (d) a relative figure
which expresses the 191 7-18 collection as a percentage of the
1916-17 collection for the same city.
The totals of this table show that in the 96 cities included
in the tabulation 10 per cent less garbage was collected in 191 7-18
than in the previous year. The figures demonstrate a genuine
conservation of food by the urban population of the country
during the past year, in the sense that 10 per cent of the usual
wastage in the preparation of food and in the incomplete usage
of food after its preparation was eliminated. The gross tonnage
figures do not, however, give a true picture of the real amount
of conservation or of the effectiveness of the Food Administra-
tion's teachings. This can only be demonstrated by the grease
figures to which we shall come presently.
Of the 96 cities included in Table I, 81 showed smaller collec-
tions in 1917-18 than in 1916-17, and 15 had larger collections.
The distribution of relative figures for these 81 cities was that
shown in Table II.
Table II
Distribution of Relative Figures of Cities Showing Smaller Collections
in 1917-18 than in 1916-17
Relative Figure Number of Cities
50-59 2
60-69 2
70-79 14
80-89 31
90-99 32
Roughly speaking, three-fourths of these 81 cities had relative
figures of 80 or above, indicating reduction of collections from
1 to 20 per cent. The four cities giving relative figures under
70, namely, Manchester, N. H., Galveston, Texas, Terre Haute,
Ind., and San Diego, Cal., make very creditable showings in-
deed.
The 15 cities showing an increase in garbage collections in
1917-18 are separately treated in Table III, which has the same
arrangement as Table I.
Table III
Fifteen Cities in which the Annual Ga
1918 Relative to 1917, in Order of Increase
Tons
May
1917-
April
City 1918
Tampa, Fla 18,081
Nashville, Tenn 410
Washington, D. C 46.732
Niagara Falls, N. Y 2,900
AUentown. Pa 12.591
Cedar Rapids, Iowa 2 , 282
Worcester, Mass 6.992
Passaic, N. J 28,987
Houston, Texas 30,203
Charlotte, N. C 9,420
Philadelphia, Pa 114,160
Akron, Ohio 10.084
Wilmington. Del 18,986
Pasadena, Cal 2,727
Springfield, III 47.910
Of these 15 cities, the first seven may at once be dropped
out of account as the increase is very small, 2 per cent or less.
Of the remainder, 5, namely Passaic, Philadelphia, Akron,
Wilmington and Springfield, 111., are places which have received
considerable increments of population within the last year on
account of war activities of one sort or another, such as muni-
tion making and the like. The effect of such sudden increase
Collections
Increased
Relative
figure
OLLECTED
1917-18
May
to
1916-
1916-17
April
taken
1917
as 100
18,023
100.3
406
101
46,293
101
2,865
101
12.340
102
2.230
102
6,828
102
27,599
105
28.567
106
8,612
109
101.678
112
8,529
118
14,187
134
1,865
146
28,315
169
Nov., iqiS
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
929
in population on garbage collection is obvious. To show its
effect in detail, Table IV has been prepared, which gives the
monthly collections for the four industrial cities showing the
greatest increases in garbage collections.
Table IV
The 4 Industrial Cities Showing the Greatest Increase in Garbage
Collection in 1918 Relative to 1917, Giving Collections by Months
Springfield, III.
Wilmington, Del.
Akron,
Ohio Philadelphia. Pa.
Tons
Tons
Tons
Tons
col-
Rela-
col-
Rela-
col-
Rela-
col-
Rela-
lected
tive
lected
tive
lected
tive
lected
May
1917
3,690
293
923
77
1,005
172
8,017
102
May
1916
1,260
1.203
583
7,823
June
1917
3,528
280
970
83
894
J48
9,588
ii9
June
1916
1,260
1,165
604
8,053
July
1917
2,322
158
1,200
93
864
ios
11,042
iii
July
1916
1,474
1,287
825
8,434
Aug.
1917
2,393
224
4,120
222
1,094
i ii
14,883
iio
Aug.
1916
1,068
1,853
967
10.604
Sept
1917
919
124
3,582
208
1,165
iis
13,690
i«
Sept
1916
742
1 .722
985
9.665
Oct.
1917
2,745
235
1,436
97
1,069
129
11 .183
iii
Oct.
1916
1.170
1,476
828
8,498
Nov.
1917
2,650
iii
1,995
183
792
96
8,174
107
Nov.
1916
1,872
1,089
829
7,655
Dec.
1917
3,438
102
1 ,282
i39
630
122
6,647
90
Dec.
1916
3,375
925
515
7,423
Jan.
1918
2,217
58
927
io6
539
i02
7,928
ioi
Jan.
1917
3,792
876
528
7,702
Feb.
1918
3,220
06
743
89
576
133
7.054
'67
Feb.
1917
4,912
838
432
10,559
Mar.
1918
11,280
253
799
'84
698
iii
7,962
ioi
Mar.
1917
4,450
952
613
7,879
Apr.
1918
9.508
323
1,009
i26
759
'93
7,992
ios
Apr.
1917
2.940
801
820
7.374
Table V gives the monthly collections in the 10 largest cities
covered in the statistics, with the relative figures for each month,
comparing that month in 1917-18 with the corresponding month
in 1916-17.
Table VI
Total Tons of Garbage Collected in 96 Cities, by Months. May 1916
to April 1918
Garbage Collected (tons)
1917-18 1916-17 Relative
May 191,129.06 226.066.56 85
June 209,937.90 230,724.72 91
July 233,853.45 245,198.66 95
August 265,409.63 278,948.91 95
September 241,317.59 258,751.64 93
October 220,943.29 234,148.73 94
November 190,012.89 209,090.07 91
December 170,391.67 200,067.75 85
January 156,711.35 200,096.45 78
February 148,785.15 167,391.84 89
March 177,392.25 181,306.00 98
April 183,119.69 177,342.50 103
Totals 2.388.931.92 2,609.133.83 92
From this diagram and table it is possible to get considera-
ble information as to the normal distribution of the garbage
production in the different months of the year. The month of
maximum collection is August and the month of minimum col-
lection is February. Following February, the curve begins
to rise and goes up rather steadily along something approach-
ing a straight line to the maximum point. The fall from the
maximum point in May to the minimum point in February is-
again nearly a straight line.
Table VI also enables one to see in what month the conserva-
tion propaganda has been the most effective. In the months of
May and June and December and January, the degree or ex-
tent of the lowering of the 191 7-1 8 collections, as compared with
the 1916-17 collections, is largest. During the other months
of the year the curves run very closely parallel. During the
last month of the fiscal year the two curves cross; that is to
<
garbage
Jollec
tions frc
m the 10 Largest Cities, G
iviug
Comparisons
by Months
New York.
Chicago,
Philadelphia
St. Louis,
Boston,
Cleveland,
Los Angeles
Balti
. Pittsburgh
San Fran-
N.
Y.
111
Pa
Mc
Mass.
Ohio
Ca
I.
Md.
Pa
cisco,
Cal.
Tons
Tons
Tons
Tons
Tons
Tons
Tons
Tons
Tons
Tons
col-
Rela-
col- Rela
R.-li
col-
Rela-
col-
Rela
col-
Rela
- col-
Rela-
col-
Rela
- col-
Rela
col-
Rela
lected
tive
lected
Tive
lected
tive
lected
tive
lected
tive
lected
tile
lected
tive
lected
live
lected
tive
lected
tive
May
1917
36,602
81
2,990
27
8,017
102
2,794
70
4,416
89
4,165
74
3,451
91
2,886
96
5.490
88
10,803
87
1916
45.197
11, 177
7,823
3.997
4,980
5,660
3,812
3,006
6.244
12,438
June
1917
44.590
93
8,386
65
9,588
119
3,882
92
4,042
88
4,613
89
3,454
'si
3,199
97
6.019
95
10,211
83
June
1916
48.099
12,826
8,053
4,205
4,572
5,176
4.120
3,307
6,303
1 1 . 760
July
1917
49,295
94
11,239
79
11,042
iii
4.631
84
3,870
87
5,431
90
4.453
'isi
4,854
97
6,728
99
10.318
Si
July
1916
52,173
14.302
8,434
5.540
4,440
6,068
5,337
5,012
6,810
12,078
Aug.
1917
51,545
97
12,583
78
14,883
iio
6.247
'88
4,265
9i
5,680
89
5.431
95
5,063
9i
7,340
"96
11.846
86
Aug.
1916
53,368
16.093
10,604
7,078
4.680
6,384
5,729
5,473
7.652
13,780
Sept
1917
45.903
94
12.142
82
13,690
142
5.591
99
4,310
92
5.639
93
5,167
ioi
4,567
97
7.623
102
11,121
S2
Sept
1916
48.934
14.774
9,665
5.645
4,668
6,069
5,111
4,709
7,481
13,541
Oct.
1917
42.971
96
11,259
90
11,183
152
3.815
94
4,033
87
5,955
1119
4,440
'97
3,833
o;
7,440
106
11,861
SS
Oct.
1916
44.629
12,462
8,498
4,075
4.632
5 , 473
4,596
4,041
7,045
13,482
Nov.
1917
35.551
90
8.967
95
8,174
107
2.495
'si
3,631
'si
4,580
92
3,395
'96
2,099
95
5,877
97
10.926
90
Nov.
1916
39.299
9.663
7,655
3.081
4,368
4,973
3,779
2,216
6,034
12,173
Dec.
1917
28.739
83
6,661
91
6,647
90
1.896
'74
3.415
79
4.165
ioi
3,481
'96
1,787
89
4,613
79
11,414
80
Dec.
1916
34.691
7,280
7,423
2,575
4,332
4,012
3.862
2,011
5,840
13,347
Jan.
1918
24.935
'76
2,388
30
7,928
ioi
1,362
'57
2,910
63
3,751
'si
3 , 605
'96
1 .780
76
4,095
69
11.537
84
Jan.
1917
32,975
7,897
7,702
2 , 403
4,608
4,485
4,026
2,357
5.907
13.696
Feb.
1918
22,350
85
4.347
74
7,054
67
1.498
'96
3,093
'si
3,352
ioo
3,246
9i
985
si
5,362
117
in. 211
90,
Feb.
1917
26.399
5,904
10,559
1,668
3.812
3.366
3.498
1.899
4,586
11,313
Mar.
1918
29.283
98
6,051
02
7,962
ioi
2.011
ioo
4,175
ioi
3,552
87
3.721
99
1.769
9i
5,988
132
10,800
89
Mar.
1917
29.995
5,936
7,879
2.020
4,051
4.087
3.740
1.905
4,539
12,092
Apr.
1918
33.650
106
6,222
01
7.992
108
2,434
107
4,175
ii9
4,583
iio
3,501
ioi
1.763
B9
6,037
i i-i
10,605
■->■>
Apr.
1917
31.692
6,182
7.374
2,268
3 , 507
3,955
3,452
1.979
5,317
10.715
The first noteworthy feature of this table is the considerable
variation among the different cities as to the constancy of the
relative figure for the different months of the year. In some of
the cities it maintains a fairly even level throughout the year,
notably in Baltimore and San Francisco, and to a lesser degree,
Boston. The seasonal fluctuations in savings in these cities,
as indicated by the relative figures, follow rather closely the
general seasonal distribution of the garbage collections in the
cities named. Others of the cities show widely varying figures
in this respect, notably in Philadelphia, where, in the course of
the year, the relative figure changes all the way from 57 to 142.
Some general features of the seasonal distribution of garbage
collection are indicated in Table V. The normal seasonal
curve of garbage production, however, is better shown by the
sums by months of all the cities covered in Table I. This is
done in Table VT, where there are exhibited the total collec-
tions of garbage for the 96 cities reporting, in each month of
the two fiscal years for which reports are available.
say, tin- April 19x8 collections were slightly larger than the
April 1 91 7 collections. This is probably due chiefly to the
fact of an increased use in April 19 18 of various vegetable
foods with a comparatively large amount of inedible refuse,
which increases in turn resulted from the shortage of wheat and
wheat flour. People were urged to substitute and undoubtedly
did so to a very considerable extent, vegetables for the scant
cereals. This was particularly true of potato consumption.
Another factor in the case is undoubtedly the increase of the
population in a considerable number of the cities of the United
States as a result of the war conditions, munitions making, ship-
building, etc.
We may turn now to a consideration of the grease recovery
from garbage. The grease is the profitable constituent of gar-
bage as it is ordinarily handled. The raw material also, of
mtains valuable protein and carbohydrate, but In the
11^1 1.1I methods of reduction the tankage from which the grease
has been extracted goes to fertilizer. Unfortunately, only
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. io, Xo. n
i of Garbage Grease Recovered i
Table VII
12 Cities for the 2 Years May 1917-April 1918 and May 1916-April 1917
City Population
Boston, Mass 781 .628(a)
Buffalo, N. Y 468. S58
Chicago, 111 2.497.722
Cleveland, ' Ihio
Columbus, Ohio
Dayton, Ohio
Indianapolis, Ind . .
New Bedford, Mass.
Pittsburgh, Pa...
Philadelphia, l'a
Schenectady. N. Y
Wilmington, Del
674.073
220.000(a)
] J5,000 a
.'71 . 7SK
118,158
579,090
,709,518
105,000
94,265
April 19(8
46,335
15,382
93,235
55,466
17,295
15,677
19,929
8,774
72,612
114, 160
4.111
18,986
April 1917
52,650
21,817
124.496
59,708
20,393
16.621
23.267
10.162
73,758
101,678
4,419
14,187
Tons op Grease Recovered
May 1917- May 1916- Rclativ
April 1918 April 1917 Figure
481,962
523,156
1 , 40 1
314
1,656
1.415
)54
250
454
199
1,554
1,178
84
49
B 906
2,140
494
2,869
1,821
355
270
2.117
92
12,843
Totals 7,684,771
(a) Population 1918.
(6)' Relative figure expressing the monthly collection for the present year as a percentage of that of the
under' 100 mean smaller collections and figures over 100 mean larger collections.
Percentage of <".
REASE
May 1917-
May 1916- Relative
April 1918
April 191
7 Figure(6)
3 02
4 . 06
74
2.03
2.26
90
1.77
2.30
77
2.55
3.05
84
2.04
3.13
65
1.59
2.13
75
2.27
67
2.26
85
2.14
2.87
75
i en
1.14
90
2.04
2.04
100
0.25
0.65
38
1.85
2.45
76
th last year; that is.
relative figures
comparatively few cities have municipal reduction plants and
are able to furnish statistics of grease recovery. Such data
as it has been possible to collect are exhibited in Table VII.
The arrangement is the same as that of the earlier tables in this
paper.
The data of Table VII show in the clearest manner the re-
markable effect of the conservation campaign. The 12 cities
show a reduction of 30 per cent in the gross tonnage of grease
recovered from garbage in 1917-18 as compared with 1916-17.
The average percentage of grease in the garbage dropped from
2 .45 to 1 .85. The figures demonstrate that not only was there
a quantitative conservation of food affected during the last
year, but also, and even more important, there was a propor-
tionally much greater qualitative conservation. There must
have been in these 1 2 cities a very great reduction in the amount
of meats and fats going into the garbage can.
The two cities showing the greatest qualitative food conserva-
tion, as indicated in garbage statistics, were Columbus, Ohio,
and Wilmington, Del., with relative figures of 55 and 53, re-
spectively. In these two cities the garbage in 19 17-18 con-
tained only a little more than half as much fatty material in
1917-18 as in 1916-17. This is truly a remarkable record.
Putting all the data together, it appears that, in sd far as the
sampling of cities may be considered representative of the urban
portion of the country as a whole, there has been a substantial
conservation of food by the American people during the past
year. A reduction of 10 per cent in the gross tonnage of gar-
bage, and of 30 per cent in the tonnage of fat recovered can
only have been accomplished by a real and widespread saving
and utilization of food materials which ordinarily go into the
garbage can
School op Hygiene and Public Health
Johns Hopkins University
Baltimore, Md.
COTTON OIL INDUSTRY IN THE WAR'
By David Wesson
Many things have been turned upside down by the war.
The cottonseed industry is one of them. Before the war there
was a constant competition between the oil mills for seed.
Money was advanced to seed buyers, and the seed, in many
instances, was accepted containing large quantities of foreign
matter, which had to be taken and paid for or else the mills
would shut down
Since the Pood Administration has Income very much inter-
ested in tin value of the products of the cottonseed for supply-
ing this country and our Allies with food and ammunition ma-
terials, they have taken the industry under control and estab-
lished a department of the Food Administration in Washing-
ton dealing specially with cottonseed products.
the war, if oil mill men got together and decided they
could pay a certain price for the seed, they were sent to jail
1 Presented al the !6th the American Chemical
nd, 1 1 '. 1918
under the anti-trust laws of the various states. If the refiners
of the crude oil who made their product into lard compounds
got together and attempted to regulate the prices of their prod-
ucts in order that there might be some profit left in the business,
they violated the anti-trust laws and were apt to find Canada or
some foreign clime far more salubrious than the good old U. S. A.
Now all of this is changed. The oil mill men go down to Wash-
ington and with the Food Administration agree on a price which
they can afford to pay for cottonseed. They also agree with the
Food Administration on a suitable price to charge for their
oil, meal, and hulls. The Government tells them how much
oil, meal, hulls, and linters they should produce per ton of
seed. The prices are arranged so that the manufacturer, work-
ing with ordinary good management, should make a profit.
The agreement is, in a sense, a gentleman's agreement, and there
is no law against breaking it, but all the manufacturers are
licensed and if they should break the agreements they would
lose their licenses. The effect of this arrangement is to stabilize
prices and to secure the largest possible production.
The approximate yields per ton of seed are at present:
Oil 41 to 43 gal.
Meal 960 lbs.
Hulls 480 lbs.
Linters 145 lbs.
Before the war 40 or 50 lbs. of linters were considered a reason-
ably good yield, while the hulls used to be about 600 lbs. per
ton.
Although the title "Cotton Oil Industry in War" was selected
the words "Vegetable Oil Industry" would have been fully as
appropriate, because at the present time cottonseed oil repre-
sents approximately only about two-thirds of the oils handled
in the plants, which were originally started to crush cotton-
seed and refine its products.
In 1900 this country crushed 2,480,000 tons of seed, costing
$II-55 Per ton, and produced products worth §42,412,000.
During the crushing season just passed about 4,200,000 tons of
seed were handled, for which was paid $65 per ton, and the com-
bined value of the products was in the neighborhood of
$400,000,000, or about ten times as great as in 1900.
The cotton oil industry proper gives the country from the
seed about 3,200,000 barrels of edible oil, 2.000,000 tons of
cake and meal, 1,000,000 tons of hulls used as cattle feed, and
280,000 tons of linters which furnish much of the cellulose for
the manufacture of explosives.
In refining the oil there are obtained 192,000 barrels of fatty
acids used in the soap industry, and last, but not least, about
3,800,000 lbs. of glycerin used in the manufacture of ex-
plosives
The great muscular activity of the men in the armies and
those in the iron and steel and shipbuilding industries calls for
a great amount of food which will furnish energy. This is largely
supplied by edible fats and oils Before the war the daily, the
cotton oil industry, and the packing houses furnished a normal
Nov., 191S
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
93a
supply for this country and exported considerable to Europe.
Since the war has started, between short crops of cotton and
the big demand for edible fats, materials other than cottonseed
oil have been drawn upon to keep up the supply. All told,
something like 1,700,000 barrels of vegetable oils were imported
during the year either as oil or in the form of oil seeds such as
copra, peanuts, sesame, and soy beans. Coconut oil has en-
tered the country largely as copra and much of it has been
crushed in cottonseed oil mills. Peanut oil has been imported
in large quantities from the Orient and has also been crushed
from the peanuts grown in the South and West. The refined
oils have gone largely into butter substitutes, some into lard,
and some into soap.
Besides furnishing the best edible oils, lard, butter substi-
tutes, cattle feed, cellulose for explosives, soap material, and
glycerin to aid the war, the cotton oil industry is furnishing
men from its mills, and the places of many of the men are being
taken by women.
The Southern Cotton Oil Company
120 Broadway, New York City
THE. BUREAU OF FOREIGN AND DOMESTIC COMMERCE
ITS RELATIONS TO AMERICAN CHEMICAL INDUSTRY
Papers presented before the New York Section, A
Chemical Society. October 11, 1918
GOVERNMENT TRADE-BUILDING INFORMATION
By Chauncey Depew Snow
Assistant Chief, U. S. Bureau of Foreign mid Domestic Commerce
In my work in the Bureau of Foreign and Domestic Com-
merce since the outbreak of the European war I have had more
to do with business men connected with the chemical industry
than with those connected with any other American industry.
Back in 1914 and 1915, when I had just returned from an official
visit of observation in Germany, it was dyestuff manufacturers,
prospective dyestuff manufacturers, or chemists chiefly interested
in dyestuffs, who most frequently came to the Bureau. In the
three years following business men connected with every branch
of the chemical industry and the chemical equipment industries
have had some occasion to deal with the Bureau of Foreign and
Domestic Commerce. The detailed analysis of import statistics
of dyestuffs which was made for the Bureau and the chemical
industry by Dr. Thomas Norton, combined with his reports on
atmospheric nitrogen and some minor Bureau contributions on
particular sides of the chemical industry, put this government
bureau in the minds of a great many men in the industry. The
success of the dyestuff census led to the request by your Society
for a survey of all chemical imports. Your Society, unlike
many of the others, backed its convictions by raising funds to
help cover the expense of the inquiry, so the Bureau was glad
to pitch right into the work on such a survey. Dr. Pickrell will
tell you more about that a little later. Xaturally the fact that
the Bureau was engaged in this study has had a tendency to
interest others of your members in our work and visits to the
Bureau by your members have been even more frequent. Not
long ago these visits from chemists and others interested in
chemicals became so numerous that the Chief of the Bureau re-
marked it would soon become necessary in our examination
requirements for Bureau positions to specify a knowledge of
chemistry.
Your committee has requested me to tell here to-night what
the Bureau of Foreign and Domestic Commerce has to offer
to the American chemical industry. As at present organized
the Bureau came into existence in 1912 by Congressional action
consolidating the Bureau of Manufactures and the Bureau of
Statistics. The Bureau of Manufactures had been charged by
law with the duty of fostering, promoting, and developing the
manufacturing industries of the United States The Bureau of
Statistics had been charged with collecting and publishing the
statistics of imports and exports and tonnage of tin I nited
States. Since the consolidation, Congress has laid all the
emphasis on trade and the promotion of manufacturing industry
by means of promoting trade. The appropriations for the
Bureau have been made primarily "ill' ■' view to enlarging our
information about foreign markets Tin great bulk of the
work during ii; nas been the promotion of the
export trade ol the ' nited stairs. Tin- appropriations have
related chiefly to the foreign field, and the Bureau has not been
given any permanent organization for direct promotion of
domestic commerce. In fact, the one little appropriation
which we did have for collecting the statistics of the internal
commerce of the United States was withdrawn. As matters
stand to-day the Bureau of Foreign and Domestic Commerce is
the official center of information for all questions pertaining to
the movement of goods into the United States from abroad, the
movement of goods from the United States to foreign countries,
and the movement of goods between the main block of territory
of the United States and our non-contiguous territory. Further
the Bureau is the chief source of information in this country
concerning the trade, industries, and natural resources of foreign
countries. We get the information concerning the outward and
inward movements of goods in the United States, as most of
you know, through the United States customhouses. Declara-
tions of value and quantity are required for statistical purposes
in connection with exports, as well as imports. Returns from
the customhouses are made to the Bureau of Foreign and
Domestic Commerce, which takes care of final compilation and
publication of returns. Information concerning the trade,
industries, and resources of foreign countries comes through a
variety of channels.
The Bureau receives tin- official statistics, official gazettes,
principal trade papers, and other non-official publications,
from practically every country and important colony on earth.
There is a staff of trained readers, translators, and research
statistical clerks working continuously on this incoming stream
of printed matter from foreign countries.
Then there is the large number of reports that are constantly
coming from the American consular offices which dot the world.
liven at this time, when of course we have no consulates in Ger-
many and the other enemy countries, we have over two hundred
anil fifty active consulates, and one hundred and fifty more
consular agencies. A good many of our business men are apt
lo smile at mention of the consular service, but the really well-
informed American business nun who have had much contact
with the consular service will till you that it is a remarkably
good organization We need more consuls, and a larger st.ill
in many of the existing consulates. The consuls have a multi-
tude of dutii bi really responsible representation
o! the Governmenl to purely notarial functions. They are re
quired to make commercial reports, both with regard to general
commercial condition ii th places where they arc stationed
and with regard to market opportunities for the sale of American
goods. The consuls havt clearlj denned local territories to
covet in their reports Some of our consuls are so pressed with
othei routine work thai thej an Forced to neglect i>>
mercial matters Others givi perhap thi bulk of theii time to
i ,1 matti ■ I "UMi iple ol jreai . since our
entry into the war, th< consuls have had so many .nl1M10n.1l
duties imposed upon them that matters of trade information
93 2
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. n
and trade promotion have of necessity pretty much gone by the
board. But the importance of the consular service in our
scheme and mechanism of trade promotion and trade informa-
tion should be recognized and appreciated. For current reports
on local matters of importance to American commerce it is to
the consuls that we must look.
In addition to the consuls we have, at the principal embassies
and legations, officers who are known as commercial attaches.
Everybody now knows what military and naval attaches are.
Well, the commercial attache is the accredited representative
of the Department of Commerce attached to the staff of the
embassy or legation to report on commercial developments of
national importance and look out for national commercial in-
terests of the United States. He acts as commercial adviser
to the ambassador and at the same time keeps the Department
of Commerce, and through the Department the business men
of this country, fully informed about developments of general
significance to American trade. The commercial attache is
under the Department of Commerce and plays with regard to
commerce a part corresponding to that taken by the military and
naval attaches with regard to military and naval matters.
Unlike the consul, the commercial attache has as his field an
entire country. Unlike the consul, also, the commercial attache
has no other functions beyond those of promoting the conj-
merce of the United States. The commercial attache is a
resident trade representative and exclusively a trade representa-
tive.
Another very important part of this mechanism of keeping
American business men informed as to the trade and industries
of foreign countries is the staff of commercial agents. The
commercial agent is a trained specialist in some particular line
or phase of commerce who has a distinct assignment to visit
certain foreign countries and report on things pertaining to his
line of trade or industry which have interest for the American
manufacturers and merchants. Thus, when we undertook to
make a study of the subject of atmospheric nitrogen in Germany
and the Scandinavian countries, we had the investigation made
by a chemist of recognized standing and fitness for the work.
Similarly, when we had a survey made of South American
markets for drug products, patent and proprietary medicines,
surgical instruments, and dental supplies, we picked a com-
mercial agent who had had technical experience in connection
with those lines. Our study of oils and seed products in foreign
countries was made by a man who was known throughout the
trade for the work which he had done in that connection. I
have taken a few instances relating directly to the chemical
industry. In like manner we have had specialists report on
foreign markets for agricultural implements and machinery,
machine tools, electrical goods, canned goods, cotton and other
textiles, boots and shoes, and so on. For some of the more im-
portant industries we have had our commercial agents cover
practically all countries.
I have described the sources of information of the Bureau of
Foreign and Domestic Commerce. I will now touch briefly
on the nature of our organization in Washington for handling
information and making it available to the business men of the
country. In the Washington office, where we have between 150
and 200 workers, we are organized partly on a geographical basis
ami partly on a subject basis. More interest has been taken in
Latin America than in any other foreign field. This is reflected
in our appropriations and in our organization. Our Latin
American Division is one of the largest and one of the best in-
formed and busiest parts of our organization. It is in charge
of a man who has for years specialized on Latin American trade,
and is personally familiar with the entire Latin American field.
He lias a number of assistants who have been in Latin America
and the necessary translators ami clerical assistants. There is
undoubtedly in this Division more trade information with
reference to the countries of Latin America than anywhere else
in this country, and probably than in any foreign country.
This year Congress gave us a special appropriation which made
possible the creation of a Far Eastern Division. The Far
Eastern Division has been organized, has developed its files,
and correlated the available information with reference to the
Far East somewhat after the fashion of our Latin American
Division. As Russian commercial affairs have loomed so large
in the past few years we have developed our Russian information
files very largely In addition to our geographical divisions we
have a Division of Foreign Customs Tariffs, which supplies
information with regard to tariff rates and customs require-
ments, consular regulations, and regulations affecting com-
mercial travellers in any foreign country or colony In this
division we also have the information with regard to foreign
patent and trade-mark requirements. In the past couple of
years our little foreign trade-mark section has done yeoman
service in helping American manufacturers to protect their
trade-mark rights in foreign countries where German com-
petitors were pirating them under foreign laws by which reg-
istration rather than use is the test of validity. We of course
have our Division of Statistics, which is the central office for
United States trade statistics. Foreign statistics in general are
handled by our Division of Research, which also has our in-
formation files with reference to foreign countries not covered
by specialized divisions. Our Division of Trade Information
handles all the non-technical correspondence. We have lists
of foreign buyers, classified, for practically every important
foreign city. The value of the lists has been lessened, of course,
recently by the ever-changing enemy trade prescriptions of the
belligerent countries. We have a big collection of trade direc-
tories and a list of American manufacturers known to be in-
terested in exporting what we call our Exporters' Index. Inci-
dentally, we have our trade information files very thoroughly
indexed and cross-indexed, in order that inquiries may receive
the best possible attention. Then we have our Editorial Divi-
sion, which gets out our daily paper, Commerce Reports, with
which many of you are familiar, and the reports of the foreign
representatives that I have mentioned. The organization of
the Bureau in Washington is for service. The Divisions that I
have talked about are arranging the material that comes in from
abroad in order to make it helpful to American business men.
The Chief of the Bureau's Editorial Division, Mr. Hopkins, will
explain to you more in detail some of the aspects and possi-
bilities of that work
Whereas in former years most of our inquirers were interested
exclusively in foreign markets for American manufactured
goods, more recently a large percentage of inquirers have been
interested in foreign sources of supply for materials to be used in
manufacturing in this country. This has been strikingly true
as the shortage of ship space has curtailed trade with the more
remote parts of the world and has made necessary the use of
nearer sources of supply and of new materials that are more
readily available with less use of ship tonnage than the custom-
ary materials. Our representatives abroad pass on information
about new industrial materials, new processes, and new uses of
old materials. The Bureau of Foreign and Domestic Com-
merce is making such information available to manufacturers
here.
In short, if there is any phase either of competition from
foreign countries in foreign markets or from foreign countries in
American markets or any information about needed supplies
of old or new raw materials for manufacture in this country,
the Bureau of Foreign and Domestic Commerce either has the
information or the means and disposition to obtain it.
I have talked at some length and at the risk of going too much
into detail in order to make quite plain to you the extent of the
trade information and trade promotion service which the Bureau
Nov., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
933
carries on. Questions are sometimes asked as to whether this
is all worth while, and both in Congress and elsewhere, occasion-
ally questions are put as to whether there is an actual money
return for the funds which are expended in this work. It is
hardly a fair test to apply, but the work that the Bureau of
Foreign and Domestic Commerce has done will stand even this
test. The letters from American firms who have been helped
by the Bureau and who have quite spontaneously expressed their
gratitude run into thousands. The sales of American mer-
chandise in foreign countries as a direct result of the trade
opportunities that are pointed out to American manufacturers .
by the Bureau have from year to year run well into millions of
dollars. There have been instances of single sales that have run
up into seven figures. This tangible result is not counted by
the Bureau as the main result of its work, however. The
Bureau officials believe that they have accomplished more by
keeping American manufacturers awake to the importance of
foreign trade and of doing it on the best ethical and technical
basis than by means of this trade opportunity service. The
settling of commercial disputes between traders in the United
States and traders abroad has been a line of service carried on
by the Bureau which has produced remarkably good results.
The good that was done by the American commercial attache in
Australia in the trying years between 1914 and 191 7, before we
entered the war, can never be calculated in dollars and cents.
It was largely through the efforts of this representative of the
Department of Commerce that American national good will in
commerce was preserved there in spite of vigorous propaganda
against the United States and its commercial methods. There
is no calculating in dollars and cents the value to American
foreign trade in general when individual American concerns are
aided by the Bureau to change their export methods so as to
conform to the best practice.
We are prone in this country to view our own Government as
rendering less assistance to trade than the governments of
foreign countries. I am inclined to believe that this is charac-
teristic of business men everywhere. In England for years it
has been the practice of business men to knock the Board of
Trade, the organization in England which corresponds to our
Department of Commerce. In Germany the average manu-
facturer has always professed to despise government assistance.
Here we have pointed to Germany and England as examples of
how governments help trade. In England they point to us and
to Germany as examples of how government helps trade. In
Germany they have pointed to England and to the United
States as examples of how government helps trade. So it goes.
When I went to Germany to take part in an investigation of
the German pottery industry I went somewhat with the idea
that I was going to find government subsidies to trade, which,
with starvation wages, had been proclaimed before our Ways
and Means Committee as the reason for German success in
foreign trade. I made a point of talking with German manu-
facturers on the subject of the help they received from the
government. I never found a manufacturer who would concede
that the government was helping him at all — instead he was
usually growling at the burden of government taxation and
interference. In this very industry that you gentlemen are
engaged in in this country there is a disposition to point to
Germany and to say that the German government is directly
subsidizing the German manufacturing industries and that there
is no hope of competing with German manufacturers under these
conditions. The tradition that the government was backing
all the German trading and manufacturing companies, and that
to this was due the success of German industry in the
world market, is a dangerous and regrettable thing. Then
too many American manufacturers who without knowing the
facts are inclined to cry, "Wolf, wolf," and demand govt rnmenl
support or government protection on that false basis. In
British countries in the course of the liquidation of German
concerns there has been a direct effort to trace out the extent of
government assistance. To date I have seen nothing as a result
of the work of liquidators that has been at all convincing evi-
dence that German success abroad was due to direct govern-
ment help. In fact, one of the British official liquidators at
Hong Kong who made a deliberate attempt to ferret out evi-
dence of government participation in German trade in that
colony admitted frankly that the books and papers of the
liquidated concerns gave reason rather for the contrary con-
clusion. We do not know all the facts about the German
methods of commercial penetration, and possibly we never shall.
We do know that the German government has shown a very
sympathetic attitude toward the big commercial interests, has
encouraged them in many ways, has given material encourage-
ment to German shipping, and has worked with pretty definite
governmental commercial policies, all in the interest of increased
national efficiency. Admit all this, however, and yet on the whole
we have got to admit further that German commercial and manu-
facturing success has been chiefly attributable to energy and
careful planning in private organization. It will be a bad thing
for the American manufacturer to fool himself into abject de-
pendence on government support in getting and holding his
business. The American manufacturer in the long run, just like
the manufacturer in any other country, must organize better,
produce better, and sell better than his competitors. I am not
going to enter into any discussion of the merits of government
protection and government subsidies, each of which may have
its place in carefully organized governmental commercial policy,
but I do wish to mention the need of a cultivation of a spirit of
self-reliance and confidence in manufacturing and selling ability
among the American manufacturers. Our Government can
help a manufacturer in a variety of ways. I have to-night
pointed out some of the ways in which the Bureau of Foreign and
Domestic Commerce can render assistance. I think that in the
field covered by the work of the Bureau our Government has
done as much and as effective work as any foreign government.
Times and circumstances have been greatly changed as a result
of the war. Other governments are reorganizing and preparing
to spend large sums in promoting their interests in after-war
trade. From all that we know of the past and present attitude
of our own Government I should say that we have no reason to
believe that our Government will not expand its own service,
give it variety and new lines of activity, just as much as the
national interests require. We must not look to the Govern-
ment to do the business for us, but at the same time we cannot
afford to ignore or underestimate the value of what the Govern-
ment is prepared to do and is actually doing.
OUR PUBLICATIONS AND THEIR BEARING ON THE
CHEMICAL INDUSTRY
By O. P. Hopkins
Chief, Editorial Division, Bu
1 of Foreign and I h i [i I
The recent wonderful development of the chemical industry in
this country has awakened in our chemists a desire to be better
informed on the relations of the American industry to that of
the rest of the world. They have a vision of a permanent and
self-contained industry here at home, but they now realize
that this vision will never be made a reality by ignoring what is
going oil in other countries, by making themselves believe that
the future is assured no matter what plans, what commercial
campaigns, what trade tendencies may be attracting attention
elsewhere. They realize, in short, that the time lias come for
the chemical industry, along with almost every Othd industry
to accustom itself to a much broader view of affairs,
b tdopt a world point of view.
This has led to the suggestion that the industry is now ready
THE JOURNAL OF INDUSTR1 I/. AND ENGINEERING I HEMISTRY Vol. 10. No. u
i more sc-riou- i of ore in foreign-trade
statistics and information in general bearing on the exportation
and importation of chemicals, raw materials, and machinery
and apparatus. The members 9l thi Section will suspect at
once that the suggestion comes from Dr. Herty and Dr. Hesse,
and such suspicions are well founded. In response to their
suggestion I am going to call attention to the wealth of material
published by the Rureau of Foreign and Domestic Commerce
and offer a few practical suggestions for making use of it.
I suppose the interested members may be divided into two
classes: Those who intend to make a practical commercial use
of our data, and those who simply wish to keep up with the times,
to be well informed on all matters pertaining to their calling,
whether or not it will ever mean dollars and cents to them.
Roth groups will be kept in mind as far as possible.
Our Bureau is the original source of all statistics relating to
American foreign trade, and its figures are issued monthly,
quarterly, annually, and bi-aiiiiually. If a chemist or chemical
manufacturer wishes to keep his finger on the pulse of our foreign
trade as it rises and falls from month to month, he will turn to
the "Monthly Summary;" if he wishes to follow in considerable
detail the ebb and flow of imports only, he will study the "Quar-
terly Statement of Imported Merchandise Entered for Consump-
tion;" if he wishes to review the trade for a whole year as com-
pared with previous years, he will examine the annual "Com-
merce and Navigation;" and if he wishes to go rather deeply into
our trade with any particular country or countries, he will turn to
"Trade of the United States with the World," which has been pub-
lished every two years, but in the future will be published yearly.
MONTHLY STATISTICS
The "Monthly Summary" shows imports and exports by
quantities and values for the latest month compared with the
corresponding month of the previous year and also for the
months of the current fiscal or calendar year ended with that
month. For instance, the May number this year gave the trade
lor May as compared with May of last year, and also the total
trade of the eleven months ended with May as contrasted with
similar periods in 1017 and 1916. In June tin- total was shown
for the twelve months of the fiscal year contrasted with the two
fiscal years immediately preceding, although in much less de-
tail than will be shown in the annual report when it is issued!
In July, however, in addition to the statistics for the month,
there is shown the total for the seven months of the calendar
year, which plan will be followed until the calendar year is fin-
ished, when periods of the fiscal year will again be considered.
Countries of origin and destination are shown only for arti-
cles moving in great quantities, and this rule unfortunately
affects a great many articles in which the chemical manufac-
turer is interested. Just recently, however, it was decided to
- show the destination of our rapidly growing dyestuff exports
and this feature has attracted considerable attention. Coun-
tries are also shown for some of the oils, naval stores, rubber,
and the most important metals and ores.
\ already stated, these figures enable a manufacturer to
keep his finger on the pulse of our foreign trade, but they are
just the bald statistical facts. They are not analyzed in any
way Analysis is left to the reader, perhaps to a greater extent
than is necessary. At any rate it will be a wise plan for the
chemist who wishes to gel the most out of the figures to devise
some plan of his own for separating out the material in which
he is most interested An outline for a compact little continuous
table can easily be made and filled in from month to month, for
one article or for some logical group of articles. Percentages
of increases or decreases can be shown conspicuously in a num-
ber of different ways. Personally, I think .1 graph is the most
satisfactory way of tracing movements of this kind, and it is
my understanding that chemists are pretty keen at devising
things of that son.
QUARTERLY STATISTICS OF IMPORTS
The quarterly statistical statement relates only to imported
merchandise entered for consumption in the United
It is designed primarily for Congress and such government
officials as may be interested in tariff legislation, for it gives
not only the rate of duty for each item imported, but the total
amount of duty collected as well. It is not likely that many
members of the American Chemical Society are interested in
the tariff statistics, but there is one feature of the quarterly
statistics that should not be overlooked. The classes are sub-
divided to a much greater extent than in the "Monthly Sum-
mary." For instance, under the heading "Chemicals" in the
"Monthly Summary" only two acids are named, oxalic and
carbolic, whereas in the Quarterly there are thirty-two. That
is an important feature, and one that is very commonly over-
looked. The Quarterly, however, does not indicate origin in
any case, nor is any comparison made with quarters of previous
years. The imports are simply set down in some detail for a
quarter of the fiscal year, alongside the preceding quarters of
the same year. If it happens to be the first quarter, then no
comparison is attempted. If a person decides that he wants to
keep his finger on the pulse of the import trade in a certain line
of chemicals and finds that there is not adequate information
available in the "Monthly Summary," he can turn to the Quar-
terly and if he wants to go to the trouble of keeping a graph he will
soon be able to trace the important developments in his line over
a considerable period. For the busy man it ought to be possi-
ble to assign the work of keeping the graph or compiling a con-
tinuous table to a secretary' or clerk. It would take very little
time in any event.
ANNUAL STATISTICS BY ARTICLES
The annual "Commerce and Navigation of the United
is an imposing volume of nearly a thousand large pages of solid
statistics. It is so formidable in appearance that many people
hesitate to trust themselves to find in it the information they
wish, and prefer to write in to the Bureau and have us look up
the data. But it really isn't complicated at all. For the chem-
ist, who is accustomed to prying into all sorts of mystifying
secrets, this book ought to be a very simple matter. I am sure
it has proved simple to any who have tried it.
The three annual tables of prime interest to the chemical
industries are No. 3, "Imports of Merchandise," by articles
and countries; No. 5, "Exports of Domestic Merchandise." by
articles and countries; and No. 9, "Imported Merchandise En-
tered for Consumption," by articles.
Two features of the tables "Imports of Merchandise" and
"Exports of Merchandise" make the volume invaluable to any-
one who wishes to make a serious study of our foreign trade. In
the first place, all of the countries of origin and countries of
destination are given for each article — there are no baffling
"other countries" to contend with. In the second place, a com-
parison is afforded with each of the four years immediately pre-
ceding the last. Another feature that deserves mention is the
recapitulation under each article showing the imports or exports
by continents.
The list of articles in these two annual tables is about the
same as that in the "Monthly Summary," but not as
detailed as in the Quarterly. Quantities are shown wherever
possible, and values in all cases. The tables are used for the
most part in making studies of the origin and destination of
the goods that enter into our foreign trade. If the chemist
wishes to find out where our quebracho imports originate, he
turns to the index for the page he wishes and soon comes upon
the quantity and value of the imports for each contributing
country for the last five J
The third annual table mentioned as being of interest to the
chemist is No. 9, which is an annual compilation of the quarterly
statistics already described. It has the same ad\, I
Nov.. 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
93 5
feature of great detail and the same disadvantages of not fur-
nishing a comparison with preceding periods and of not indica-
ting the origin of the imports. If all the countries of origin
were shown for all the articles given and comparisons made with
preceding years, this table alone would be larger than the en-
tire volume now devoted to the annual statistics. Possibly the
day will come when such a table will be issued, but the demand
from many industries will have to be much stronger than it is
to-day.
There is also included in this volume a table showing our ex-
ports of foreign merchandise, that is, our re-exports of foreign '
goods. It may occasionally happen that items in that table
will interest the chemist. There are twenty-one other tables
that need not be described. A good index prevents any con-
fusion that might otherwise result from gathering so many
tables under one cover.
STUDIES OP COUNTRIES
The "Commerce and Navigation" is intended to facilitate
commodity studies, and is not well suited for studies of coun-
tries. If a chemical manufacturer wished to study our trade in
caustic soda he would find his information in "Commerce and
Navigation;" but if he wished to survey our chemical trade
with Argentina, say, he would be almost obliged to turn to our
"Trade of the United States with the World," in which each
country is taken up separately and its import and export trade
with the United States shown in detail by articles.
This work has been published every two years in two vol-
umes, one for imports and one for exports. There is no particu-
lar reason why it should not be published every year, and from
now on it is going to be.
The statistics are for fiscal years and comparison is made
with returns for the year immediately preceding the last.
COMMERCE REPORTS
For the chemist who wishes to have something more than
just the statistics of our foreign trade in chemicals there is
available the Bureau's daily "Commerce Reports." which relies
for its material upon the American consuls, traveling special
agents, commercial attaches, trade commissioners, and the ex-
perts in the Washington office.
The reports from these various sources cover practically all
phases of foreign trade, but for the most part may be said to
aim at promoting the sale of American goods in foreign markets.
A fair proportion of them bear directly on markets for chem-
icals and allied materials and products, although there are not
as many on heavy chemicals as there will be when the manufac-
turers of those lines go in for foreign trade on a large scale. When
the demand for information increases, the supply will increase.
Reports on the markets for such lines as medicinal preparations
and pharmaceutical supplies are much more numerous, while on
such allied products as paper there is no end of information.
The reports vary widely in character. There may be one on a
pressing temporary shortage of caustic soda in Brazil, while
another may review at some length the conditions that govern
the use of caustic soda in that country, with an opinion as to
future developments that will affect the market. I Hhcrs may
throw light on the subject of packing chemicals for certain
markets or on tariff regulations.
Sources of raw materials also receive attention and not a few
reports are devoted to the appearance of new products in the
various countries and to new manufacturing processes.
Actual opportunities for selling goods or forming busil
nections are featured in a separate department, usually made
up i thi la i page of the paper. Millions of dollars' worth of
American gootls have been sold through these trade opportuni-
da goodly share has been chemicals 01 allied products
Hut of course tin papi r appeal
merely glances over it, and perhaps misses a numbei 1 1 ionally,
he will not gain more than a very general impression of what
is going on in the foreign trade. If he wishes to follow develop-
ments more carefully and get practical results, he must devise
some way of getting together the material in which he is most
interested and keeping it easily available. It is at that point
that many manufacturers, chemists among them probably, de-
cide not to see it through.
It happens that I do not know a chemical manufacturer with a
working method for extracting the good metal from this
mass of ore, but I do know of a system devised by one of our
largest hosiery manufacturers. He, the president of the con-
cern himself, spends two or three minutes each morning in
marking material in Commerce Reports for filing. His stenog-
rapher then clips the marked passages and pastes them on
colored paper. White paper is used for reports on hosiery,
yellow for reports on miscellaneous wearing apparel, and green
for any reports on general conditions that might possibly have
a bearing on the demand for hosiery. These are filed by coun-
tries and take up very little room. When he wishes to brush
up on the hosiery business in Argentina, there is his informa-
tion right at hand in the most convenient form imaginable.
There seems to be no reason why some scheme of this sort would
not be just as convenient and valuable for the chemical manu-
facturer.
However, there is a quarterly index that simplifies matters
greatly for those who do not care to establish a file, especially
if a set of bound volumes is maintained.
Annual reviews of the trade and commerce of the various
countries are printed separately as supplements to Commerce
Reports, one for each country. These vary in size according
to the commercial importance of the country, but the contents
are rather uniform, as the business conditions of the year are
reviewed and statistical and other information is given as to domes-
tic production and foreign trade. Special attention is given to
the progress American goods make in the market, and the pros-
pects for the future. These reviews are really up-to-date little
commercial handbooks and are extremely valuable in re-
viewing current commercial progress in any country. The
chemical trade of course receives its share of attention in coun-
tries where it is comparatively important.
SPECIAL REPORTS
The Bureau issues a great many special reports, the majority
of which are devoted to the markets for specified lines of goods in
specified countries, or districts, although some are devoted to
studies of basic economic conditions and some are on unusual
but opportune subjects, of which Dr. Norton's reports on the
dyestuff situation in this country and the census of dyestuff
imports are examples.
The special reports on markets are written by consuls, com-
mercial attaches, and traveling special agents, principally the
last named. These traveling agents are specialists in certain
lines, such as cotton goods, agricultural machinery, and shoes.
Unfortunately, there has never been in the past a sufficient demand
from the industry to warrant a special investigation of the for-
eign markets for American chemicals, but there is such a study
011 the program for Latin America for the present fiscal year
and if sufficient intrust is shown in that there will probably be
■ iili' 1 , 10 follow. The pressure brought to bear on the Bureau
foi uch inve tigations is the only index it has as to the atti-
tude of the industry,
The catalog of the Bureau's publication will show what
i .( to the chemist have been pub-
lished iii the past, ami announcements of new reports are i" mini
I ' !
MM MARY
\ aL formation pub-
Bureau "i Foreign and Dorm itic Commerce can
936
THE JOURNAL OF 1 SDVSTRIAL AND ENGINEERING CHEMISTRY Vol. io, No.
be approached at two different angles by the chemist. He may
not be after practical results, as figured in dollars and cents.
He may simply wish to keep abreast of the new expansion of the
industry in which he is engaged, to know what is going on. A
great many people are going to take that sort of interest in for-
eign trade in the future, just as the average Frenchman or
Englishman keeps himself fairly well posted on foreign invest-
ment markets, whether he has any money invested abroad or
not. We ought to take at least a cultural interest in the great
industrial and commercial developments of the country.
But many chemists are going to look at the matter in a very
practical manner. To lay a sure foundation for future success
they must familiarize themselves with conditions in foreign
fields. They must come to look upon business with Argentina,
or China, or South Africa, as they now look upon business in
the Pittsburgh territory, or the Chicago territory, or the New
England territory. It really is not much different when you
become accustomed to the longer focus.
The practical minded chemist will also find it necessary to
study the facts of our own import trade if he is to make sure
progress in his efforts to manufacture here at home the chemicals
we formerly purchased abroad. The forthcoming census of
imported chemicals is being made to the order of the American
chemists.
As the chemists get along in their studies of the Bureau's
data they will soon be able to make suggestions for additional
service, and I can assure them that the sooner they come the
better the Bureau will like it.
THE METHOD OF PREPARATION OF THE CENSUS OF
CHEMICAL IMPORTS
By E. R. PlCKRKLL
Special Agent, Bureau of Foreign and Domestic Commerce
It was with pleasure that I accepted the invitation of Dr.
Herty to state briefly for your information the method of prepara-
tion of the Census of Chemical Imports. As you gentlemen
well know, the idea of this census was conceived by your
fellow member, Dr. B. C. Hesse. Upon request of representa-
tives of the American Chemical Society, the Department
of Commerce undertook for the benefit of American chemical
manufacturers this monumental statistical work. The Census
of Dyestuffs which was published in 1916 by the Bureau of
Foreign and Domestic Commerce was the initial undertaking
of this kind by any branch of the United States Government.
How well Dr. Norton accomplished this vital and timely task
is shown by the fact that requests for copies of the dyestuff
census have been received even from foreign countries. To-day
the domestic dyestuff manufacturers have at their disposal
information concerning the importation of dyestuffs into the
United States which is of inestimable value for the development
of a permanent domestic dyestuff industry.
The Census of Chemical Imports is a much greater and more
difficult task than the dyestuff census, for it entails the procure-
ment of information relating to a vast and varied number of
articles. The statistical data presented by this census will be
of value not only to chemical manufacturers but also to the drug
manufacturers, synthetic medicinal manufacturers, perfumery
manufacturers, paint and varnish industries, oil industries, and
fertilizer industries.
During the fiscal year 1913-1914, chemicals, allied chemicals,
drugs, and medicinals imported into this country totaled in
value $176,000,000. This total was divided as follows:
Chemicals, drugs, dyes, and medicines $95,000,000
Oils 46,000.000
Fertilizers 23, 000,000
Tanning materials 2,000.000
Perfumes 2,000,000
Paints 2 000 000
Glue 2.000,000
Grease and oils 1 , 000 , 000
Soap 1,000,000
Olcostearin. dyewoods, beeswax, and blood (each) 500,000
Inasmuch as the object of the Census of Chemical Imports
was to show the quantity, value, country of origin, and per cent
of the quantity imported from each foreign country of every
chemical, drug, allied chemical, and medicinal imported into this
country for the fiscal year 1913-1914, the last normal year,
and since there was no available statistical data in this country
setting forth this information, it was necessary to examine every
invoice filed at the different customhouses in this country
during that one fiscal year.
In view of the fact that more than sixty per cent of all the
articles imported into the United States come through the Port
of New York and that probably seventy-five per cent of all the
chemicals imported are entered here, it was deemed advisable
that the clerical staff engaged on the census personally examine
the New York entries.
The original request was made to the Secretary of the Treasury
that all invoices, some 700,000, received in the United States
for the fiscal year 1913-1914 be forwarded to the Port of New
York for examination by the staff engaged on the census. That
official was of the opinion this procedure would not be advisable
because of the increased liability that some of these very valuable
records might be lost or destroyed in transit. The alternative
procedure was then adopted of sending circular letters of in-
struction, with an appended alphabetical list of 3500 chemicals,
allied chemicals, drugs, and medicinals to the collectors of the
headquarters ports of the forty-eight customs districts into
which the United States and its territorial possessions are
divided, requesting that invoices covering all these articles be
forwarded to Newr York.
It is the aim of the census to amplify Schedule E of Imports,
that is, Table 9 of the Commerce and Navigation Reports
published by the Bureau of Foreign and Domestic Commerce,
maintaining the same classification as closely as possible, but
always keeping in mind that the purpose of the census is
purely commercial. Consequent^ the commercial classification
has had precedence over scientific terminology. It would have
been a much easier task to have devised and employed a strict
scientific classification and disregarded entirely Table 9, which
follows more or less closely the Tariff Act of October 3, 1913.
This amplification is to show the quantity, value, and per
cent imported from a foreign country of every chemical, allied
chemical, drug and medicinal imported into this country during
the fiscal year prior to the European war. In other words,
the seventy-five classes covering these articles provided for in
basket clauses in Table 9 are to be amplified into over three
thousand articles. By means of this amplification each article
will be specifically designated instead of being grouped to-
gether, as formerly, in general terms or basket clauses. For
example, Table 9 now provides for 32 acids by name. The
Census of Chemical Imports will show more than 60 acids by
name. Every acid imported into this country in the fiscal year
1913-1914 will be provided for in the census. This same table
lists 21 soda compounds. The census has already more than
52. There are an unlimited number of articles, many of which
are of common chemical usage which will be provided for
definitely in the census and which are at present hopelessly
lost in the basket clauses. Table 9 does not show more than
half a dozen synthetic medicinals; the census will show every
synthetic medicinal imported during that year. Whereas in
Table 9 medicinal compounds, preparations, and salts to a
value in excess of $315,000 were grouped together in one general
class, the census will completely subdivide this class so that
probably more than 150 different medicinal preparations will be
shown. Then again, crude drugs valued at over Si, 000,000
were imported during the fiscal year 1913-1914. These drugs,
which were divided into two general classes in Table 9, will be
completely separated into over 250 different articles.
To gather this tremendous amount of detailed information
a staff of 24 clerks has been employed, some since March 1918,
Nov., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
937
in translating and transcribing the necessary information from
more than 35,000 invoices gathered from every customs district
in the Union.
For every single article mentioned in each entry an individual
card was made, stating thereon the country of origin, the quantity
and value, and the English name as translated from the foreign
language. More than 90,000 such cards were made out. These
90,000 cards were then assembled into groups containing the same
articles, and the quantities and values, according to country of
origin, were totaled. This information was then transcribed to
larger cards and the foreign monetary and quantitative terms con-
verted into American dollars and units of weight. The quanti-
ties from the various countries of exportation were ascertained
and expressed in percentages employing the entire quantity im-
ported as the equivalent of one hundred per cent. The follow-
ing are examples of the information to be presented in the census
and the manner of presentation :
Quantity Country Per
Value Lbs. of Origin cent
Titanium Potassium Oxalate 8839 4,859 Germany 53.9
England 46 . 1
Carbon Tetrachloride $32,616 657,409 Germany 97.9
Italv 1.9
Canada 0.2
Tartaric Acid $218,856 906,614 Germany 39.1
England 19.8
Italy 17.1 j
Austria 9. 1
Netherlands 7 . 8
France 7.1
The mass of statistical data collected was so great it was
deemed advisable to incorporate in the body of the census only
those articles having a total value in excess of Sioo. At present
there are over 3,000 articles having a value of over Si 00, as
compared with 75 classes now provided for in Table 9. The
number of articles is steadily increasing and will approximate
about 4,000. Those articles having a total value less than
Sioo will be listed alphabetically as an appendix to the census.
The grand total value of all these articles less than $100 will be
shown in the census.
It is hoped *that this Census of Chemical Imports will clearly
present to domestic manufacturers of chemicals, allied chemi-
cals, drugs, and medicinals what they may expect in the way of
foreign competition when this world conflict is over; that this
information will be in such detail and so definite that American
production of these commodities will be stimulated; that every
American manufacturer dependent upon these commodities will be
able to obtain them as a result of American production ; and that
an American chemical industry brought into existence through
extraordinary circumstances will remain and grow to be one
of the bulwarks of American industrial progress and development.
Would it not be advisable to present to the American manu-
facturers in a series of half a dozen well-stated publications,
covering the chief classes of materials provided for in the census,
such as coarse chemicals, paints, perfumes, oils, fertilizers, and
synthetic medicinals, the information contained in the census
relating to these articles, the quantities and values of the same
imported during the year 19 17-19 18, and the quantities and
values produced and consumed in the United States during the
same year, so that each manufacturer of a particular class of
articles will be cognizant to a minute degree of all factors affect-
ing his trade?
CURRLNT INDUSTRIAL NEWS
By A. McMillan, 24 Westend
ANALYSIS OF WHITE METAL
As rapid analyses of white metal are frequently made, the
following note on the subject, which appeared in the Z. angew.
Chem., for April 30, may be of interest. About 1 g. of the metal
borings is dissolved in 10 cc. nitric acid, density 1.4, the solu-
tion being diluted with 50 or 100 cc. hot water, boiled for 5
min., and then filtered. The moist precipitate (consisting of
oxides of tin and antimony) is washed into a conical flask,
heated and diluted with water; about 2 g. of pure powdered
iron are then dropped into the flask and the liquid is kept at
80° C. for about 1 hr., air being excluded. The tin will have
dissolved as stannous chloride, which is estimated by ferric
chloride, while the antimony is precipitated as metal on the
excess of the iron which is extracted with hydrochloric acid.
The original filtrate contains the lead, copper, iron, and zinc
of the white metal. Sulfuric acid is added to the solution which
is evaporated to dryness and redissolved in water. The lead
remains insoluble as sulfate and the other metals pass into solu-
tion. The copper is precipitated by sulfureted hydrogen;
the iron is oxidized by bromine water and precipitated as hy-
drate by caustic soda. The zinc is finally precipitated from
the filtrate, previously made acid with hydrochloric acid, by
soda.
LUBRICATING OIL
Oil of a quality suitable for aeroplane motors is being obtain' '1
in Russia largely from hcmpsccd. The press., produci 1 yield
of from 5 to 6 per cent of a dark gray colored oil. Refilling and
filtering processes give as a pure lubricating product, 30 per
cent of a clear yellow oil. The crude residue is used fur soap
making. As the manufacture has been carried on mainly by
Austrian prisoners of war, the processes will soon be made
known in Austria and Germany where, consequently, large
quantities of seed are already available.
Park St, Glasgow, Scotland
VENEZUELAN TRADE INQUIRIES
The British Consul at Caracas reports that a firm of com-
mission agents in that city desires to represent in Venezuela,
firms dealing in drugs and medicines, hardware, etc., also that a
firm at Barquisimets would be glad to get into touch with firms
interested in importing castor-oil beans. These latter have
recently, in not inconsiderable quantities, been shipped to the
United States, and in view of the good market obtained, this
plant, previously regarded as a weed, is now being assiduously
cultivated in Venezuela. The oil furnished by these beans is
said to be the only one which satisfies all the requirements for
lubricating aeroplane engines.
POTASH SALTS IN CHLLE
The existence of nitrate of potassium as a by-product of the
nitrate of sodium industry has been engaging the attention of
chemists and mining engineers in Chile for some time past.
According to the Canadian Weekly Bulletin, one of the best known
scientists in Chile claims to have discovered a process for its
extraction by refrigeration and is proving the efficiency of the
process by practical application. From his investigations he
has ascertained that potash exists in all the nitrate regions, be-
ing most plentiful in the Tarapaca region, followed by Taltal,
Antofagasta and Tocopilla in rotation of importance. Out of
165 oficinas, there are at least 100 whose caliches contain 1 to 2
per cent of potassium nitrate I [e estimates that in the residues
of the saltpeter industry. 600,000 tons thrown
away yearly. Analyses made of saltpeter ready for shipment
proved the existence in this of 0.7 to 3.6 per cent. If an aver-
age of 1 per cent be taken out of 3,000,000 tons of sodium ni-
trate exported, there art |O,OO0 tons of potassium nitrate given
H tin- 000,000 tons thrown away in the residues of the
oficinas supposing that only 60 per cent is utilized, there remain
' t ation 360,000 tons.
93»
THE JOURNAL Of INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. n
NEW CONCRETE MIXER
A machine recently brought out by Messrs. Winget, 25 Vic-
toria St., London, says the Times Trade Supplement, is designed
particularly for the efficient mixing of semi-wet concrete, though
it is also adapted to the mixing of concrete of any consistency
to the other extreme of wetness. It consists of six patent chain
paddles rotating at 35 r. p. m. in a semi-circular trough. Pad-
dles of this form, it is stated, increase the mixing by more than
100 per cent as compared with the solid spades previously used,
and also present the advantage that no stone can wedge be-
tween them and the trough so that aggregate of any shape or
description can be used. The cement and aggregate are fed
into a hopper above the trough into which they are discharged
by the depression of a lever, and water is added at any stage in
any quantity by turning a tap in an overhead pipe, which in-
sures even distribution. The mixed concrete is finally dis-
charged by pulling a second hand lever, which rotates the trough
on its trunnions. At present the machine is being made in
one size only, with a capacity of 3 cu. ft. Through this 60
completely mixed charges can be passed in an hour, equivalent
to 67 cu. yds. per working day of 10 hrs. The machine, which
weighs i1/* tons complete, is driven by a 2' '•> h. p. paraffin
engine. A larger size with a capacity of '/» cu. yd. is now being
tested and will, it is expected, be ready for commercial manu-
facture shortly; its weight complete is about 3 tons and it is
driven by an 8 h. p. paraffin engine, which is arranged through a
friction clutch also to rotate the trough on its trunnions for
discharge.
COMBUSTION OF COAL
It has been shown by experiment, says the Engineer, that the
sulfur contained in coal in the form of pyrites is not the chief
source of spontaneous combustion, as was formerly supposed,
but the oxidation of the sulfur in the coal may assist in breaking
up the lumps of coal and thus may increase the amount of fine
coal which is particularly liable to rapid oxidation. Even this
opinion is not unanimously endorsed. In spite of experimental
data showing that sulfur is not the determining element in spon-
taneous combustion, the opinion is widespread that, if possible,
it is well for storage purposes to choose a coal with a low sulfur
content.
BATIK DYEING PROCESS
A special display of textiles dyed by the Batik process was
exhibited at the Leipsic Spring Fair this year and in a statement
issued by the Textil Zeitung information was given that the use
of the process was spreading rapidly among manufacturers and
was likely to become a great and important branch of the textile
industry after the war. "Batiking" is well known to United
Kingdom manufacturers and United Kingdom firms were the
first to offer to the Straits Settlements, where it was originally
introduced from Java and is exceedingly popular, goods dyed
either by the same or a modified batik process. The Textil
/filling claims that the process has been amplified and perfected
in Germany during the war. Certain tissues, which hitherto
would not take certain colors, can now be dyed. Stuffs, blouses.
stockings, hats, etc., can be redyed by it when they are old and
can take a lighter color or be entirely changed. It has been
possible to use apparently useless or faded goods. The follow-
ing account of the batik process written by an authority in the
Netherlands Hast Indies is of interest: To batik signifies to
cover a cotton fabric with a thin ground of wax before plunging
it into a bath of dye so as to preserve from the latter certain
parts of the stuff thus forming a design. This operation, re-
peated several times in succession but with a dye of different
color on each occasion, and with the stuff recoated so as to pre-
serve different portions from the dye, finally produces a design
which is often of real artistic value.
LAMP TESTS
In the Schweizerische Eleklrotechnische Zeilschrift, for January
5 last, is given a summary of the results obtained from tests
of various lamps with the orthochromatic plates and silver eosin
plates prepared by two German firms. The tables show wattage
and candle power of various lamps and their actinic value, abso-
lute and per watt and per Hefner candle power for both kinds
of plates with and without yellow filters. The lamps tested in
this way were the Hefner lamps, vacuum and gas filled, tungsten-
wire lamps, arc lamps with solid carbons and yellow and white-
flame carbons, enclosed arcs and quartz-enclosed mercury arcs.
NEW RADIOACTIVE ELEMENT
The Client. Trade Journal, 62 (1918;, 512, quoting from the
Munehener Xewste Nachrichten, says that after a number of
unsuccessful attempts by several scientists to discover the
mother substance of actinium, recent efforts have succeeded
not only in isolating this substance but also a new radioactive
element of great emissive power. L. Meitner states that the
material taken as a starting point for the investigation was the
residue, insoluble in saltpeter and acids of pitchblende, which
forms the raw product of radium. This residue was subjected to
treatment which finally left undissolved only the substance of
the tantalum group, and this final residue showed a radiation,
at first weak but afterwards increasing greatly though grad-
ually, which mainly proceeds from the evolution of actinium,
showing that the element contains actinium and must, indeed,
be its mother substance. The new element has been named
Protactinium. Its period of semi-integration, i. e., length of
time which elapses before half the atoms are separated from
one another, probably fluctuates between 1,200 and 18,000 yrs.
The production of protactinium requires large quantities of
raw material; for about 1 kilo of the pitchblende residue insolu-
ble in saltpeter and acids 73 milligrams of protactinium are
obtained. The substance is obtained in the form of a white
powder which contains the new element at first only in very
small proportions and with a large admixture of earthy acids.
Experiments for the separation of the element from the acids
will be undertaken immediately.
RUBBER-SEED OIL
The report of the Federated Malay States Agricultural De-
partment shows evidence of the growing tendency to apply
scientific methods to the rubber industry'- A description is
given of the method of manufacture of rubbtr-seed oil and its
residual product with a view to putting it on a commercial
basis. It would seem, from the report, that this high-grade
oil requires hardly any refining, is obtained from a waste product
available in great quantity, easy to collect, transport and store
and easy to crush. It would certainly pay in normal times
to ship the seeds or kernels but, as the prospects of ft eight
facilities for some years do not present a bright outlook, it
would seem that shipping the oil is the better proposal. Oil
keeps better than seeds and is more easily stored. Experiments
with a consignment of 30 tons of seeds sent to England resulted
in $250 per ton being obtained for the oil, while $40 per ton was
realized for the residual cake. At the time unseed oil stood
at $300 per ton. The difference of $50 per ton may be put down
to the prejudice with which all new products have to contend.
As far as can be foreseen, rubber-seed oil will occupy .1 place
but little inferior to linseed oil as soon as the world's markets
have acquired confidence in the new product. Finally, the
production of rubber-seed oil would not interfere with the
market for coconut oil or sesame, as these oils are used essen-
tially as human foods in the form of margarine and cooking
fats. These oils are never used [as rubber-seed oil is likely to
be"! for paints, varnishes, red and white lead, packing composi-
tions for joints, soft soap manufacture and the like
Nov., 1018
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
THE SCHOOP METAL-SPRAY PROCESS
According to a note by K. Matzinger in the Anzeiger fiir
Elecklroteknik und Maschinen-Bau, April 28, 1918, by increasing
the "atomizing pressure" in the pistol of the Schoop appara-
tus, metal deposits of very fine grain and high density and
strength have recently been obtained. The pistol is a blow-
pipe in which the metallic bead, fused by the flame, is torn away
and atomized by the current of compressed air. The ordinary
working pressure of the air is 3 . 5 atmospheres, but the pistol
operates on the injector principle and the actual atomizing
pressure was so far only 1 . 5 atmospheres. This pressure has
recently been raised to 2 . 5 and 3 atmospheres without increas-
ing the working pressure, with very promising results. A lead
pipe, 1 mm. wall thickness, made by the improved process, was
filled with hydrogen at 5 atmospheric pressure while lying in
water; no hydrogen escaped while hydrogen bubbles forced
their way through a lead pipe made by the old process. In
another experiment plates of sheet iron were covered with lead,
one or two coatings at pressures of 1.5 or 2.5 atmospheres.
The one or two coatings of the old process did not prevent sub-
sequent rustings of the iron, but both the one coating and the
two coatings of lead deposited at the higher pressure kept the
plates free from rust when they were placed in water.
CATALYTIC PROCESSES IN GERMANY
The Badische Anilin Company is developing some promising
catalytic processes, says the Gas World. When a mixture of
two volumes of carbon monoxide and one volume of hydrogen
is passed over asbestos impregnated with cobalt or osmium
oxide and some caustic soda, at temperatures from 300 ° to 420 °
C. and pressures from 100 to 120 atmospheres, the result is the
production of water, carbonic acid, methane, higher hydrocar-
bons and oxygenated compounds such as aldehydes. The hydro-
carbons are saturated and unsaturated with a boiling point
above 2500 C. If carbon dioxide is used instead of carbon
monoxide, the yield of hydrocarbons is reduced. By adding
nitrogenous or sulfur-containing components to the gas mix-
ture employed, nitrogenous or sulfur-containing organic com-
pounds are produced by the catalyzers. Catalyzers of higher
heat conductivity, such as rods or wires of metals or carbides,
especially those of the iron group, tend to prevent the reaction
from hanging back.
CADMIUM IN BRASS
As much of the zinc now imported into France contains con-
siderable proportions of cadmium, Leon Guillet (Comptes rendus,
March 6, 1918) has investigated the influence of cadmium on
the mechanical properties of brass. He prepared alloys contain-
ing 70 to 60 per cent copper, 28 to 40 per cent zinc, and up to
4.54 per cent cadmium. The high percentage of cadmium is
accompanied by a relatively high percentage of lead to which
Guillet does not draw attention. The other impurities were
iron and tin, neither present in more quantity than o 1 per
cent. He found that cadmium had little influence on the proper-
ties of the brass, as long as cadmium did not exceed 1 per cent,
and higher percentages are fortunately rare. The influeo
cadmium was distinctly deleterious. It lowered the hardness
and general strength and this was particularly noticeable 111 the
impact tests which were made on notched bars. 1 h< ' longation
was hardly affected as long as the cadmium remained below 2
per cent. For low percentages the cadmium could bl
in fine lines surrounding the grains of alloy; when the per©
went higher the cadmium was Been to be isolated in round grams
It would appear that the cadmium enters into olid olution
when present in small proportions The detrimental effect
of the pn lenci ol cadmium wert more striking in an a than in
an a-0 brass.
ACID RESISTING FERROSILICONS
The publication by Camille Matignon in Comptes Rendus of
May 2i, 1918, of the results of corrosion tests of his comes some-
what late. He conducted tests in 1913 with the alloys then
obtainable and the analyses and corrosion values are interesting.
His alloys contained between 13 and 17 per cent silicon, nearly
1 per cent manganese and in addition to the usual phosphorus
and sulfur only the constituents we mentioned. The rnetilluie
of Adolphe Zouve contained 2 .5 per cent aluminum; one of the
two elianites (an Italian product) contained 2 . 2 per cent of
nickel and seemed to be less corrodible, owing to this constit-
uent; the other ferrosilicons were ironac and duriron. Matignon
further tested a ferroboron containing 70 per cent iron, 15 .4 per
cent boron, 4 . 9 per cent silicon, and 3 . 3 per cent manganese ;
and Borcher's metal, a nickel chromium alloy containing 64 . 6
per cent nickel, 32.3 per cent chromium, 0.5 per cent silver,
1 . 8 per cent molybdenum. The corrosion tests were made in
boiling nitric acid and in boiling acetic acid and butyric acids,
concentrated and diluted. The ferroboron was easily attacked;
the Borcher's metal differed from the other alloys by resisting
diluted acids better than concentrated acids, but was not other-
wise superior to them. The best metillure was a very homo-
geneous alloy. None of the alloys resisted hydrochloric acid,
and there is no mention of sulfuric acid. Some of the tests
were continued for a period of 360 hrs.
NEW NORWEGIAN INDUSTRIES
A recent exhibition in Christiania illustrating Norwegian in-
dustrial self-help shows that an extensive work has been under-
taken to make Norway more independent of foreign supplies.
A factory for the making of crucibles based on artificial graphite
from the Arendal Smelting Company will soon commence opera-
tions at Langesund. Ferromanganese was formerly imported,
but is now made at the Fiskaa Works, several concerns having
taken up the manufacture of electrodes, of which 8,000 tons
were formerly imported per annum. The requisite quantity of
sulfate of aluminum, some 400 tons per year, is now being made
within the country. Chloride of lime, soda lye, glue and various
dyestuffs, red lead, etc., will be manufactured on a basis which
will leave some for export, after the country's requirements
have been met. Iodine, which formerly it did not pay to manu-
facture on account of the powerful Iodine Trust which the war
has broken, will now be made on a scale large enough to supply
all Scandinavia. A Holmestrand concern has worked out new-
methods for the preparation of bismuth and various prepara-
tions from it. Nitrocellulose and collodion 'cotton are now being
made from ordinary cellulose, which seems to yield a suitable
product. Formerly Norway imported her entire requirements
of grinding materials, especially from America, Germany, and
Austria, but now these are being entirely covered by home
manufactures. The exhibition also comprised electric lamps,
porcelain articles for electro-technical purposes, and material
for the complete equipment of electric installations, electric
cables, etc.
NEWFOUNDLAND COD-LIVER OIL
The Imperial Institute, London, 1- calling the attention of
importers to Newfoundland cod-liver oil. Hitherto the bulk
of tin- refined medicinal 1 od liver oil used in the Empire has been
of foreign origin. Newfoundland having devoted attention chiefly
to the production of industrial cod-liver oil for currying leather.
The Oldest British colony has, however, now taken its cod -liver
oil industry seriously in hand and is in B position to providi
oo< onlj the industrial oil, foi which it is famous, but also refined
oil equal in quality to the finesl medicinal oil produced in Nor
The Imperial Institute 1 1 prepared to supplj analj
oi Newfoundland oil, 1 1 ol 1 tportera ind otha information
on the subject to importers interest d in thi branch of trade
94°
THE JOURNAL OF INDUSTRIAL AND ENGINEERI N(i CHEMISTRY Vol. 10, No. n
NATIONAL METAL AND CHEMICAL BANK
The directors of the National Metal and Chemical Bank have
issued a circular, says the Chemical Trade Journal, detailing the
objects of the bank. For the purpose of its business, it is to
assist "in the coordination of British interests in the base metal,
chemical and allied industries." It has already acquired ex-
tensive interests in undertakings producing iron ore, coal and
the principal nonferrous metals and, through its associated
concerns, is in a position to arrange for the smelting and refining
of gold, silver, lead, bullion, lead ore, zinc ore, etc., and to sup-
ply all descriptions of manufactured lead, zinc and alloys. The
bank is also largely interested in chemical undertakings, pro-
ducing dyes of all kinds, sulfuric acid in large quantities, and in
superphosphate works in course of construction.
DISCOLORATION OF WHITE PAINT
Zinc-white enamels frequently turn yellow and brown, espe-
cially in warm atmospheres both in the light and dark. In some
cases this discoloration is merely a staining of the paint with
atmospheric dust and dirt. In others it is not without reason
attributed to the presence in the pigment or oil of traces of
lead. Dr. D. F. Twiss discussed the question in the Journal of
Chemical Industry, June 29, 1918, and found that lead cannot
in all cases be responsible, since the discoloration sometimes pro-
ceeds in the absence of all sulfureted hydrogen and is not ac-
celerated by its presence. The linseed oil and varnish them-
selves tend to turn brown when absorbed by dry filter paper
and kept for a few hours at 60° C, and the brown color appeared
quite as readily when this experiment was performed in sealed
tubes, charged with pure carbon dioxide as under ordinary con-
ditions; thus the presence of oxygen and the action of high
temperature which would polymerize the oil, are not at all es-
sential, contrary to expectation. On the other hand, it proved
possible to bleach the brown tint again by the light rays from a
quartz-mercury lamp. For this reaction the presence of oxygen
is necessary as was expected, the real bleaching agent being the
ozone. Dr. Twiss was able to repeat the discoloration and bleach-
ing experiments several times with the same specimens. The
effects might also be due to the presence of manganese or of
alkalies, but the experiment in carbon dioxide is against the
latter assumption and, even if radioactivity should be con-
cerned in the phenomena, which is not unlikely, the color change
would ultimately be the manifestation of a chemical change in
the pigment or medium.
GAS IN GLASS INDUSTRY
At the annual meeting of the Society of Chemical Industry,
Dr. Morris Travers gave an account of the establishment of
-one of the three large British glass works which have been
brought into existence since the war began. Dr. Travers said
that in the early experiments at one factory oil-fired furnaces
were used, but eventually it was decided to put down a gas-
Bred furnace which was built and running in seven weeks and
was capable of turning out 5 tons of glass per week. This was
a non-recuperative furnace, but a later one was recuperative.
The greater control and quicker working which gas gave opened
up the prospect of knocking off the night shift which was now
necessary in this industry. Discussing the requirement in re-
gard to chemical glass, Dr. Travers commented on the fact
tli.it every chemist wanted an infinite range of beakers. That
meant that blowing machines could harly be used in the industry
because the large variety meant that only a comparatively-
few of each could be made. If it were possible, as he believed
it was, to have beakers in three si^es only, between the liter
and 50 cc, instead of eight, blowing machines could be intro-
duced which would considerably reduce the cost of manufac-
ture.
HEATING IN A LIQUID
There has been prepared by Messrs. J. Wright & Company,
Birmingham, says the Gas Journal, a useful booklet on the "Use
of liquids, consisting of fused salts or mixtures of salts for the
heating, quenching and tempering of carbon steel and high
speed steel." Attention is drawn to the advantages of heating
in a liquid and there are brief descriptions of various kinds of
melts that have been evolved for different purposes. There
are numerous difficulties encountered in the use of a lead bath
for heating, and these are pointed out. Barium chloride is
used for heating high-speed steel and "Pyromelt" for carbon steel
or carbonized work. The latter is so light that the trouble ex-
perienced in the case of lead of articles floating on the surface
does not arise. Then there is "Feusalt" for quenching high-
speed steel, for tempering and for heat treatment; "Tempermelt"
for tempering and for heat treatment; and patent "Quenchoid"
for tempering carbon steel and for heat treatment. The book-
let also contains illustrations of Wright-Brayshaw furnaces for
the various salts, and the final page is devoted to a comparison
of the Centigrade and Fahrenheit scales. Copies of the book-
let may be had on application to the firm.
SOURCES OF ORE
According to Metall und Erz, new sources of mineral wealth
are to be found in European Turkey. Copper ore exists in
great quantity in Turkish Rhodope in the neighborhood of
Yardimli. In the Turkish Balkans, ores of nearly all the metals
occur, while gold is found in Markova Reka, south of Uskub.
In the neighborhood of Kratova, gold, and galena, containing a
fairly high percentage of gold, have been found. Chromium ore
in abundance has been discovered near Xiausta on the Salonika-
Monastin railway. The mountain range of Southern Macedonia
is especially rich in chromium ore and there are also ores of
iron, antimony and lead.
BOLIVIAN WOLFRAM INDUSTRY
According to the latest available figures, nearly 25 per cent
of the output of wolfram in Bolivia is enemy-controlled. The
total production in 1916 compiled from figures giving the output
of the mines was: in non-enemy mines, 2,388 metric tons, of
which 1,364 tons were sent to the United States and 1,360 to
the United Kingdom; in mines belonging to the enemy, 658
tons were consigned to the United States.
GAS AND PETROL ENGINES
A series of vertical gas and petrol engines are described and
illustrated in a catalog sent by the Keighley Gas and Oil
Engine Company, of Keighley. They are made with one, two.
or four cylinders, and while the one- and two-cylinder types are
arranged for thermo-siphon cooling with radiator, water cir-
culation is employed in the four-cylinder type, a centrifugal
pump being driven from the cam shaft, as is the magneto, by a
silent chain. In the two- and four-cylinder engines oil is forced
under pressure to all the bearings by means of a geared pump
driven from the cam shaft by skew gears, while in those with a
single cylinder a pump of the plunger type is employed. A
centrifugal governor, totally enclosed with all its connections in-
side the crank case, is coupled direct to the throttle value in
the carbureter and varies the mixture to suit the load. A
number of self-contained electric generating sets, with the en-
gine, dynamo and all accessories mounted on a cast iron base
plate, are illustrated in the catalog, which also describes similar
self-contained air compressor and pumping sets, together with
stationary, semi-portable and portable engines for farm and
estate duty.
Nov., 1018
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
041
ANTIFRICTION METALS
A French report on new antifriction metals includes trials of
alloys consisting chiefly of aluminum, cadmium, magnesium,
and especially of zinc. Such alloys were designed to reduce
as far as possible the use of copper, tin, lead, and antimony,
and the most satisfactory results are stated to have been given
by a compound of 63.3 per cent zinc, 21.3 per cent tin, 12 per
cent lead, and 3.3 per cent copper.
HYDROSULFITES
At a meeting at King's College, London, Mr. F. Rogers said
that the value of hydrosulfites in their application to industry
seems to have been fully recognized by German chemists and
that much labor had been expended in the problem of solidifying
them. French and American chemists had also worked at the
problems with the result that they were now obtainable in a
stable form. Sodium hydrosulfite is extremely valuable as a
reducing agent, one of its principal uses as such being in dyeing
with indigo. It is also used for clarifying sugar, molasses,
edible oils, soaps, etc. It is a valuable straw bleacher and is
prepared in a convenient form for the removal of stains. Up
to the present time, English chemists have never taken sufficient
interest in the compound but now it can be obtained in large
quantities, thus enabling industries to be carried on, which
otherwise would have been crippled.
METALLIC LIQUIDS
A pamphlet received from Messrs. George Lillington & Co.,
of 40 Holburn Viaduct, E. C. 1., describes their "Metalo" liquid
which in various forms is used for hardening concrete and cement,
for waterproofing and hardening external and internal walls,
roofs and old work, for waterproofing wood and preserving it
from rot, decay and vermin, for hardening wood and plaster and
rendering them waterproof and fire-resisting, and for preserving
iron and steel work. Some tests are quoted showing the effect
of the liquid, which is merely added to the water used in mixing,
on the strength of concrete. Briquettes made of three parts
of sand to one of cement, which gave under pulling tests 275
lb. per sq. in. after 14 days, and 345 lb. per sq. in. after 28 days,
gave 316 lb. per sq. in. after 14 days and 388 lb. per sq. in. after
28 days when a 1 to 5 solution was employed. A 6-in. cube of
concrete, containing three parts of aggregate to one of cement,
together with 5 per cent of the liquid, had a crushing strength
of 43 . 6 tons at the end of 28 days, whereas the crushing strength
of a similar cube not treated with the liquid was only 33 tons
after the same time.
STARTING RHEOSTATS
A list received from the British Thomson-Houston Company,
of Rugby, describes two forms of starting rheostats for electric
motors, in both of which the switch and resistance are enclosed
in such a manner as to prevent access of dust and give complete
protection to all live parts. In one form, intended for use with
motors from 0.25 to 7.5 h. p., the contact brush is of the skate
type, pressed on the contacts by means of a steel spring, and
the starting period allowed is 30 seconds with normal full cur-
rent. In the other form for motors of 3 to 40 h. p. the contact
brush is made up of a carbon portion, which reduces sparking to
a minimum, and of a brass portion which carries practically all
the current; a starting period of 40 seconds is allowed. These
rheostats comply with the Home Office Rules for the use of
electricity in factories, and with the British Engineering Stand-
ard's Association's specification for normal duty rheostats.
They can be used for starting and stopping motors as often as
four times an hour, though this starting duty docs not repre-
sent the limit since the resistance units are constructed to with-
stand excessive temperatures without damage.
AIR RAH) SIGNALS
Engineering publishes some interesting particulars of the Chal-
lot rotating vanes and the series of horns forming the sirens
now mounted on monuments in numerous French towns to give
warning of the approach of hostile air craft. The siren consists
of a casing or stator within which an aluminum rotor revolves on
ball bearings. The stator and rotor each have a number of
openings generally rectangular. Vanes for canalizing the air
start from the center of the rotor and end at the rotor openings.
, When the rotor revolves centrifugal force drives the air through
the openings and the flow is alternately permitted or interrupted
according as the openings in rotor and stator coincide or not.
The rotor is driven by an electric motor of 12 to 15 h. p. Conical
horns of suitable shape and length are connected to each opening
of the stator in order to amplify the sound. The Paris sirens
have a total weight of 1,700 lbs. and in the city cannot be heard
beyond a radius of 1 .5 km. (under 1 mile), although in the open
the range may be as high as 8 to :o km. Hand-operated sirens
have also been built for giving the alarm in small towns.
OXIDATION OF AMMONIA
At the British Scientific Products Exhibition held in London
during August, a unit plant for the oxidation of ammonia to
oxides of nitrogen was exhibited. Such a plant was not ex-
tensively used outside Germany before the war and there is
reason to believe that the Germans have relied on it very largely
for their output of nitric acid for explosives, as well as in the
manufacture of sulfuric acid by the chamber process. The
method is now in use in this country and several large firms
such as Brunner, Mond and Company and the United Alkali
Company are using apparatus similar to the plant shown at the
Exhibition.
SYNTHETIC RUBBER
At a recent meeting of the German Bunsen Society held at
Berlin, the question of synthetic rubber was discussed and its
possibilities as a substitute for the natural product were con-
sidered. The world's requirements before the war amounted
annually to some 145,000 tons. Since 1914, however, the de-
mand apart from the needs of the Central Powers has increased
to 220,000 tons. Of this quantity America takes the greater
part. In the period 1910-12, according to the Client. Trade
Journal, 63 (1918), 162, attempts were made by Frantz Hoff-
man at Leverkusen to produce a substitute by synthetic pro-
cesses. These were in large measure successful but the constant
fall in prices of the natural product resulted in the partial
abandonment of the experiments. The enormous demand
brought about by war conditions and the shortage in Germany
and Austria have given fresh impulse to this promising new
branch of industry. In spite of the difficulty of obtaining
materials 150,000 kilos of methyl rubber are produced monthly.
It was not at first a wholly satisfactory substitute, for it became
oxidized in air and was somewhat refractory in the process of
vulcanization. These objectionable qualities have, however,
been in large part removed by improvements in manufacture.
By the addition of other substitutes a useful hard rubber, it is
said, is now produced, equal in firmness and durability to the
natural product, and 20 per cent better for electrical insulating
purposes. The accumulator boxes used in submarines are made
of this hard rubber. Soft rubber is more difficult to make.
At ordinary temperatures the product is not elastic but leather-
like. It becomes elastic as its temperature is raised. The
addition of dimethyl aniline and toluidine increases the elasticity
of the manufactured material. It is now used for tires for heavy
road motors. A factory of large extent has been built at Lever-
kusen, capable of producing 2000 tons annually.
942
I III. mi RNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol! 10. No. n
CORROSION OF BRASS TUBES
Two cases of condenser tub which had been badly
corroded by electrolysis, says Engineering, were examined by
the Mater ialprufungsamt, near Berlin, in 1916. One of the
brasses originally contained the following percentages of metals:
copper, 70.5; zinc, 28.8; lead, 0.21; tin. 0.28; iron, 0.08. The
corroded alloy contained copper, 97.4; zinc, 0.69; lead, 0.06;
tin, 0.46; iron, 0.08. The other brass gave the following analysis:
copper, 59.2; zinc, 40.37; no tin; iron, 0.32; lead, 0.24. The
corroded alloy had the composition: copper, 96.76; zinc, 1.29;
no tin; iron, 0.10; lead, 0.05. In both cases, hence, the corrosion
had bleached out the zinc and had also diminished the small
percentage of lead, while there was little or no change in the iron.
That the ordinary water of the supply main may give rise to
considerable differences of electric potential is shown by the water
of Charlottenburg, a suburb of Berlin. In this water, couples of
zinc and brass acquire a potential difference of 0.888 volt. In
view of the actual wide uses of substitutes for metals and alloys,
the Prussian government has drawn attention to this danger of
electrolysis.
TOOL STEELS
Two varieties of tool steel are described in folders sent out by
Messrs. Kdgar Allen and Co., Sheffield. One of these, known
as Red Label, is a tungsten crucible steel for twist drills, taps,
milling cutters, and similar tools. It possesses the qualities of
deep-hardening and density of structure, and, as compared with
ordinary carbon tool steels, shows from 75 to 100 per cent more
torsional resistance; and, though it is not a high-speed steel, it
will take a much higher friction heat than ordinary carbon
steel. After being heated carefully and thoroughly to darkish
cherry-red, say 1400° to 14360 F., it is hardened in clear water at
about 60 ° F. though small sections may be hardened at an even
lower temperature. The second steel, K 90, is intended for tools
in which extreme accuracy is required, and with it the expansion
and contraction ordinarily set up in the hardening process are
stated to be practically eliminated. It should be heated slowly
and thoroughly to a cherry-red heat, say 1436 ° to 1472°, and
quenched in oil. Both steels are sent out annealed and ready for
machining.
COMPRESSION STRENGTH OF GLASS AND QUARTZ
Some new experiments on the crushing strength of glass and
quartz conducted by G. Berndt, Berlin-Friedeman, were com-
municated last December to the Deutsche physikalischc Gesell-
schaft. The experiments were made on the Amsle testing
machine, maximum load 30 tons, first with cubes of the glasses
and quartz and then with cylinders. It was observed that when
cubes were used the strength decreased as the cube edge was
increased, in steps from 5 mm. up to 15 mm.; the cylinders
afterwards used had a diameter of 5 mm. and the same height.
The faces were either all polished or only those faces were
polished to which pressure was applied; this made little difference
and the rate of applying the load had likewise little effect on
Its, With stained glass, but well annealed, the strength
was smaller by 10 per cent with quick loading than with slow
loading. The final crushing to powder took place with almost
explosive violence. A borosilicate glass showed an average
strength of 15,200 kg pel sq. cm when strained and a higher
average of 16,900 kg (maximum, 18,400 kg.) when well annealed.
In the case of quartz the crushing strength was smaller by
25,000 kg. per sq. cm. when compressed parallel to the optical
axis than when the pressure was at right angles to the axis
(25,000 kg. to 27,000 kg.). These values for quartz are somewhat
higher than those found by Winkelmann, but lower than those
found for glass.
FATS AND OILS IN GERMANY
Before the war, says the Zeitschrift fur iingeuandte Chemie,
the annual production of vegetable oils in Germany was about
20,000 tons of animal fats, exclusive of cheese, about 1,000,000
tons, of mineral oil some 150,000 tons. To meet the demand
there were imported 270,000 tons of animal fats, 570,000 tons of
vegetable oil and 1,000,000 tons of mineral oil The demand
for animal fats may be satisfied by home production which in
times of peace may be greatly increased. Among the imports
of animal fats, American produce figures largely. Vegetable
oil came for the most part from overseas, but largely in the
form of fruit from which the oil was extracted in Germany, such
as linseed, rapeseed, cottonseed, palm kernels, soy beans, sesame,
etc. These have been imported from Africa, South and East
Asia, and the Argentine. In recent years, oil instead of soy
beans has been imported from East Asia. The chief source of
mineral oil has formerly been the United States; in future it is
likely to be Roumania.
DAMASCENE STEEL
In the Middle Ages, Indian steel, famous under the name of
damascene steel, was a product of great importance. A note
on the subject by Col. N. T. Belaieus appears in the Journal of
the Royal Society of Arts The Hindoos, particularly, seem to
have excelled in the manufacture of iron and steel, and the famous
wrought iron pillar at Delhi and other instances of their skill
still exist. In some of the specimens high carbon crucible steels
were undoubtedly used. Small cakes of the steel were ex-
amined by Reaumur and also by Faraday whose investigations
led to useful results. The fine watering of these Damascus
blades shows the great amount Of mechanical treatment to which
they were subjected, the Oriental maker never exceeding a
temperature of about 700° C. From the point of view of after-
war trade, the damascene process is of considerable interest.
CHINESE PENCIL FACTORY
An Anglo-Chinese enterprise has been started in Shanghai
to manufacture lead pencils. This is the first undertaking of
this character in China though there are several such factories
in Japan. The raw materials used at present are American
wood and graphite, while the machinery was made in Japan.
Though the factory is at present on a very moderate scale, the
possible output is estimated at 100 gross pencils per day and
there seems to be no reason why these China-made pencils
should not compete successfully with the foreign-made
articles chiefly imported from enemy countries before the war
It will, at any rate, be possible to turn out a very cheap article
and the quality promises to be sufficiently good to satisfy the
needs of the China market
JAPANESE-CHILEAN NITRATE ENTERPRISE
It is reported by the Japan Advertiser that efforts are being
made to undertake an enterprise for the working of niter deposits
in Chile under Japanese and Chilean joint management. There
has been a steady increase in the import of Chilean niter into
Japan In 1914 it amounted to no less than 24,000 tons, but
the figure for last year increased to 53,000 tons. At present the
total consumption of niter in Japan amounts to about 60,000
tons It is said that to obtain this quantity by working deposits
in Chile requires a capital of no more than Si, 000,000 and some
Tokyo business men are making efforts to undertake the enter-
prise in cooperation with Chilean business men. The Chilean
government sold 15 niter concessions by tender on August 1,
1918.
Nov., 1018
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
DRYING OVENS
Gas-heated drying ovens for enameling, lacquering, core
drying, armature drying, and other operations carried out at
temperatures up to 500 ° F. are described in a list published by
the Davis Furnace Company, of Luton, England. The most
usual types are the double-cased, with two casings, the inter-
vening space being packed with 2 in. of non-conducting material
and the products of combustion circulating through the heating
chamber on their way to the flue outlets; and the treble-cased,
in which the space between the two outer casings is packed
with non-conducting material and the products of combustion
circulate round the inner casing, so that the burnt gases do not
come in contact with the work to be heated. Natural draft
burners consuming gas at ordinary main pressure are employed
for heating, though the burners can be modified to use producer
gas when necessary in places where town gas is not available.
A thermometer is provided in each oven for temperature regula-
tion which can be accurately effected. To facilitate handling
and reduce transport charges, the ovens, the double-cased type
of which are made in various standard sizes ranging up to 9
ft. by 6 ft. by 6 ft. over all and the treble-cased up to 6 ft. by
5 ft. by 7 ft., are supplied in sections to be bolted together on
arrival.
RIVETING RECORDER
There is danger in riveting steam boilers by hydraulic pres-
sure that the pressure on the cup may be released before the
shank of the rivet has had time to cool. In such an event the
plates may spring apart to such an extent that the shrinkage
of the rivet in cooling is not sufficient to ensure a tight seam.
In a German technical paper a description was recently pub-
lished of an automatic recorder designed to overcome this
possible defect of hydraulic riveting. Pressure upon the warm
head of the rivet is transmitted through piping to clockwork
and sets a pointer in motion until the required pressure is reached.
This pressure is kept constant until a predetermined number
of seconds has passed when a red pointer indicates that the
pressure may be released and the pointer returns to zero. This
result is graphically recorded upon a traveling paper band from
which the pressure and the period of compression can easily be
read.
PLATINUM SUBSTITUTE
A platinum substitute tested, according to the Chemical Trade
Journal, in Amsterdam, was an alloy of 89 per cent of gold with
1 1 per cent platinum. This material, called platino, withstood
sulfuric, hydrochloric, and nitric acids, and other reagents used
in chemical work and was unaffected by heating for '/2 nr-
in a smoky petroleum-gas flame. It proved equal or superior
to platinum in ware for the chemist's laboratory except for the
large loss by corrosion when used in contact with a mixture "I
sulfuric and nitric acids.
NEW SOUTH AFRICAN INDUSTRIES
During the year 1917, the following new industries, ao ording
to the Report of the Industries Advisory Board, arc known 1"
have been initiated in the Union of South Africa and. in many
cases, to have commenced production: manufacture of calcium
carbide, chloride of lime, alcohol motor fuel, shoe and floor
polishes, sulfate of ammonia, asbestos, ai enic, tarch from
maize, paints and distempers from local materials, glue and iiae,
wax, also tin and antimony, smelling, wattle bark 1
tad detinning of scrap tin. Iii addition, a cemenl
capable of manufacturing 720,000 bags of [88 lb each !
commenced work nciir Mafeking.
AEROPLANE CONSTRUCTION
A catalog issued by Messrs. Accles and Pollock, Birmingham,
gives full-size illustrations, with equivalent diameters of the
special sections of weldless steel tubing they make for aero-
plane construction and other purposes. The sections are to be
numbered in hundreds and are of all forms — square, rectangular,
round-end oval, pointed oval, D, half-round stream line, etc.
There are tables giving the areas of sections of circular tubes
and the approximate weight in lbs. per ft. of all outside diameters
■from '/i6 in. UP to any size in i6ths for Imperial standard gauges
No. 6 to No. 26, and illustrations are added of wire strainers and
other ferrules made from solid drawn weldless steel tubing and
of various polished aircraft parts manufactured by the firm.
NEW STEAM MOTOR
A new form of steam motor which is expected to supersede
the internal combustion motor has been invented according
to the Danish press, by a well-known Danish engineer. The
new motor is mobile and the steam is supplied by pumping
water intermittently into a spiral where it is vaporized by a
blowpipe flame. The water circulates and is used again as in
a motor cooler and in much the same quantity. The motor has
three cylinders but has the same effectiveness as a six cylinder
internal combustion motor. It does not weigh more nor occupy
more space than an ordinary benzene motor. It is capable of
using the most inferior crude oils as fuel. It is simple in working,
can be easily controlled, and is said to be specially suitable for
use in fishing boats. Patent rights have been sold both in
Norway and Sweden.
A NEW PLASTIC COMPOUND
The nouinflammable and odorless plastic material described
in a late French patent is made from gelatin, glue, or other
animal product by the action of suitable chemicals. After
melting the gelatin or glue on a water bath at about 2000 F., a
decoction of hop flowers is prepared and added in a mixture
with dilute oxalic acid. Impurities are thus caused to settle
at the bottom. The liquid gelatin is poured into sheets or
strips, dried in cold air, and then colored with natural or artificial
dyes. The sheets are then treated with a bath of 25 to 30 per
cent or more each of formaldehyde, water, and alcohol, with a
little oxalic acid, tannin, and glycerin, after which they are
dried in hot air.
IRON AND STEEL TRADE OF ADEN
The iron and steel trade of Aden can not be considered as
large nor as offering a growing opportunity for manufacturers.
but, due to the cessation of practically all civilian building.
,, , ,1, to the difficulty in getting material, a field will be open to
manufacturers who can make prompt after-war deliveries.
The iron and Steel used a1 Aden is principally for construction of
lighters and buildings, for the repair and maintenance of small
plants used for manufacture of ice and condensing of water, and
foi repairs to ships. The slight increase noted recently in
impoits of nails, rivets, washers, etc., is due largely to the fact
that as no material is obtainable f'>r construction of new lighters
,in tomato extensive repairs to the present lighters.
ii,, deweasi in imports of "bar and channel iron" and "beams,
,, indi at hew the normal demand for building
materials have fallen ofl Several builders have expressed n
i import it. .11 and steel for building purposes from the
1 nited State., but have been deterred bj the high freight rati
and the COSt "f material.
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. n
SCIENTIFIC 50CILTIL5
RESOLUTION CONCERNING ORGANIC NOMENCLATURE
Editor of the Journal of Industrial and Engineering Chemistry:
The following resolution was passed unanimously by the
Division of Organic Chemistry at the meeting of the American
Chemical Society, held at Hotel Statler, Cleveland, Ohio,
September 12, 1918:
Whereas, The Journal of the American Chemical Society and
Chemical Abstracts have adopted and consistently employ the
pure English terms "benzene," "toluene," and "xylene," in-
cluding all of their derivatives, in place of the hybrid forms
"benzol," "toluol,'" "xylol," etc.; and
Whereas, these English terms alone are to be found in
publications devoted to pure organic chemistry, both in this
country and Great Britain; and
Whereas, industrial and technical journals have become
lax in their use of these strictly correct English forms; and
Whereas, the one-time confusion between the words
"benzene" and "benzine" now no longer exists, owing, primarily
to the discontinuance of preparation of this latter named prod-
uct, and, again, to a recent and well-made suggestion of the
term "benzolene" for this same petroleum benzine fraction, if
later to be placed on the market;
Therefore be it Resolved, that the members of the Division of
Organic Chemistry of the American Chemical Society shall
hereafter encourage the use of these English terms exclusively,
where and whenever opportunity permits.
It is requested that a copy of this resolution shall be sent
to the Editor of the Journal of Industrial and Engineering
Chemistry, with the hope that the German terms aforemen-
tioned may be replaced by the English throughout the pages
of the Industrial Journal, both in its editorial and advertising
matter. By this means we shall maintain a consistency in
organic nomenclature throughout all publications of our Society.
As stated herein, it is the wish of our Division that you and
your associate editors immediately consider our resolution and
transmit the same to other journals of the industrial chemical
world. William J. Hale,
Secretary
The above resolution was unanimously endorsed by the Division
of Industrial Chemists and Chemical Engineers at the Cleve-
land Meeting (see page 866, October issue), and has also been
endorsed by the Advisory Committee of the American Chem-
ical Society. In view of this unanimous expression of opinion we
shall endeavor to carry out the recommendation contained in this
resolution in the editorial columns of This Journal. — [Editor. ]
AMERICAN ELECTROCHEMICAL SOCIETY
34TH GENERAL MEETING, ATLANTIC CITY
SEPTEMBER 30 TO OCTOBER 2, 1918
The meeting at Atlantic City, September 30-October 2, 1918,
was another demonstration of the feasibility and desirability of
war-time scientific meetings. Eighty-two members and thirty-
two guests constituted an interested body which listened at-
tentively to the papers, started lively discussions, and gave an
air of atteution-to-business to all the proceedings.
Princeton had been selected for the meeting place, and a full
and interesting program had been arranged to the last detail,
but the commandeering of colleges and universities by the Gov-
ernment on October first made Princeton unavailable, and a
quick change to Atlantic City was effected at the last moment.
Headquarters were at the Hotel Traymore, and many members
attending the Chemical Exposition at New York the previous
week found a welcome relaxation in spending Sunday at the
shore. The sessions were held in the convenient Belvedere
room, whose windows command a spacious view of the island
and surf-edged beach.
Monday morning's program included papers on "An Appa-
ratus for the Separation of Radium Emanation and its Deter-
mination Electroscopically" by J. E. Underwood and Prof.
Schlundt, of the University of Missouri; "Notes on the Heter-
ogeneous Equilibrium of Hydrogen and Oxygen Mixed with
Radium Emanation" by S. C. Lind, of the Bureau of Mines,
Denver; "Processes Within the Electrode which Accompany
the Discharge of Hydrogen and Oxygen," by Prof. Donald P.
Smith, of Princeton; "The Sign of Potential," by Prof. O. P.
Watts, of the University of Wisconsin. The discussion of the
latter paper was particularly lively, Prof. Watts pleading for
the retention of the usual designation of the stronger metals as
the more electropositive and the retention of the parallelism
between chemical activity and electrical potential. His main
argument was the uniformity thus introduced in the signs of
the electrodes and the direction of the current in consonance
therewith, in electrolytic and battery cells.
In the afternoon session F. C. Kelley read a paper on "The
Hardness of Soft Iron and Copper Compared," in which he
showed that annealing in hydrogen gave unexpected softness to
pure iron. E. Kilburn Scott described at length "Nitrogen
Fixation Furnaces," touching on the salient and characteristic
features of various types of arc furnaces in a masterly manner.
W. R. Mott, of the National Carbon Company's research labor-
atory, contributed a remarkable paper on "The Relative Vol-
atilities of Refractory Materials," in which he tabulated ten
different methods or lines of observation which give data on
the volatilities of various refractory metals and oxides in the
electric arc. The long paper -contained a mass of new and in-
teresting observations and data, from which perhaps only a
fraction of the possible conclusions and inferences were drawn by
the author; a number of such were brought out in the discussion.
In the late afternoon, at a meeting of the Board of Directors
of the Society, the 1919 Spring Meeting was scheduled for New
York City, the Fall Meeting for Chicago, coincident with the
Fifth National Exposition of Chemical Industries, and a $2000
subscription to the Fourth Liberty Loan was voted.
The evening gathering in the beautiful Rose Room (which
happened to be lined with an exhibit of the wonderful Farre
airplane pictures) furnished relaxation in the form of moving
pictures: "The Fixation of Atmospheric Nitrogen at Niagara
Falls,'' by courtesy of the American Cyanamid Co.; "Canadian
Shawinigan Falls Power Development and Electrochemical In-
dustries," by courtesy of the Shawinigan Water and Power Co.;
and "The Triplex (Bessemer-Open Hearth -Electric) Steel Pro-
cess at South Chicago," by courtesy of the V. S. Steel Corpora-
tion. The pictures formed a very satisfactory substitute for the
usual visits to industrial plants; such exhibitions are valuable
adjuncts to a scientific meeting.
Tuesday was given, morning and afternoon, to discussing
"Electrochemistry After the War." A. H. Hooker, of Niagara
Falls, discussed the chlorine and alkali industry; Van R. Kokat-
nur, of Niagara Falls, the multitudinous uses of chlorine; W I.
Landis, of the American Cyanamid Co., air nitrates; F. A. J.
FitzGerald, of Niagara Falls, the electric furnace; J. A. Mathews,
of the Holcomb Steel Co., Syracuse, electric steel; Robert Turn-
bull, of St. Catherine's, Canada, electric furnace pig iron (the
low-phosphorus pig made in steel-melting furnaces from steel
scrap); C. A. Winder, of Niagara Falls, the power situation;
J. W. Beckman, of San Francisco, the same topic, from the
Pacific Coast standpoint; Grinnell Jones, of the L". S. Tariff
Commission, tariff problems of the electrochemical industries;
Lt.Col. W. D. Bancroft, U.S.A., scientific research; Dr. Mees,
of Rochester, the question of cooperative industrial research.
The general note in all these discussions was optimism, tempered
by a realization of the magnitude of the tasks and the necessity
of scrapping old ideas and facing bravely the new situations
which have arisen.
Nov., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
94 5
In the evening Dr. E. F. Northrup, of Princeton, gave an
informal account of how he came to devise his interesting and
potentially important "Oscillatory Current Induction Furnace."
His non-mathematical presentation, giving a direct and clear
insight into the characteristics of the furnace, held the
attention of the gathering for nearly two hours. The next
morning the meeting of the Society adjourned direct to Tren-
ton, N. J., where Dr. Northrup, at the works of the Pyroelectric
Instrument Company, concluded his lecture by demonstrating
the furnace in operation, melting a charge of nickel. A visit to
the Thermoid Rubber Company plant, after lunch, concluded a
meeting which was a pleasure and an inspiration to everyone
fortunate enough to be in attendance.
J. W. Richards
Lehigh University
South Bethlehem. Pa.
THE MILWAUKEE MEETING OF THE AMERICAN INSTI-
TUTE OF MINING ENGINEERS
On October 7 to 12, 1918, Milwaukee was host to the Amer-
ican Foundrymen's Association, the American Institute of Min-
ing Engineers — the Institute of Metals Division and the Iron
and Steel Section, and the American Malleable Castings Asso-
ciation. In addition to the joint and separate meetings of these
bodies, the huge auditorium hall was filled with an industrial
exhibition of metals and metal-working accessories which was
worth going a long way to see.
All the Societies joined in an opening session on Tuesday
morning, at which President Backert, of the Foundrymen's
Association, presided ; Governor Philips, of Wisconsin, welcomed
the visitors in a patriotic speech; a long and interesting letter
from Captain R. A. Bull, a former president of the Association
and now in France, was read, and a ringing resolution was
passed, to be telegraphed to President Wilson, pledging anew
to the Government every resource of the allied metal trades
until "the abject and unconditional surrender of the enemy."
Following this, the gathering resolved itself into various sec-
tional meetings, unfortunately scheduled simultaneously, thus
rendering it impossible to hear all the papers in which one
might be interested. Several in this predicament were heard
drawing a parallel between this convention and a four-ting
circus. The criticism was a valid one; the program should have
had the sectional meetings arranged consecutively, using both
mornings and afternoons, so as to prevent the keen disappoint-
ment felt by those forced to choose between one meeting and
another.
The Foundrymen's Association had a schedule of papers on
various subjects, from moulding sands to core ovens, electric
furnaces, and pyrometers. Owing to the impossibility of being
in three places at once, the writer can only report what was
verbally reported to him, viz., that the attendance on these
technical sessions was poor and the discussion of the papers
tame, excepting the discussion on casting semi-steel shrapnel
shells. Evidently the foundrymen are stronger in action than
they are at talking, a virtue which, we will readily admit, has its
commendable features.
The Institute of Metals Division of the Mining Engineers
(W. M. Corse, Chairman) , on the other hand, held well attended
sessions at which discussion was lively and the interest so great
that they extended an hour or more beyond the normal closing
hours. Almost all the papers on the program had been printed
in advance in the Bulletin of the Institute, giving ample oppor-
tunity for preparation of careful and well-considered discussion.
Professor Zay Jeffries described "The Metallography of Tung-
sten," attempting therein to show the causes of its lnittleness;
Sir Robert Hadfield, of Sheffield, England, communicated lome
discussion mainly bearing on the explanation of the effect of
tungsten on the electrical properties of steel. S. L Hoyt dis-
cussed in a new way the ever-present problem of "The Con-
stitution of the Tin Bronzes;" his conclusions did not find
unanimous approval. Jesse L. Jones, of the Westinghouse Com-
pany, considered "Babbitt and Babbitted Bearings," his main
point being that the genuine "Babbitt" was improved by reduc-
ing its tin content by the addition of 1 per cent of lead. Two
papers by S. Skowronski treated of "Oxygen and Sulfur in
the Melting of Copper Cathodes" and "The Relation of Sulfur
to the Over-Poling of Copper;" N. B. Pilling discussed "The
Action of Reducing Gases on Copper."
Another session was devoted to a "Symposium on the Con-
servation of Tin." A dozen men prominent in the white metal
industry read carefully prepared addresses, and a general dis-
cussion of a most interesting nature followed, the session lasting
from 10 a. M., to 1.30 p. m., and being continued into the
afternoon session at 3 p. M. The savings possible by reducing
the tin in solders, using substitutes for tinfoil, packing dry
foods in cartons instead of tin boxes, using copper-coated iron
for boxes intended to be printed, saving the fumes from melting
down old tin scrap to sash-weight-iron, making dry tin skim-
mings, etc., etc., almost ad infinitum, were thoroughly con-
sidered. It was a unique session of absorbing interest.
At the concluding session, Dr. John Johnston read an inter-
esting resume of the existing data on "The Volatility of Zinc
from Brass," and discussed the figures in an able manner.
Although the data are scanty, yet they allow some definite
conclusions to be drawn as to the vapor tension of zinc from
these alloys at various temperatures, and the consequent lia-
bility to loss of zinc in melting and pouring them. Dr. J. W.
Richards discussed the question from the thermodynamic stand-
point, pointing out that the vapor tension curve of pure zinc
was well known, and that if the heats of combination of zinc
with copper to form these various brasses were determined
calorimctrically, the vapor tension of zinc from these alloys
could be calculated with precision; further, if their latent heats
of fusion were also determined, the vapor tension of zinc from
the solid brasses could be calculated. The further discussion
emphasized the advisability of cooperative industrial research,
subsidized by the brass manufacturers, to determine such lack-
ing data and make them available to the industries. G. C.
Stone, of the New Jersey Zinc Co., described "The Effect of
Impurities on the Hardness of Cast Zinc;" C. A. Hansen's paper
on "Electrolytic Zinc" was, in the absence of the author, read by
title; Prof. C. H. Fulton's paper on "The Condensation of Zinc
from its Vapor," was a valuable contribution towards the
explanation of a difficult problem; G. F. Comstock discussed the
important question of "Non-Metallic Inclusions in Bronzes and
Brasses;" Dr. G. K. Burgess and L. J. Gurevich, of the Bureau
of Standards, "Fusible Plug Manufacture." Dr. Arthur W.
Gray had a long and painstaking paper on "Dental Alloys,"
principally the amalgams and their properties. Hill and Luckey
described how minute quantities of lead can be determined in
copper by boiling off the lead from a weighed sample, in an
electric arc, and noting with a stop-watch the time required
until the spectroscope shows the absence of the lead lines — a
most interesting and novel method of quantitative chemical
analysis.
The Iron and Steel Section (Dr. J. W. Richards, Chairman)
was scheduled for two sessions, one dealing principally with
iron and steel and the other with coal and coke. The first ses-
sion opened with an exhibit of moving pictures of the Triplex
Steel Process (Bessemer-Open Hearth -Electric) at the South
Chicago works of the Illinois Steel Company, Dr. Richards fur-
nishing explanations of the process and the pictures. Dr. John
Johnston, of the National Research Council, read a paper on
the work of the Council, written by H. M. Howe. Papers on
"The Limonite Deposits of Mayaguez Mesa, Porto Rico," and
"Recent Geologic Development on the Mesabi Iron Range."
] by title. "The Manufacture of Ferro- Alloys in the
B," by R. M. Keeney, was an up-to-date pre-
946
THE JOURNAL 01 INDUSTRIAL AND ENGINEERING > HEMISTRY Vol. ic.
sentation of a very important topic containing particularly new
information concerning ferro-uranium. "The Manufacture of
Silica Brick," by H. LcChatelier and B. Bogitch, was mostly
a detailed discussion of the microscopic characteristics and the
constituents of bricks burned at different temperatures — itshould
have brought out an active discussion, but it did not. Two
ing papers followed on partly distilled coal — carbo coal
and semi coke, by C. T. Malcolmson and G. VV. Traer, respec-
tively. The discussion was lively and brought out very clearly
the fact that such products are looked to, in the Middle West,
to replace anthracite coal for household use — an object of great
national importance. W. H. Blauvelt's paper on "The By-
product Coke Oven and its Products," dealt with nearly the
same topic. H. R. Collins, of the Fuller Engineering Company,
discussed "The Use of Coal in Pulverized Form," which led to
considerable discussion, in which Mr. Adams, of Milwaukee,
described the installation of powdered coal firing in locomotive
boilers in .Southern Brazil, using coal with 4 to 5 per cent sul-
fur. Mr. Adams also invited all present to visit the Milwaukee
Power Station, where a steam boiler was running regularly on
powdered coal, at high thermal efficiency. Those accepting his
invitation saw a very simple and effective installation, which
will doubtless soon be copied in power plants all over the country.
The meeting as a whole was a great technical success and ful-
filled admirably its function of instructing and stimulating to
greater industrial and scientific achievement the metallurgists
and engineers in attendance J. W. Richards
Lehigh University
South Bethlehem, Pa.
October 15, 1918
REPORT OF THE COMMITTEE ON RESEARCH AND
ANALYTICAL METHODS, FERTILIZER DIVISION,
AMERICAN CHEMICAL SOCIETY
llld, September II, 1918
Two subjects have been under consideration by thU Com-
mittee:
The first was the report of Mr. H. C. Moore, who was ap-
pointed to work out a suitable method for the determination of
sulfur in pyrite to replace the faulty Lunge method. His work
developed the value of a modification of the Allen and Bishop
method and has been under way for several years. The co-
operative work this year has given results which are even more
satisfactory, if anything, than those of previous years and are
being reported by Mr. Moore in a paper to be read before the
Division at this meeting, with the recommendation that the
method be adopted.
The other was the DeRoode method for determining potash,
which was brought to the attention of the Committee from several
quarters A modification of this method was published by
T. F. Keitt and H. F. Shiver in the Journal of Industrial and
Engineering Chemistry for March 1918.
The results obtained by this method are, in general, con-
siderably higher than those obtained by the official method and
the results of preliminary work do not indicate that this is
due to impuritcs or other sources of error.
I'ail Ki i>Mck. 1 ha
1 K C uibron
A I PaTTSn
C. H. JONBS
J M. McCanih.Kss
NOTLS AND CORRESPONDENCE
THE CENSUS OF CHEMISTS
Editor of the Journal of Industrial and Engineering Chemistry:
General Sibert directs me to extend to you the thanks of
the Chemical Warfare Service of the United States Army for
your assistance in the census of American chemists recently
made by this arm of the service. Without the aid of your
Journal it would have been impossible to have gained such wide
publicity for the enterprise, or to have obtained such a prompt
and altogether satisfactory response from the great body of
loyal chemists of this country. Well over half of the question-
naires have been answered, and the rest are daily being re-
ceived in such numbers as to indicate the completion of the
task at a not far distant date. The War Department is
thus put in possession of an invaluable set of records at ex-
tremely small expense.
W'liile the purpose of the questionnaire has been understood
by nearly all of those who have replied to it, there have been
a few instances in which it has been mistakenly interpreted as
a call to immediate service. In order to avoid any misunder-
standing it should be explained that the purpose of the census
is primarily to put the War Department in control of complete
information as to tin chemical 1n.u1 power of the country, not
to gain immediate recruits foi the Chemical Warfare Service.
At the present time the \ .leam ies ill the Service are compara-
nd 1\ few in number. When vacancies occur in the future,
reference will be bad to the tabulated information gleaned from
the present census, and appointments will be made from the
names 011 file, attention being paid to the applicant's technical
qualifications, desire to set .
i hi great majority of American chemists will undoubtedly
never be called upon to sei ve in a military capacity in the present
war. The Government, however, must have complete informa-
tion concerning all chemists, in order that it may select those
best fitted to perform its work, and at the same time interfere
as little as possible with established essential industries The
chemist who, after returning his complete questionnaire, re-
ceives no call to service, may take it for granted that the Gov-
ernment cannot, for the time being, utilize his ser\ :
the meantime three things are asked of him:
1 — To keep the Chemical Warfare Service informed of any
change in his address, his employment, his draft status, or any-
thing else which might have a bearing on bis 1
2 — To notify the Chemical Warfare Service at once if he is
drafted and called to camp. In such a case he should rive hi*
complete military address
3 — To help stabilize the industry of the country by con-
tinuing steadily at essential work until the Government notifies
him that his services are needed elsewhere.
In addition it is requested that all persons send to the Chem-
ical Warfare Service the names and addresses of any chemists
of their acquaintance who have not already received the ques-
tionnaire. Chemists who have already received the question-
naire but who have not yet returned it should do s
order that the Government may not be put to the trouble of
sending out a large number of "follow up" letters Any chemist
who has not received the questionnaire should write for a copy,
addressing Ins request to the Personnel Section. Administration
Division, Chemical Warfare Service. U. S A . 7th. and B Struts,
N. W . Washington, D. C.
F F. Brsithot
Major. Chemical Warfare S<
Chief of Personnel
Washington-. IV C.
September <(), I 'MS
No v. , i o 1 8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
94;
DEFERRED CLASSIFICATION AND FURLOUGHS FOR
GOVERNMENT AND STATE CHEMISTS
The Chemical Warfare Service has been duly authorized, by-
order of the Secretary of War, to make the necessary arrange-
ments through the Adjutant General's Office, to secure the
furlough, without pay or allowances, of such chemists as are
necessary in such government bureaus as the Bureau of Stand-
ards, Bureau of Chemistry, Bureau of Mines, United States
Patent Office, where such chemists are engaged in chemical
work for the government or state bureaus concerned, essential
to the prosecution of the war. At the same time they are ad-
vised that the new Selective Service Regulations, to be pub-
lished shortly, will emphasize to the draft boards the fact that
skilled employees of war industries should be placed in deferred
classification. The induction into the military service of skilled
men necessary to essential industries or occupations, to be sub-
sequently furloughed back to their industries or occupations, in-
volves an expense to the Government, and the men concerned
lose time from their necessary work. The bureaus concerned
are authorized by the Selective Service Regulations to submit to
the draft boards affidavits and written proof to maintain their
contention that their employees should be placed in deferred
classification and it is believed that they should be encouraged
in securing deferred classification rather than securing the fur-
lough of the men after they have been inducted into the mili-
tary' service.
All communications in regard to information from those de-
siring any details should be addressed to Major Victor Lenher,
Chemical Warfare Service, U. S. A., Chief, Governmental and
State Relations Branch, Unit F, Corridor 3, Floor 3, 7th and B
Sts., N. W, Washington, D. C.
CHEMICAL INDUSTRY IN THE NETHERLANDS
In a recent number of the Dutch publication, In- en Uitvoer,
Mr. Jan Straub gives a brief history of the chemical industry in
the Netherlands. The writer points out that the present back-
wardness of the industry is the natural result of the lack of
minerals in the country and of the fact that in the Netherlands,
agriculture and trade have for ages been the principal sources
of wealth. In Germany, on the contrary, the great mineral
wealth furnishes valuable opportunities for the employment of
the growing population. The chemical industry in the Nether-
lands owed its origin to the needs of agriculture, but its progress
was retarded by the ease with which chemicals could lie imported
from Germany and from oversea countries, as well as by Un-
limited demand at home. The Dutch simply followed tin-
practical maxim according to which it is better to buy cheaply
than to produce dearly. In recent years, however, the demand
for chemicals has increased greatly in Holland, particularly for
export to the colonies, and the war has induced the Dutch t"
make extensive investigations in order tn ascertain what chem-
icals and preparations could be made at home just as cheaply
as elsewhere. The methods and processes of production have
been studied during the war in various establishments, and the
factories are ready to begin production as soon as peace returns
and the raw materials Income available.
The manufacture of essential oils is a comparatively new
branch of the chemical industry which is always cer-
tain of a market for its products. It supplies soap factories,
manufacturers of artificial fruit flavoring'., and distill' 1 with the
means (or the refining of their products. The manufacture of
aps, fruit syrups, and fine liquors is on the increase,
and the demand for 1 ind compound ethers is grow-
ing. The oils and tin 1I1 an prepared undei cientinc super-
vision, and the manufacturers are profiting bj I
of their customers. They will lie in a position to competl until
foreign producers after the war.
The production of pure chemicals and drugs has developed
rapidly under the stimulus of the war. The increasing demand
for all sorts of inorganic and organic preparations both for in-
dustrial and medicinal use will provide a market for these prod-
ucts also in times of peace, both at home and in the Dutch East
Indies. It may well be that many of these preparations, when
peace returns, will be obtainable from abroad at a price below
the domestic cost of production. In that casa, even if domestic
production shall be discontinued, some good will have been
.accomplished nevertheless; the Dutch purchasers will know the
limits of the prices which may be demanded of them.
Only a few of the coal-tar dyes were formerly manufactured in
Holland here and there, but the necessary intermediate products
had to be imported. During the war, steps have been taken to
build up the industry systematically from the simplest raw ma-
terial to the finished product. The increased production of
the Limburg mines, the new coke ovens, and the expansion of
the tar-distilling industry promise to furnish a sufficient quan-
tity of intermediates. For the present the intermediate products
are given the chief attention, as they have their own markets,
and the production of finished dyes, one after the other, will
follow later. The first products will doubtless be. taken by the
Dutch textile factories, which will thus become independent of
foreign or rather German producers. The Dutch factories are
also getting ready to produce various perfumery articles, drugs,
and tar distillates, but refrain from making known the results
achieved until the time comes when they may begin deliveries.
PORTRAIT OF CHARLES M. HALL FOR THE CHEMISTS'
CLUB
On the evening of October n, 191S, previous to the regular
meeting of the New York Section of the American Chemical
Society, a portrait of the late Charles M. Hall, presented to
the Chemists' Club by the Aluminum Company of America,
was unveiled. Mr. Ellwood Hendrick, President of the Chem-
ists' Club, in his introductory remarks, spoke briefly of the life
of Mr. Hall and of his work on aluminum. He then called upon
Mr. Duggan, Chairman of the House Committee, to unveil the
portrait, after which the artist who painted the portrait, Mr.
Rood, was asked to tell something of the process of making a
likeness of a man whom he had never seen. This. Mr. Rood
explained, he had done by means of various photographs of Mr.
Hall and of talks with men who had known him.
In the absence of Mr. Arthur V. Davis, President of the
Aluminum Company of America, who had expected to lie pres-
ent to give personal recollections of Mr. Hall. Mr. Hendrick
called upon Dr. C. F. Chandler, who told the story of Mr. Hall's
discovery, at the age of twenty-two, of the solubility of alu-
mina in fused cryolite and all that this discovery has meant
industrially.
The portrait of Mr. Hail now hangs in the Lounge Room of
the Chemists' Club. He is the third Perkin Medalist whose
portrait has been hung on the walls of the Club, and Dr. Chandler
said that he hoped to live to sec a portrait of each one of them
111 the Club.
COOPERATION REQUESTED BY THE ALIEN PROPERTY
CUSTODUN
Editor of the Journal of Industrial and Engineering Chemistry:
I will greatly appreciate it if you will call the attention of
era of your publication to tii il the "Trading
with tin Enemy Act," which provides that all money or other
property held by, for, or for the account of, 01 tin benefit of, an
enemy or ally of enemy, should in- immediate^ reported to this
office. This includes patents, trade marks, copyrights, prints,
! iii. 1 , and rli
948
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. n
In connection with the last named, the following persons are
required to make report to this office:
All persons who are in any manner interested in the use or
operation of any enemy-owned patent, trade-mark, copyright,
print, label, or design, including joint inventors, where one
of the inventors is an enemy within the provisions of the "Trad-
ing with the Enemy Act."
Assignees of an undivided part or share of an invention, or
right to carry on a process or operate under a trade-mark,
copyright, print, label, or design, within and throughout a
specified portion of the United States, when such patent or
process is enemy-owned.
Mortgagees and licensees of enemy-owned patents, trade-
marks, copyrights, prints, labels, or licenses.
The above includes guardians, executors, and administrators.
Any information regarding the enemy interests in any patents
trade-marks, copyrights, prints, labels, or designs, should be
forwarded immediately to Francis P. Garvan, Director of the
Bureau of Investigation, Alien Property Custodian's Office,
Washington, D. C, even if the information is only gossip or rumor.
Oftentimes a clue to important enemy interests is obtained in
this way. I feel sure than I can count upon your cooperation
in the work of uncovering money and property of enemy charac-
ter. The money thus obtained is invested in Liberty Bonds,
and is made to fight for our country, instead of against it.
Sixteenth and P Streets, X \V. A. MITCHELL PALMER
Washington, d. c. Alien Property Custodian
October 1, 1918
AN ALINEMENT CHART FOR THE EVALUATION OF
COAL— CORRECTION
In the article of the above title, This Journal, io (1918),
627, the 4th line in "Directions for Use" under the cut should
read "Price per dry ton" instead of "Cost per million B. t. u."
September 12, 1918 A. F. BLAKE
PERSONNEL, RESEARCH DIVISION, CHEMICAL WAR-
FARE SERVICE— CORRECTION
It is regrettable that in the rush of assembling the names of
the men engaged in work for the Research Division of the
Chemical Warfare Service, for publication in the September
issue of This Journal, the name of Professor Treat B. Johnson,
of Yale University, was omitted from the list.
WASHINGTON LETTER
By Paul Wooton, Union Trust Building, Washington, D C.
No hedging against the end of the war is being done by the
Government. Contracts are being let, plants are being built,
and all plans are being made as if it were sure that the war will
last two years more. While this is no more true of chemical
activities of the Government than of any of its other war
activities, it can be stated on the best of authority that the
apparent collapse of the Teutonic fighting machine has in no
way been reflected in the activities of the agencies conducting
the chemical work being done by the Government. Incidentally,
the ban on publicity, which has been clamped over this work
since the beginning of the war, remains in place. Matter,
which would be 90 per cent useful to the chemists of the United
States and 10 per cent useful to Germany, is withheld with all
rigorousness, along with much information which apparently
would not be of value to the enemy.
The War Minerals Bill became a law at 2 P.M., Oct. 5. This
Act, which affects importantly nearly every chemical industry,
must await the issuance of regulations before its effects are felt
generally. At this writing (Oct. 16) the President's proclama-
tion, which will designate the agencies to administer the Act,
is being expected daily. It is regarded as probable that power
will be divided between the Bureau of Mines and the War
Industries Board. Certainly price fixing and allocation of
materials will go the the War Industries Board as it already is
handling all such matters for the Government.
Prices for sulfuric and nitric acids have been agreed upon
by the War Industries Board and the Committee on Acids
of the Chemical Alliance, effective until the first of the year, as
follows :
Sulfuric Acid, 60° 816.00 per ton (2000 lbs.)
Sulfuric Acid, 66° 25.00 per ton (2000 lbs.)
Oleum. 20 per cent 28.00 per ton (2000 lbs.)
Nitric Acid, 42° 8>/» cents per lb,
The same provisions for shipment in drums, carboys, in car-
load and less than carload lots as were made effective for the
quarter ending September 30 are to continue for the last quarter
of the year, but with these new prices fixed for bulk shipment
used as a base for package prices.
Senter, Mich., has been selected for the site of a new Govern-
ment tetryl plant. The value is to be §250,000, which is to be
divided between the cost of buildings and equipment.
A Si, 000,000 addition to the Frankford Arsenal has been
authorized.
The Federal Trade Commission continues to insist on the
discontinuance of what it terms unfair methods of competition
when prices are offered which are "unwarranted by trade condi-
tions and so high as to be prohibitive to small competitors."
The American Agricultural Chemical Co., of Connecticut, and
the Brown Co., Inc., of Trenton, N. J., manufacturers of ferti-
lizers, are among the latest concerns to be accosted by the Com-
mission. The Commission states that it found that the Ameri-
can Agricultural Chemical Company is the owner of all the
capital stock of the Brown Company and that prices were being
offered at Philadelphia and at Atlantic City for raw materials
which were "calculated and designed to, and did, tend to de-
stroy certain small competitors."
Licensing of the platinum industry is proceeding more rapidly
than had been expected. The fact that the same plan has been
applied to other materials, as well as the wide publicity given
the regulations, is responsible for most of those concerned being
conversant with the steps they are required to take. It is
estimated that 150,000 licenses will be issued.
That gas masks being used by the American Army give twenty
times the protection afforded by German gas masks is a fact
attested to in a formal statement issued by the War Department.
It is stated further that there is not a single case on record of an
American soldier falling victim to a gas attack when protected
by the mask that is now being manufactured in the United
States on a vast quantity basis. This fact has been so
thoroughly established by repeated experiences that military
authoritk-s place the blame for gas poisoning on the carelessness
of the victim. A great many officers in the United States
Army insist that in most cases the men who get gassed should
be court-martialed, not decorated.
It is an interesting fact that American gas masks stand up
under tests that German masks cannot meet. German masks
will not give protection against a high concentration of gas.
This was demonstrated recently when the British assembled a
sufficiently large battery of projectors to put seventy tons of
phosgene into the air at once, with consequences quite well
known to the German General Staff. There is no concentration
of gas that American masks will not defy. This has been proved,
not only on the battlefield, but in the experimental stations in
this country, where determined attempts to break down the
resistance of United States Army masks by heavy gas con-
centrations were absolutely unsuccessful.
Importation of French optical glass is to be controlled by" the
War Industries Board. Orders for the French product must
Nov., iqiS THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
949
pass through the hands of the War Industries Board and the
War Trade Board. Regulations for the importation of French
optical glass adopted following conferences between the Military
Optical Glass and Instruments Section of the War Industries
Board, of which George E. Chatillon is chief, and the Bureau of
Imports of the War Trade Board, provide:
1 — All import orders for French optical glass should be placed with the
Service Geographique, who will distribute them among the various French
manufacturers.
2 — The order, together with the application for import licenses, should
be forwarded to the War Trade Board, Bureau of Imports, to the attention
of Air. Reardon.
3 — The applications should state in detail the purpose for which the
glass is intended.
4 — The War Trade Board will in all cases consult with the .Military
Optical Glass Section of the War Industries Board before applications are
granted.
5 — Orders placed direct will not have the approval of the Military
Optical Glass Section nor the necessary endorsement of the War Trade
Board to allow the glass to be imported from France.
6 — If glass of a special manufacturer is desired, it may be noted on the
order.
at a price of $3.50 per bushel. With the harvesting of the crop it has been
found that this price does not provide sufficient remuneration to the grower.
After careful consideration of the matter by a board of the Bureau of
Aircraft Production, Mr. W. C. Potter, the Acting Director of Aircraft
Production, has established a price of $4.50 per bushel of 46 lbs. As
specified in the original contracts, beans are to be delivered hulled and
sacked, in carload lots, f. o. b. the nearest railroad station to the land on
which they are grown.
Most of the planting of castor beans was done under sub-contracts with
the general contractors. The price of $4.50 now established is to be paid
to the actual growers of the beans. The remuneration of the general
contractors for their services in connection with the crop is in addition to
this sum.
Hope had been expressed that the shipping situation would be
sufficiently relieved this winter to allow increased importations
of nitrate of soda. While the shipping situation has improved,
in so far as additional tonnage is concerned, beyond expectations
of a year ago, the demands on that tonnage also have increased
beyond all estimates. For this reason, it is improbable that any
large amount of nitrate of soda for other than Government use
will be brought in this winter.
Drugs and medicines used by the Army Medical Corps are
being tested by the Bureau of Chemistry of the United States
Department of Agriculture at headquarters here and at its
offices in other cities. Several chemists have gone from the
Bureau to accept commissions in the Army and perform the work
directly for the War Department. Chemists and inspectors are
being instructed for Army and Navy work and special investiga-
tions are being conducted on problems concerning foods, leather,
fabrics, paper, and other products in military and naval demand.
In a new ruling of the War Trade Board ( W. T. B. R. 254 ), the
importation into the United States of varnish gums 1 Kauri,
Copal, Damar, Zanzibar, Manila, Congo, Fentiansk, Bengurlla,
Sandarao, and East India or Borneo gum) is restricted as to ship-
ments made after October 10, 1918. AH outstanding licenses
have been revoked as to ocean shipment after that date and no
new licenses will be issued except to cover the following: (1)
Shipments made from abroad on or before October 10, 1918,
(2) shipments for the use of the United States Government, (3)
shipments from Mexico or Canada by other than ocean trans-
portation, (4) shipments from Europe or Mediterranean Africa
when coming as return cargo from convenient ports where
loading can be done without delay, (5) shipments of Copal or
Manila gum when shipped from the Philippine Islands, and (6)
shipments of Kauri gum not to exceed a total of 3,000,000 lbs.
during the calendar year 1918.
Licenses for the amounts of varnish gums permitted to come
forward, pursuant to the foregoing, will be allocated by the
Bureau of Imports of the War Trade Board in accordance with
the recommendations, as to distribution and price, of the War
Industries Board. Varnish gums are accordingly added to the
list of commodities excluded from the terms of license PBF 27.
A voluntary increase in the price of castor brans !
announced by the War Department, 'litis action will save
serious loss to the majority of those who embarked in the new
enterprise of growing castor beans, it is believed, and will make
for a continuance of the industry in the South. The War De-
partment's statement in this connection is as follows
In order to procure an adequate supply of castor oil for usi
nection with tip .' ttion program, dui
were let last spring for the raising of castor beans in the Southern Suites.
The list of restricted imports No. 1, item 64, issued by the
War Trade Board, provided that prior to October 1, 191 8,
licenses might be issued for the importation of 125,000 long tons
of pyrite. Since licenses have not been issued for the full amount
so permitted, the War Trade Board has authorized the issuance
of licenses during the remainder of the present calendar year,
when the applications are otherwise in order, for the importation
from Spain of the unimported balance of the amount originally
authorized, which is approximately 56,400 tons.
To provide for more prompt chemical analysis of food products
for use by the Army and Navy, a new arrangement has been
made by the Bureau of Chemistry, which is described in the
following announcement:
Arrangements have been made by the Subsistence Division
of the Quartermaster Corps whereby the laboratories of the
Bureau of Chemistry, Department of Agriculture, throughout
the rutted States are to be more fully utilized by the Army.
Through this arrangement the inspection of food products which
requires chemical analysis will be made to a greater extent under
the direction of the general supply depots at the source of manu-
facture. Delays occasioned under the former procedure of
having inspection made at the delivery point will thus be avoided,.
At times cars of greatly needed food products have been held up
pending report of analyses. Under the new system such prod-
ucts will have been completely inspected at point of purchase.
The new system will be particularly effective in handling
canned milk, putting milk upon the same basis of inspection as
canned meat products in large packing houses. Further at range-
ments have been made whereby, if it develops that any stations
of the Department of Agriculture are too remotely situated t"
alTord the proper service, stations will be promptly established
by the Bureau of Chemistry to givi '• service. This
arrangement is another of the steps which the Quartermaster
Corps is taking to coordinate all government departments in
securing lite best supplies and service for the troops.
In thi anization of the Ordnance Depa
Lt. Col. W. C. Spniance has been placed in charge of chem-
icals.
PERSONAL NOTL5
Dr. Ernest G. Genoud died at his home in Dorche fo r, Mass.,
on October 12, of pneumonia following Spanish influenza. Dr.
Genourl was born in Boston, February 23, 1889 Aft
uation from tin in [908,
t\ ing the degree oi doctoi of et
at Charlottenburg in [911. He had become a red
specialist on fermentation processes and was a membei "i the
Staff of A. D. Little, [m
The Colleg< of the City of New York announo tin following
additions i<> the department of chemistrj Henrj
formerly of Rose Polytechnic [nstitute, B li tan I professor of
i chemistry; Herman C. Cooper, formerly of the Uni-
versity oi iyrai I phyi it al chemistry;
Carl R. McCrosky, formerly of Oregon Vgricultural College,
and '1 ilv "i tie Department of Agricul-
instructoi in 1 hi mi tt \
95°
THE JOURNAL OF INDl STRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. n
Mr Carleton B. Edwards, formerly head of the chemistry
department at Guilford College, is now doing chemical engi-
neering work in smokeless powder with E. I du Pont de Nemours
and Co., at the Hopewell Plant, City Point, Va.
Mr. Benton Dales, formerly head of the chemistry department
of the University of Nebraska, is now research chemist for the
B. F. Goodrich Co., Akron, Ohio.
Miss Jessie E. Minor has resigned her position as associate
professor of chemistry at Goucher College to accept a position
as chief chemist for the Hammerschlag Paper Mills, Garfield,
N. J.
Mr. Seward G. Byam, formerly chemist for the Revere Plant
of the United States Rubber Co., Providence, R. I., is now
employed as aeronautical chemist at the General Laboratories,
Bureau of Aircraft Production, Pittsburgh, Pa.
Mr. Ralph Brown, formerly employed in the laboratory of the
Eagle-Picher Lead Co., Joplin, Mo., is now running a small lead
smelter for the estate of James Robertson, Galletta, Ont.,
Canada.
Mr. R. R. Henderson, formerly chief chemist of the Vreeland
Chemical Co., has resigned his position with that firm in order to
devote his whole time to consulting practice. Mr. Henderson
specializes in the development of chemical processes and the
application of automatic machinery to chemical productions.
His headquarters are at Little Falls, N. J.
Mr. Richard L. Wing, formerly chief chemist for the Holmes
Mfg. Co., New Bedford, Mass., is now Engineer, Area "E,"
U. S. Government Explosives Plant "C," Nitro, West Vir-
ginia.
Mr Paul J. Carlisle, who for the past two years has been
engaged in research for the Roessler and Hasslacher Chemical
Co., Perth Amboy, N. J., has been transferred to St. Albans,
W. Va., and placed in charge of a new department which the
company is adding to its plant in that city.
Mr. Arthur P. Harrison, formerly chemist and bacteriologist
with the National Soil Improvement Co., Charlottesville, Va.,
is now supervising the synthetic preparation of certain dye
intermediates for the du Pont Dye Works, Wilmington, Del.
Mr. Philip G. Wrightsman, formerly instructor in chemistry
at Iowa State College, is now in the Chemical Warfare Service
working on toxic gases in the Research Division, American
University, Washington, D. C.
Mr. H. M. Freeburn has resigned as assistant engineer of the
Pennsylvania State Department of Health to become associated
with the engineering staff of Wallace and Tiernan Co., Inc.,
New York City, manufacturers of chlorine control apparatus and
sanitary engineering specialties.
Dr. Arthur M. Pardee has resigned his position as professor
of chemistry at Tarkio College, Tarkio, Mo., and has been
appointed professor of chemistry at Washington and Jefferson
College, Washington, Pa.
Mr. H. L. Walter, formerly of the U. S. Bureau of Chemistry,
has been appointed chief chemist of the State Food and Drug
Department of Tennessee. x
Mr. Harry L. Barnitz, consulting engineer on oxygen and
hydrogen, has severed his connection with the International
Oxygen Co. and is conducting business under his own name
at 617 West 152 St., New York City.
Mr A. G. Frericks, formerly chief chemist for the Palmer
Tire and Rubber Co., St. Joseph, Mich., is now doing chemical
inspection work in the Explosives Section of the Ordnance
Department.
The Association of British Chemical Manufacturers has
elected officers as follows: President, The Right Honorable
Lord Moulton, K. C. B., G. B. E., etc.; Chairman, Mr. Robert
Grosvenor Perry, C. B. E.; Vice Chairman, Tin- Right Honorable
J. \V. Wilson, M. P.
Mr. L. S. Munson, who for the past eleven years has been
with the Ault and Wiborg Co., Cincinnati, <>., has recently
accepted the position of assistant superintendent of the Deep-
water Point, N. J., plant of the du Pont Dye Woi ks
L. D. Sale, Los Angeles, Cal., ha:* been named chairman of
the chemical, oils, and paints section of the Los Angeles dis-
trict of Sub-Region No. 14. Region No 19, of the resources and
conversion division of the War Industries Board.
Hi. Walter Taggart has been appointed consulting chemist-at-
F01 the 1 trdnance I lepartment.
Mr. Alex H. McDowell, formerly with Wiley and Co., is now
chemist at the Ashepoo Fertilizer Works, Charleston, S. C,
of the American Agricultural Chemical Co.
Mr. Lawrence C. Stahlbrodt has been appointed by the
Pfaudler Co., Rochester, N. Y., to take charge of its publicity
department.
Mr. P. W. Bruckmiller, formerly assistant professor of chem-
istry at the University of Kansas, is now chemist for the Standard
Oil Co. (Indiana), at Sugar Creek, Mo.
Mr. C. C. Vogt is on leave of absence from the industrial
fellowship on dental supplies of the Lee S. Smith and Son Mfg.
Co. in order to engage in gas investigations at the American
University Experiment Station.
Professor H. F. Moore, of the Engineering Experiment Station
of the University of Illinois, has been appointed by the National
Research Council chairman of the committee to investigate
the fatigue phenomena of metals.
Mr S. M. Evans, vice president of the Eagle-Picher Lead
Co., with headquarters in N. Y., has been relieved of duty with
his company for the duration of the war and is now with the
U. S. Fleet Corporation, with headquarters at Philadelphia,
as chief statistician.
Dr. C. A. Brautlecht, professor of chemistry in the Florida
College for Women, has been called into the Sanitary Corps as
First Lieutenant. He is stationed at the Rockefeller Institute for
Medical Research in New York City.
Mr. James K. Lawton, formerly chemist with the J. H. Pratt
Laboratory, Tampa, Fla., has been commissioned Second
Lieutenant in the infantry, United States Army, and assigned
for duty with the Chemical Warfare Service, Edgewood Arsenal,
Edgewood, Md.
Dr. Frank T. F. Stephenson, past president of the Detroit
Section of the American Chemical Society, has been com-
missioned Captain in the Medical Corps.
Mr. Max L. Towar, formerly of Parke, Davis & Co., Detroit,
Mich., is now with the National AnUine Company, of Buffalo.
Mr. Chas. H. Jumper, formerly secretary of the Detroit
Section of the American Chemical Society, and chief chemist
with the General Motors Co., Detroit, is now connected with the
Calco Chemical Co., Bound Brook, X.J.
Mr. S. B. Chadsey, chairman of the Toronto Section of the
Society of Chemical Industry and formerly assistant to the general
manager of the Massey-Harris Company, has been appointed
manager of the Massey-Harris Company's plant at Brantford,
Ont.
Mr. G. Hallberg, formerly with the Riordon Pulp and Paper
Company, Limited, Hawkesbury, has been appointed chemist
at the Mattagami Pulp and Paper Company's sulfite mills at
Smooth Rock Falls, Ont.
Mr. Harold B. Gammell, formerly stationed at Indian Head,
Md., has been assigned to duty under the inspector of powders,
East Coast, as sub-inspector at the plant of the Standard Textile
Co., Glens Falls, N. Y. This work is under the Navy in which
he enlisted in April 1917.
Mr. Win. Garratt, formerly chief chemist for the Latrobe
Electric Steel Co., Latrobe, Pa., now has a similar position with
the Fulton Steel Corporation, Fulton, N. Y.
Mr. James S. Curry for some time supervising chemist for
the du Pout Company at Wilmington, Del., died of pneumonia
on October 12, 1918,
Mr. W. W. Jones, formerly manager of the New York office
of Frederick Steam and Co., has accepted the appointment
of manager of the Essential Oil and Gum Department of the
National Aniline and Chemical Co., Inc., 21 Burling Slip, New-
York.
Mr Charles Crew has resigned his position with the Central
Testing Laboratory and has taken charge of the consulting work
on chemical engineering for The Stillwell Laboratories, Inc..
New York.
Miss Elvira Weeks, formerly with the New Jersey Zinc Co.,
Franklin, N. J., is now in the Research Department of the
Carborundum Co., Niagara Palls, X. V
Mi Harold W. Baldwin, formerly with the National Aniline
and Chemical Co., Inc., Boston, Mass., is now in the Army
and doing research work at the American University Experi-
ment Station
Nov., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
95 1
Dr. J. Bishop Tingle, professor of chemistry at McMaster
University, Toronto, died on August 6, in Ottawa, Ont. He
had been a prominent figure in the scientific world for many
years. For three years he was at Johns Hopkins University
where he did organic research work and edited sections of the
American Chemical Journal. Since the outbreak of the war,
recognizing the part that chemistry was to play, he had laid
special emphasis on training students for laboratory positions
in war industries.
In addition to the silver service which was given to Dr. M. C.
Whitaker on his retirement from the presidency of the Chemists'
Club, an exquisite illuminated memorial, designed by Mr.
Edward B. Edwards, has also been presented to him. The
center is a Latin text written by Professor McCrea of Columbia
University and the border decoration consists of portraits of
Gerber, Bacon, Lully, and Paracelsus in the four corners and
alchemistic symbols interestingly worked into a decorative design.
Mr. Arthur Given, formerly chief chemist for Morris Herr-
mann and Company and recently chemical engineer with Stevens-
Aylsworth Company, has been appointed First Lieutenant in the
Ordnance Department and is stationed at Picatinny Arsenal.
Mr. Edward W. Weiler has given up his position as research
chemist for the United States Industrial Alcohol Co., Balti-
more, Md., to enter the Chemical Warfare Service.
Mr. B. A Dunbar has recently been made head of the chem-
istry deparment at the South Dakota State College.
Mr. M. Cannon Sneed, formerly assistant professor of chem-
istry at the University of Cincinnati, is now head of the division
of general and inorganic chemistry at the University of Minne-
sota.
Professor J. B. Rather, formerly head of the department of
agricultural chemistry in the University of Arkansas, has ac-
cepted a position as chemist with the Standard Oil Company,
New York.
Dr. M. L. Crossley, associate professor and acting head of the
department of chemistry at Wesleyan University, Middletown,
Conn., has resigned to accept the position of chief chemist for
the Cako Chemical Co., Bound Brook, N. J.
In addition to those noted in the February issue of This
Journal, the following members of the staff of the depart-
ment of chemistry of the College of the City of New York have
gone into war work : Martin Meyer, 2nd Lieutenant, U. S. A. ;
Benjamin Rayved, Ensign, Paymaster Division; Leon J.
Smolen, Nathan Rauch, Moses Chertcoff, Martin Kilpatrick,
Hyman Storch, Joseph L. Guinane, Samuel Yachnowitz,
Privates, Chemical Warfare Service ; Julius Leonard, Alexander
Lehrman, Yeomen, U. S. N.
Mr. E. J. Quinn, formerly research chemist at the Montana
Agricultural Experiment Station, has accepted an appointment
as assistant professor in the department of chemistry at the
State College of Agriculture and Mechanic Arts, University of
Montana, Bozeman.
Ricketts & Co., Inc., formerly of 80 Maiden Lane, have
moved their offices to 280 Madison Avenue. Mr. Charles E.
Wagstaffe Bateson, Dr. M. L. Hamlin, and Mr. T. A. Shegog,
formerly assistant professor of chemistry and metallurgy at the
Royal College of Science, Dublin, and professor of chemistry
and metallurgy for the County of Monmouth, are associated
with them.
Mr. F. W. Bunyan has resigned his position as testing chemist
for the Southern Pacific Railway Company to accept a position
as assistant chemist with the Noble Electric Steel Company,
Heroult, Shasta Co., Cal.
Mr. H. A. Noyes, research associate in horticultural chem-
istry and bacteriology at the Purdue Agricultural Experiment
Station, has resigned to accept an industrial fellowship with the
Mellon Institute, University of Pittsburgh.
Mr. Edward P. Bartlett, formerly assistant professor of
chemistry at Pomona College, Claremont, Cal., has been com-
missioned Captain in the Military Intelligence branch of the
Army.
Dr. Arthur L. Day has resigned as director of the Geophysical
Laboratory, Carnegie Institution of Washington, to do research
work for the Corning Glass Works, Corning, N. Y.
Dr. H. C. McNeil, of the chemical department of the Bureau
of Standards, has been appointed professor of chemistry at
George Washington University, as successor to Prof. C. E.
Munroe, who is giving all his time to the investigation work
of the Committee on Explosives of the National Research
Council.
Professor Moses Gomberg, professor of organic chemistry
at the University of Michigan, has been commissioned Major
in the Ordnance Department and is stationed in Washington.
Dr. H. S. Washington, of the Geophysical Laboratory, has
been appointed chemical associate to the scientific attaches
at the American embassies in Paris and Rome.
Professor M. F. Coolbough, of the department of chemistry,
Colorado School of Mines, is in Washington on leave of absence
and is engaged in war work at the Bureau of Mines.
Dr. H. M. Loomis, formerly of the Bureau of Chemistry,
Department of Agriculture, has been made chief inspector
of the sardine canneries of Maine and Massachusetts, for the
Food Administration.
Mr. F. C. Teipel, recently associated with Bush, Beach and
Gent, Inc., has rejoined Dana and Co., Inc., N. Y., as manager
of their chemical department.
Lieutenant Colonel Charles F. Craig, who until recently
has been stationed at Fort Leavenworth, Kansas, has been
placed in charge of the Yale Army Laboratory School, the new
school for bacteriologists and chemists.
Dr. Joseph C. Bock, formerly instructor at Cornell Uni-
versity Medical School, has been appointed professor of
physiological chemistry in the school of medicine of Marquette
University, Milwaukee.
Dr. F Mollwo Perkin has been elected president and Mr.
H. A. Carwood secretary of an association, which has been
organized in England, of chemists engaged in the oil, color, and
allied trades.
Mr. Charles L. Raiford, head of the department of chem-
istry at Oklahoma Agricultural and Mechanical College, Still-
water, Okla., has been elected associate professor of chemistry
at the University of Iowa.
Dr. E. B. Spear, professor of inorganic chemistry at the Massa-
chusetts Institute of Technology and consulting expert to the
Bureau of Mines, delivered an illustrated lecture on "Some
Problems of Gas Warfare" at the Brooklyn Institute of Arts
and Sciences on October 19.
INDUSTRIAL NOTES
Alfred I. du Pont, the owner of the Grand Central Palace,
N. Y., has announced that, notwithstanding the fact thai th(
Government is to take over the building for the pa Li
war as a base hospital for the Army and Navy, he int
proceed with his plans for creating there a center for world
commerce after the war in an Allied Industries Corporation.
Japanese manufacturers have well developed ill'"
industries since the war. They 1m
and an investment of more than $7,470,000. It is hoped that
some plan may in- di vised whereby they may
invasion of foreign products after the war.
The Labor Department announces thai th nlustries
of Niagara Kails. N. Y., are in great need of won
The survey of the plan by represent
Inderal I) acting under the direction of the Women
in Industry Service of the Department of Labor.
American dyestuffs are gaining a hold on the Japanese market,
which has heretofore been dominated by German products
obtained through neutral countries This gnin is clearly shown
by the figures of imports of dyestuffs into Japan for the Oral
I hi is now a permanent factor in the 111.11111
ictun "i cotton md silk piece goods ami the importance of
building up a market then foi American dyestuffs cannot l><
mphasized.
Reorgani/c is of the Federal Dyestuff and Chemical Corpora-
tion, of Kingsport, Term., have decided to call their new com-
pany the Union Dyestuff and Chemical Corporation. It is
"1 that the company anticipates some lai
from the Government for chemicals.
The \\ ai Department has awarded .1 contract i" I <
ican I'ln Philadelphia, foi 'ion of a
phosphorus plant at Fairmont, \\ V*a
952
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. ,o. No. n
List oh Applications Made'.to tub Fkdiirai. Trade Commission for Licrnshs 1'ndbr'Enbmv-Contkoi.i.kd Patents Possuant to the "Trading with
the Enemy Act"
Year Pat. No. Patentee Assicnee
1908 896,807 K.al Dieterich, Helfen-
Saxony, Germany.
[909
943,163
782,739
812,554
Aclolph Schmidt, Dresden,
Germany.
Emil Fischer, Berlin, Ger-
Alfred Einho
Germany.
Munich,
Otto J. Graul, Ludwigs-
hafen - on - the - Rhine,
Germany.
Otto Schmidt, Ludwigs-
hafen - on - the - Rhine,
Germany.
Otto Schmidt, Ludwigs-
hafen - on - the - Rhine,
I-Mn,
Chemische Fabrik Helfen-
berg, A. G., formerly
Eugen Dieterich.
E. Merck, Darmstadt, Gcr-
Farbwerke vorm. Meister,
Lucius & Bnining,
Hochst - on - the - Main,
Germany.
Badische Anilin & Soda
Fabrik, Ludwigshafen-on-
the-Rhine, Germany.
Badische Anilin & Soda
Fabrik, Ludwigshafen-
on-the-Rhine, Germany.
Badische Anilin 8: Soda
Fabrik, Ludwigshafen-
on-the-Rhine, Germany.
Knoll & Co., Ludwigshafen-
on-the-Rhine, Germany.
Patent
Improvement in agar-agar-
cascara products and pro-
cesses of making same.
Improvement in agar-agar-
. products.
CC-Dialkylbarbituric acid
and process of making
same.
Process of making cyan-
methyl derivatives of
Digitalis extract.
I c h t h y o 1 Gesellschaft Trade-mark "Ichthyol" for
Cordes, Hermanni & medicated soap.
Co., Hamburg, Ger-
Ichthyol Gesellschaft Trade-mark "Ichthyol" for
Cordes, Hermanni & plasters and certain medi-
Co., Hamburg, Ger- cinal preparations.
Ichthyol Gesellschaft Trade-mark "Ichthyol" for
Cordes, Hermanni 8: medicinal sulfonic acids
Co., Hamburg, Ger- and their salts.
many.
Vereinigte Chininfabriken Trade-mark "Euquinine"
Zimmer 8: Co. Ges. mit for derivatives of cin-
beschrankter Haftung, chona alkaloids.
Frankfort - on - the -
Main, Germany.
Applicant
Reinschild Chemical Co.,
47-49 Barclay St., New
York City.
Reinschild Chemical Co..
47-49 Barclay St., New
York City.
Fellows Medical Manu-
facturing Co. Inc., 26
Christopher St., New
York City
Fellows Medical Manu-
facturing Co., Inc., 26
Christopher St., New
York City
National Aniline & Chemi-
cal Co., Inc., 21 Burling
Slip, New York City.
E. C. Klipstein 8: Sons
Co., 644 Greenwich St.,
New York City.
E. C. Klipstein & Sons
Co., 644 Greenwich St.,
New York City.
Merck & Co., 45 Park PI.,
New York City.
Takamine Laboratory*, Inc.,
120 Broadway, New
York City.
Takamine Laboratory, Inc.,
120 Broadway, New
York City.
Takamine Laboratory'. Inc.,
1 20 Broadway, New
York City.
Takamine Laboratory, Inc.,
120 Broadway, New
Y'ork City.
The Pacific Electro Metals Company is now operating a
silicon-manganese furnace and will in the very near future be
operating another furnace making ferromanganese. Each of
these furnaces has a capacity of 3,000 kilowatts. In addition,
three 300 kilowatt furnaces are being installed in which ferro-
nickel, ferromolvbdenum, ferrochrome, and ferrotungsten will
be made as the raw materials are available. To make the plant
self-contained and independent of outside sources for elec-
trodes, an electrode plant has been erected and local raw ma-
terials have been applied to the manufacture of electrodes.
The directors of the company are C. D. Clarke, San Francisco,
President; J. M. Kroyer, .Stockton, Cal., Vice-President; Henry
Koster, San Francisco, Treasurer; C. F. Potter, San Francisco,
and J. W. Beckman, San Francisco.
A new chemical firm financed by Des Moines, Iowa, capital
has entered the field. It is known as the Consolidated Chemical
Products Co., of Alton, 111.
To encourage the production and distribution of manganese
used extensively in production of munitions, steel, and other
war supplies, the Railroad Administration has ordered a reduc-
tion of about 20 per cent in rates on manganese ore from western
producing fields to eastern manufacturing centers.
The Puerto Cortes consulate has been advised by residents
that they have discovered and denounced a rich deposit of
se within 2 miles of the Honduras National Railway.
I'll. \ claim that this ore is mixed with graphite, gold, and
copper.
The New Jersey Zinc Company has issued a series of pamph-
lets explaining the composition and uses of zinc dust, zinc pig-
oiled zinc, spelter and other zinc products, and will send
the booklets free to those interested.
The vVesI End Mining Co., San Francisco, is preparing to
in tall 1 quipment and begin the development of potash beds in
tin' Searles Lake district along lines endorsed by the Govern-
ment.
The I sl( "i Pim promises to become an important producer
Of iron, copper, and othei ores. Eleven mines have already been
located, though only two are being actively dl «
Tin Cuban government is taking a most active interest in the
development of these mines.
kiiiiku, Inc., has incorporated under the laws of Delaware to
manufacture dyes, chemicals, and colorings of all kinds
$10,000; incorporators, C. I. Rimlinger, F. A. Armstrong, B. A.
Spangler.
Two sulfuric acid plants are to be erected in Pennsylvania,
one at Emporium, the other at Mt. Union, under the super-
vision of the Construction Division of the Army. The esti-
mated cost for both plants is S3,ooo,ooo. The Emporium plant
will consist of eight units on a site on Driftwood Creek, close
to the plants of the Aetna Explosives Company and the Em-
porium Iron Company. The Mt. Union plant will be erected
adjacent to the plant of the Aetna Explosives Company.
Twenty acres of laud have been purchased at S56 an acre. The
contract has been awarded to the Leonard Construction Com-
pany. The preparation of all plans and specifications, in
addition to the supervision of the work, will be under the direc-
tion of the Construction Division.
At Copenhagen, Denmark, there is being held an exhibition
of products made from the nettle plant, which, in these times of
great shortage of raw material for the textile industry, is of
considerable interest. In the department for readymade stuffs
are to be found tablecloths, napkins, and towels in most diverse
patterns The nettle cloth is snow white, pliable, and pleasant.
The exhibits show that practically all of the material is used,
as. in addition to that consumed in making textiles, some is
ground for fodder and some used in the paper industry. This
is an entirely Danish industry and the people in the different
districts are taught how to prepare the nettles for delivery to
the factories.
Since 19 16 the cane sugar industries around Lake Maracaibo,
which formerly produced for local markets, have been exporting
large quantities to England and the United States owing to the
present high prices and scarcity of sugar.
Linoleum manufacturers have been asked by the Conserva-
tion Division of the War Industries Board to cut down the styles
from 3 patterns to one and to do away with inlay linoleum.
In addition to this they have been asked to cut down their use
of chrome.
The large chemical companies manufacturing sulfuric acid
and the powder manufacturers who depend upon the American
production of sulfur for use in making explosives were con-
siderably disturbed by reports that the Louisiana plant of the
Union Sulfur Co., at Lake Charles, had been partly destroyed
by a cyclone the latter part of August. Repairs are in progress
and the plant will soon be restored to its normal condition.
M. Lechner Co., Manhattan, X. V.. has incorporated to deal in
dyes, dyestuffs, powder, oils, etc.; capital, >io,ooo; incorpo-
rators, R. Lechner, A. Schmidt, B. Schneir, 200 Fifth Ave.
Nov., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
953
John R. Rettig and Co., Stockholm, has started to manu-
facture the electric-insulating material, micanite.
In order to increase the domestic supply of bromine, the
Government had additional brine wells drilled in Michigan early
in 1918. A large part of the output is marketed in the form of
potassium bromide, sodium bromide, and other salts.
Peach pit and coconut hull charcoal are said to be more
efficacious than ordinary charcoal in the soldier's gas mask
and the United States has undertaken to furnish the special
charcoal to the Allies. A nation-wide campaign for the collecting
of this material is in progress.
A process for making a substitute for leather out of cotton
is now being used by a company formed for that purpose.
Machines have already been designed for making shoe laces,
belts, and straps, and it is hoped that material several inches
wide may soon be made.
At a recent meeting of the House of Commons a vote on the
supplementary estimates for the Board of Trade of £1,000,000
($4,866,500), the first installment of an advance for the de-
velopment of the British dye industry, was agreed to. The
object of this advance is to establish the dye industry on a sound
basis within a reasonable time after the end of the war.
Plans are under consideration by the Solvay Process Co.,
Syracuse, N. Y., for the construction of a large plant in Grand
Rapids, Mich., for the manufacture of picric acid.
The New England Chemical Co., Boston, has been incor-
porated with a capital of $500,000 to manufacture, export, and
deal generally in dyestuffs and chemicals.
An explosion occurred in the chemical plant of the Barrett
Manufacturing Co., Philadelphia, on September 17, 1918.
Two men were killed and the blaze which followed the explosion
threatened at one time the Government munition plant at the
Frankford Arsenal.
The so-called Krayseska method, a new means of drying eggs,
fruit juice, and blood, has been found worth while in Germany.
The drying is done in a large iron cylinder, 5 meters in diameter,
in which a pair of large metal wings rotate rapidly, driven by a
steam turbine. The fluid is lashed to foam and dried by the aid
of a current of hot air which is continually passed through the
cylinder. The dried product is in the form of a powder, which
will keep for a long time and can be most economically trans-
ported.
The Florida Fertilizer Milling Company has been incorporated
with a capital of Sioo.ooo. The incorporators are F. D. M.
Strachan, Geo. F. Armstrong, and Clarence Camp.
Dr. Richard B. Moore of the United States Bureau of Mints
has announced that mesothorium is an excellent substitute in
many ways for radium. He believes that this substance should
be used instead of radium in luminous paints, gun sights, and the
dials of watches, compasses, and airplane instruments.
From recent experiments it has been shown that worth while
extracts of potash may be obtained from the common wild
desert grease-wood shrub growing in Texas.
The American Indian Oil and Gas Co., Poteau, Okla., is to
install machinery for the manufacture of carbon from natural
gas.
A new fertilizer called tetraphosphate is being manufactured
in Italy, which is considered equally as good if not better than
superphosphate. It was invented in 1914 by Professor Stop
of Bologna, and the process was patented and purchased by an
Italian company. Considerable progress has since been
notwithstanding the present difficulties in obtainh
phaterock and necessary reagents. From the eleven plants now in
operation there is a yearly output of 500,000 quintals and four
new plants are under construction.
ive phosphate deposits on Nauru or Pleasant Island and
Ocean Island, located northwest of New Zealand, are said to be
tin most valuable deposits of the kind in the world
quantity of phosphate available is estimated at 501 '.000,000
tons, and as fertilizer the deposit is said to rival the famous
nitrate fields of Chile.
Production of toluene has been commenced bj 111' 1 1 11 nil
Walker and Sons Chemical Co., Walkerville, 1
aim 0 ttion is to furnish tolut ai foi r u « iea ami
lop an after the war trade in dyes am! chi m
Swift and Co., Chicago, have let a contract for the con-
strue li'.n "I a 1 lad oil plant at Charlotte, N. C, costing $75,000.
Fire occurred on September 21 at the plant of the Ames
Chemical Laboratory, Glens Falls, N. Y., manufacturers of
nitrate of silver.
On October 5 fire completely destroyed the Charleston
Chemical Plant, at Bello, near Charleston, W. Ya. The plant
had been operated by the Government for several months.
The natural steam and water of the "soffioni" of the volcanic
area of Tuscany contain large quantities of boric acid and are
being used as a source of the acid which is produced about 99
per cent pure. The acid is treated with sodium carbonate to
obtain borax which is manufactured in the form of crystals and
powder. Ammonium carbonate is also manufactured and re-
search work is being done to determine the radioactivity of the
gases and the possibility of the separation of helium which is
also present.
The Bureau of Mines has requested an elimination of wheat
flour from the manufacture of high explosives other than "per-
missibles." This flour has been used in making dynamite and
other explosives employed in mining and engineering operations.
It is estimated that this will save more than 16,000 barrels.
Several factories are being built for extracting wax from
candelilla weed, which grows in great profusion upon many
thousands of acres of land bordering the Rio Grande in Texas.
An important feature of this industry is that it has recently
been discovered that the ash residue contains probably the
highest percentage of potash of any known species of vegetation.
The dried bagasse of the candelilla is used for fuel in the factory',
and from the ashes, it is claimed, enough potash may be ob-
tained to pay the entire expense of operating.
The Medical Research Board of the Division of Military
Aeronautics, after recent experiments with lenses for air pilots'
glasses, has announced that it has been able to effect the casting
of certain substances in thin sheets which, while not glass, can
be used as such and may afford a practical substitute for goggles.
Thin sheets of the material have been produced which can even
be ground and polished. The substance is hard and non-in-
flammable and insures practically a non-shatterable lens for the
protection of the pilots' eyes.
The manufacture of calcum carbide is being resumed near
Germiston, South Africa, as the difficulty of producing a suit-
able electrode has been overcome. It is expected that after a
few changes are made 2Y2 tons of carbide will be produced per
24 hrs.
The British Minister of Munitions has issued an order pro-
hibiting the purchase, sale, or delivery of any radioactive sub-
stances, luminous bodies or ores without a permit.
A ruling of the War Trade Board restricts the importation
into the United States of dyewoods and vegetable dye extracts
as to shipments made after Oct. 10.
The Southern Acid and Sulfur Co., East St. Louis, 111., is
planning the development of sulfur properties and the manu-
facture of sulfuric acid at Port Arthur and Texarkana, Texas.
The Porterite Efficiency Products Corporation, New York
City, manufacturers of paints, oils, and varnishes, has been
incorporated with a capital of $500,000. The incorporators are
W. J. Eldrcdge, P. J. Dobson, and J. A. Martin.
As a result of the increasing lemon crop, a plant has been built
at Corona. Cal . for manufacturing citric acid and also for making
and experimenting with other products.
The Hercules Powder Company, Landing, N. J., has recently
1 fifty women from various colleges throughout
the United States to act in the capacity of chemists.
I'll, business of the New Ungland Paint, Oil, and Yaruish Co.,
has been purchased by the du Pout Company.
As the result of a terrific explosion of T X T at the T. A.
Gillespie Loading Company's plant at Morgan, X. J., nearly
one hundred persons were killed and 325 of the 700 buildings
were destroyed.
The volcanic island of Sautoriui, in tile Aegean Sea, produces
a natural cement call.. I ' p.n 1 ,. l.ma," which, mixed 1
ubstitute
lh. high price of imported cement has
brought this product into promirn
The gathering of moss in Sweden is now organized on a large
scale. About 50,000 school children will be occupied in this
work during tl.. uonths and it is estimated 111. it Hi' y
tons of moss, to be used as cattle feed
954
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No.
3
GOVERNMENT PUBLICATIONS
By R. S. McBridb, Burea
NOTICE — Publications for which price is indicated can be
purchased from the Superintendent of Documents, Government
Printing Office, Washington, D. C. Other publications can
usually be supplied from the Bureau or Department from which
they originate. Commerce Reports are received by all large
libraries and may be consulted there, or single numbers can be
secured by application to the Bureau of Foreign and Domestic
Commerce, Department of Commerce, Washington. The regu-
lar subscription rate for these Commerce Reports mailed daily is
$2.50 per year, payable in advance, to the Superintendent et
Documents.
PUBLIC HEALTH SERVICE
Official Control of Antipneumococcus and Antimeningococcus
Serums. G. W. McCoy. Public Health Reports 33, 13 13-
iji6. Issued August 9.
GEOLOGICAL SURVEY
Gravel Deposits of the Caddo Gap and De Queen Quadrangles,
Arkansas. H. D. Miser and A. H. Purdue. Bulletin 690-B.
From Contributions to Economic Geology, 1918, Part I. 15
pp. Published June 14
New Determinations of Carbon Dioxide in Water of the
Gulf of Mexico. R. C. Wells. Professional Paper 120-A,
from Shorter Contributions to General Geology, 1918. 16 pp.
Published June 20.
The Upper Chitina Valley, Alaska. F. H. Moffit. With a
Description of the Igneous Rocks by R. M. OvErbeck. Bulletin
675. 82 pp. Paper, 25 cents.
The only minerals yet found in this district that may be of
possible economic importance are copper, gold, and molybdenum.
No copper ore has been mined nor is any likely to be mined
in the near future, for practically no work has been done on the
copper deposits except the assessment work necessary to hold
a few claims. The present price of copper, however, should
stimulate the search for that metal in this district.
A little gold has been produced, but it is doubtful if the
quantity recovered has been sufficient to pay more than a small
part of the cost of production.
A vein of molybdenite is reported by a prospector who spent
part of the summer of 1915 in the upper Chitina Valley. The
vein, which is about 8 miles from the lower end of the largest
of the Canyon Creek glaciers, is in granite and is reported to be
8 feet wide and to consist of quartz and molybdenite. The
molybdenite forms a solid vein, 12 in. thick, between the
quartz and the hanging wall and occurs in stringers and bunches
through the quartz and in disseminated flakes in the quartz.
There is no timber near the property, and the best source of
supply would be Young Creek, which is separated from Canyon
Creek by a low, flat divide that could be easily traversed. Sleds
afford the only method of transportation now available in
winter, and any ore produced from the vein will have to be
brought out over the glacier ice to Canyon and Young Creeks and
carried thence to the railroad at McCarthy.
Some Manganese Deposits in Madison County, Montana.
RDBB Bulletin 690-F. Being .1 Separate from Con-
tributions to Economic Geology, 1918, Part I, pp. 131-143.
Published July S, 1918.
Platinum and Allied Metals in 1917. J. M. Hill. Being a
Separate from Mineral Resources of the United States, 191 7,
Part I, pp. 11-21. Published June 21, 1918.
Crude platinum was produced in Alaska, California, Oregon
and Washington in 1917. Buyers and refiners report purchases
amis from pioducers in these States, which, at the
[ of Standards, Washington
average price (S90 an ounce), would have a value of $54,450.
Incomplete returns from placer mines that produce crude
platinum indicate that the production in 191 7 fell off about
100 ounces from that of 1916, when it was 710 ounces. In view
of the high prices for crude platinum in 1917 this decrease is
rather difficult to understand, but part of it may be due to the
fact .that some of the miners held their platinum for higher
prices.
Dealers and refiners reported sales in 1917 of 72,186 ounces of
secondary platinum metals derived from refining scrap and
sweeps. The figures that make up this total probably represent
some duplication, as the same metal may be handled as scrap
several times in a year. The large increase in the sales of
scrap metals indicate cleaily that, owing to the greatly de-
creased imports of crude platinum and the high prices paid for
scrap, much attention was given to the collection and refining
of all kinds of scrap containing platinum metals.
The imports of platinum and allied metals for consumption in
1917, exclusive of the 21,000 ounces of Russian platinum re-
ceived in December, which do not appear in the reports of the
Bureau of Foreign and Domestic Commerce for 1917, were about
57 per cent of the imports in 1916 and about 25 per cent of the
pre-war imports.
The quoted price of refined platinum in the New York market
was $80 to S82 a troy ounce in January 1917, but it increased
to S102 to $105 in February and remained nearly stationary
throughout the year. The average price for the year was
$102.80 a Troy ounce.
After the War Department had commandeered all crude and
refined platinum on March 2, 1918, a maximum price of $105
an ounce for all imports was set by the War Industries Board.
Refined palladium was quoted at $70 to $85 a troy ounce at
the beginning of 1917, but prices advanced continuously through-
out the year, being $115 to Si 25 for the period from August to
November and reaching a maximum of S130 to $135 the last of
December. Refined iridium was apparently sold only by special
bargaining, and no very definite information is available con-
cerning its price. Apparently Si 10 was the nominal quotation
in January, but sales in the last months of 191 7 are said to have
been made at $180 to $185 an ounce.
Quicksilver Deposits of the Phoenix Mountains, Arizona.
F. C. Schrader. Bulletin 690-D. Being a Separate from Con-
tributions to Economic Geology, 1918, Part I, pp. 95-109.
Published June 26, 1918.
Cadmium in 1917. C. E. Siebenthal. Being a Separate
from Mineral Resources of the United States, 1917. Part I,
pp. 49-53. Published July 12, 1918.
Cadmium was first produced in the United States by the
Grasselli Chemical Company in 1917. One by one other com-
panies began the recovery of cadmium until there are now six pro-
ducing companies, as follows: American Smelting & Refining
Co.; Grasselli Chemical Co.; Krebs Pigment & Chemical Co.;
Mammoth Copper Mining Co.; Midland Chemical Co.; and
United States Smelting, Refining & Mining Co. As cadmium
residue resulting from the production of electrolytic spelter is
accumulating at several plants there will doubtless be other
producers before long.
Cadmium is produced in the United States in two forms —
metallic cadmium and the pigment, cadmium sulfide The
domestic production of metallic cadmium in 1907 was nearly
sufficient to supply the home demand, a fact shown by the small
imports for that year, but in 1908 the quantity of cadmium im-
ported was almost doubled, and in 1009- 191 2 the imports were
Nov., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
955
back at the figures that prevailed before cadmium had been
produced in the United States. Since 1912, however, the
domestic production has made great strides, and as a result
the imports of cadmium are again small. As the imports came
largely from Germany they have been practically stopped for
the last four years.
Complete statistics of the exports of cadmium are not avail-
able, but it is known that domestic cadmium has been largely
exported during the war. According to the Bureau of Foreign
and Domestic Commerce the following quantities of cadmium
were exported through the port of New York in the last quarter
of 1916: In October, 33,244 pounds, valued at $55,259; in
November, 4,900 pounds, valued at $5,100; and in December,
1,044 pounds, valued at $1,530. Of the exports in October,
23,210 pounds went to France, 9,984 pounds to Italy, and 50
pounds to Dutch Guiana.
Unrefined cadmium in cadmium residues has also been ex-
ported, as noted above.
The price of stick cadmium throughout the first half of 191 7
was listed in retail lots as nominal at $1.50 a pound. During
the last half of the year the quotations remained practically
stationary at $1.40 to $1.75 a pound. The average price for
1917 as calculated from sales was $1.47 a pound, as compared
with an average of $1.56 a pound in 1916. The price in London
during the first four months of 1917 was 7s. 7'Ad. ($175) a
pound; during the next five months it was 8s. il/A. ($1.90) a
pound, and for the remainder of the year it was from 7s. 3d. to
7s. 7'/2d. ($1.70 to $1.75) a pound.
The average selling price of cadmium sulfide in the United
Sta'es in 1917 was $1.41 a pound, as compared with $1.26 a
pound in 1916.
The value of the output of cadmium in the United States in
1917, calculated at the average selling price, was $305,097, as
compared with $210,931 in 1916, and the value of the cadmium
sulfide produced was $70,939, as against $27,942 in 1916.
The total value of the output , of metallic cadmium in the
United States since the beginning of production in 1907 is
$830,673 and of cadmium sulfide $151,389, both together equal
to nearly a million dollars.
Manganese and Manganiferous Ores in 1916. D. F. Hewett.
Being a Separate from Mineral Resources of the United States,
1916, Part I, pp. 731-756. Published July 18, 1918.
As an indication of the condition of the domestic manganese
industry during 1916 it may be said that probably in no other
mineral industry has there been the same inducement for change
in source of supply, price, and manner of utilization. The con-
tinued elimination of established foreign sources of manganese
ore and ferromanganese has caused the country to depend al-
most entirely on the ore deposits in Brazil. As prices of ore and
ferromanganese more than doubled within the year, there has
been strong incentive to utilize less desirable domestic supplies
of ore. As a result, domestic production of each grade of ore in
1916 was nearly three times that of 1915. Although this is still
only a small part of the country's needs as expressed in terms of
manganese metal, the production is much larger than many
competent observers thought possible several years ago.
The domestic shipments of manganese ore in 1916 were
2(>,997 gross tons; of ferruginous manganese ore, 176,130 tons;
and of manganiferous iron ore, 372,673 tons Most of this
material is used in the iron and steel industries.
Gems and Precious Stones in 1916. W. T. Smaller. Being
a Separate from Mineral Resources of the United States, 1916,
Part II, pp. 887-899. Published June 27, 1918.
Talc and Soapstone in 1917. J. S. DillER. Being a Separate
from Mineral Resources of the United Stales, 1917, Part II,
pp. 81-84. Published July 12, 19:8.
The sak-s of talc in 1917 amounted to 198,613 tons, valued :it
■1,889,673, a gain, as compared with 1916, of nearly 3 per cent
in quantity and of more than 7 per cent in value. Thirty-
seven producers reported to the Geological Survey, of whom 7
were 'in California, 6 in Georgia, 1 each in Maryland, Massa-
chusetts, and New Jersey, 4 in New York, 6 in North Carolina,
2 in Pennsylvania, 5 in Vermont, and 4 in Virginia.
The highest average priced talc, including that which was
cuf for gas tips, pencils, and insulators, was sold from Georgia,
North Carolina, and Vermont, and the highest prices ranged
from $50 to $200 a ton. The lowest priced material was sold
as rough talc (crude) at prices ranging from $3 to $8 a ton, or
on an average of $5.58 a ton. Its value was greatly increased
by grinding and ranged, when ground, according to quality,
from $5 to $20 a ton, although the general average was only
$9.11 a ton.
Magnesite in 1917. C. G. Yale and R. W. Stone. Being
a Separate from Mineral Resources of the United States, 1917,
Part II, pp. 63-69. Published July 19, 1918.
Until 1917 practically all the domestic magnesite was pro-
duced in the State of California, but in that year the newly
developed deposits in Stevens County, Wash., yielded nearly
one-third of the domestic output. Formerly this county im-
ported from 250,000 to 350,000 tons of magnesite (stated in
terms of crude material), mostly from Austria-Hungary and
Greece. Practically all the California output was consumed
on the Pacific Coast, mainly as a digestei for wood pulp in paper
mills, but to some extent as plastic material for flooring, plaster,
and cement. The freight rate to eastern points from California
was prohibitive, in view of the cheapness of the imported ma-
terial. Since the opening of the war, however, and especially
since the United States became involved in it, the importation
from Austria-Hungary has ceased, and, except for a com-
paratively small quantity derived mostly from Greece and
Canada, the country has been compelled to rely upon the
domestic product. The natural result of this condition has been
renewed activity in the larger mines and the opening and de-
velopment of numerous new properties.
At the beginning of 1917 the crystalline magnesite from
Washington was new on the market and untried. It so quickly
proved its value that the market consumed all that the new
quarries could produce. Toward the end of the year, however,
embargo against shipments into the freight-congested district
east of Chicago and north of Ohio and Potomac Rivers began
to delay and limit shipments from both California and Wash-
ington, for many of the plants that make refractory products
from magnesite are east of Chicago. In spite of this embargo
the continued demand caused an increase of more than 100
per cent in production in 191 7 over 1916, the previous record
year.
The crude magnesite produced and sold or treated in the
United States in 1917 amounted to 316,838 short tons, valued
at $2,899,818, as compared with 154,974 tons, valued at
$1,393,693, in 1916. In 1917 California produced 211,663
tons, valued at $2,116,630, and Washington 105,175 tons,
valued at $783,188. California's increase in quantity over the
production of 1916 was 37 per cent. Washington began pro-
duction in December 1916, 715 tons being shipped by the end
of the year.
The Nesson Anticline, Williams County, North Dakota. A.
J, Collier, bulletin 691-G, from contributions to Economic
Geology, 1918, Part II. 6 pp. Published August 15. As it is
generally recognized that the highest parts or crests of anti-
clines or arches in the rocks are the most likely places to find
accumulations of natural gas, it would seem advisable that one
or more wells be drilled about four miles cast or southeast of the
Nelson well in search of a In
The Santo Tomas Cannel Coal, Webb County, Texas. G. H.
Ashley. Bulletin 691— I, from contributions t" Kconomic
Geology, 1918, Pari [I. 19 pp. Published Inly 25.
956
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. n
Gold and Silver in 1916. (General Report.) H. I). Mc-
Caskey and J. P. Duni.op. Separate from Mineral Resources
of the United States, 1916, Part I, pp. 679-721. Published
May 7.
Chromite in 1917. J. S. D11.1.ER. Separate from Mineral
Resources of the United States, 1917, Part I, pp. 37-47. Pub-
lished August 8.
The domestic production in 191 7, so far as may be judged
from reports already received by the Geological Survey, was
43,725 long tons. It came mainly from California, where the
output was more than 36,700 long tons. Oregon ranks second,
with a production of about 6,700 long tons. Alaska produced
nearly 1 ,000 tons, and the remainder, less than 300 long tons, came
from Washington, Maryland, ami Xorth Carolina. As a con-
siderable number of supposed producers have not yet reported,
ible that the total production may turn out finally to be
somewhat greater. It seems probable that the total domestic
production in 1917 was about 3,000 tons less than in 1916. If
so, the decline deserves special consideration in view of the con-
stantly increasing demand.
To discover, if possible, the causes of decline in the production
of chromite in 191 7, the United States Geological Survey sent
out a questionnaire to all the chrome producers on its list, ask-
ing for statements of the maximum possible production of the
mine during the last quarter of 191 7 and the actual shipments
of chromite from the mine during the same period, the difference
being the deficiency in production due to one or more causes,
of which the following may be noted: Bad weather, poor roads
in winter, lack of funds, lack of shipping facilities, especially
lack of cars as the result of the freight embargo, low prices, and
uncertainty of market, particularly for low-grade ore. The
last two ate the most potent causes affecting small producers.
The price of 40 per cent chromite at the beginning of 191 7
was $15 a ton, that is, 37V2 cents a unit of chromic oxide, but
at the end of the year the price had been raised to 70 cents a
unit, or £28 a ton. The actual price reported to the Geological
Survey ranged from Sio to S50 a ton and the average price
of the ore sold during the year by producers was a little more
than $24 a ton. Early in 1918 the price for 40 per cent ore
reached 85 cents a unit (S34 a ton). The impending crisis re-
sidtiug from lack of ships to import the ore needed for war
purposes has impelled the principal consumer, the Electro-
metallurgical Co., of New- York, to advance prices greatly in
the hope of increasing domestic production.
The block chrome ore sold on the Pacific Coast in the summer
of 1917 ranged in composition from 30 to 55 per cent chromic
oxide " age composition was 42 per cent.
Of the chromite mined and sold in the United States in 1917,
22 per cent of the total quantity contained from 45 to 50 per
cent of chromic oxide, 32 per cent contained from 41 to 45 per
cent of chromic oxide, 36 per cent contained from 38 to 41 per
cent of 1 ,1 from 30 to 38
1 omic oxide.
Of the ore marketed on the Pacific Coast in 1017 nearly nine-
utaincd 38 per cent or more of chromic oxide and fell
within the price of $1.25 a unit DOW offered. Important con-
■ hromite ranging from 30 to 35 per cent chromic oxide
have recently been signed, but the prices lor that grade of ore
have not yet greatly increased. It is hoped, however, that the
large consumers of chrome ore for refractory purposes, as well
as for fcrroehrome, may further stabilize prices not only by
adopting tins scale of prices but by establishing a corresponding
minimum price for ore below the grade of 38 per cent chromic
md thus contribute greatly to the increased production
of low-grade ores and incidentally aid in promoting concentra-
tion.
The most striking feature of (he imports in 1917 is 1'
decrease in the total from [15,943 long tons in 1916 to 72,063
long tons in 191 7. This decrease is due wholly to restricted
shipping facilities on account of the war and affects particularly
imports from South Africa and Xew Caledonia, which require
long overseas transportation. On the other hand, the imports
from Canada have greatly increased and those from Guatemala
appear for the first time. Only 17 tons have come from Cuba,
but recent developments indicate that Cuba and also Brazil will
soon be large contributors to our needs of chromite.
The measure of normal annual consumption of chromite for
all the various uses before the war may best be expressed by the
sum of domestic production and imports in 1913, about 65,000
long tons. On account of the greatly augmented demands of
war conditions it has been estimated by the committee on
mineral imports and exports of the Shipping and War Trade
Boards that the needs of the United States in 1918 will be equiva-
lent to about 130,000 long tons of 50 per cent ore, of which
67,500 tons will be needed for ferrochrome, 40,000 tons for
making bichromates and other chemicals for tanning, etc., and
22,500 tons for refractors' purposes.
Gold, Silver, Copper, Lead, and Zinc in the Eastern States
in 1917. J. M. Hn.L. Separate from Mineral Resources of the
United States, 1917, Part I. 7 pp. Published July 29.
Slate in 1917. G. F. Loughlix. Separate from Mineral
Resources of the United States, 1917, Part II. 17 pp. Pub-
lished July 30.
The total value of the domestic slate sold in 1917 — $5,749,966
— was an increase of nearly 8 per cent over that for 1916, which
was an equal increase over the value in 1915. This increase
was common to all the slate products recorded but was most
marked in slate for "other uses." The increase in value, how-
ever, is in marked contrast to the prevailing decrease in quantity
of the different products sold and only indicates the degree to
which prices have been advanced to offset increased cost of pro-
duction.
Feldspar in 1917. F. J. Katz. Separate from Mineral Re-
sources of the United States, 1917, Part II. 5 pp. Published
August 7.
The marketed production of domestic feldspar in 191 7 was
the largest ever recorded. It was an increase of nearly 7 per
per cent in quantity as compared with 1916, 35 per cent as com-
pared with 1915, and 5 per cent as compared with 1914. As
reported prior to 1916, the values of the yearly production have
expressed the combined sales of crude and ground feldspar and
have, therefore, shown wider fluctuation than the quantities
because of changes from year to year in the proportions sold as
crude or ground. The value of the combined production in
1013 was the largest in the decade, and the production in 1915
dropped almost to the low level of 190S and 1909. The in-
dustry rallied markedly in 1916 and 1917, making productions
substantially as large as in the best years.
The average price for feldspar sold crude in 1917 v.
a long ton, as compared with S3. 34 in 1916 and S3-4<> m '9>5.
the range in prices during 1917 reported to the United States
Geological Survey being from S2 to S7 a long ton. The average
price of ground feldspar in 1017 was fio 15 a short ton. compared
with $9.30 in 1 010 and $8.33 in 101 s. the range in 10 17 in prices
reported to the Geological Survey being from $5.70 to Si 7 a
ton.
( If the total marketed production about 70 per cent
crude and 30 per cent ground in 191 7. compared with 63 per cent
and 37 per cent, respectively, in 1916, and 69 per cent and 31 per
cent in 1915.
Sand-Lime Brick in 1917. J. Middlkton. Separate from
Mineral Resources of the United States, 1917, Part II. 1 p.
Published August 20.
The sand-lime brick industrv. contrary to indications at the
beginning of the year, showed decrease in both output and value
Nov., iqi8
THE JOURNAL OF INDUSTRIAL
in 191 7 compared with 1916. The causes for the decrease in
output are not difficult to find. The principal cause was the
general decrease in building activities; the scarcity of labor,
likewise a general condition, was another cause, and trans-
portation conditions may be cited as a third reason for this de-
cline. The increase in the cost of production was reflected in the
increased cost to the consumer of the principal product — com-
mon brick — of $1.11 per thousand, compared with 1916. Not-
withstanding the decrease in the value of the sand-lime brick
marketed in 191 7 the value in that year was the greatest in the
history of the industry with the exception of 1916.
The decrease in the quantity of sand-lime brick sold in 191 7
compared with 1916 was 39,798,000 brick, or nearly 18 per cent,
but the decrease in value was only 853,743, or 4 per cent.
Gems and Precious Stones in 1917. W. T. Schaller.
Separate from Mineral Resources of the United States, 191 7,
Part II. 23 pp. Published July 29. This article contains a
very complete glossary of gem names.
Mica in 1917. W. T. Schaller. Separate from Mineral
Resources of the United States, 1917, Part II. 12 pp. Pub-
lished July 29.
Although the total value of all mica produced and sold in the
United States in 1917, as reported to the United States Geological
Survey, was the highest on record, the total quantity was smaller
than that for any preceding year since 1908, with the exception
of 191 2. This was due in part to the fact that a good deal of
the scrap mica mined was not sold.
The prices paid for mica in 191 7 continued, with minor fluctua-
tion's, to increase throughout the year. The prices paid for
domestic mica in the South in 191 7 were from 10 to 20 per cent
higher than the prices for similar mica in 1916. The greatest
increase was for the smaller sizes, especially for the il/± by 2,
2 by 2, and 2 by 3 in. The largest sizes showed no increase in
price.
The average price per pound of sheet mica produced in 1917
was 58 cents, a price lower than for either 1916 (61 cents) or
1 915 (68 cents), but higher than for any other preceding year.
A very large amount of punch or washer mica was produced in 1 9 1 7 ,
and as this averaged only 5 cents a pound it materially lowered
the average value of all sheet mica with which it was combined.
Graphite in 1917. H. G. Ferguson. Separate from Mineral
Resources of the United States, 1917, Part II. 29 pp. Pub-
lished July 26.
The increase in metal manufacture incident to the progress
of the war has brought a greatly increased demand for crucible
graphite, and the amount of graphite suitable for crucible use, both
domestic and imported, consumed during the year was ap-
proximately 30,000 short tons, as against 13,500 short tons in
1 91 3. The domestic production has responded to the greater
demand and during the last three years has shown a steady
increase.
Estimates furnished by the producers of crystalline graphite
show that out of the total sales of 10,584,080 lbs., 6,816,913
lbs., valued at $982,336, or about 64 per cent by weight and 90
per cent by value of the total, was flake graphite containing
from 80 to 90 per cent graphitic carbon, in large part suitable
for crucible use. The remainder, 3,767,167 lbs., valued at
u.i, dusl or low-grade flake probably averaging undei
"50 per cent graphitic carbon. The proportion of flake produced
is higher than in previous years, owing in part to im
milling methods, whereby :i larger proportion ol the [raphite
was saved as flake, and in p;irt to the fact that because of the
freight embargo during the latter part of the year such ship-
tin- Alabama producers were able to a
mainly of the better grade material.
The production of amorphous graphite during 1917 was
8,301 t"ns, valued at iared with 1,62a tons,
Valued ;it (30,723 in I'll''. As amorphous graphite is not suit-
AND ENGINEERING CHEMISTRY 957
able for use in crucible manufacture, war conditions have no
increased the demand for it to so marked a degree as for crystal
line graphite'. Moreover, the production of flake graphite for
crucible use yields a large amount of dust as a by-product, and
this dust is available for practically all uses.
Graphite is manufactured chiefly by the International Acheson
Graphite Co., which utilizes electric power generated at Niagara
Falls. The output has increased greatly in recent years and now
forms an important element in the country's graphite supply.
The bulk graphite is made either from anthracite or from petro-
leum coke and is utilized mainly in lubricants and p aints and for
foundry facings, boiler-scale preventives, and battery fillers.
Besides the graphite products that enter into competition with
natural graphite, there are a large number for which artificial
graphite is particularly adapted. Chief among these is graphite
electrodes, the demand for which has greatly increased during
the last three years on account of the remarkable growth in
certain electrochemical industries.
Domestic flake graphite brought slightly higher prices in 191 7
than in 1916. The prices received at the mines for the best
grades ranged from 12 to 18 cents a pound for No. 1 flake,
according to its grade; from 6 to 10 cents a pound for Nos. 2 and
3; and from half a cent to 5 cents a pound for dust. Flake
graphite containing 90 per cent or more of graphitic carbon
sold for considerably higher prices than the usual product con-
taining 85 per cent carbon or less.
Salt, Bromine, and Calcium Chloride in 1917. R. W. Stone.
Separate from Mineral Resources of the United States, 1917,
Part II. 12 pp. Published August 10.
Salt is so abundant and so widely distributed in the United
States that the industry can meet domestic requirements in
spite of unfavorable conditions. At some plants in 191 7 there
was shortage of labor, difficulty in obtaining fuel, and an in-
adequate supply of freight cars, yet the total production for the
country was a notable increase over that of 1916. The salt
produced and sold in the United States in 1917 was 6,978,177
short tons, valued at $19,940,442, an increase of 9.7 per cent
in quantity and 46.1 per cent in value over the production of
1916.
From the itemized figures in the table it is determined that the
increase in production of manufactured or evaporated salt in
1917 was 1.1 per cent, of brine salt 13.8 per cent, and of rock
salt 17.3 per cent. The much larger increase in rock salt is a
measure for the readiness with which the production of salt by
mining can be expanded in comparison with the production by
evaporating brine.
The average price increased $3 per cent and was $2 .86 per ton
in 191 7, as compared with $2.14 in 1916. This great increase
in price was caused by higher wages paid for labor and higher
cost of fuel and an other supplies.
The quantity of bromine marketed in 191 7 increased nearly
23 per cent over the production in 1916.
The production of bromine was retarded in 1917 by steadily
falling priii- and increasing cost of production, by railroad
in ight cot mbargo on shipments which hindered the
11 of salt, by shi ibor and fuel at some plants,
repairs, and by the extremely cold weather in Decem-
ber.
The wholesale price of bulk bromine in New York was to
d in [913, )o to 35 cents from January to August
[914, and 40 to 50 cent from Septembei in December 1914-
Tin- following I'M' shorn - a largi increa 1 in con umption
mihI ;i \o I calcium chloride in 1917:
rATKS,
1915-1917
■ ". Average Price
Yi:ak Slum Tone per Ton
1915..
I'M',
1917.. .10,503
95 1
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol.
No.
Sulfur, Pyrites, and Sulfuric Acid. P. S. Smith. Separate
from Mineral Resources of the United States, 1917, Part II.
43 pp. Published July 10.
Although precise statistics are not given, it may be said that
the domestic production in 191 7 was nearly 50 per cent greater
than in 1916 — a year during which several hundred per cent
more sulfur was produced than in any year before the war.
According to reports received from the Bureau of Foreign and
Domestic Commerce, the quantity of crude sulfur or brimstone
exported from the United States in 1917 was 152,833 tons,
valued at $3,504,661. This was the greatest export of sulfur
by this country in a single year, exceeding by nearly 20 per cent
the previous record quantity exported in 1916. The exports
in 1917 exceeded by more than 70 per cent the exports in 1913,
which may be taken as fairly representative of normal conditions
immediately before the war.
Up to 1900 the annual domestic production of sulfur was
relatively insignificant and about 175,000 long tons of sulfur
were imported each year. With the commercial development
of the deposit in Louisiana the importation of sulfur suddenly »
decreased, and in 1907 the imports amounted to only about
20,000 tons. Since that year up to and including 1916 the im-
ports of sulfur each year have been between 20,000 and 30,000
long tons. In 191 7, however, owing to the restrictions imposed
by certain of the foreign governments, the difficulty of obtaining
ships, and the quantity of domestic sulfur available, less than
1,000 tons of foreign sulfur were received in this country.
The domestic production of pyrites in 1917 was 462,662
long tons, valued at §2,485,435, an increase of about 39,000 long
tons in quantity and of about $520,000 in value, as compared
with the production in 1916. The consumption of pyritic ore in
1917 — that is, the domestic production plus imports — amounted
to about 1,430,000 long tons and was about 240,000 long tons
less than the consumption in 191 6. This decrease was largely
attributable to the great falling off in imports.
In addition to the pyritic ores reported here, returns from
manufacturers of sulfuric acid show that 708,500 long tons of
domestic copper-bearing sulfide ores, 147,531 long tons of
foreign copper-bearing sulfide ores, 594,100 long tons of domestic
zinc-bearing sulfide ores, and 152,911 long tons of foreign zinc-
bearing sulfide ores were treated in 191 7 for their sulfur as
well as for their metallic content.
The production of sulfuric acid in 191 7 was nearly twice as
great as the production in 191 3, which may be taken as a normal
pre-war year. The expansion in the industry to meet the condi-
tions imposed by the war had been begun in 1916, so that the
increase in 1917 over 1916 was much less than the increase in
1916 over 1915.
The production of sulfuric acid in 191 7 expressed in terms of
50° B6. was 5,967,551 short tons valued at $71,505,536, to which
must be added 759,039 short tons of acids of strengths higher
than 66° Be., which cannot be converted for purposes of calcula-
tion into acid of 500 Be., valued at $16,034,645. The total
value of all the sulfuric acid produced in 1917 was therefore
$87,540,181. This production shows an increase in 1917 over
1916 of the acid expressed as of 500 Be. of more than 325,000
short tons in quantity and of about $8,800,000 in value and an
increase in stronger acids of more than 315,000 short tons in
quantity and $5,225,000 in value. The value of the total pro-
duction of sulfuric acid in 191 7 was therefore more than
$14,000,000 greater than the value in 1916.
The totals given above include by-product acid — that is, acid
produced at copper and zinc smelters. The production of acids
from this source in 1917, expressed in terms of 6o° acid, was
1,336,209 short tonsf valued at $14,516,104, to which must be
added 119,048 short tons of acids of strengths higher than
66° Be., which can not be calculated in terms of acid of 60° Be.,
valued at $2,374,441 None of the stronger acids are reported
to have been produced at copper smelters, and no 50° acid was
reported to have been produced at either the copper or the zinc
smelters.
BUREAU 07 CENSUS
Chemicals and Allied Industries. Census of Manufacturers,
1914. 85 pp. One of a series of bulletins being issued by the
Bureau, presenting statistics of industries, concerning which
inquiries were made at quinquennial census of manufacturers
in 1914. Statistics are presented in three sections: Summary
and analysis, giving general data compiled for industry; special
statistics relating to materials, products, and methods of manu-
facture; and State tables, giving comparative summary, by
States, for 1904, 1909 and 1914, and detailed statistics for in-
dustry, by States, 1914.
Leather Industry. Census of Manufacturers, 1914. 63 pp.
Wool Manufacturers. Census of Manufacturers, 1914. 48 pp.
Patent and Proprietary Medicines and Compounds and
Druggists' Preparations. 18 pp.
BUREAU OF MINES
Bibliography of Petroleum and Allied Substances, 1915.
E. H. Burroughs. Bulletin 149. in pp. Paper, 15 cents.
Oil Storage Tanks and Reservoirs. With a brief discussion
of losses of oil in storage and methods of prevention. C. P.
Bowie. Bulletin 155. 68 pp. Paper, 25 cents.
Mining and Concentration of Carnotite Ores. K. L. Kithh.
and J. A. Davis. Bulletin 103. 77 pp. Paper, 25 cents.
Prepared under a cooperative agreement with the National
Radium Institute.
Initial Priming Substances for High Explosives. G. B.
Taylor and W. C. Cope. Technical Paper 162. 20 pp.
Paper, 5 cents.
The Use of Permissible Explosives in the Coal Mines of
Illinois. J. R. Fleming and J. W. Roster. Bulletin 137.
103 pp. Paper, 20 cents. This report was prepared under a
cooperative agreement with the Illinois State Geological Survey
and the engineering experiment station of the University of
Illinois.
Metal-Mine Accidents in the United States during the Calen-
dar Year 1916. A. H. Fay. Technical Paper 202. 78 pp.
Paper, 10 cents.
Quarry Accidents in the United States during the Calendar
Year 1916. A. H. Fay. Technical Paper 193. 55 pp. Paper,
10 cents.
Siliceous Dust in Relation to Pulmonary Disease Among
Miners in the Joplin District, Missouri. E. Higgins, A. J.
Lanza, F. B. Laney and G. S. Rice. Bulletin 132. 108 pp.
Paper, 25 cents.
Recovery of Gasoline from Natural Gas by Compression and
Refrigeration. W. P. Dykema. Bulletin 151. 117 PP- Paper,
25 cents. "This report treats of the compression and refrigera-
tion process for the recovery of gasoline from natural gas from the
viewpoint of the practical engineer and businessman. Condi-
tions of actual operation and the equipment in use are cited and
described so that operators, and others interested, can compare
the variations in methods of treating natural gas for its gasoline
content in the different fields and also the conditions encountered
and the features that control the methods used."
The Quick Determination of Incombustible Matter in Coal
and Rock-Dust Mixtures in Mines. A. C. Fieldner, W. A.
Selvig and F. D. Osgood. Technical Paper 144. 29 pp.
Paper, 10 cents. "An investigation of the specific-gravity
method of determining the percentage of rock dust, ash, or dry
incombustible in mixtures of coal and rock dust such as are
Nov., 101S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
959
found in the entries and rooms of mines showed that this method
was rapid and sufficiently accurate for use in controlling the
application of rock dust in mines."
Effects of Moisture on the Spontaneous Heating of Stored
Coal. S. H. Katz and H. C. Porter. Technical Paper 172.
19 pp. Paper, 5 cents. "The only recommendation of practi-
cal import to be made as a result of the matters considered in
this paper is to prevent the segregation of the fine coal in building
a pile for shortage. This has been proposed before as a means
of reducing the danger of spontaneous combustion. The con-
sideration of moisture now gives it further support."
Weights of Various Coals. S. B. Flagg. Technical Paper
184. 7 pp. "A study of the foregoing table indicates that
heavier weights may be expected for coals of high fixed carbon
content than for those of low. Increased ash content seems
to lower the unit weight. It is also true, in general, that the
coals high in moisture are fighter than those low in moisture
and the younger coals are fighter than the older coals."
Use of the Interferometer in Gas Analysis. F. M. Siebert
and W. C. Harpster. Technical Paper 185. 12 pp. Paper,
5 cents. This paper describes the outcome of some of the
investigations made by the Bureau of Mines in connection with
work on mine gases and natural gas.
Physiological Effect of Different Gases on Man. G. A.
Burrell. Large chart unnumbered. This chart shows the
pertinent physical properties and easily recognized charac-
teristics of mine gases in a form that can readily be understood
by miners.
Temperature-Viscosity Relations in the Ternary System
CaO-Al203-Si02. A. L. Fetld and P. H. Royster. Technical
Paper 189. 36 pp. Paper, 5 cents.
Analyses of Mine and Car Samples of Coal Collected in the
Fiscal Years 1913 to 1916. A. C. Fteldner, H. I. Smith, J.
W. Paul and Samuel Sanford. Bulletin 123. 478 pp.
Paper, 50 cents.
Measuring the Temperature of Gases in Boiler Settings.
H. Kreisinger and J. F. Barkley. Bulletin 145. 72 pp.
Paper, 15 cents. "This book is one of a series of publications
being issued by the Bureau of Mines for the purpose of dissemina-
ting information in regard to the methods by which the fuels in
this country may be used most efficiently."
A Convenient Multiple-Unit Calorimeter Installation. J. D.
Davis and E. L. Wallace. Technical Paper 91. 48 pp.
Paper, 15 cents.
The Diffusion of Oxygen through Stored Coal. S. H. Katz.
Technical Paper 170. 47 pp. Paper, 10 cents.
Slag Viscosity Tables for Blast-Furnace Work. A. L. Field
and P. H. Royster. Technical Paper 187. 38 pp. Paper,
5 cents. The purpose of this report is to make available to the
operator the results of the slag-viscosity measurements made in
the laboratories of the Bureau. This information, if used
intelligently, should help the blast-furnace operator to reduce
losses caused by off -grade pig iron; to improve fuel economy;
to promote operating efficiency; and to extend present-day
practice to meet the increasing need of smelting lean and com-
plex ores.
Methane Accumulations from Interrupted Ventilation. H. I.
Smith and R. J. Hamon. Technical Paper 190. 46 pp. Paper,
10 cents. This report was prepared under a cooperative agree-
ment with the Illinois State Geological Survey and the Engi-
neering Experiment Station of the University of Illinois.
BUREAU OF STANDARDS
Wave Lengths in the Red and Infra-Red Spectra of Iron,
Cobalt, and Nickel Arcs. W. F MSGGBRS and C. C. Kb
Scientific Paper 324. 14 pp. Paper, 5 cents.
The Properties and Testing of Optical Instruments. Circular
27. 2nd Ed. 41 pp. Paper, 10 cents. In recent years
many types of optical instruments have been developed and have
come into more or less common use. At the same time, a
great deal has been written in the English language on optical
subjects, but there is no general discussion of optical instru-
ments in nontechnical language for the benefit of the average
person who owns, for example, opera glasses or a camera. The
primary purpose of this circular is to correct this deficiency by
giving a simple description of the principal features of optical
instruments, to explain the causes and correctness of various
imperfections, and to indicate methods of testing for the presence
of imperfections which mar the ideal performance of optical in-
struments. This information, for the most part, can be found
in various textbooks and treatises on optical subjects, but the
fact that it is inaccessible to many people, because it is widely
scattered and generally couched in mathematical language,
is the reason for this presentation This circular should not be
mistaken for a complete treatise on optical instruments. It is
intended first of all to serve the public who use optical instru-
ments but who have had little opportunity to study the physical
theory of such instruments.
DEPARTMENT OF AGRICULTURE
Commercial Bordeaux Mixtures: How to Calculate then-
Values. E. Wallace and L. H. Evans. Farmers' Bulletin
994. 11 pp.
Tests of the Absorption and Penetration of Coal Tar and
Creosote in Longleaf Pine. C. H. Teesdale and J. D. McLean.
Department Bulletin 607. 43 pp. Paper, 15 cents. Published
June 6.
Digestibility of Some Seed Oils. A. D. Holmes. Depart-
ment Bulletin 687. 20 pp. Paper, 5 cents. Published June 28.
This bulletin records studies of the digestibility of corn oil,
soybean oil, sunflower-seed oil, Japanese mustard-seed oil,
rapeseed oil, and charlock oil. It is primarily of interest to
students and investigators of food problems.
Articles from the Journal of Agricultural Research
Influence of Gypsum upon the Solubility of Potash in Soils.
P. R. McMdxer. 14, 61-66 (July 1).
Mineral Content of Southern Poultry Feeds and Mineral
Requirement of Growing Fowls. B. F. Kaupp. 14, 125-134
(July 15).
A Comparative Study of Salt Requirements for Young and for
Mature Buckwheat Plants in Solution Cultures. J. W. Shive
and W. H. Martin. 14, 151-175 (July 22).
Composition and Digestibility of Sudan-Grass Hay. W. G.
GaesslER and A. C. McCandlish. 14, 176-185 (July 22).
Soil Reaction and the Growth of Azotobacter. P. L. Gainey.
14, 265-271 (August 12).
Effect of Different Oxygen Pressures on the Carbohydrate
Metabolism of the Sweet Potato. H. Hasselbring. 14,
273-284 (August 12).
COMMERCE REPORTS -AUGUST 1918
Special efforts are being made in Australia to increase the
production of industrial denatured alcohol by diverting plants
engaged in the manufacture of potable spirits. (P. 441)
Over one hundred dyestuff factories are in operation in Japan.
In order to protect them in the future, a high tariff is suggested.
(P- 454)
Owing to the cutting off of foreign supplies of salt, steps are
being taken in Holland to develop extensive salt beds, the
existence of which has long been known. (P. 499)
In Mexico, it is proposed to manufacture alcohol and a cattle
food, from "sotol," a plant which grows wild in unlimited
quantities. (P. 503)
960
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 11
Large deposits of lignite of good quality have been discovered
. where they will be especially valuable owing to lack
of coal deposits. (Pp. 5.12 and 667-71)
The Canadian Research Council has urged the formation of
"industrial guilds," to be made up of linns or companies in the
same or allied industries, for the purpose of conducting research
laboratories for the benefit of the members of the guild. In
some cases government aid, in the form of grants or laboratory-
space, may be furnished. (P. 580)
The syndicate which controls the sulfur industry of Sicily,
has been granted an extension of 12 years, in view of the present
unsettled condition and the increased competition of American,
Japanese and African sulfur. (P. 623)
Plans are being made for extensive development of the iron ore
deposits of Brazil at the close of the war. (P. 636)
Owing to the shortage of adhesives in Germany, glue is being
extracted from bones by treatment with sulfur dioxide, removal
of fat by benzene extraction, and then boiling the bones under
pressure. Various vegetable juices are also being used in the
manufacture of adhesives. (P. 680)
Detonation caps are being made in Sweden with an explosive
containing copper, and no mercury. (P. 685 and 808)
Arrangements have been made for the first installment of
£1,000,000 on the British loan for the development of the dye
industry, in order to promote the manufacture of those dyes
which are essential, but cannot now be produced on a com-
mercial basis. (P. 705)
A plant is to be erected in Colon for the manufacture of
coconut oil and palm oil, and soap, and by-products. (P.
709)
A new process for the production of salt, magnesium salts,
sodium sulfate, iodine and bromine, from seawater, is being
installed in Norway. (P. 820)
Bids received in Brazil for the erection of caustic soda plants,
all specified the electrolytic process, except one which proposes
to use the Solvay process. (P. 828)
Special Supplements Issued During the Month
Denmark — 4a Scotland — \9h
France— 5c Canada — 23c
Italv — 86 French West Indies — 286
Spain — 156 Honduras — 31 a
Liverpool and Sheffield — 19/ China — 52/ and g
Bradford, England — 19g
Statistics of
Mexico — 712
Antimony
Arsenic
Bones
Copper
Gold
Silver
Cottonseed cake
Guayule rubber
Hides
Horn
Ixtle fiber
Lead
Mercury
Sarsaparilla
Tin
Candelilla wax
Zinc ore
Denmark — Sup. 4fl
Chalk
Diamonds
Flint pebbles
Hides
Paper
Porcelain
Rennet
Exports to the United States
France — Sup. 5c
Dye extracts
Photographic paper
Antimony sulfide
Hides
Liverpool — Sup. 19/
Bones
Wool grease
Crude gums
Hides
Rubber
Ferromanganese
Palm oil
Rapeseed oil
Fish oil
Paper stock
Ammonium sulfate
Ammonium chloride
Cochineal
Cutch
Gum tragasol
Sodium silicate
Sodium sulfate
China
Artificial silk
Tin
China — Sup. 52/
Antimony
Beeswax
Albumen
Cantharides
Camphor
Aniline dyes
Indigo
Gall nuts
Musk
Rhubarb
Sodium benzoate
Tumeric
Hides
Pig iron
Tungsten ore
Be
i oil
Castor oil
Cottonseed oil
Peanut oil
Rapeseed oil
Wood oil
Linseed
Sesame
Zinc ore
BOOK REVIEWS
Sulfuric Acid Handbook. By Thomas J. Sullivan. McGraw-
Hill Book Company, Inc., New York City, 1918. Price,
$2 . 50, net.
This book owes its chief value to the fact that it contains
the unusually complete set of sulfuric acid tables adopted by
the Manufacturing Chemists' Association of the U. S. A.
These tables are indispensable in working out problems
connected with the manufacture and use of sulfuric acid, and
placed together in a convenient form, fill a long-felt want.
J. B. F. Herreshoff
Treatise on Applied Analytical Chemistry. By Vittorio
Villavecchia and Others. Translated by Thomas H. Pope.
Pp- 475- P. Blakiston's Son & Co., Philadelphia, Pa. 1918.
Price, $6.00.
The author of this book has endeavored to present those sub-
jects which have to do with the purchase of raw materials for
manufacturing processes. He has also given attention to the
analysis of finished products from the standpoint of impurities
and adulterations. The book is well arranged and the subjects
are presented in a very pleasing manner. It is a commendable
volume and should be of value to those interested in the problems
of analytical chemistry.
Allen Rogers
Cellulose. An Outline of the Chemistry of the Structural Ele-
ments of Plants. By CROSS and Bevan. New Impression
with Supplement. 348 pp. with 14 plates. Longmans,
Green & Co., New York and London, 1918. Price, $4.50.
This is a reprint of the third edition of this classical work
which is familial to all students of cellulose chemistry. The
new impression is extended, however, by a supplementary chap-
ter, pp. 311—331, which contains brief paragraphs on pure cellu-
lose, ester anhydrides, reactions of decomposition, physical
properties and lignocellulosc, while the summary of technical
progress since the edition of 1016, is compressed into less than
two pages. This is the more to be regretted since the authors
state that owing to "the persistent international complications"
they have not been able to complete the records which would
justify publishing a No. 4 of their series of Researches on Cellu-
lose. In view of the colossal importance which cellulose and
its compounds have acquired as war materials, and the note-
worthy special applications of paper to war purposes, it is un-
fortunate that the authors have been unable to bring the sub-
ject more nearly up to date. A. D. LiTTi.i:
The Chemist's Pocket Manual. By Richard K. Meade. 3rd
Ed. 530 pp. The Chemical Publishing Company, Easton,
Pa., 1918. Price, $3.50.
The author's extensive experience as an engineer and chemist
has enabled him to produce a book which should appeal particu-
larly to chemical engineers, works chemists, and superintendents.
It differs from other manuals in its practical character. The
customary lengthy tables of the properties of inorganic and
organic compounds are condensed and the space saved is de-
voted to matter on fuels and combustion, electricity, mechanics,
steam, steam engines and boilers, hydraulics, power trans-
mission, elevators and conveyors. There are a number of
useful conversion tables for analytical chemists and a su
article on graphic methods for saving calculation. Methods for
standardizing weights and calibrating glassware are described
The last half of the book is taken up by a description of the
methods used in the examination of iron, copper, lead, zinc
ores, etc., the analysis of iron, steel, alloys, coal, flue gases, clay,
lubricating oils, asphalts, soap, mixed paint, fertilizers, water.
and Portland cement. In the reviewer's opinion .1 better
selection of methods, both practical and accurate, (tiuld scarcely
be made. At the end of each part there is an excellent bibliog-
raphy of the more important magazine articles and books.
Nov., 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
961
The manual is seriously marred by the number of errors.
Even a casual examination 'Kill disclose quite a few. In the
section on mineralogy the proofroom eluders "camalite, prout-
site, pyroxine" may be found. The newspaper atrocity
"analine" is discovered on p. 310. "Sulfuric anhydried" appears
on p. 205. Sadtler is misspelled Sartler on p. 260. Mohr is
Moh on p. 261. One year has 265.24 days on p. 10. The
atomic weights of 1917 are used, but the table is titled 19 16
on p. 28. Many other errors might be cited.
By this time the reader's confidence in the reliability of the
tables is somewhat shaken. To investigate this point the re-
viewer examined carefully three of the tables. The first of
these, the table of logarithms, has two mistakes in the logarithms
corresponding to the numbers no and 540. The second, the
table of molecular weights on pp. 32-35, has eight incorrect
formulas. The extinct symbols A12C16, Fe2Cl6.K6Fe2(CN),2 are
used in this table, whereas the modern ones are listed in the
table of reagents on p. 303. The third table, factors on pp.
36-41, contains a number of slight errors. The factors NH4C1
to NH4, BaS04 to SO3, Zn2P207 to Zn are seriously in error.
The reagents used in analysis on p. 303 might preferably be
made up to a concentration bearing some relation to the molecular
weight, as described in A. A. Noyes' "Qualitative Analysis,"
instead of a haphazard percentage basis. Methyl red is missed
from the table of indicators.
In the directions for the determination of the specific gravity
of liquids with a pycnometer, the bottle is immersed in water a
"little above or below" the standard temperature. The
pycnometer is removed as soon as its thermometer shows the
proper temperature. This procedure can scarcely give accurate
results, since the only guarantee that the temperature of the
liquid in the pycnometer is uniform is to have a thermometer
in the bath as well as in the bottle, and both thermometers must
register the identical temperature before the pycnometer can
be removed for weighing.
The book is of handy size, is free from advertising matter,
and is well printed on strong paper. It should be in the hands
of every chemical engineer and analyst.
A. C. Langmuir
Chemical French. An Introduction to the Study of French
Chemical Literature. By Maurice L. Dolt, Ph.D., Pro-
fessor of Chemistry in the North Dakota Agricultural College,
viii + 398 pp. The Chemical Publishing Co., Easton, Pa.,
19 1 8. Price, $3.00.
Whether or not chemistry was once a French science, in later
times its language has had a decided German accent. Now-
adays, however, our interest in French chemists and French
chemistry is happily increasing and this book is opportunely
timed. It is a companion volume to the well known Chemical
German of Professor Phillips, being similarly arranged, printed
and bound.
French does not present so many new words to the speaker of
English as does German, but it is full of troublesome idioms;
these the author, who had his birth and early education in France,
is well equipped to handle.
Part I consists of four exercises reviewing in chemical language
the essentials of French grammar, and of twenty exercises
covering the various fields of chemistry. At the head of each is
a little vocabulary of new words and phrases occurring in the
exercise. Part II comprises classic selections from the French
journals, such as that of Pasteur on racemic arid and Moissan
on fluorine. The book concludes with a useful table <>f irregular
verbs and a dependable vocabulary of about 5500 terms 'which,
however, by no means includes all the words that appear in tin-
text).
Chemical French has been carefully prepared and is excellently
adapted to its purpose. It will no doubt meet with a cordial
reception. Austin M. Patterson
The Science and Practice of Photography. By John R. Roe-
buck, Assistant Professor of Physics, University of Wisconsin.
D. Appleton & Co., New York, 1918. Price, $2.00.
The sub-title of this book is "An Elementary Textbook of
Scientific Theory and a Laboratory Manual" and for the pur-
poses of a class textbook the sharp division between theory
and practice thus indicated is perhaps well adapted. The first
part, on general theory, consists of the following chapters:
Historical Development, Properties of the Gelatin Dry Plate —
Exposure and Development, Properties of the Gelatin Dry
Plate — Color Sensitiveness, Latent Image Theories, Negative
Defects, Positive Processes, Lenses, Color Photography, Good
Pictures, with an appendix on Plate Speed Numbers and De-
velopment. The second part consists of a Laboratory Manual
of exercises for students, taking them through the principal
operations and processes; also appendices on apparatus, chem-
icals, record slips, and photometers.
The book has the outstanding merit of putting the crux of
photographic science in the forefront 01 the argument. This is
of course the dependence of the density and character of the
negative upon exposure and development, and bound up with
this, the relationship of subject, negative, and positive. It is
of interest to industrial chemists that two of their number,
Hurter and Driffield, were the first to eliminate non-essentials
here, to give acceptable definitions of such photographic quanti-
ties as density and contrast, and to standardize their measure-
ment. The principles which they derived, and their mathe-
matical and graphic exposition of these, have formed the basis
of most subsequent quantitative work.
This has indeed shown that these principles are limiting ones,
completely true only under simplified conditions, and actually
subject to many deviations in the denser detail of practice. It
is, however, their great merit that they discerned an essential
reference framework through the fog of practical variations.
The author's account of these fundamental matters, in the
second chapter, is adequate and lucid. One may venture a hope,
rather than a criticism, that a future edition will show an even
more extended application of the characteristic curve, for ex-
ample, in connection with intensification and reduction methods,
for positive processes, and also for color sensitizing and color
photography. Without some illustration of the influence of
color (or wave length) upon the form and gradation of the
characteristic curve, the sensitizing curves given are apt to be
misleading.
The chemical side of photographic processes receives a less
satisfactory treatment. Equations are given somewhat baldly,
without any reference to mass action, to reversibility, or other
elements of the mechanism of the reactions. In the equation
as printed for wet plate development,
FeSO. + AgBr = Ag + Fe(S04)Br,
the ferric bromo-sulfate is surely a questionable species, while
the part played by restraining organic acids is not indicated.
The treatment of development and organic developers seems
rather brusque in a work emphasizing the desirability of scien-
tific foundations, failing which, the process of development be-
comes only a subject of empirical rules or individual guess-work.
The chapter em t li<- latent image stands out favorably by
contrast. It is an excellent and concise piece of work in which
the author concludes in favor of the colloid silver theory. It
may then be suggested that the cheiriical aspect of the book
would I"- strengthened if this occasion wen used to bring for-
u.ml the basic principles of colloid chemistry as central to plioto-
graphic processei \ sufficient claim for an elementary
1111 nt will be allowed on considering such facts as these- The
modifications of silver bromide described by Stas and others
an oil By colloidal changes due to interrelated adsorption and
subdivision. Practically all photographic images are colloidal.
962
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 11
their physical texture and color, as well as their chemical re-
activity arid stability, largely depending upon control of the
colloid condition. And virtually all photographic processes
are carried out in or upon a colloid medium.
These criticisms must be understood as made from the stand-
point of the photographic chemist. As an introduction to
photography, the book as a whole strikes one as very readable,
well balanced, and admirably adapted to its purpose as a class
textbook. This is assisted in no small measure by the well
chosen experiments of the Laboratory Manual.
There are some minor errata and misstatements requiring cor-
rection. Jean Servias Stas was an eminent Belgian chemist,
not a "famous German." H CI, incorrectly typed H C I on
p. 15, is not a desirable acid in gclatino-bromide emulsions.
Dr. Scheffer's name is misspelt, pp. 68 and 107, and in the in-
dex. Under the carbon process, the alkaline chromates are
given as sensitizers, which is misleading, since it is only as di-
chromates (or bichromates) that sensitizing is effected. Also,
the coloring matters used are pigments, not dyestuffs as stated,
which arc only used to shade them. And in the article on wet
collodion in the Laboratory Manual there is no explicit state-
ment of the necessity of saturating the silver sensitizing bath
with silver iodide.
The book is well printed on non-glossy paper, with numerous
clear illustrations, and has a good index. The footnote ad-
vices that articles such and such may be obtained from firms
so and so of Berlin, Miinchen, Dresden, etc., seem somewhat
superfluous at this date.
S. E. Sheppard
The American Fertilizer Handbook for 1918. Edited by John
D. Ten,, nth Annual Edition. Ware Brothers Company,
Philadelphia, 19 1 8. Price, $1.50.
The American Fertilizer Handbook has become a valuable
reference book in the fertilizer industry, and should be found
very valuable to anyone connected with this industry. It is
classified in the following sections: Fertilizer Materials, Direc-
tory of Allied Industries, Phosphate Rock, Fertilizer Machinery,
Fertilizer Brokers, Chemists and Engineers, Cottonseed Oil
Mills and Machinery, Packers and Renderers.
The first hundred pages are devoted to matters of general in-
terest to the fertilizer industry, giving the officers of the National
Fertilizer Association, The Southern Fertilizer Association,
Chemical Alliance Incorporated, location of the agricultural
experiment stations and the officials of these various stations.
There is also an interesting table showing the fertilizers and
tonnages by States.
This is followed by the Fertilizer Materials Statistics which
is a very complete and interesting review of the fertilizer ma-
terials market, statistics of the production, imports, consump-
tion, and prices of fertilizer materials for several years.
The Phosphate Rock, Sulfur, and Potash articles are very
complete and show clearly the status of these materials up to
1918.
The Fertilize! Manufacturers Directory is a well arranged
directory of the fertilizer manufacturers arranged by States.
The Directory of the Allied Fertilizer Trades is a buyers'
guide to the fertilizer trade.
The Phosphate Rock section includes a treatise on the pro-
duction of phosphate rock in 1916 by R. W. Stone, United States
Geological Survey, Washington, and also gives a complete list
of the phosphate mining companies, together with their addresses.
The Fertilizer Machinery section should be valuable to fer-
tilizer manufacturers interested in new construction, equip-
ment and supplil 5
The Fertilizer Materials section is merely an advertisement
of the companies handling fertilizer materials
The Brokers Section is also a list of fertilizer brokers.
The Chemists and Engineers is a section covering advertise-
ments by various chemists, assayers, engineers, constructors,
lead burners, samplers, etc.
The Cottonseed Oil Machinery section covers in a commer-
cial way the cottonseed oil and meal situation together with
statistics. There is also in this section an interesting and very
instructive article on the composition of cottonseed by Thomas
C. Law, Atlanta, Ga.
The last section in the book, entitled Packers and Renderers,
deals with the western animal ammonia market from May 1,
1917, to April 30, 1918. It also has charts showing the market
fluctuations on high-grade tankage and blood. This section
also has the directory of packing houses and rendering plants.
The book as a whole is a commercial book, a valuable addi-
tion as a reference book to anyone who desires information in
regard to the fertilizer industry.
J. E. Breckenridge
Van Nostrand's Chemical Annual. Edited by John C. Olsen,
A.M., Ph.D., Professor of Chemistry, Cooper Union, N. Y.,
and Maximilian P. Matthias, Ch.E., Lieutenant, Ordnance
Dept., U. S. R., Assistant Editor. Fourth issue. 778 pp.
D. Van Nostrand Co., New York, 1918. Price, $3.00.
When a chemical book has gone through four editions, the ap-
proval of the profession which has made this possible testifies
more emphatically to its merit than it is possible for any re-
viewer to do. In this case, therefore, the work of the latter can
be confined to the pleasant task of approving of the public's
discernment and of calling attention to the advances made in
the present over former editions.
The standard tables have, of course, been revised and ex-
tended in accordance with the latest information obtainable,
making use therein of much of the data published by the Bureau
of Standards. The new matter includes tables on the physical
constants of the radioactive elements, critical data of gases, rela-
tive hardness of the elements, the calibration of glass vessels,
indicators for volumetric analysis, weight of dry air at differ-
ent temperatures and pressures, properties of the wrought cop-
per alloys, specific gravity standards, refractometer readings
and density of cane sugar solutions, composition of sea water,
density and volume of pure water, reduction of weighings to
vacuo, pressure of saturated aqueous vapor, weights and mea-
sures, capacities of tanks, values of electrical, mechanical, and heat
units, conversion of Centigrade to Fahrenheit degrees, freezing
mixtures and freezing point of brines, latent heat of vaporiza-
tion, and the composition and heating value of natural gas.
Directions are given for using logarithms and the slide rule.
The section on Stoichiometry has been revised and explana-
tions of the use of the various tables have been inserted through-
out the book. A feature of this issue as of others is a complete
list of the more important American and foreign books which
have appeared since the third issue of the Annual in 1913. The
frontispiece of this issue consists of an excellent recent likeness
in sepia of Professor Ira Remsen.
Richard K. Meade
Sir Wm. Ramsay as a Scientist and Man. By T. A. Chaudhuri,
Professor of Chemistry, Edward College, Pabna, with intro-
duction by Panchanan Neogi, Government College,
Rajshahi. ix + 66 pp. Butterworth and Company, London
and Calcutta, 1918. Price, 1/8 net.
This is an exquisite, short but accurate, oriental biography
of a man, who not oidy interpreted, but added much to our
technical knowledge of Nature. Students could profitably be
directed to read this booked monograph not alone for informa-
tion, but as an illustration of delightful literary style. It is "an
estimate of the sublime lesson of the life and life-work of the
British savant within a small compass."
Charles Baskerville
Nov., 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
963
NLW PUBLICATIONS
By Clara M. Gupfy, Librarian, Mellon Institute of Industrial Research, Pittsburgh
Alloys: Introduction a l'Etude des alliages. W. Broniewsky. Price,
18 fr. Delagrave, Paris.
Analysis: Course of Instruction in the Qualitative Chemical Analysis of
Inorganic Substances. A. A. Noyes. 7th Ed. 8vo. 124 pp. Price,
$1.50. The Macmillan Co.. New York.
Chemistry: Senior Chemistry. G. H. Bailey and H. W. Bauser. 2nd
Ed. 8vo. 526 pp. Price, 5s. University Tutorial Press, London.
Color in Relation to Chemical Constitution. E. R. Watson. 8vo. 197
pp. Price, $4.00. Longmans, Green & Co., New York.
Conservation of Food Energy. H. P. Armsby. 12mo. 65 pp. Price,
$0.75. W. B. Saunders Co., Philadelphia.
Electric Motors and Control Systems: A Treatise on Electric Traction
Motors and Their Control. A. T. Dover. 8vo. 388 pp. Price,
16s. Sir Isaac Pitman & Sons, New York.
Engineering Drawing. T. E. French. 2nd Ed. 8vo. 329 pp. Price,
$2.50. McGraw-Hill Co., New York.
Farm Engines and How to Run Them. J. H. Stephenson. 12mo. 252
pp. Price, $1.00. F. J. Drake & Co., Chicago.
Machine Design: Elements of Machine Design. H. L. Nachman. 8vo.
Price, 9s. 6d. Chapman & Hall, London.
Mechanism: Principles of Mechanism. W. H. James and M. C. Mac-
kenzie. 8vo. Price, 7s. Chapman & Hall, London.
Metallurgists and Chemists' Handbook: A Reference Book of Tables and
Data for the Student and Metallurgist. D. M. Liddell. 2nd Ed.
16mo. 656 pp. Price, $4.00. McGraw-Hill Co., New York.
Metals: Chemical Combination Among Metals. Michele Giua and
Clara Giua-Lollini. Translated by G. W. Robinson. 8vo. 341 pp.
Price, $4.50. P. Blakiston's Son & Co., Philadelphia.
Metals: Les Metaux. Leurs conditions d'emploi dans l'industrie
moderne. Jean Oertle. Price, 10 fr. Librarie Aeronautique, Paris.
Petroleum, Asphalt and Natural Gas. Kansas City Testing Laboratory.
12mo. 248 pp. Price, $2.00. The Author, 1013 Grant Ave., Kansas
City. Mo.
Pocket-Book for Mechanical Engineers. D. A. Low. 16mo. 740 pp.
Price, $3.00. Longmans, Green & Co., New York.
Rural Water Supplies and Their Purification. A. C. Houston. 8vo.
151 pp. Price, 7s. 6d. Bale, Sons and Danielssohn, London.
Steel: Fabrication de l'acier. H. Noble. 2nd Ed. 632 pp. Price,
25 fr. H. Dunod et E. Pinat, Paris.
Steel: Trempe, Recuit, Cementation et Conditions d'emploi des aciers.
L. Grenet. Price, 20 fr. Ch. Beranger, Paris.
Synthetic Dyestuffs and the Intermediate Products from Which They are
Derived. J. C. Cain and J. F. Thorpe. 4th Ed. 8vo. 440 pp.
Price, 10s. Charles Griffin & Co., London.
Testing, Fault Localization, and General Hints for Wiremen. J. Wright.
New Ed. 18mo. 88 pp. Price. Is. 6d. Constable & Co., London.
Zinc Industry. E. A. Smith. 8vo. 223 pp Price, $3.50. Longmans,
Green & Co., New York.
RECENT JOURNAL ARTICLES
Alizarin. J. F. Springer. Color Trade Journal, Vol. 3 (1918), No. 3,
pp. 326-333.
Automatic Shell Heat-Treating Furnaces. W. J. Harris. Iron Age, Vol.
102 (1918), No. 10, pp. 565-568.
Bactericidal Efficiency of Soap Solutions in Power Laundry. H. G.
Elledge and W. E. McBride. American Journal of Public Health,
Vol. 8 (1918), No. 7, pp. 494-498.
Benzo Fast Scarlets. C. S. Wehrly. Color Trade Journal, Vol. 3 (1918),
No. 3, pp. 323-325.
Blast-Furnace Charge at the Bunker Hill Smeltery. C. T. Rics. Engi-
neering and Mining Journal, Vol. 106 (1918), No. 10, pp. 436-438.
Boiler Plates: A Cause of Failure in Boiler Plates; Effect of Grain Growth;
Alteration of Crystalline Structure by Mechanical Deformation; Some
Remedies. Walter Rosenhain and D. Hanson. The Iron Age,
Vol. 102 (1918), No. 11, pp. 632-636.
Coal Storage in Large Quantities: Methods, Equipment and Typical In-
stallations. H. J. Edsai.i.. Industrial Management, Vol, 56 (1918),
No. 3, pp 193-200.
Condensing Quicksilver from Furnace Gases. L. H. Duschak and C. N.
SchuSTTB. Mining and Scientific Press, Vol. 117 (1918), No. 10, pp.
315-323.
Conveyors. R S. Lewis. Mining and Scientific Press, Vol. 117 (1918),
No. 11, pp. 349-355.
Copper Refining: Recovery of Selenium and Tellurium in Copper Re-
fining. M II Mkhhiss anij II. T, !'.l.M>i;i' / Mining
Journal, Vol 106 (1918), No. 10, pp. II
Correcting Air Volume for Blowing: the Adjustment of Air Supply to a Blast
Furnace is Governed Accurately by a New Constant-Volume Corrector,
Independent of Temperature, Barometer, and HnmiditJ
STEIN Ihr Iron Iradr Rmr:r, Vol ft! 1 9 1 £
Cottrell Processes of Electric Precipitation, with Especial Regard to the
Application to the Recovery of Potash as a By-Product. J. S. Grasty.
Manufacturers Record, Vol. 74 (1918), No. 12, pp. 70-72.
Dyeing: Use of Organic Dyestuffs in the Preparation of Color Lakes.
Barrington de Puyster. Color Trade Journal, Vol 3 (1918) No 3
pp. 320-322.
Dyeing of Feathers and Furs. R. W. Smith. Color Trade Journal Vol
3 (1918), No. 3, pp. 304-310.
Electric Brass Melting: Present Status of Electric Brass Melting. H. M.
St. John. Chemical and Metallurgical Engineering, Vol. 19 (1918),
No. 6, pp. 321-328.
Electric Steel Production for Small Units. A V. Farr. The Blast Furnace
and Steel Plant, Vol. 6 (1918), No. 9, pp. 381-383.
Electric Welds. E. E. Thum. Chemical and Metallurgical Engineering,
Vol. 19 (1918), No. 6, pp. 301-308.
Examination of Commercial Dextrin and Related Starch Products. F. W.
Babington, Alfred Tingle, and C. E. Watson. Journal of the Society
of Chemical Industry, Vol. 37 (1918), No. 15, pp. 257-258.
Explosives: Handling and Storing of Explosives. Arthur La Motte
Engineering and Mining Journal, Vol. 106 (1918), No. 11, pp. 488-493.
Fuel Economy in Blast Furnace Practice. T. C. Hutchinson. The Blast
Furnace and Steel Plant, Vol. 6 (1918), No. 9, pp. 378-380.
Gas-Firing: Methods of a New System of Gas-Firing: Method of Ob-
taining Uniform and Constant Gas Mixture for Proper Combustion
Explained. A. C. Ion-ides. The American Drop Forger, Vol. 4 (1918).
No. 9, pp. 365-367.
Glass: Gas Firing and the Glass Industry. J. W. Cobb. Journal of the
Society of Glass Technology, Vol. 1 (1917), No. 4, pp. 223-238.
Glass: Some Notes on the Annealing of Glass. Solomon English and
W. E. S. Turner. Journal of the Society of Class Technology, Vol. 2
(1918). No. 6, pp. 90-102.
Iron in Santo Domingo. R. B Brinsmade. Mining and Scientific Press,
Vol. 117 (1918). No. 11, pp. 356-358.
Lead Plating: Some Information Regarding the Electrolytic Deposition
of Lead. Bureau of Standards, Washington, D. C. The Metal
Industry, Vol. 16 (1918), No. 9, pp. 410-411.
Lighting Textile Mills in Wisconsin; General Lighting System of Indirect
Type Commonly Used. J. A. Hoeveler. Textile World Journal
Vol. 54 (1918), No. 10, pp. 75-77.
Manganese: Conserving Manganese in Steel Production. A. N. Diehl.
The Blast Furnace and Steel Plant, Vol. 6 (1918), No. 9, pp. 366-367.
Molybdenum: Determination of Molybdenum in Ores. W. J. Crook
and M. L. A. Crook. Mining and Scientific Press, Vol. 117 (1918),
No. 10, pp. 313-314.
Nickel and Cobalt Determination in Steel; Elimination of the Bulk of the
Iron by Means of Sodium Carbonate. W. R. Schoeller and A. R.
Powell. The Blast Furnace and Steel Plant, Vol. 6 (1918), No. 9, pp.
359-360.
Niter Cake for Pickling Metal; How a Practical Man Eliminates Sulfuric
Acid. G P. Butler. The Metal Industry, Vol. 16 (1918), No. 9, p. 418.
Oil: Reclaiming Oil from1 Metal Turnings. C. L. Smith. The Iron
Age, Vol. 102 (1918), No. 10, pp. 558-559.
Oxide Film Lightning Arrester. Crosby Field. General Electric Review,
Vol 21 (1918), No. 9, pp. 597-601.
Oxide Film Lightning Arrester. C. P. Steinmetz. General Electric
Review, Vol. 21 (1918), No. 9, pp. 590-596.
Peat: Utilization of the Peat Resources of Canada. B. F. Haanbl.
Journal of the Society of Chemical Industry, Vol. 37 (1918), No. 15, pp.
2581-2611.
Plating: Government Specifications for Copper and Nickel Plating. C.
H. Proctor. The Metal Industry. Vol 16 (1918), No '). pp. 407-409.
Potash: Availability of Potash in Some Common Soil-Forming Minerals.
Effect of Lime Upon Potash Absorption by Different Crops. J. K
Plummer. Journal of Agricultural Research, Vol 4 (1918), No. 8, pp
297-316.
Potash: Possibilities of Developing an American Potash Industry. A.
W. STOCKETT. Manufacturers' Retard, Vol. 74 (1918), No. 12. pp. 68-6V.
Potash: The Recovery of Potash as a By-product in the Manufacture
of Portland Cement. J J PoSTBR. The American Fertiliser, Vol 40
(1918). No. 5, pp. 58-72.
Potash: A Wet Process for Extracting Potash from Cement Dust. I (.
Dean. Chemical and Metallurgical Engineering, Vol 19 (1918
pp 1 19 IK'
Powdered Coal: A Diversified Application of Powdered Coal. I
Vol. 102 (1918), No. I I. pp 61!
Producer Gas, Its Manufacture and Use: An Interesting Discussion on the
Chemical Analysis of Producer Gas; Methods of Burning It and Results
Obtained as Compared with Other Gases; Relative Specific Heats of
Gas Mixtures Given, C S Palhbi Ih, American n>,
Vol 4
964
MARKET REPORT— OCTOBER, 1918
WHOLESALE PRICES PREVAILING IN THE NEW YORK MARKET ON OCTOBER 19, I918
INORGANIC CHEMICALS
Acetate of Lime 100
Alum, ammonia, lump 100
Aluminum Sulfate, (iron free)
Ammonium Carbonate, domestic
Ammonium Chloride, white
Aqua Ammonia, 26°, drums
Arsenic, white
Barium Chloride
Barium Nitrate
Barytes, prime white, foreign
Bleaching Powder, 35 per cent
Blue Vitriol
Borax, crystals, in bags
Boric Acid, powdered crystals
Brimstone, crude, domestic Long
Bromine, technical, bulk
Calcium Chloride, lump, 70 to 75% fused. . . .
Caustic Soda, 76 per cent 100
Chalk, light precipitated
China Clay, imported
Feldspar
Fuller's Earth, foreign, powdered
Fuller's Earth, domestic
Glauber's Salt, in bbls 100
Green Vitriol, bulk 100
Hydrochloric Acid, commercial
Iodine, resublimed
Lead Acetate, white crystals
Lead Nitrate
Litharge, American
Lithium Carbonate
Magnesium Carbonate, U. S. P
Magnesite, "Calcined"
Nitric Aoid, 40«
Nitric Acid, 42*
Phosphoric Acid, 48/50%
Phosphorus, yellow
Plaster of Paris
Potassium Bichromate
Potassium Bromide, granular
Potassium Carbonate, calcined. 80 @ 85%.. .
Potassium Chlorate, crystals, spot
Potassium Cyanide, bulk, 98-99 per cent
Potassium Hydroxide, 88 @ 92%
Potassium Iodide, bulk
Potassium Nitrate
Potassium Permanganate, bulk, U. S. P
Quicksilver, Bask 75
Red Lead, American, dry 100
Salt Cake, glass makers'
Silver Nitrate
Soapstone, in bags
Soda Ash, 58%, in bags 100
Sodium Acetate, broken lump .
Sodium Bicarbonate, domestic 100
Sodium Bichromate
Sodium Chlorate
Sodium Cyanide
Sodium Fluoride, commercial
Sodium Hyposulfite 100
Sodium Nitrate, 95 per cent, spot 100
Sodium Silicate, liquid, 40* B* .'
Sodium Sulfide, 60%, fused in bbls
Sodium Bisulfite, powdered
Strontium Nitrate
Sulfur 100
Sulfuric Acid, chamber 66° Be
Sulfuric Acid, oleum (fuming)
Talc, American white
Terra Alba, American, No. 1 100
Tin Bichloride. 50°
Tin Oxide
White Lead, American, dry
Zinc Carbonate
Zinc Chloride, commercial
nominal
7.00
Lb.
nominal
Lb.
9>/« @
17
Ton
75.00 @
90.00
Lb.
12 @
14
Ton
30.00 @
35.00
Lb.
4'/i @
5
Lb.
9'A @
9>/«
Lb.
7 'A @
ioy«
Lb.
7»A @
8»A
Ton
nominal
Lb.
75 @
Ton
20.00 @
22.00
Lbs.
4.40 ®
4.50
Lb.
4>A @
5
Ton
20.00 @
30.00
Ton
8.00 @
15.00
Ton
nominal
Ton
20.00 @
30.00
Lbs.
2.10 @
3.00
Lbs.
2.00 @
2.25
Lb.
C. P. nominal
Lb.
4.25 @
4.30
Lb.
20
@
30
Ton
60.00
@
65.00
Lb.
7«A
Lb.
8>A
Lb.
7 'A
@
9
Lb.
1.10
@
1.15
Bbl.
2.00
@
2.50
Lb.
44
@
46
Lb.
n
>mm
al
Lb.
60
a
70
Lb.
3.75
a
4.00
Lb.
27
@
30
Lb.
1.85
<4
2.00
Lbs.
125.00
@
130.00
Lbs.
11.25
<a>
11.50
Ton
17.50
a
22.00
Ox.
63 'A
®
65
Ton
10.00
@
12.50
Lbs.
2.65
a
2.75
Lb.
20
m
21
Lbs.
3.60
a
3.70
Lbs.
2
60 @
3.60
Lbs.
4
42 'A @
5.00
3>A @
3'A
Lb.
nominal
12 @
14
Lb.
25 @
30
Lbs.
2
25 @
4.60
Ton
18.00
Ton
32.00
Ton
15.00
Lbs.
1.17V.
ORGANIC CHEMICALS
Acetanilid, C. P.. in bbls Lb.
Acetic Acid, 56 per cent, in bbls 1 00 Lbs.
Acetic Acid, glacial, 99'A% 100 Lbs.
Acetone, drums Lb.
Alcohol, denatured, 180 proof Gal.
9.30
19.50
1.00
10'A
9.55
19.70
Alcohol, sugar cane, 188 proof Gal.
Alcohol, wood, 95 per cent, refined Gal.
Amyl Acetate Gal.
Aniline Oil, drums extra Lb.
Benzoic Acid, ex-toluol Lb.
Benzol, pure Gal.
Camphor, refined in bulk, bbls Lb.
Carbolic Acid, U. S. P., crystals, drums Lb.
Carbon Bisulfide Lb.
Carbon Tetrachloride, drums, 100 gals Lb.
Chloroform Lb.
Citric Acid, domestic, crystals Lb.
Creosote, beechwood Lb.
Cresol, U. S. P Lb.
Dextrine, corn (carloads, bags) Lb.
Dextrine, imported potato Lb.
Ether, U. S. P. 1900 Lb.
Formaldehyde, 40 per cent Lb.
Glycerine, dynamite, drums extra Lb.
Oxalic Acid, in casks Lb.
Pyrogallic Acid, resublimed, bulk Lb.
Salicylic Acid, U. S. P Lb.
Starch, corn (carloads, bags) pearl 100 Lbs.
Starch, potato, Japanese Lb.
Starch, rice Lb.
Starch, sago flour Lb.
Starch, wheat Lb.
Tannic Acid, commercial Lb.
Tartaric Acid, crystals Lb.
OILS, WAXES, ETC.
Beeswax, pare, white Lb.
Black Mineral Oil, 29 gravity Gal.
Castor Oil, No. 3 Lb.
Ceresin. yellow Lb.
Corn Oil, crude 100 Lbs.
Cottonseed Oil, crude, f. o. b. mill Lb.
Cottonseed Oil, p. s. y 100 Lbs.
Menhaden Oil, crude (southern) Gal.
Neafs-foot Oil, 20* Gal.
Paraffin, crude, 118 to 120 m. p Lb.
Paraffin Oil, high viscosity Gal.
Rosin, "F" Grade, 280 lbs Bbl.
Rosin Oil, first run Gal.
Shellac, T. N Lb.
Spermaceti, cake Lb.
Sperm Oil, bleached winter, 38* Gal.
Spindle OU, No. 200 Gal.
Stearic Acid, double-pressed Lb.
Tallow, acidless Gal.
Tar OU, distilled Gal.
Turpentine, spirits of Gal.
METALS
No. 1, ingots Lb.
Antimony, ordinary Lb.
Bismuth, N. Y Lb.
Copper, electrolytic Lb.
Copper, lake Lb.
Lead, N. Y Lb.
Nickel, electrolytic Lb.
Platinum, refined, soft Or.
SDver Or.
Tin, Straits Lb.
Tungsten (WOi) Per Unit
Zinc, N. Y
4.90
91 'A
4 20
a
9
nominal
a
20
8 9
nominal
27 ®
16'A Gov't 1
60 9
41
a
00
a
13
@
12' ,
9
9'A
9
nominal
65
9
82
9
33»/«
a
34
17
a
18
17.75
a
18.00
17 'A
&
—
21.00
a
22.00
1.15
a
1.25
3.45
a
3.55
9> .
a
10
40
a
41
15.10
a
15.20
75
a
76
13
A 9
14
3
50
26
26
9
9
9
8.05
1
a
53
1
a
nominal
.81 'A
nominal
56
0
00
a
24
DO
0
40
a
9
CO
FERTILIZER MATERIALS
.Sulfate 100 Lbs.
Blood, dried, f. o. b. Chicago Unit
Bone, 3 and 50, ground, raw Ton
Calcium Cyanamide Unit of Ammonia
Calcium Nitrate, Norwegian 100 Lbs.
Castor Meal Unit
Fish Scrap, domestic, dried, f. o. b. works.. . .Unit
Phosphate, acid, 16 per cent Ton
Phosphate rock. f. o. b. mine: Ton
Florida land pebble, 68 per cent Ton
Tennessee, 78-80 per cent Ton
Potassium "muriate," basis 80 per cent Ton
Pyrites, furnace size, imported Unit
Tankage, high-grade, f . o. b. Chicago Unit
6.95
37.00 ® 37.50
nominal
and
20c
16.50 9 1750
nominal
5.00 9 600
7.00 9 8.00
300.00 @ 310.00
nominal
6.75 9 6.80
The Journal of Industrial
and Engineering Ghemistry
Published by THE AMERICAN CHEMICAL SOCIETY
Volume X
DECEMBER 1, 1918
No. 12
Assistant Editor: Grace MacLeod
Editor: CHARLES H. HERTY
Advertising Manager: G. W. Nott
ADVISORY BOARD
H. E. Barnard H. K. Benson F. K. Cameron B. C. Hesse A. D. Little A. V. H. Mory
Published monthly. Subscription price to non-members of the American Chemical Society, $6.00 yearly; single copy, 60 cents
Price per single copy to American Chemical Society members, 50 cents. Foreign postage, seventy-five cents, Canada, Cuba and Mexico
Entered as Second-class Matter December 19, 1908. at the Post-Office at Easton, Pa., under the Act of March 3, 1879
Acceptance for mailing at special rate of postage provided for in Section 1103. Act of October 3, 1917. authorized July 13, 1918.
All communications should be sent to The Journal o! Industrial and Engineering Chemistry.
Telephone: Vanderbilt 1930 35 East 41st Street, New York City
Subscriptions and claims for lost copies should be referred to Charles L. Parsons, Box 505, Washington, D. C.
Eschbnbacb Printing Company. Ea
TABLE OF CONTENTS
Editorials:
A Victory of Arms, Not Yet of Ideals 966
National Self-Containedness 966
A Special Meeting of the Council 967
A Golden Opportunity 967
An Experiment in Publicity 967
An Embargo on Research Work 968
The Return of the Chemists 96S
An Institute for Cooperative Research as an Aid to
the American Drug Industry:
A National Institute for Drug Research. John J.
Abel 969
An Institute of Chemotherapy. P. A. Levene 970
Drug Research and the Bureau of Chemistry. C. L.
Alsberg 971
An Institute for Research in Synthetic Organic Chem-
istry. A. S. Loevenhart 97 1
An Institute of Therapo-Chemical Research. Frank
R. Eldred 973
Institute for Research on Synthetic Drugs. D. W.
Jayne 975
Remarks Concerning Suggestion for Central Medicinal
Research Laboratory. E. R. Weidlein 976
Chemical Markets of South America:
The Chemical Markets of Colombia, Ecuador, tin
Guianas, Venezuela, and Paraguay. O. P. Hop-
kins 977
Original Papers:
A Study of the Conditions Essential for the Com-
ial Manufacture of Carvacrol. Arthur W.
HLxsou and Ralph H. McKLee 982
Tlic Seeding Method of Graining Sugar. H. E.
Xitkowski 992
A Study of Sources of Error Incident to the Lindo-
Gladding Method for Determining Potash. T, E.
Kcin and It. E. Shiver 994
Di termination of the Value of Agricultural Lime. S.
I >- Conner 996
The 1 1 romide and Iodine
NuiTii. on Oil as a Means of Identifying
the Species of Canned Salmon. II S. Bail
J. M. Johnson 999
Composition ol the Waters of the [nter-Mounl
on I E Greavt tnd C T Hii 1 1001
On Con tituents of Oil of Cassia II Francis D
Laboratory and Plant:
Method "i An 1! Industry
IV 'l| M. Weiss
A New Illuminator for Mi ider
Silverman toi \
A Special Stopcock for Dropping Liquids Arranged for
Equalizing the Pressure above and below the Out-
let in the Stopcock. Harry L. Fisher
A New Timing Device for Simplifying the Ther-
mometric Reading of Calorimetric Determinations.
Chas. A. Myers, Jr
Addresses:
Some Applications of Physical Chemistry in the Coal-
Tar Industry. Wilbert J. Huff
A Manufacturer's Experience with Graduate Chemical
Engineers. S. R. Church
Current Industrial News:
Burmese Monazite Sands; Incandescent Lamps.
Aluminum and Its Alloys; Peat Fuel; Oils from Coal
Tar; Soda and Sulfite Pulp; Ferromanganese
Manufacture in Spain; Electric Lamp Industry in
France; German Enterprise in the Ukraine; Anneal-
ing Aluminum; Tanning Material in Germany;
Japanese Camphor; Nickel Steel; Gas-Fired Brazing
Table; A Chinese Perfume Plant; The Schoop
Metal-Spraying Process; New Source of Alcohol
Bichromate Manufacture in Sweden; Beechnut nil
in the Netherlands
Scientific Societies:
French Section, American Chemical Society; Iota
Sigma Pi; Society of Chemical Industry. New Ynrk
Section
Notes and Correspondence:
An Opportunity to Help the French; New Aftei Wai
Preparations in the Chemical Industry of Germany
'I'Ih' American Dyestufl Industry and It. Pri
The Journals of the American Chemical N
Theft of Platinum 01 Research Work;
Cooperation between Manufacturers and
versities; Invention Problems; Safet] of TNT as an
Explo en in the Chemical in. in 1
mil. Two Letters on Effect of Coal Ash mi tin
Nature of Cement Mill Potash. .
Washington Letter
l Noti
govbrnmi
impound "i \i ■ nil and Vntimony; The
1918 Edition
[ONS
Market Rbpi if i
1
Si BJBC1 I ' DI '■■
1014
1015
1 016
1019
1035
IO37
IO38
IO39
1040
104 1
IO46
o66
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 12
EDITORIALS
A VICTORY OF ARMS, NOT YET OF IDEALS
Thanks be to God, a new day has dawned! The
forces of domineering might which at one time threat-
ened to engulf the world have suddenly crumbled.
Fantastic dreams of universal domination and world-
wide loot have been dispelled by cold steel, high ex-
plosives, and the blood of those who believe in the
brotherhood of mankind.
To those of our own and of our Allies who have
made the great sacrifice of their lives our hearts
turn first in this moment of victory. In spirit
tluy will live forever honored among us. For those
who soon will be returning a welcome awaits such as
this country has never before given to any of its sons.
It is not yet possible to grasp the full meaning of
the mighty events of the past month: the change is
too stupendous. How far the actual change has pro-
gressed it is difficult now to tell. Certainly the mili-
tary power of the Teuton has been crushed for genera-
tions; but has his heart been changed? We believe
not. Has the Kaiser abdicated? We know not.
Certainly no authentic publication of his abdication
paper has appeared. The question has no military
significance, but it has important bearing on the good
faith of a nation which is now about to begin its
elementary acquisition of this useful commodity;
progress in this line cannot be made in his presence.
Has defeat really beta accepted by Germany? In a
way, yes, but only in a way. The "solfings" of Dr.
Solf, daily flashed to us by the wireless, show plainly
that we are still facing the same German heart, have
still to guard against the same machinations, have still
to witness the same stupid psychology by which at
oiii time we as a nation were charitable enough al-
most to be deceived.
No, Germany has not yet gone down through the
dark valley of suffering where alone she can cleanse
herself for fellowship in the great family of nations.
Until that day is reached let us be on our guard.
The sacrifices already made for civilization must not
be in vain.
NATIONAL SELF-CONTAINEDNESS
For the past four years we have advocated the
doctrine of national self-containedness. The vast and
varied natural resources of this country justify the
conviction that economic independence can be attained
if opportunity is afforded the chemist to exercise his
skill upon this raw material. Lack of independence
resulted not long ago in serious economic disturb-
ances; preparedness for the future demands that re-
cent progress toward independence, intensified by war
conditions, continue unabated. Ultimate reaching of
the goal depends upon two factors, our ability as
chemists and the cooperation of the body politic.
The first of these two factors is our own responsi-
bility; the second has for its foundations a sympathetic,
well-informed public opinion, confidence in the ability
of American chemists, patience to wait through the
unproductive days of investigation, and willingness to
meet perhaps higher costs of production during the
period of development of research results into sound
and efficient manufacturing practice. Without at-
tempting a systematic survey let us make candid
inquiry as to the present state of security of these
foundation stones.
Certainly public opinion is to-day better informed
and more sympathetic than ever before. So, too, is
there abundant evidence not only of confidence but of
pride in the ability of the chemist. The constant
increase in the number of industrial research labora-
tories bears witness to increased willingness to wait
upon investigation. So far so good. The last stone,
however, the willingness to meet temporary higher
costs of production, seems to be wabbly. Evidently
an insufficient amount of cement has been used to give
it firm setting. That some cement has been used is
evidenced by the prompt action of consumers in
joining in the request for a protective tariff in order to
insure independence in dyestuff supplies. But what
about potash and duty-free imports for educational
institutions?
First, as to potash, real progress has been made in
the procurement of a domestic supply, but support
has not been received from the great organizations
of the chief consumers, the farmers. Why is this?
We will not attempt to answer, for it would bring us
into the region of surmises. Perhaps a partial answer
is found on page 2 of the U. S. Official Bulletin, October
25, 1018. Summarizing the conference on potash held
in the offices of the Department of Agriculture, the
Bulletin states:
" * * * the view of the Department of Agriculture is that the
Government should do all that is possible to encourage the pro-
duction of potash from the cheapest sources in this country in
order to enable farmers to obtain it at a low price, because foreign
supplies are now unavailable." (Italics are ours.)
The reading naturally suggests the thought, What will
be the attitude when foreign supplies are again avail-
able? The cement is weak, very weak.
Second, at the Urbana meeting of the American
Chemical Society the matter of "duty-free imports"
for educational institutions was thoroughly discussed
and a committee appointed to find some way of re-
moving this obstacle to the development of American
manufacture of laboratory supplies. Up to date,
however, we have heard of no action by the Associa-
tion of American Universities or by the heads of the
chemistry departments of these institutions. Our
constant plea is that Americans should stand by the
American chemical industry. Should we not practice
among ourselves what we preach to others? More-
over, can we put the right spirit into the students we
are training for the American industry when the
"import" atmosphere pervades the whole laboratory?
This seeming saving through "duty-free imports" is
one of the costliest endowments our educational in-
stitutions possess, in that it cuts at the very heart of
independence through instilling the spirit of de-
pendence in the chemists of the future.
Dec, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
967
A SPECIAL MEETING OF THE COUNCIL
At the outbreak of the war the American Chemical
Society led the way in a prompt tender to the Gov-
ernment of a wealth of information, through the census
of chemists and their qualifications, compiled in co-
operation with the U. S. Bureau of Mines, which
has proved of inestimable value. Now it is incumbent
upon this great organization of American chemists
to do its part in the reestablishment of normal con-
ditions. With this in view, there has been called a
meeting of the Council of the Society at New York
City on December 14, 1918, which will doubtless prove
the most important in the history of that body. The
Secretary's notice of the meeting contains the follow-
ing salient paragraphs:
The Advisory Committee of the American Chemical Society
has requested President Nichols to call a meeting of the Council
at as early a date as practicable, in order that the Council may
carefully consider the whole question of the Society's opportunity
and duty in regard to the reconstruction of conditions chemical
which are to follow after the war. The American Chemical
Society has had an influence, fully admitted by all, during the
war; and now that the war is over and peace is in sight other
great problems are before us in the solution of which the Society
can again serve our country.
Accordingly, you are all asked to discuss these problems
with the other chemists of your local section, or with anyone
whose ideas are worth while, and to come to the meeting of the
Council in New York prepared to present and elucidate your
views. You are requested particularly to have a meeting of
your local section called in advance of the Council meeting and
to take up there with the members the general problem in order
that the full force of the American Chemical Society may be
felt in this matter.
You will find an interesting article by Dr. B. C. Hesse in the
November issue of the Journal of Industrial and Engineering
Chemistry which you should read. If possible, send to me in
writing any ideas which may be evolved, to reach this office on
or before December 10, in order that they may be brought be-
fore the Directors of the Society to be duly formulated with
others in advance of the Council meeting.
Large problems loom before us which must be con-
sidered from the new viewpoint which a world freed
from the scourge of Teutonic ideas presents. No
one man or small group of men is qualified to decide
such matters. Decision must be based upon a thor-
ough knowledge of the views of all chemists, presented
and discussed where common counsel can be deliber-
ately taken and policies carefully formulated.
Much material for discussion should be furnished
in the suggestions received by the Philadelphia Sec-
tion in response to their effective action following Dr.
Hesse's address, "Preparation for After the War,"
published in our last issue. It should be borne in
mind, however, that at that Council meeting any
subject which bears upon the welfare of this country
through chemistry is in order for discussion. Now
is the time, therefore, for meetings of local sections, at
which every phase of this subject should be canvassed,
insuring thus that the gathering in New York City
on December 14 will be thoroughly representative,
not simply of the personnel, but of the views of the
membership of the Society.
In this connection it should be noted that th
visory Committee meets in the early pari
month, and that the committee would gladly wel-
come at any time suggestions from
councilors, or individuals.
A GOLDEN OPPORTUNITY
As a Nation we have just expressed on Thanksgiving
Day our gratitude that peace has been justly restored
to a war-torn world. Again we approach that natal
day whose century-old maxim is "Peace on earth, good
will toward men." Shall these expressions of thank-
fulness and good will stop with mere lip service? We
never wish it so, but often know not where to turn to
find that human objective which will give to our
' sentiments the glorifying touch of personal applica-
tion. On page 1024 of this issue Secretary Parsons
outlines the work of the American Ouvroir Funds,
w.hich is seeking the "adoption" of those French
orphans whose fathers were technical men, graduates
of l'ficole Polytechnique who have fallen at the front.
The plan is so direct, so practical, and so filled with
the human touch that it will grip the heart-strings of
all who give it even a cursory reading.
The American Chemical Society has been asked
to lend its aid in securing as many as possible of these
"adoptions," which may be undertaken either by in-
dividuals or by groups. We are now in the midst of
meetings of our local sections held for discussing
constructive plans for the new period in the world's
history into which we are about to enter. Could any
more fitting prelude to these discussions be found
than a warm-hearted presentation of the righteous
claims of these orphans; could any nobler record ap-
pear upon the minutes of any local section than the
statement of the number of these orphans "adopted"
by the section or by its individual members? We
would waive all precedent, all by-law requirements,
and suggest that the first item of business at the im-
portant meeting of the Council on December 14, 1918, be
reports from the Councilors of the number of orphans
"adopted."
Six "adoptions" by members of the Society have
already been recorded. May the number increase
tenfold within the month!
What do we not owe to France, who for four years
stood at the gateway of civilization and with all her
resources, human and material, kept back the marauder?
Silent in her great losses and suffering, cheerful in
even the gloomiest days, determined in every fiber
of her national being, she stands triumphant at last.
Problems of reconstruction now confront her, and in
at least one of these, the care of her orphans, it is our
great privilege to share. Perhaps the little Jeans
and Maries of to-day may prove to be the ties of strength
which will bind Prance and America in closer union
than could be possible through diplomatic scroll or
statesmen's strivings.
AN EXPERIMENT IN PUBLICITY
Another experiment in chemistry has been in prog-
ress, and the results arc indeed interesting.
e April 1918 meeting th Directors of the
appropriated $2500 for a revival and con-
ni publicity work during this year. Ad-
mittedl; was in the nature of an
und rtakes 1 ■ mse o( ' tie belie! that a
more sympathetic bond should be established between
968
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 12
the public-at-large and the chemists. It was felt that
this purpose could be served best by seeking to de-
velop in each Local Section talen.1 for popular presenta-
tion of chemical facts. Contributions of short arti-
cles were therefore asked of the members, and a
payment of $5.00 was offered for each article accepted.
The results of the experiment have just been com-
piled for the Directors. These show, first, that the
administration and mechanical carrying on of the
work is a much less formidable undertaking than was
originally supposed, hence funds for continuance of
this part of the work can be largely curtailed next
year. Fifty bulletins have been issued to date. Re-
turns from the clipping bureau, necessarily incom-
plete, show that the bulletins were used in varying
numbers by 120 newspapers and magazines distributed
through 72 cities in 26 states. Nineteen of the fifty
bulletins were contributed by members of Local Sec-
tions other than the members of the General Com-
mittee or its office staff. All of the nineteen were re-
ceived after July 30, 1918, and most of them origina-
ted within the Minnesota Section, not, we believe,
because that Section has any special monopoly on
popular writing but because it took hold of the matter
in a live way and put some real punch into the effort.
This is best illustrated by the following extracts from
an announcement sent out in mimeograph form to
each member of the Section:
Does S5 .00 look good to you?
Now that you are interested we will tell you how you can make
that much money in less than 30 minutes. You are a chemist;
you have a chemical hobby; you think it is really the only phase
of chemistry worth working at; you feel sorry for others because
they can't see all of the interesting phases of your work; you
are even in a line of work which is of great scientific and practical
value to the nation.
Sit down and write a 500-word article full of interest with lots
of "news punch" about your favorite line of science and write
it so that people may not only be interested but that they may
also gain some information as to the importance of chemistry
in its relation to the every-day things of life.
.Send this article to Chairman Publicity Committee, American
Chemical Society, 35 East 41st St., New York City. If the
article is of general interest and is accepted you will receive
S5.00 in the return mail.
If you don't need the money, write an article anyhow and buy
Thrift Stamps with the proceeds.
We are asked by the Society officers to do all that we can to
bring chemistry home to the people. Pay your annual dues by
writing two articles of general interest. The Chairman of the
Committee on Publicity has requested that we bring this
to your attention. Individuals and local sections will re-
i1 i.M aco pled articles. These articles will be pub-
lished all over the country. If you have chemical items of
loeal interest, don't fail to write them up.
If each Local Section in preparation for the new year
would followr the worthy example of the Minnesota
Section in presenting this matter directly to each
onfidenl thai headquarters would be
i with material for consideration, and that
deniable value would be secured, whether
or noi were accepted.
Try your hand, who knows?
AN EMBARGO ON RESEARCH WORK
We print, here a Letter > ed from
a research chemist ion precludes
tig classified >nic kicker:
I think the following letter from a manufacturer may in-
<M, as it indicates what amounts to a government em-
bargo, in all probability unintentional, on research work in
chemistry in the United States.
"We cannot ship you any phosgene for the reason
that the Government has put in new regulations regard-
ing shipments of phosgene gas.
"The new regulations provide that this must be
shipped in special trains accompanied by messenger.
Hence you can see the impossibility of our making ship-
ment."
I deem it imperative that this restriction on the transport of
all chemicals, at least as far as universities and the chemical
industry are concerned, be removed at the earliest possible date,
and I trust your Journal will consider this question of sufficient
importance to give publicity to the law herewith concerned,
and will also suggest whatever remedy the situation may warrant.
Furthermore, I am certain chemists will be interested in know-
ing just what chemicals come under this embargo. I know that
metallic sodium, as well as phosgene, is under the ban. Now
how far can the organic chemist go without sodium? If we
consider its use in the manufacture of veronal, luminal, adalim,
and phenyl ethyl alcohol, substances for which there is a great
demand and a limited supply, I think the predicament of the
research chemists in this country, who may be engaged in de-
veloping methods for the manufacture of these important
pharmaceuticals, is sufficiently emphasized. We are progressing
with giant strides in building up chemical industries in the
United States, but we should not lose sight of the fact that the
only solid foundation on which successfully to rear a permanent
business in this direction is research.
Before the war there was a way to get any chemical from
Germany to our laboratories. It is true there were certain
rules that had to be observed in reference to containers, but the
important fact is there was a "way" to get phosgene, metallic
sodium, picric acid, etc. The question arises, would it not be a
happy solution of the problem in hand for the Government to
call to its assistance a few representative chemists and have
them indicate how the needs for chemicals of every description
which our laboratories and industrial plants require may be met?
All the chemicals at present under embargo, with the proper
safeguards, have been in the past, and could be now, transported
without extra hazard.
It may be interesting to call attention to the fact that, if I
am correctly informed, the only practical way for the manu-
facturer to obtain metallic sodium is to incur the expense of an
auto truck to and from Niagara Falls.
The point raised is one which will affect every re-
search laboratory. With the early return to the uni-
versities from war service of professors and graduate
students, general research should soon get under full
swing, but this important work will be sorely handi-
capped if a change from conditions here depicted is
not quickly obtained. It is therefore earnestly urged
that the proper officials of the Railroad Administra-
tion modify existing regulations so as to give the
necessary re
THE RETURN OF THE CHEMISTS
In the development of the Chemical Warfare S
vice into an effective war machine invaluable service
was rendered by Major Allen Rogers, chief of the
Industrial Relations Branch, in establishing
ble balance between the supply of chemists for -
vice in the military ranks and in essential industries.
Now that the demobilization of this great fore
soldier chemists is about to begin, it is fortunate that
the work is to remain in charge of the same efficient
officer, as noted from the following announcement:
When the United Slates entered the European War one of the
first problem- to be considered was the effect of the draft upon
our essential industries It was early appreciated that in order
to maintain our full efficiency it would be necessary to conserve
Dec, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
969
as far as possible our skilled workers and men with technical
training. In order that we might not suffer from the depletion
of our ranks, steps were taken to secure deferred classification,
and later on provision was made to furlough back to industry.
This arrangement made it possible for chemical industries to
maintain their efficiency and has contributed largely to the
effectiveness of our forces in the field.
Up to the time of cessation of hostilities the Industrial Rela-
tions Branch of the Chemical Warfare Service had recommended
for deferred classification 641 chemists and skilled workers.
These recommendations were favorably considered, as a rule, by
the Local Boards, and as a result about 90 per cent of the men
so recommended were put in a deferred class.
Many cases, however, were not brought to the attention of
this branch until the men had actually been called into service.
Such chemists or skilled workers as were essential to industry
were then furloughed in order that the production of war ma-
terials might not be retarded. Through this method 156 men
had been returned to industry, and at the time of the signing
of the armistice 120 more cases were pending in the Adjutant
General's Office.
►»As hostilities cease we naturally must again turn to peace
time conditions and look forward to the future development of
chemical industry in America. The problem now before the
Industrial Relations Branch of the Chemical Warfare Service is
to assist chemists in service to secure positions where their
training and experience can be used to the best interests of the
Government. This enormous readjustment is rendered possible
through the information gathered by Dr. Charles L. Parsons,
secretary of the American Chemical Society, and through the
questionnaires sent out by Major F. E. Breithut of the Personnel
Division of the Chemical Warfare Service.
In order to accomplish results the chemists now in military
service who desire to return to chemical industry are being
requested to inform the chief of the Industrial Relations Branch
concerning their future prospects, while the manufacturers are
being asked to designate their requirements for chemists. The
administration of this work will be carried out by the Industrial
Relations Branch. Any information desired may be obtained
by writing to Major Allen Rogers, Chief, Industrial Relations
Branch, Chemical Warfare Service, 7th and B Streets, N. W.,
Washington, D. C.
Here is a definite problem of readjustment of the
utmost importance, and we congratulate the Chem-
ical Warfare Service on the promptness with which it
has moved. We are led, however, to wonder what
plans are being made for the demobilization of the
large number of chemists secured recently for war
purposes in other branches of the government service,
for example, the Ordnance Department. Up to the
present time we have not heard that specific steps
have been taken, although the problem is fully as im-
portant in these other departments.
AN INSTITUTE FOR COOPERATIVE RESEARCH
A5 AN AID TO THE AMERICAN DRUG INDUSTRY
Addresses delivered before the New York Section of the American Chemical Society, November 8, 1918
At the meeting of the New York Section of the American Chemical Society on November 8, 1918, a sym-
posium was held upon the subject of an institute for cooperative research by chemists, biologists, and manu-
facturers as an aid to the development of the American drug industry. The basis of the discussion was an editorial
in the September 1918 issue of This Journal entitled "War Chemistry in the Alleviation of Suffering." At the
conclusion of the regular program Dr. E. R. Weidlein, Acting-Director of the Mellon Institute, upon invita-
tion, spoke of the early steps in the foundation of that institution. He traced its continuing growth, outlined
the conservative principles which had proved such wise safeguards for its well-being, and in a spirit of enthusi-
astic support of the movement offered to aid to the fullest extent desired in the formulation of the policies of the
proposed institute. In the following report of the meeting there is included a communication subsequently re-
ceived from Dr. Weidlein.
As the matter under discussion was of national rather than of local import, the resolutions adopted at the close
of the meeting were referred to the Advisory Committee of the American Chemical Society.
The feeling of those present at the meeting seemed to be epitomized in the remark of a prominent manufacturer
who said, "Something has been started to-night." — Editor.
A NATIONAL INSTITUTE FOR DRUG RESEARCH
By John J. Abbl
I am greatly interested in the plan for a national
institute in which chemists would cooperate with
specialists in the medical sciences to produce new
remedies for the alleviation of human suffering.
The need for such an institute is very great and its
opportunities arc boundless.
Among the many problems which it might undertake
would be the isolation of powerful drug principles,
like the so-called hormones, problems which cannot
be solved without the help of the funds and the EaciU
ties offered by a great central institute. For example,
the investigator who attempts to isolate the active
principle of the pituitary gland,' thi
uterine stimulant known to medicine, find thai the
price of the raw glands is six dollars a pound in the
Chicago slaughter houses and that he must be on hand
with the proper equipment to work up the fresh glands
as they are gathered. Considering the large amount
of material necessary and the cost of all the operations
involved, it is plain that the individual investigator
would have no chance to solve a problem of this sort
without generous financial assistance.
This is but an example of the innumerable problems,
all of the greatest scientific and practical importance,
that lie all aboul us. There are a great number of
crinlc drugs known 1o barbarous, as well as civilized
which should be exhaustively studied in the
ml h si it'll' 1 and medical prad ICC I'm'
v., ii h the know Li dge thai ii alr< adj a1 hand,
the joinl labor of phai mai ologists and 01 ganic chemists
should lead to the synthetic production of a very
: leu number of drugs of the most diverse qualities
97°
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 12
and remedial powers and hence of the greatest service
to mankind, or, stated more precisely, combining
the chemo-therapeutic data already in hand with the
innumerable hints that are given by nature's own
remedies should yield an enormous return in new syn-
thetic products.
The time at my disposal does not permit me to elabo-
rate this theme as much as I could wish or to cite
examples in illustration. The wonderful work of
Ehrlich in giving us organic arsenical derivatives
for the cure of syphilis is an illustration of what was
accomplished by the combined labors of pharmacolo-
gists and chemists supported by adequate funds.
What has been done in our own country in the way
of the isolating of active principles from natural sources,
as well as in the production of synthetics, should make
us certain that from the large number of trained pharma-
cologists and organic chemists among us a group of
men could be selected who would turn out brilliant
work in a national institute such as has been proposed.
What are the requirements for a successful national
institute of therapeutics and pharmacology, or what-
ever it might be called?
I — A large endowment, the income of which should
be sufficient to finance the following groups of workers.
II — Workers: Group 1 would consist of phar-
macologists who should have some knowledge of
chemistry as well as of medicine. With this
group must- be associated a certain number of
pathologists, bacteriologists, biological chemists, and
such other specialists from the medical and biochemical
field as the needs of the work require, a fluctuating
number, at least in subordinate capacities. Biological,
chemistry, however, would play such a large rdle
that this first group would always contain at least
one eminent leader in this field.
This first group would in the course of time naturally
divide itself into various sub-groups each devoting
its energies to a special field, but all working in close
cooperation. Thus, it is evident that there would
be a sub-department for pharmacological and toxi-
cological testing of new drugs and poisons. Such a
sub- department could very easily train young men to
take positions with manufacturing firms which more
and more require the service of such men. This de-
partment of the institute could also undertake the
pharmacological and toxicological testing for individuals
and firms who have no laboratories of their own.
Group 2 must be made up of capable and highly
trained organic chemists and their main work would
be in perfecting various syntheses, the hints for which
would probably be derived from the work of the first
group. Individuals of the two groups would naturally
pair off to work together on some given problem.
In 1 his second group there would also develop various
subdivisions; thus, one or more men would take charge
of the microchemicaJ and ultimate analysis. In time
there might even be a division for the prosecution
of pharmaceutical chemical research; a subdivision
of this character could be depended on to stimulate
c pharmacy in this country.
I will not new elaborate further on the various sub-
divisions of a national institute of the character under
discussion. I would, however, emphasize that the
two important things to be borne in mind are:
(1) A sufficient endowment to make the institute
independent of any outside influences.
(2) The Board of Trustees of this institute must
see to it that those selected for the leading positions
are men of ability and promise, whose one interest
is research of a high order, whether in the field of pure
or of applied science.
It is evident that an institute of this kind must
do work in both pure and applied science as indicated
in the above outline.
While I have attempted to give a brief outline of
what seems to me a feasible scheme for the development
of our proposed institute, I would welcome any modi-
fication, however extensive, which would be found
advisable by those selected to man such an institute,
for we shall all agree that these men must be the very
best that the country can furnish. Men of this caliber
must be given great freedom of action.
Johns Hopkins University Medical School
Baltimore, Maryland
AN INSTITUTE OF CHEMOTHERAPY
By P. A. Levene
The thought that the American chemical industry,
in order to be successful and impregnable against
foreign competition, needs the most careful utiliza-
tion of all intermediary products, is not novel and re-
quires no new advocates. It is also well recognized
that the most profitable utilization of the intermediary
products of chemical industry lies in their conversion
into drugs. The problem which confronts us to-day
is how to establish the American drug industry on a
solid basis.
It is needless to say that in order that the production
of a drug shall be profitable to American industry
the drug must be American in origin, and in order to
be successful it must equal and, if possible, excel the
corresponding drugs of foreign origin.
Naturally, as in every other enterprise, one must
have a certain faith that the work has promise of
success. Fortunately every one of the more success-
ful remedies is far from the state of perfection, and
new fields of application of chemical remedies in con-
nection with preservation of health or with treatment
of disease are being discovered every day.
Thus the chemical knowledge of the cardiac vaso-
active remedies is in an elementary state; the field of
anesthetics, though it has received some attention,
remains rich in promise of fruitful results; there is
much to be discovered in the field of antiseptics;
the chemical treatment of infectious disease is a field
all new and most attractive to the chemist; and
those substanees known as accessory food elements
or vitamines, have as yet not emerged from the dark-
ness of mystery.
However, several conditions have to be met in
order that the enterprise may end in success:
First, the existence of a chemical industry furnishing
the intermediary products.
Dec, i9 iS THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Second, the existence of facilities and equipment for
pure scientific research in the field of medical chemistry.
Third, the existence of trained specialists for the
required work, and finally, the existence of ample and
generous material support of the work and of the
workers.
The chemical industry has come to stay in this
country, hence one of the conditions is already met.
The question of capital is not the domain in which
the biochemist is at home. I shall dwell principally
on the plan of organization which will aim to satisfy
the two remaining conditions.
Every one intimately familiar with the development
of medicinal remedies realizes the fact that there are
very few, if any, individual workers who possess all
the technical skill and the theoretical information
required for the development of any one remedy.
As a rule, drugs are poisons. Both their toxic and
therapeutic properties may be altered by the mode of
administration or by chemical modifications. The
rules which govern the toxicity or therapeutic proper-
ties of drugs are not constant, hence before any remedy
is offered to the profession, all its toxicological, physio-
logical, therapeutic, as well as chemical properties,
have to be established. For the efficiency and ex-
pediency of the work it is most desirable that all the
work should be done in close cooperation with a group
of specialists, preferably housed in the same insti-
tution.
I therefore suggest the organization of an institute
of chemotherapy in the broader sense of the term.
The aim of the institute should be on one hand to pro-
mote this branch of science, on the other to offer the
facilities to industrial institutions to solve specific
problems which they may encounter.
To meet this double function the institute is to
consist first, of a permanent staff of investigators
engaged in free, independent, and undisturbed re-
search; and second, of groups of workers employed
by their individual industries for special investiga-
tions. The aim of the first group will be principally
to advance theoretical knowledge, which ultimately
may establish the correlation between chemical struc-
ture and biological action, and furthermore, to train
younger investigators.
The second group shall consist of temporary units
employed by the industrial institutions, but working
under supervision or control of members of the per-
manent staff. These temporary units may then serve
as a nucleus for development of laboratories housed
in the respective industrial institutions.
This plan is offered as one of three possible alter-
natives, the other two being the cooperation of the
existing industrial laboratories with either the medical
college or with the government laboratories.
In order to appreciate my objection to the medical
school it is necessary to recall the history of modern
medicine. Medicine of to-day became a science with
the development of the microscope and galvanometer
Cellular pathology, electrophysiology, and bacteriol-
ogy are the foundations of recent medicine. These
subjects dominate the horizon of the medical school.
It is perhaps right that it should be so. True, those
of us who are chemists are inclined to think that the
chemical mode of reasoning will some day acquire
ascendency in the medical mind, but this is a dream
of the future. For the present, in the majority of
medical schools, with few exceptions, the teachers
and students think in terms of cellular pathology or
electropotentials. This mode of thinking is scarcely
conducive to the development and stimulation of
chemical visions. There are other arguments against
cooperation with the colleges, but time does riot permit
to analyze them all.
Against the cooperation with the government bureaus
I have no argument of principle. I feel, however,
that the existing Bureau of Chemistry is already so
overtaxed with a multiplicity of functions that it can
scarcely be expected to do justice to all. Besides,
it is a difficult and unpromising task to educate a
government to a more generous and liberal treatment
of the scientist.
Rockefeller Institute for Medical Research
New York Citv
DRUG RESEARCH AND THE BUREAU OF CHEMISTRY
Abstract of Address by C. L. Alsberg
Dr. C. L. Alsberg, chief of the Bureau of Chemistry,
United States Department of Agriculture, spoke
extemporaneously of his deep interest in the subject
of the evening, as for many years he has been par-
ticularly interested in the development of the synthetic
pharmaceutical industry in the United States. In
his own Bureau work along related lines has been under-
taken, for the benefit of agriculture, in the production
of insecticides and fungicides. The work of the
Bureau's color laboratory was described and the
hope expressed that with this work well established
its next development would be in the closely related
field of synthetic medicinals.
Dr. Alsberg agreed with previous speakers that part
of the work contemplated in the subject of the evening
could not be carried on under government auspices,
as he felt that the federal laboratories could not be util-
ized for the study of specific problems for the benefit of
individual manufacturers. He was confident, however,
that the work of his Bureau would dovetail into the
work of the proposed institute, and expressed his best
wishes for the success of the movement which had
within it many possibilities of lasting blessings.
Bureau of Chemistry
Washington, D. C.
AN INSTITUTE FOR RESEARCH IN SYNTHETIC
ORGANIC CHEMISTRY
By A. S. LOBVSHHAKI
In my work a1 nan University Experi-
ment Station I have seen how satisfactory and ei
research work in close cooperation between chemists
and pharmacologists may be. The object toward
which we are working there is the development of
k destructive of life, but the thought naturally
thai if this cooperative work is so effective
972
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 12
in war time for the development of offense weapons,
in peace time such cooperation would be of enormous
value in promoting the security of life and its com-
forts.
I may briefly recount the way in which the work
at American University has been conducted. Most
of the materials are produced by chemists working
in the Station. Formal conferences are held twice
a week between pharmacologists and chemists, and
there are informal conferences each day. At these
conferences it is decided what substances should be
prepared. When the materials are synthesized they
are turned over to the Pharmacological Section for
every sort of test. The results of these tests are then
made known to the chemists and the possibilities of
improving the materials are then discussed. I may
say that the work has been eminently success-
ful from every standpoint, and that the cooperation
has been delightful. One can hardly realize until he
has experienced it how the pharmacologist and chemist
working together mutually stimulate one another.
I am therefore prepared to testify that cooperation
of the kind proposed is not only practicable, but
is the ideal condition for productive research. The
question then presents itself: What should be
the character of the proposed institution? What
fundamental ideas should guide in its organization?
The previous speakers have mentioned several possi-
bilities. I propose to bring up for discussion a some-
what different type of institution. The proposition
under consideration has interested me for many years,
and I have only been awaiting the time when a realiza-
tion of this dream might be possible. This is the
propitious time for establishing such an institute, at the
close of the great war, when we must face the great re-
construction period. Bold ideas, and large development
along chemical lines are in order. The marvelous
struggle that Germany has been able to put up against
the rest of the world has to be attributed largely to
her fostering of synthetic organic chemistry, during
the last fifty years, so that they have been able
to develop every manner of substitute for essential
things. The great war has brought home to every
one the thought that national security rests largely
upon chemical development and especially upon the
fostering of synthetic organic chemistry. Since the
fostering of this subject is essential for national security,
every patriot must do what he can to see that the sub-
ject is developed so that our country shall not only
be independent of the rest of the world but that it
shall lead if possible in this line of work. Such organiza-
tions as the National Security League should have
brought to their attention in the most forcible manner
possible the essential character of organic chemistry,
in order that they may not devote their entire energies
to the building up of an army and navy, but may
apply some effort to the mure subtle and less obvious
forces required for the national security, and which
also in time of peace shall be a source of great value
mil profit to the world at large.
The question then naturally presents itself: How may
the production of organic chemicals be built up into
a great industry in this country? In this connection
we may for a moment consider what factors have
played a rdlc in Germany in building up their im-
mense development in this field of endeavor. While
the establishment of such an institute will be
a wonderful stimulus and factor, it alone will not
suffice. It is obvious that one of the most important
factors will be the filling of our chairs of organic chem-
istry in the universities with the truly inspirational
type of teacher, and provision must be made that he
shall receive more for his service than the niggardly
salaries which the universities at present pay. I
understand that when the University of Heidelberg
desired to obtain the services of Victor Meyer as
professor of chemistry they asked him under what
conditions he would come. He stated that he would
require a salary of 25,000 marks; that a new chemical
laboratory should be built in addition to the old one
of Bunsen; and that his first assistant should be a full
professor. In Germany the professor receives in
addition to his salary the fees of his students, which
in the case of Victor Meyer probably amounted to
7 5, 000 marks a year. On the supposition that this
story, which I have from one of Victor Meyer's old
students, is correct, Victor Meyer was receiving up-
wards of 100,000 marks a year, in addition to whatever
income he may have received from his patents. It
must be borne in mind that this occurred about
thirty years ago, when the purchasing power of the
mark approximated that of the dollar. This story
is told merely to indicate that when the German uni-
versity desired to have a man to fill the chair of chem-
istry the authorities ascertained under what conditions
he would come and met his conditions. Teachers of
this type should not be allowed to go into the industries
in order to receive the compensation which their talents
justify.
The lack of cooperation which has existed between
men in university chairs and manufacturing concerns
has been due to many factors. The university man
had to feel absolutely certain that his name and uni-
versity connection would not be used in any way for
advertising purposes. Again, many of our best drug
firms have been in the habit of making unwarranted
statements in their advertising which were not borne
out by the facts. The drug firms, like other
commercial enterprises in this country, spent far
more money and laid more stress on their ad-
vertising and salesmanship departments than on
research to insure that they had a product which
would stand on its own merit and which would require
less advertising and not such a high order of salesman-
ship in order to place it on the market successfully.
The recent campaign for honest advertising in all
lines has produced splendid effects, and the work of
the American Medical Association through the Council
on Pharmacy and Chemistry and. the issuing of New
and Non-Official Remedies has done a wonderful ser-
vice which cannot be praised too highly.
The need for an institution of the type proposed
is obvious when one realizes that there is no institution
in America to day where the therapeutic value of a
Dec, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
973
drug can be determined in a manner acceptable alike
to scientific men and physicians. To my mind such
an institute should not only foster the production and
testing of remedial agents, but every phase of synthetic
organic chemistry should be considered within its
domain. This is necessary because remedial agents
may be found among any group of organic chemical
products. Remedial substances do not fall entirely
within the field of the coal-tar series, as many chemists
seem to think.
I will briefly and roughly outline what I think should
be the scope of the proposed institute. In the first
place, it must be endowed. The initial endowment
should be at least $1,000,000, but preferably not less
than $5,000,000. The institute should be entirely
independent of any existing institution, but it should
establish very close working relations and cooperation,
especially with the following institutions: the Ameri-
can Chemical Society, the American Medical Associa-
tion, the American Pharmaceutical Association, the
Hygienic Laboratory of the Marine Hospital Service,
the Bureau of Chemistry of the Department of Agri-
culture, the Chemical Warfare Service of the War
Department (in case this is continued in peace times),
all university departments of chemistry, research
chemical institutions and industrial concerns.
There should be many departments, all headed by
men of the highest rank who have the full confidence
of the scientific and medical men of the country.
The institute should not only encourage organic chem-
istry within its own walls, but in all universities and
industrial concerns. To this end it Should maintain
the largest possible collection of organic chemicals,
which would be furnished to any university or in-
dustrial concern at cost in smaller quantities. It
should also be willing to synthesize for chemists any
substances which they require for their work, these
substances to be furnished at cost. This idea is
prompted by the tremendous advantage German
chemists have had in securing from industrial con-
cerns any substances which they require in their
work in almost any quantities, wThereas this has been
denied the best American investigators.
Another important function of the institute should
be the obtaining and administering of patents by
organic chemists. Any scientific man should be able
to turn over to the institute any patent relating to
synthetic organic chemistry on the basis that he re-
ceive as a maximum fifty per cent of the profits, or
any less amount that he may elect, the remainder
of the profits being his contribution to the research
fund or the general fund of the institute. This would
ultimately result in an institute of great financial
strength, which is a matter of great importance. The
institute might handle its patents by licensing a
limited number of concerns to use them, or in special
cases it might itself manufacture, in case existing
manufacturers hesitated to "make use of a given patent.
One of the departments of this institute should be
devoted to pharmacology and toxicology, and H
be necessary in order to make the final therapeutic
tests acceptable to the medical profession to control
a hospital devoted to experimental therapy, to which
only selected types of cases would be admitted. This
feature alone would indicate the necessity of the insti-
tutes becoming financially strong in order to bear the
expense of such a hospital.
In conclusion, I may say that I am willing and glad
to do anything in my power to further such a project
as this, because I have the feeling that it is a matter
of the utmost importance, not only for the security
of our national life but for the benefit of the world at
large.
American University Experiment Station
Washington, D. C.
AN INSTITUTE OF THERAPO-CHEMICAL RESEARCH
By Frank R. Eldred
In an editorial in the September issue of the Journal
of Industrial and Engineering Chemistry, under the
title "War Chemistry in the Alleviation of
Suffering," Dr. Chas. H. Herty points out the need
for a research institute for the pharmacological and
clinical testing of medicinal substances.
In discussing such an institute from the stand-
point of the manufacturer of medicinal products,
I shall not attempt to dwell at length upon its re-
lations with the manufacturer, since successful co-
operation would depend entirely upon the organiza-
tion and policy of the institute and the character of
the work done.
If an institute of this kind is to attain a high degree
of usefulness, its organization and management, both
administrative and scientific, must receive the most
careful consideration. Its field of work should be
distinct from that of other similar institutions already
established. It is of prime importance that the pro-
posed institute be essentially a chemical institute.
It should be organized and conducted under the spon-
sorship of the American Chemical Society and
should in some manner be closely affiliated with that
organization. Upon the above propositions will rest
the success of the undertaking.
During the past four years we have made wonder-
ful strides in all branches of chemical industry and
with the coming of peace, steps must be taken to
make these achievements permanent assets to our
country and to assure continued progress.
In the branch of chemical industry devoted to the
alleviation of human suffering the proposed institute
would thus have a twofold function: to aid in making
us as far as possible independent of all other countries
in the production of necessary and valuable medicinal
products, and to encourage, as well as take an active
part in, researches directed towards the discovery
of more effective agents for the prevention and cure
ie, Oi thi le two functions the latter is un-
doubtedly the more important. With proper govern-
mental protection the manufacturer can be trusted to
make this country independent in the production of
medicinal chemicals which have an established use,
bul it is in the development of new medicinal
that the great difficulties and great opportunities lie.
d is not for
974
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 12
more drugs but for better — and fewer — drugs. It
would be of slight value to establish an institution
merely for the purpose of testing, pharmacologically
and clinically, new or old drugs which might be sub-
mitted to it, but it would be difficult to estimate the
immense value of a great research center for the study
and improvement of our present chemical agencies
for combating disease. In the ultimate analysis all
agencies for this purpose are chemical agencies, just
as the life processes are chemical processes, and it is
for this reason that the institute should be so organized
and supervised that all of the problems which come
to it will be attacked from the chemical standpoint.
It is a rather disquieting thought that we know
almost nothing about the mechanism of the action
of medicines and that our present medicines have been
developed by empirical methods. The effects of
many drugs now widely used were discovered accident-
ally, while certain synthetic drugs were apparently
developed for the purpose of utilizing a cheap by-
product or a readily available intermediate, and still
others were discovered by trying, more or less in-
discriminately, one substance after another until one
was found which had the desired action. Only a few
of the many German synthetic drugs have proved to
be of real value, while the larger number have been
foisted upon the public by clever propaganda. It
is not desirable that an institution should be estab-
lished to foster this kind of research. Probably no
one but a drug manufacturer knows how many remedies
are proposed by chemists and others not chiefly occu-
pied in the development or production of medicinal
substances and therefore without any broad knowledge
of the needs of medicine. No excuse can be found
for many such proposals; some are based upon un-
sound reasoning and others are entirely lacking in
originality, frequently to the extent of having been
previously tried and discredited. It would only in-
crease the number of drugs and at the same time
lower their average efficacy if drugs inferior to those
already available were placed upon the market. A
research institute such as we are considering must not
therefore lend its influence to the multiplication of
drugs of doubtful value nor waste time in the investi-
gation of many of the remedies which might be pro-
posed. *
Although little is known in regard to the manner in
which medicines produce their physiological effects,
animal experimentation and clinical tests have yielded
a great mass of facts in regard to the effects which are
produced by various drugs and this forms the founda-
tion of our present efforts in the development of remedial
substances. Such facts are of course very important
and must not be disregarded. As a result of such
studies it has been possible to correlate molecular
structure with physiological action in such a way that
it has become a most valuable guide to the chemist
working in this field, but when substances of such
diverse constitution as cocaine, quinine, novocain,
benzyl alcohol, and magnesium salts all act as local
anesthetics, it becomes apparent that we must look
more deeply for the cause of their physiological action.
The problem is one for the physical chemist, and until
the methods of physical chemistry are applied to the
study of drugs and the actual mechanism of their
action is investigated, we cannot hope for real progress
in this most important field. Pharmacology, the
study of the action of drugs, then becomes a study
involving the application of recognized physical
and chemical laws to the investigation of the reactions
occurring between the living organism and the chemical
agents employed. It is along such lines that an in-
stitute of pharmacology or therapo-chemistry should
be developed rather than along the more superficial
lines usually thought of in connection with pharma-
cological work.
It is evident that animal experimentation of the
conventional type is necessary in order to establish
the action and value of drugs and that connections
with hospitals of the highest class must be maintained
so that clinical trials can be carried out under the most
favorable conditions, but this part of the work, while
indispensable, should be subordinated to the funda-
mental researches already mentioned.
If an institute were organized in which fellowships
could be established by manufacturers or others for the
study of specific problems, the usefulness of the insti-
tute would largely depend upon the support which the
institution received in this way as shown by the number
of fellowships maintained. It is safe to say that an
institute of the character which has been outlined,
under the management of men having the proper
conception of the work and the necessary training
and experience for directing it in an efficient manner,
would receive the support of the manufacturers. It
would of course be necessary to guarantee to those
establishing fellowships, advance reports of the work
and proper patent protection. This would give
the manufacturer without research facilities an oppor-
tunity to secure the advantages of research of the high-
est type and at the same time to contribute something
to the sum of knowledge in the field from which all
or part of his livelihood is derived. The manufacturer
with research facilities would often welcome an oppor-
tunity to supplement the work carried on in his own
laboratories by establishing fellowships in a well-
equipped and competently supervised institute.
If this branch of the chemical industry is built up
in this country along the lines indicated, it will add
to our national prosperity and at the same time con-
tribute to the welfare of mankind. To bring about
this result the manufacturer must receive the support
and protection which will enable him to make his
business profitable. It must be remembered that
with the exception of a very few drugs which have come
into general use by the laity, the volume of sales of
any one medicinal substance is very small when com-
pared with the relatively enormous sales of many
technical chemicals and other manufactured commodi-
ties. The responsibilities and almost endless detail
entailed in this branch of manufacturing are also
out of all proportion to the returns. The commercial
possibilities are therefore not sufficient to justify
expensive research and the installation of costly manu-
Dec, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
975
facturing equipment unless the manufacturer can se-
cure, for a limited time, a monopoly in the sale of the
products which he originates. Indeed it often happens
that on account of the limited demand for many
well-known medicinal chemicals their manufacture
cannot be made profitable if engaged in by more than
one manufacturer. The drug manufacturer must
therefore receive the full measure of protection accorded
to other manufacturers. He must not be discrimi-
nated against in the matter of patent protection as
has been advocated in certain quarters. No other
factor could be more potent in preventing progress
in this branch of industry than the elimination of
product claims from chemical patents. Since the
progress of the industry depends upon the success of
the manufacturers engaged in it, one of the most
important duties of the institute would be to assist
the manufacturer of medicinal products in every way
consistent with the objects to be accomplished.
An institute organized for the purpose of promoting
the welfare of the industry and at the same time the
health and welfare of the people, and conducted along
the most strictly scientific lines could not fail to have
a far-reaching influence. It would be a unique in-
stitution of which the founder, the American Chemical
Society, and the Nation could be justly proud.
Dr. Herty deserves great credit for discerning the
need for such an institution and for laboring so un-
selfishly to make it a reality.
Eli Lilly and Company
Indianapolis, Indiana
INSTITUTE FOR RESEARCH ON SYNTHETIC DRUGS
By D. W. Jaynb
My contribution to this subject is an endeavor to
give the viewpoint of the manufacturer of synthetic
drugs, or the manufacturer who could, under certain
conditions, properly become a producer of these drugs.
There is no doubt that the field of synthetic drugs,
especially of a coal-tar origin, has been largely over-
looked by American chemical manufacturers. Many
concerns have entered the manufacture of dyestuffs,
and that industry has, no doubt, come to stay, but
many of the dyes that are still lacking are those of
comparatively small tonnage. It is the tonnage of
an article that usually first attracts the American
manufacturer, and synthetic drugs cannot be con-
sidered from a tonnage standpoint. With the coming
of competition on the items of larger tonnage the
products used in smaller quantities are turned to,
and have frequently been found to be more remuner-
ative than the larger volume items.
The coal-tar drugs which are made here to-day, are,
like the dyes, merely copies of those formerly imported
from Germany. With the coming of competition
on the old lines in the dyestuffs, the manufacturers
:ire putting more and more effort on research work
"1.0 discover new dyes, and it is a safe prediction that
the results of our American chemists' work in re-
search on dyes, will lead to new things in that field.
It is also safe to believe that if American chemists
begin in earnest on research in drugs, surprising re-
sults will be obtained. The field is certainly broad
enough to give ample opportunities to satisfy both
the pure scientist and the investor.
This turning to the coal-tar and other synthetic
drugs by present chemical manufacturers, especially
of dyestuffs, is certain to come. Peace time uses
for the vast resources of this country developed for
war purposes are sure to be sought. This field, how-
ever, can be pressed forward to the attention of manu-
facturers, and it should be.
I express, I believe, the thought of our Chairman,
when I say it is right and proper that the forces which
wrought for destruction in war time, should, in peace
time, turn to the conservation of the health and
happiness of the human race.
The great obstacle to the development of the syn-
thetic drug industry from the manufacturer's point
of view is, in my opinion, the inability to properly
try out the results obtained in the laboratory. In
research on dyestuffs, a new product or an old one
can be definitely tested in the manner of its intended
use, but lacking any constructive theory, the applica-
tion of the results of the research chemist in drugs
can be determined only in an unsatisfactory way at
present.
I am, therefore, of the opinion that the establish-
ment of such an institute as we are discussing, if prop-
erly carried out, would be the greatest stimulus to the
rapid creation and development of a real American
synthetic drug industry.
I believe that this institute should have two functions:
First, research in the pure science, to determine the
general effects on the human system of each class of
chemical compounds, and the probable relative effi-
ciency of these compounds by classes against certain
ailments; second, the determination of the efficiency
for the purpose proposed of any drug submitted to it
by a manufacturer, with a simultaneous determination
of any side- or after-effects of the use of such drugs.
Under the first head would come, for example, the
determination as to whether the introduction of the
acetic acid radical tends to increase the febricidal
efficiency of given compounds, and how that increase
in efficiency compares with the introduction of, say,
a formic acid radical.
Under the second heading would come the sub-
mission of a drug, claimed, for example, to be more
efficient than salvarsan. This would require consider-
able work, not only to determine its efficiency as a
specific, but to establish the quantities to be used
over a given period to secure results without conse-
quent side effects. This would imply that the de-
termination of the proper dose should be a part of
such investigations.
Both of these functions would require the highest
integrity and ability in the institute as an organiza-
tion, and in its personnel individually, li
in pure research should be recognized as the best
authority. The results of such research would then
make more evident to the chemists in the industry
the direction in which to make their effort, either in
finding a drug for a specific purpose, or finding a pur-
976
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. Xo. 12
pose for a drug which would be especially fitted for
their manufacturing conditions.
The second-mentioned function, that of reference
for report, also makes it essential that such an institute
be conducted on the highest plane, to insure the confi-
dence of the manufacturers and also of the medical
profession, which above all must be convinced of the
merits of the drugs, in order to provide a market for
them not based merely on clever advertising.
I am not attempting to detail the method by which
the research in the pure science should be carried on,
whether by fellowships or otherwise, except that the
central organization should be big enough and strong
enough to pass on any work done, and approve or
disapprove of the results in the name of the institute.
This same central organization would also necessarily
be charged with direct supervision of the work done
on drugs submitted to it. The manufacturer who
submitted a drug would pay for the report on it, but
the institute should not submit to limitations on the
work to be done. The results, of course, would be-
long to the manufacturer, and if the report showed
lack of merit of the product, or harmful effects from
its use, it would be for the information of the manu-
facturer, a favorable report also being his. for use with
proper and necessary restrictions.
The institute could cover synthetic flavors and per-
fumes, as well as drugs, as, especially in the case of
flavors, the absence of toxic or other harmful effect
is a necessary requisite.
It is also entirely possible, even probable, that
certain natural products now used in food, can be
nearly duplicated synthetically, and such products
would certainly be proper ones for submission to the
institute.
It has also occurred to me that this same institute
could fill another want, that of the investigation of
industrial diseases, due to working in various chemicals.
No doubt many concerns had unlooked-for trouble
with occupational diseases when they began the manu-
facture of dyestuffs and explosives ingredients. The
effects of working in nitro compounds are well recog-
nized, but what effects should be expected in the manu-
facture of other and more complex compounds should
be studied and made available to prospective manu-
facturers, as well as methods of avoiding and com-
bating these troubles.
The effect of these various compounds on the man
working in them is certainly a parallel problem to
the use of certain finished products to purposely pro-
duce a result on the human system.
No doubt the results of the research of such an
institute would shortly lead to an ability to definitely
predict results in the manufacture or use of any given
product .
I — Chemical manufacturers should be encouraged
to enter the wide field which exists in the production
of synthetic drugs.
II To secure rapid and proper development, a
ink should be formed between the manufacturers and
the medical profession.
III An independent organization of the highest
type of men is needed to form this link.
I V If formed, it would undoubtedly be used by
the manufacturers, and should shortly become the
leading factor in the situation.
The Barrett Company
New Yore City
REMARKS CONCERNING SUGGESTION FOR CENTRAL
MEDICINAL RESEARCH LABORATORY
By E. R. Weidlein
The various papers presented on the necessity for a
central medicinal research laboratory were exceedingly
interesting and show conclusively the need for such
an organization. The matter has come to my mind
several times since the meeting, and, while my few
remarks were along the lines of cooperation with me-
dicinal manufacturers, I do not believe that the impor-
tance of this cooperation was sufficiently emphasized.
The industrialist needs all possible assistance in under-
taking and developing research work as a means of
enlarging his output and improving its quality. How-
ever, in order to be effective, this assistance must in-
crease his independence and power of initiative and be
so given as to enlist his active support. It has been
the cooperation of progressive industry with science
which has led to the practical application of the re-
sults obtained in the laboratories of scientific men.
Fortunately the policy of industrial secrecy is now being
more generally regarded in the light of reason and more
liberal views are taken, thus bringing about a closer
union between science and industry. Nevertheless,
large corporations will not be willing to enter into
such a scheme of cooperation until they have a vivid
and broad comprehension of the need of the efficiency
which the scheme represents and a realization that the
scheme itself is founded on sane and practical consid-
erations.
It is also equally important that the central medicinal
research laboratory should have complete control over
its work, and especially, over how the results shall be
used. The introduction of a commercial atmosphere
or the use of its results for advertising purposes would
soon prove fatal to such an institution.
It is important to realize that investigations on a
large scale ultimately bring considerable benefit to the
community generally, that every scientific discovery
applied through industry results to the public gain,
and that, consequently, industrial organizations will
be justified in supporting a movement to carry on such
investigations, since it is only where there are large
aggregations of capital that the most extensive and
productive research facilities can be obtained.
The Mellon Institute of Industrial Research is willing
at all times to cooperate and render any informative
service necessary for the establishment and organiza-
tion of such a laboratory. A spirit of cooperation
should be encouraged among all types of research
laboratories, as no greater good to society can arise
than from a wider distribution of the duties and
responsibilities of research.
Mellon Institute for Industrial Research
Pittsburgh. Pa.
Dec, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
CHEMICAL MARKETS OF 50UTH AMERICA
By O. P. Hopkins,
THE CHEMICAL MARKETS OF COLOMBIA, ECUADOR,
THE GUIANAS, VENEZUELA, AND PARAGUAY
Received October 30, 1918
Excluding Paraguay, the countries considered in this
article form the northernmost portion of the continent
and all fall within the tropics. They are not so well
developed as the countries treated in previous articles
of this series, although like them, they have great re-
sources awaiting outside capital and direction. The
fact that they are within comparatively easy reach of
American ports gives our traders an advantage that
they do not possess in the countries farther south, and
make the markets much more attractive than might
at first thought be suspected. This is particularly
true of the markets for medicines, toilet articles, paper,
and so forth.
To most of these countries the war has meajit in-
creased prosperity, as their products have been in
unusual demand. Capital has accumulated . as the
result of shipping restrictions which have cut down
their imports, and it is reasonable to assume that the
coming of peace will find the inhabitants with more
money to spend than ever before and a pent-up desire
to spend it. Trade with Colombia and Venezuela,
which has always been attractive to Americans, should
be even more so when normal conditions are restored.
While trade with the other countries will increase, it
will not be of great importance, comparatively, for
many years to come.
Paraguay, which does not belong to this group of
countries geographically, is nevertheless included to
make the series complete. It should perhaps have
been considered in the first article with Argentina,
Brazil, and Uruguay.
As in the other articles, there is given for each coun-
try a table showing the imports of chemicals and allied
products from all sources, compiled in each case from the
official statistics of the country under consideration.
These figures are in some cases meager, are never very
nearly up to date,andarein somerespectsnotparticularly
accurate. They should be used only as a general
guide to the extent of the markets. The tables show-
ing the trade with the United States are compiled from
statistics published by the Bureau of Foreign and
Domestic Commerce of the United Stales Depart-
ment of Commerce.
COLOMBIA
Lack of transportation, an indifferent labor supply,
and small white population have in the past n
the development of Colombia's m mineral
s, upon which depend the prosperity of the
country. In recent years, hov
decided change for the better, in whi
ital and machinery have been promin n1 ' tors. The
opening of the Panama Canal has I i1 help,
and since the reaction that foil
the war the counli U pro I
Washington, D. C.
Gold is the principal product and silver is mined to
some extent. As the only important source of plat-
inum outside of Russia, the country has aroused much
interest in Allied circles. Emeralds are also an im-
portant product, and there are supplies of iron, coal,
salt, and petroleum, although they have received but
little attention. Manufacturing and agriculture are
comparatively unimportant.
Considering the size of the white population, Colom-
bia has been a rather important purchaser of the
products considered in these articles, and American
houses have done the bulk of the business, although
previous to the war Germany's share was not incon-
siderable, as is shown in the following table, which is
a compilation from the Colombian official statistics
for the latest available calendar year.
Colombian Imports of Chemicals and Allied Products
Articles 1914 1915
Chemicals, Drugs, Medicines,
Druggists' Articles $750,123 $797,07
France 137,890
Germany 1 34 , 323
United Kingdom 87,930
United States 325.992
Colors, Paints, Inks, Varnishes. . 118,909 150,78
Germany 33 ,489
United States 62,594
Soaps and Perfumery 112,249 87,72
France 16,673
United Kingdom 21 ,291
United States 65,012
Explosives 79,281 86,82
United Kingdom 37,835
United States 30,940
Oils and Fats, Exclusive of Min-
eral Oils 194,749 180,71
United Kingdom 16,357
United States 135,625
Mineral Oils and Combustibles. . 540,081 590,84
Germany 43,811
United Kingdom 57.175
United States 344.776
Glass and Glassware. Earthen-
ware. Stoneware 481.890 242,39
Germany 124,510
Uiiited Kingdom 95,164
United States 180,512
Paper, Cardboard, and Manufac-
tures of 551,582 494,67
Germany 1
United States 195.458
That the war greatly increased the dependence upon
supplies from the United States is shown in the next
table, which is based upon American statistics for the
fiscal years 1914 and 10 17. The marked gains under
the heading "Chemicals, drugs, dyes, etc.," are in a
measure due to high prices, but may in part be at-
tributed also to thi ■• European sources
ad to the Ead thai the purchasing
capacity of the country had increased. It is unfor-
hat the mosl striking gain under this head is
entered as "All other." The most impressive increase
in the list is shown for paper, $85,165 to $688,310.
Colombia is a market that deserves close atl
from America
sideratio
for platinum, of which ■ on and a half
11,17. Rubbei and tani
978
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 12
American Products Sold in Colombia
Articles 1914
Aluminum and manufactures $ 228
Babbitt metal 640
Blacking, shoe paste, etc 7,246
Celluloid and manufactures 1 ,221
Cement, hydraulic 126,333
Chemicals, drugs, dyes, etc.:
Acids:
Sulfuric 5,328
All other 3,212
Dyes and dyestuffs 55
Medicines, patent or proprietary 254,643
Petroleum jelly, etc 765
Roots, herbs, barks 195
Soda salts and preparations ....
All other 92,232
Explosives:
Cartridges, loaded 8,681
Dynamite 7,483
Gunpowder 25,461
All other 9,218
Flavoring extracts 5 , 1 43
Glass and glassware 56,034
Glue 1 ,182
Grease:
Lubricating 7 , 525
Soap stocks and other 5 , 639
India-rubber manufactures 38,212
Ink 6,412
Leather, patent 9,232
Naval stores 49,457
Oilcloth and linoleum 10, 345
Oils:
Animal 74
Mineral:
Crude 97,527
Gas and fuel 161
Illuminating 148,045
Lubricating, etc 67 , 946
Gasoline 33 , 709
Other light 1,184
Vegetable:
Cottonseed 2 , 523
Linseed 6,629
All other fixed 4,362
Volatile 2,263
Paints, pigments, etc.:
Dry colors 4 , 634
Ready-mixed paints 23,416
Varnish 4,562
White lead 789
Zinc oxide
All other (including crayons)... . 6,538
Paper and manufactures 85 , 1 65
Paraffin and paraffin wax 55 , 750
Perfumery, cosmetics, etc 17.325
Photographic sensitized goods 7 , 290
Plumbago and manufactures 916
Soap:
Toilet 28,675
AU other 32,096
Stearin, vegetable ....
Sugar and molasses 5 , 374
Wax and manufactures 1,350
1917
$ 21,793
1,680
11 ,312
50,603
122,277
6.757
32,222
24.372
342,157
5,858
4,053
65,594
540,863
9,400
33,401
17,440
145,255
10,343
233,804
5,238
17,040
2.923
107,603
23,255
33,719
81,112
14,443
646
150,014
6,467
45,609
38,050
81,047
911
5.424
33,077
20,077
6,656
19,128
45,691
7,319
1.636
6.719
54,106
688,310
130.259
37.159
14,796
5,978
44,875
14,413
5.573
17.616
9.188
Ipecac, which grows wild, is exported to the extent
of fourteen or fifteen tons annually, but no imports
into the United States are shown separately in the
statistics. The following table shows imports from
Colombia into this country for the fiscal years 1014
and 1917:
Colombian Products Sold in the United States
Articles 1914 1917
Chemicals, drugs, dyes, etc.:
Extracts for tanning $25,494 $142,064
Chicle .... 515
Indigo ... 6,128
Copper 841 5,886
India rubber, etc.:
Balata 243,322
India rubber 175,870 492.432
Oils:
Animal .... 4.650
Vegetable .... 239
Platinum:
Unmanufactured 398.657 1,524,039
fagots, bars, etc. .... 12.383
Tanning materials, crude:
Mangrove bark. 80 9, 169
Quebracho wood .... 2 887
All other ' 300
Zinc 114 5.168
ECUADOR
Ecuador is the smallest country on the West
Coast and has a white population of not much more
than two hundred thousand, the market for imported
goods is naturally limited, and it would be an exaggera-
tion to say that much improvement in that respect can
be expected in the near future. The mineral resources
have barely been scratched, agriculture in the main
has received little attention, and, aside from the
Panama-hat industry, which does not require imported
equipment or materials, there is very little manufac-
turing. Cacao beans make up more than half of the
exports ordinarily, the other principal products en-
tering the export trade being Panama hats, ivory nuts,
coffee, rubber, gold, and hides, the total in normal
times not amounting to much more than thirteen mil-
lion dollars.
Very little in the way of chemicals is imported, but
such business as there was in normal times was fairly
evenly divided between the United States, France,
England, and Germany, in the order named. In drugs
and medicines the United States has had the advantage
of all competitors. Belgium was formerly most suc-
cessful in supplying the demand for soap, England has
a virtual monopoly of the candle business, and Ger-
many was favored in orders for paper, as the following
official Ecuadorian figures show:
Ecuadorian Imports of Chemicals and Allied Products
Articles 1913 1915
Chemicals, Drugs, Medicines $299,558 $284,184
Drugs and medicines 139.534 195.436
France 26.432 54,331
Germany 22,814 113
United Kingdom 15,265 11,515
United States 65,315 114,072
Chemicals, n. e. S' 54.776 12,132
France 17,296 1,659
Germany 8,698 ....
United Kingdom 10,800 119
United States 17,560 9,786
Soaps 136,888 158.521
Soap, ordinary 126.016 143,338
Belgium 51.189 10.348
Germany 24.103 97
United Kingdom 35.992 24.209
United States 4.416 53.885
Soap, perfumed 10.872 14,572
United States 9.699 13,593
Paints and Varnishes 34,659 33,900
House paints 24,866 20.966
France 8,468 4.727
United States 7,070 10,742
Asms, Ammunition, Explosives. .. . 86,960 42.193
Dynamite 12,787 14.616
United States 12.787 14.616
Stearin Candles and Paraffin.. . 109.230 164.003
Stearin candles 106,322 151.700
United Kingdom 89.721 143,920
United States 1,625 5.741
Oils, Animal and Vegetablb 77,901 74,400
Olive oil 20,830 25.520
Italy 14.214 17,747
Spain 4.020 6.179
Machine oil 24.919 13.397
United States 16.733 12,915
Oils, Mineral, and Combustibles. 330,067 327,176
Gasoline 57,768 56.015
United States 2.958 _ 605
Kerosene, refined petroleum 72,821 76,525
United States -71.643 75,542
Glass, Glassware, Earthenware.. 99,655 41.880
Sheet glass 10.783 7.563
Belgium 2,602 3,179
Germany 6.645
United States 291 3.723
Paper and Cardboard 152.400 119.968
Printing paper 47.718 26,458
Belgium 7.761
Germany 28,557 3,347
lulled States 9,284 20,369
Writing paper 21.813 11.662
Belgium 5.227
United States 5.831 6.695
Perfumery and Toilet Articles. . 73,400 199.075
While the sales of American chemicals and allied
products are not imposing, there has been a substan-
tial gain all around since the war started, and as our
exporters are more advantageously situated geograph-
ically than their competitors there is no reason to
suppose that the increased business cannot be main-
tained, at least in part, when normal conditions are
restored. The effect the war has had on the trade is
shown by the following fiscal year American figures:
1 Not elsewhere specified.
Dec, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
979
American Products Sold in Ecuador
Articles 1914 1917
Aluminum and manufactures $ 44 $ 2,138
Blacking, shoe paste, etc 3,224 14 971
Candles 19 3,'410
Celluloid and manufactures 632 16,849
Cement, hydraulic 9,198 59 [790
Chemicals, drugs, dyes, etc.:
Acids 510 6,666
Copper sulfate 270 1,309
Dyes and dyestuffs 124 7,578
Medicines, patent and proprie-
tary 98,454 71,564
Soda salts and preparations (a) 13.588
All other 31.082 141,877
Explosives:
Cartridges, loaded 8,720 13.115
Dynamite 60,142 13,210
Gunpowder 4,058 30,597
All other 3,733 8,564
Glass and glassware 7,426 76,076
India-rubber manufactures 48,289 42,265
Ink 2,077 7,250
Naval stores 6,544 11,612
Oilcloth and linoleum 4,691 22,517
Oils:
Refined mineral:
Illuminating 67,855 66,660
Lubricating 19,825 21,669
Vegetable:
Linseed 561 5,296
All other 6,164 10.862
Paints, pigments, etc.:
Dry colors 265 7 , 709
Ready-mixed paints 5,878 7,314
All other (including crayons) 7,093 15,923
Paper and manufactures 78 , 089 293 , 344
Paraffin and paraffin wax 321 22,026
Perfumeries, cosmetics, etc 11,802 52,917
Photographic sensitized goods 693 5,137
Soap:
Toilet 13.103 23,516
AU other 1,081 46,633
(a) Not stated separately in 1914.
The next table, also based upon American returns
for the fiscal years 19 14 and 191 7, shows that of the
materials under consideration rubber alone is exported
to the United States in anything like an appreciable
quantity.
Ecuadorian Products Sold in the United States
Articles 1914 1917
Bones, hoofs, horns .... $ 2 , 1 74
Chemicals, drugs, dyes, etc.:
Extracts for tanning .... 1 .... 2 , 538
All others 12,893
Copper 17.570 991
India rubber, etc.:
Balata 3,908
India rubber 136,903 296,208
India-rubber scrap .... 80
Tungsten-bearing ore .... 5 ,300
BRITISH GUIANA
Of the three Guianas, the British colony is the most
important, but it does not offer an extensive market
for American goods. Sugar makes up the bulk of the
exports from the country, although there are some
shipments of gold, rum, balata, and rice. England
ordinarily furnishes about half the imports and, with
Canada, takes the major portion of the exports. The
imports of chemicals and allied products from the
United Kingdom and the United States in 1913, 1914,
and 1916 are shown in the following table, other de-
tails of origin not being available.
Imports of Chemicals and Allied Products into British Guiana
Articles 1913 1914 1916
United Kingdom:
Medicines and drugs (not
containing alcohol):
Patent and proprietary... $ 18,877 $16,959 $20,440
All other, and chemicals.. 42,402 66.317 93.641
Oils, all kinds 32.450 38.724 45.856
Soaps, all kinds 94,035 113.432 129,096
Paints, colors, pigments 23 , 805 23 . 1 74
Paper and stationery' 53,534 59.180 87.154
Glass and glassware 14.974 16,109 19.369
United States:
Medicines and drugs (not
containing alcohol):
Patent and proprietary... 8.457 13.721 17.333
All other, and chemicals.. 18,963 29,336 112.038
Petroleum, refined 106,551 99,494 138.819
tber 110.787 148.647 204
1 Does not include printing paper, which, however, is not shown
elsewhere.
The next table shows that the United States has
improved its share of the trade in chemicals and allied
products since the war started. These are fiscal year
American figures.
American Products Sold in British Guiana
Articles 1914 1917
Blacking, shoe paste, etc $6,281 $ 6,091
Candles .... 3 , 1 06
Cement, hydraulic 5,617 36,293
Chemicals, drugs, dyes, medicines:
Acids:
Sulfuric 6,491 26,095
All other 8,303 25,361
Medicines, patent or proprietary. . 18,166 14,893
Petroleum jelly 1,419 1,550
Soda salts and preparations of. . . . (a) 3,627
All other 10,373 140,103
Explosives 3,733 2,487
Fertilizers 100 18,836
Glass and glassware 960 15,625
Grease :
Lubricating 539 3,537
All other 245 355
India rubber, manufactures of 8,940 17,689
Matches 35 3,255
Naval Stores:
Tar, turpentine, pitch 4,598 5,736
AU other 1,194 2,356
Oils:
Animal 1 , 845 3 , 726
Mineral:
Fuel and gas 1,297 7.119
Gasoline 31,736 13.887
Illuminating 95,950 86,454
Lubricating, etc 14,878 30,281
Vegetable:
Corn 4,769 102,725
Cottonseed 98,357 20,930
All other 57 2,628
Paints, pigments, colors, varnishes:
Ready-mixed paints 721 2,971
All other (including crayons)... . 1,270 5,615
Paper and manufactures 6.417 56,986
Perfumeries, cosmetics, etc 6,701 15,703
Photographic goods 244 6,544
Salt 4,833
Soap:
Toilet 2,110 5,227
Allother 10 8,657
Sugar, refined 12,002 16,430
(0) Not stated separately in 1914.
Sugar and balata are the only materials of the sort
under consideration imported into the United States
from British Guiana, as the following table, for fiscal
years, shows.
Products of British Guiana Sold in the United States
Articles 1914 1917
Clays or earths .... $ 3,577
India rubber, unmanufactured:
Balata $58,284 150.102
India rubber .... 23 , 543
Sugar, cane 125 737.456
DUTCH GUIANA
Conditions in Dutch Guiana do not differ greatly
from those in the British colony and do not promise
to improve sufficiently in the near future to make the
market an attractive one for chemical products. Ba-
lata is the principal product of the country, followed by
Imports of Chemicals and Allied Products into Dutch Guiana
Total Imports from
Imports Nether- United
Articles 1913 lands States
Chemicals, Drucs, etc.
Acid, acetic, and vinegar f 3,635 $ 3,474 ....
Alcohol, cthvl 50,525 45,393 $ 564
Alcohol, methyl 490
c s 33,610 20,708 6,523
r and chloroform 64 63 ....
Fertilizers 20,859 8.531 1.044
Opium 3.382 3,202
Perfumery 7,022 5.015 1.251
Oils, Vegetable
.matic 1.240 1,000 110
Coconut, linseed, olive, rape, nia-
67,601 45.990 15.651
olini . . 4,535 1,024 2,006
1,754 19 1.727
44.420 2 41.954
Explosives:
i,)wdcr 3,900 3,898
.... 32,318 30.544 82
873 795 50
and Glassware 7,626 7,080 248
20,570 18,211 1,864
980
THE JOURNAL OF INDUSTRIAL AND ENGINEERING < HEMISTRY Vol. 10. No. 12
sugar, gold (which is mined in a primitive manner).
and cacao. Manufacturing and agriculture are of lit-
tle importance.
A glance at the preceding table will show that the
market for chemical products is of little consequence
and that such trade as there is, is dominated by the
mother country. The statistics here given are for
1 91 3, the latest available in the official records of the
country.
The next table shows that the colony has been
forced by the war to turn to the United States for sup-
plies, but the total is, of course, not impressive even
now. These figures are for fiscal years and are from
American records.
American Products Sold in Dutch GtJIAHA
Bli
Candle
Articles
eking, shoe paste, etc $
ulic
Cement, hydr;
Chemicals, drugs, dyes, medicines:
Acid, sulfuric
Copper sulfate
Medicines, patent or proprietary
All other . .
Glass and gla
1914
368
1,291
India
1,1, he
ufaetures of.
Oils
Mineral:
Fuel and gas
Gasoline
Illuminating
Lubricating, etc
Vegetable:
Cottonseed
Linseed
All other
Paints, pigments, colors, varnishes:
Readv-mixed paints
All other
Paper and manufactures
Perfumeries, cosmetics, etc
Soap:
Toilet
All other
Sugar, refined
512
1,448
5,533
2,339
649
753
658
4,652
1,797
46,966
281
9,312
967
506
3 . 1 22
8,661
$ 2,914
7.019
8.225
360
6^252
22.430
3,403
1,554
5,491
8,522
12.068
88 , 283
12,152
70,397
5,010
2,882
J. 787
4 , 366
20,426
2,197
1.986
9,301
8,900
Sugar, cacao, and balata are the only materials of
any importance imported into this country from Dutch
Guiana, as the following table shows.
Products op Dutch Guiana Sold in the L'nited States
Articles 1914
Cacao, crude $473,883
India rubber, unmanufactured:
Balata 375,747
India rubber 12
Sugar, cane 7,617
1917
S492.I63
398,670
23,639
692,382
FRENCH GUIANA
Most of ; he trailing with French Guiana is, under
normal conditions, controlled by France, but, as is the
i Chemicals and Allied Products into
Articles 1913
Chemical Products SI4 , 164
British Colonies.
Prance
I nited !
Soaps and Pi:,-
rvES
ite
Gunpov. ■
STABLE
Cottonseed
United
oi
1 1 1 1
i Mhe, fixed
' kLS, Miner u
I
no Glassware.
Paper and P ipbr Wake
France
80
41 ,524
616
244
17.1,-14
125
409
59
19.034
1 J, 719
11 .724
French Guiana
1914
$10,387
45, l"i)
347
6,196
1 1 . 550
case with the other Guianas. it is unimportant. Gold
is the most valuable product, the output approximat-
ing some two million dollars a year. Primitive meth-
ods prevail in the industry. There are important tim-
ber resources, as yet but little exploited. Rosewood
is exported to France in considerable quantities nor-
mally and there used in the manufacture of rosewood
extract. This extract is produced to some extent in
the colony also. Balata and phosphate rock are ex-
ported.
The official statistics of the country prove that
chemical products are not imported in large quantities,
the preceding table showing such details as are avail-
able for 1 913 and 19 14.
The following table shows that the war has increased
the demand for American cottonseed oil in the colony.
Even if complete data were available there would
probably be no other features sufficiently interesting
to note. These are official American figures for the
fiscal years 19 14 and 191 7:
American Products Sold in French Guiana
Articles
Cement, hydraulic. . .
Chemicals, drugs, dye
Mineral — illuminating .
Vegetable — cottonseed .
Quicksilver
1914
34
139
1917
S 2.125
780
11.439
68,596
5.052
Materials imported into this country from French
Guiana are of very little value, and information as to
their exact nature is not readily available.
VENEZUELA
In the extent of its foreign trade Venezuela is a
close second to Colombia among the countries dealt
with in this article. The country is sometimes con-
sidered as comprising three zones: The Coastal Zone,
the principal products of which are coffee, cacao and
sugar; the Orinoco River Zone, largely pastoral; and
the Forest Zone, from whence come India rubber, balata,
tonka beans, vanilla, and copaiba, and in which are
found the mineral deposits, which only in recent years
have begun to attract foreign capital. Manufacturing
is not at all well developed.
Before the war the United States furnished about a
third of all the goods imported into the country, but
in 191 7 the American share was seventeen out of
twenty-live millions. In compiling the following table
from the original Venezuelan statistics it was not found
able to show the principal sources of origin for
the individual items, but some idea of the c.
which the different competing countries divide the
trade can be gained from the entries under "Total of
all Imports," which includes all lines imported into
Venezuela. As an importer of the finer chemical
products Venezuela is rather important,
are shown.
LAN Imports OR CHEMICALS AND A;
Articles
Total op All Imports (I
Prance
Germany
Netherlands
l'nited Kingdom
United States
Chemicals, i>ki ros, M, 011
Aeid, sulfuric
\> ids. other
Calcium carbide
1414
.11 II.
4. MM 419
Dec.
191S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
981
Venezuelan Imports op Chemicals and Allied Products (Concluded)
Articles 1914 ,9,7
Chemicals, Drugs, Etc. (Concluded)
Carbonic acid gas 12, 103 13 961
Chemicals, drugs, medicines,
_.".■?•■••■. 550,855 875,032
Disinfectants 30,320 45 929
Epsom and Glauber salts 2,295 7 373
Perfumery 131,445 202' 153
Quinine... „ 52,540
Soda, bicarbonates of 3 , 569 6 390
Soda, common, caustic, crystals. 30,305 68*275
Soda, silicate of 6,246 8-617
Colors and Varnishes:
Paints and colors
Varnishes
Explosives:
Dynamite 14,523
Gunpowder 9 , 689
Oils, Mineral:
Benzene and gasoline 51 ,632
Kerosene 190. 025
Lubricating oil 35 , 279
Paraffin 1 ,730
Oils, Vegetable:
Linseed
319,795
199,252
48,054
101.798
Oliv
Other
Glass and Glassware:
Bottles
17,804 29,387
119,381 168,581
5,329 6,924
Gl;
Sheet glass
Paper and Cardboard:
Cardboard
Paper, printing
Paper, all other
(a) Not shown separately in 1914.
70,306
89,198
12,316
72,630
54,600
18,438
32,014 36.405
36,580 154,298
177,705 358,697
The following table for the fiscal years 1914 and
191 7 shows that Venezuela is no exception to the rule
that South American countries have turned to the
United States for chemical and allied products since
the war started. Imports of almost all lines have in-
creased in value, some of them in a very marked man-
American Products Sold in Venezuela
Articles 1914 1917
Aluminum and manufactures $ 51 $ 5,206
Blacking, including shoe paste 2.808 5,167
Candles 8,674 8,393
Celluloid and manufactures 478 15,711
Cement, hydraulic 48,870 69,316
Chemicals, drugs, dyes, etc.:
Acids:
Sulfuric 473 5,364
All other 952 35,382
Calcium carbide 28,877 24,792
Copper sulfate 1,692 8,851
Dyes and dyestuffs .... 30. 101
Medicines, patent and proprietary. 173,613 299,408
Petroleum jelly, etc 191 3,982
Roots, herbs, barks 254 4,067
Soda salts and preparations (<j) 85,675
All other 70,145 434,467
Explosives:
Cartridges, loaded 70,073 40,572
Dynamite 1,267 520
Gunpowder 11,862 25,740
All other 5,250 18,032
Flavoring extracts and fruit juices.. . 5,101 8,458
Glass and glassware 16,079 141,738
Grease :
Lubricating 4,766 13.814
Soap stock and other 1,934 7,700
India-rubber manufactures 42,377 224,487
Ink 6,058 14,156
Leather, patent 8,551 84,326
Metal polish 14') 12,221
Naval stores 55,508 59,977
Oilcloth and linoleum 6,494 7,951
Oils
Mineral:
Illuminating
Lubricating, etc
Gasoline
Other light..
Vegetable:
Cottonseed
Linseed
Other fixed
Volatile
Paints, pigments, etc.:
'ilors
Ready-mixed paints
Varnish
Zinc oxide
All other (including crayons)..
Paper and manufactures
Paraffin and paraffin wax
Perfumeries, cosmetics, etc
Photographic sensitized goods
-• and manufactures
ToHel
tabl
! manufacture*
(0) Not stated separately in 1914.
198,295
26,348
38,652
1,759
I , 133
I ,106
2 . 596
2 , 85 1
15,348
4,427
195,932
62.522
287.877
1,114
4,342
32.399
6.057
8,739
18,535
33,575
7,069
5,066
47,521
483,754
113,551
33,466
.IS, 441
51 .4. '(I
■ ner, and the problem here is the same as in the other
countries — to retain the advantage when European
competition returns.
Sugar, india rubber, balata, copper, and "All other
chemicals" (including probably tonka beans, vanilla,
and copaiba), are the principal items of Venezuelan
export to the United States that can be considered of
interest to the chemical industry. The extent to which
they enter the American market is shown in the fol-
lowing table covering the fiscal years 1914 and 191 7:
Venezuelan Products Sold in the United States
Articles 1914 1917
Asphaltum and bitumen 425,060 258,205
11,271
Bones, hoofs, horns
Chemicals, drugs, dyes, etc.:
Chicle
Other gums
All other chemicals
Copper
Dyewoods, in crude state
Fertilizers
Fish sounds
Hide cuttings and other glue stock
India rubber, etc.:
Balata
Guayule gum
India rubber
India-rubber scrap
Sugar, cane
28,975
23,324
7,515
71,056
304,369
208,364
507.369
1,260
4,086
11,222
116,709
7,822
37,404
3,518
211,794
341 .220
3,985
128,063
249,867
80
703
10
1.126,788
PARAGUAY
Imports of all kinds into Paraguay in 19 14 totaled
only five million dollars, the United States ranking a
rather poor fourth after Germany, England, and Ar-
gentina as a source of supply. Such export trade as
there is consists of animal and forest products, fruits,
petitgrain oil, tobacco (a German source of supply),
and yerba mate (Paraguayan tea). As the following
Paraguayan figures show, the United States has had
the advantage in sales of chemicals, drugs, medicines,
and explosives, while Germany has been favored in the
glass business. The statistics are inadequate and do
not represent actual market values.
Paraguayan Imports op Chemicals and Allied Products
Articles
Che*
als. Drugs, Medicines 1226,528
Germany.
United Kingdom
United States
Arms. Ammunition, Explosives.. . .
Germany
United States
Glass, Glassware, Earthenware..
France
Germany
United States
1914
1915
>26,528
$113,636
42,299
4 . 1 59
33,017
24,339
80,961
50,402
58,674
3,532
12,993
7
23,342
1 ,156
71,442
13,294
10,949
3,151
51,410
1,326
393
515
Such details as are available in the American sta-
tistics of exports to Paraguay for the fiscal years 1914
and 1917 are shown in the following table:
American Products Sold in Paraguay
Articles 1914 1917
Blacking, shoe paste, etc .... $ 2,702
Chemicals, drugs, dyes, etc $15,550 15,050
• led cartridges 17,193 7.1KI
Illuminating oil 8.394
As (he exports from Paraguay pass through Argen-
tina and Uruguay, and arc credited to those countries
in our <<■ 1 difficult to determine I he
extent ti Pai uayan products are sold in this
country, but it is 1 ebracho extract and
petitgrain oil are received in fair quantities. Thi t. in-
ning-extract industry has developed rapidly ill
years. An item of 1,108 tons of muriate of potash,
valued at $43,161, was recorded as ■
Paraguay in 10 14, but it has not 10
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol! io, No. 12
ORIGINAL PAPERS
A STUDY OF THE CONDITIONS ESSENTIAL FOR THE
COMMERCIAL MANUFACTURE OF CARVACROL
By Arthur W. IIixson and Rai.i-ii II McKee
Received June 21, 1918
Carvacrol is closely related both chemically and
physiologically to thymol. The latter substance is
used as a specific for hookworm disease and as the
principal ingredient in many antiseptic preparations.
Hookworm is probably the greatest handicap to the
full use and occupation of the tropics by the white
races. On account of the general use of thymol in
antiseptic manufacture and the widespread organized
effort being made in many countries to combat the
enormous inroads of the hookworm disease, the de-
mand for it has become so great that the supply from
present sources is entirely inadequate.
Attempts have been made to produce thymol
synthetically, but up to the present time no process
of any promise commercially has been developed.
Recent comparative tests1 have shown carvacrol
to be practically equal to and, in some cases, to possess
greater antiseptic value than thymol. Its importance
as a substitute for this substance is sufficient to warrant
an investigation of its production.
Carvacrol is found as an ingredient in the essential
oils of many labiate plants and particularly in those
of the species Origanum. There are two kinds of
Origanum oil2 known commercially, namely, Trieste oil
containing from 60 to S5 per cent of carvacrol, and
Smyrna oil containing from 25 to 60 per cent. Both
of these oils contain cymene. Carvacrol is also found
in the oil of thyme from Thymus vulgaris in which it
sometimes replaces all of the thymol.3 The quantity
of carvacrol available from these natural sources,
however, is very small and of practically no com-
mercial importance. These facts indicate that if
carvacrol is to be used in the place of thymol a process
for its synthetic preparation on a commercial scale
must be developed. The prospects were such as to
encourage a study of the synthetic preparation of
carvacrol and the conditions essential for its com-
mercial production, which is the object of this re-
search.
Carvacrol was first prepared synthetically by
Schweizer4 who found that the same oil was obtained
by treating caraway oil with potassium hydroxide,
phosphoric acid, or iodine. Claus5 heated camphor
with iodine and obtained a product which he called
camphor-creosote which was identical with the product
made by Schweizer. Muller6 while comparing cymene
and thymol obtained from different sources, sul"
1 The average results of four viability tests using the organisms B
typhosus, B communior, and slaphylococus pyogenes aureus, furnished through
courtesy of Dr A. K. Halls, Department of Bacteriology, College of Physi-
cians and Surgeons. Columbia University, and Dr A. M Buswell, Depart
ment of Chemical Engineering, Columbia University, New York City.
■ U. S Dispensary, 19th Edition, 1905, 1432
' Ibid , 19th Edition, 1905, 1571.
• J. prakl. Chem.. 14 (1841), 257.
• Ibid . as (184.'), 264.
• Ber., 3 (1869). 1 10
fonated pure cymene, made the sodium salt, fused it
with sodium hydroxide and obtained an oil which hej
identified as carvacrol. Kekule and Fleischer1 treated 1
carvone obtained from caraway oil with orthophos-
phoric acid and produced carvacrol. From cymene.
obtained from camphor, Pott2 made potassium cymene
sulfonate, which he fused with potassium hydroxide.
He poured the fusion mass into water, neutralized with
sulfuric acid, and obtained a small amount of
yellowish liquid which distilled at 230 ° C. He rec-
ognized it as an isomer of thymol. He also observed
that if a few drops of an alcoholic solution of the oil
were added to a solution of ferric chloride, a charac-
teristic green coloration would be produced. Rey-
chler3 found that when carvo-chlorhydrate is distilled,
hydrochloric acid split off and the distillate contained
carvacrol. Etard4 treated monochlorcamphor with a
10 per cent solution of zinc chloride and heated it.
By distilling the mass and agitating the distillate with
caustic soda he obtained carvacrol. Mead5 and
Kremmers converted pinene into nitroso-pinene and by
hydrolyzing this substance produced carvacrol. The
yield was about 60 per cent. Wallach6 made amido-
thymol from oxydihydrocarvoxime, treated it with
sulfuric acid, and found carvacrol to be one of the
products. Harries7 passed steam for a long time over
hydrobromcarvone and produced a small amount of
carvacrol. McKees has patented a process for the
manufacture of carvacrol based upon the use of spruce
turpentine as the source of cymene.
A careful examination of these methods showed
that in each case, with the exception of that of McKee,
the raw materials used were of such a nature as to
make them impracticable for the production of carva-
crol on a commercial scale. However, the discovery
that spruce turpentine consists mainly of cymene and
the fact that it is produced in large quantities as a
by-product in the manufacture of wood pulp by the
sulfite process indicated that a method, along the line
suggested by the experiments of M Ciller, Pott, and
McKee might be capable of commercial development.
For these reasons an investigation was made to de-
termine whether a method based upon the following
reactions could be carried out on a commercial scale:
I — Formation of cymene 1 -sulfonic acid by treating
spruce turpentine with sulfuric acid.
II — Removal of the excess sulfuric acid used in (I)
and formation of calcium cymene sulfonate by treat-
ment with finely divided limestone.
Ill — Formation of sodium cymene sulfonate in solu-
tion and removal of calcium as carbonate by treating
with soda ash.
' Ber., 6 (18731, 1087.
■Ibid., 9 (1876). 468.
' Chem.Centr.. 63 (189.
< Compl. rend . 116 11893). 1156.
t Am Chem. J . 17 (1895). 607.
• Ann , 191 UR96). 54S
' Per.. 34 U901) 19:4.
• U. S. Patent No. 1,263,800, May 14, 1918.
Dec, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
IV — Formation of sodium carvacrolate by fusing the
sodium cymene sulfonate with caustic soda.
V — Formation of carvacrol by treating the fusion
products of (IV) with sulfuric acid.
A study of these basic reactions indicated that the
following fundamental operations would be necessary:
1 — Sulfonation of cymene.
2 — Disposal of the sulfonation products.
3 — Formation of calcium cymene sulfonate solu-
tion and precipitation of calcium sulfate.
4 — Filtration and disposal of the filter cake.
S — Formation of sodium cymene sulfonate solution
and precipitation of calcium carbonate.
6 — Filtration and disposal of filter cake.
7 — Evaporation of the sodium cymene sulfonate
solution and disposal of the solid salt.
& — Fusion of the solid sodium salt with caustic
alkali.
9 — Disposal of the fusion products.
10 — Neutralization of the fusion product solution
and formation of carvacrol.
11 — Separation of the carvacrol.
12 — Purification of the carvacrol.
EXPERIMENTAL
The experimental work consisted of the determina-
tion of the relative importance of the preceding opera-
tions and the conditions under which they could be
carried out with maximum efficiency.
materials — All of the materials used in the experi-
mental work were of standard commercial purity, such
as can always be obtained on the market, without
difficulty in normal times, with the exception of spruce
turpentine, which up to this time, although produced
in large quantities as a by-product, has had no com-
mercial value.
The spruce turpentine used was a steam-distilled
product obtained from the New Process Gasolene
Company, of Philadelphia, and was purchased in the
crude form by that company from the J. and J. Rogers
Company, of Au Sable Forks, N. Y. This product
was clear and nearly white. After remaining in the
laboratory for several months a distinct yellow tinge
appeared. The product was used in the "as received"
condition without treatment of any kind. A fractional
distillation of 1.5 liters gave the following results:
Temperature Fraction
Degrees C. Cc. Per cent
Below 171.5 50 3.33
171.5-178.5 1250 83.34
Above 178.5 200 13.37
Kertesz' found spruce turpentine to contain 80 per
cent of cymene, from 10 to 12 per cent of sesquiterpene,
and the remainder diterpene. The fractionation re-
sults show that nearly 80 per cent of the material came
off at about 1 75 ° C, the boiling point of cymene.
sulfonation — The prime variables in this opera-
tion arc (a) strength of acid, (b) temperature, (r) time,
(d) proportional amount of acid, (e) amount of stir-
ring, (/) type of sulfonating vessel.
strength of acid — The adoption of 66° Be\ sul-
furic acid as the most practical strength for the sul-
fonation of benzene in phenol manufacture led to the
' Chem. Zls., 40 (1916). 945.
belief that this strength would also be the most practical
in the sulfonation of cymene. 400 cc. of commercial
66° Be. acid (checked by titration with standard
alkali) were placed in a liter Erlenmeyer flask with 200
cc. of spruce turpentine. This was placed in a water
bath and heated to 96° C. A two-blade glass propeller
stirrer was placed in the vessel below the level of the
acid and was run at a speed of 700 r. p. m. in the
direction that would throw the acid toward the top
of the flask. At the end of 3V2 hrs. sulfonation was
complete. This proved that 66° Be. acid could be
used. A similar experiment with 60° Be. acid showed
that sulfonation was less than 50 per cent complete
at the end of 1 2 hrs. Acids of greater strength were
not tried although it was obvious that the reaction
period would be shortened somewhat by their use.
The fact that 66° Be. acid can normally be obtained at
less expense and trouble than the stronger acids and
that it can be handled in a plant with less difficulty
prompted its adoption for all of the sulfonation experi-
ments.
temperature — The apparatus described in the
preceding section was used. The sulfonation vessel
was filled with 200 cc. of spruce turpentine and 400 cc.
of acid. The stirrer was run at 700 r. p. m. Four
hours was the standard time. At the end of the
reaction period the stirrer was removed and acid
allowed to settle and separate from the cymene and the
sulfonated portion. The upper layer was then siphoned
off, shaken well, and 25 cc. removed by means of a
pipette. This was placed in a graduate and 75 cc.
of water added, shaken well, and allowed to stand for
12 hrs. The unsulfonated cymene formed a layer
at the top and its volume was read directly. The
following table and curve, Fig. i, show the results:
Table I
sulfonated
portion
Per cent
Cc.
sulfonated
19.3
22.80
14.5
42.00
7.8
68.80
2.0
92.00
0.2
99.20
Trace
99.5 +
The rate of sulfonation varied almost directly with
the increase of temperature up to 90°. Between this
temperature and ioo° C. the rate was highest, indicating
that the temperature should be kept within this range
for efficient sulfonation. This temperature being near
the boiling point of water makes it an easy one to
maintain in both laboratory and plant. Sulfur
dioxide is evolved at all temperatures. The amount
was slight at low temperature and increased as the
temperature was raised.
time — With the same apparatus and the same
quantities of materials, time experiments were run.
The data in the preceding table indicate that a tem-
perature between 90° and 100° would give the shortest
time required for complete sulfonation. 96° C. was
chosen for the reason that it was convenient to main-
tain. The extent to which the reaction had pro-
ceeded was determined by the same means used in the
preceding experiments, that is, 25 cc. portion wen
taken from the upper layer which had been separated
984
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 12
s
0
•X
I
Tern
tet -i
fa re
-5ul
fona
t-fon
Curl
e
/
/
Degrees C.
Fig. 1
from the acid and, after diluting and standing for 12
hrs., the volumes of the unsulfonated portions were
read. The results are given in Table II.
Table II
Unsulfonated
portion
Per cent
Cc.
sulfonated
18.4
26.40
12 4
50.40
4.3
82.80
1.2
95.20
0.1
99.60
Trace
99.6 +
These data show that a 4-hr. period is sufficient for
complete sulfonation at 96° C. with efficient stirring.
The results are shown graphically in Fig. 2.
amount of acid required — 200 cc. charges of spruce
turpentine were sulfonated at 96 ° C. with quantities
of acid varying from 400 cc. to 150 cc. Sulfonation
was complete with amounts down to 200 cc. With
amounts below this complete sulfonation could be
obtained, but the time required was greatly increased.
Many batches were run using equal volumes of acid
and cymene and complete sulfonation was obtained
in 4 hrs., with the temperature at 96° C. These re-
sults show, contrary to previous records, that a volume
of 68° B€. acid equal to that of the cymene is sufficient.
It is to be noted also that the decrease in the amount
of acid used to the equal volume limit did not decrease
the rate of reaction.
amount of stirring — McKee1 has shown that the
rate of sulfonation of hydrocarbons is distinctly de-
pendent upon efficient stirring, other things being
equal. By increasing the efficiency of his stirring
device he was even able to sulfonate kerosene with
ease. No experiments were made to determine the
effect of different degrees of stirring upon the rate of
sulfonation of cymene, but the type of stirrer used,
the speed at which it was run, and the shape of the
' Science, 35 (1912), 388.
reaction chamber insured an extremely intimate con-
tact of reacting materials.
type of sulfonating vessel — To determine
whether a cast iron or steel sulfonating vessel could be
used, one was made by screwing a cast iron cap on the
lower end of a 6 in. length of 4 in. pipe. A similar cap
provided with stuffing-box openings for a stirrer and
the thermometer was used for a cover. A two-blade
stirrer of the propeller type was used. The blades
were set at such an angle that when run at speeds above
500 r. p. m. the liquid was thrown against the cover of
the vessel. To the stem a series of pulleys of different
diameters was fastened in order to use different speeds.
The stirrer was driven with an electric motor. A
thermometer was placed in the vessel at such a depth
as to be well in the liquid, and it was held in place
by a stuffing-box similar to that used for the stirrer.
When the cover was screwed on well the vessel was gas-
tight. The vessel was set into a water bath to such a
depth that the surface of the water came to the lower
edge of the cover. The water bath was heated by an
ordinary Bunsen burner and the temperature was
controlled within two degrees without difficulty.
With this apparatus many runs using 300 cc. of
spruce turpentine and 300 cc. of acid were made.
The temperature in all cases was from 96 ° to 98 °.
With the stirrer running 500 to 600 r. p. m. sulfonation
was complete in from 3V2 to 4 hrs. A larger amount
/
/
|
/
^
^
J
/
1
1
/
/
Time - 5ulfonatton Curve
> 1 1 1 • 1
Fig. 2
of sulfur dioxide was given off than with the glass
vessel. When all openings in the cover were tightly
closed, a considerable pressure was developed. It
was observed that although a considerable surface
of the sulfonator was above the surface of the water,
the temperature inside of the vessel during the opera-
Dec, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
98S
tion was less than one degree below that of the bath.
When the sulfonation products were poured into a
glass vessel and allowed to cool, a white solid settled
to the bottom of the acid layer. This was found to be
ferric sulfate. . The iron had reacted with an excess
of concentrated sulfuric acid forming ferric sulfate and
sulfur dioxide. This accounted for the increased
amount of sulfur dioxide observed during the reaction
period. The amount of ferric sulfate formed varied
from 3.55 to 5.6 g., representing a loss of iron of from
0.73 to 1.57 g. The weight of the sulfonator was
3500 g. The loss was quite small and undoubtedly
in a larger vessel of special cast iron would be still
less on account of the relatively smaller contact area
and refractory skin on the surface of the vessel. The
presence of this iron was not objectionable. If for
any reason its removal might be desired this could be
done at practically no increase of cost by the addition
of a small quantity of lime just after the precipitation
of the calcium sulfate in the next operation.
sulfonation products — When sulfonation was com-
plete and the mixture allowed to stand for a short
time, two distinct layers formed. The lower, lighter
colored layer contained the greater portion of the
excess sulfuric acid and about 20 per cent of the total
amount of the cymene sulfonic acid. The upper,
darker colored layer contained the greater part of the
cymene sulfonic acid, some sulfuric acid, and ma-
terials resulting from the action of the acid on the
impurities in the spruce turpentine. The formation
of the layers took place rapidly when the materials
were hot. When cold, the upper layer became very
thick and viscous. When allowed to stand for a few
days at 20 ° C. the cymene sulfonic acid began to
crystallize and finally the whole layer became solid.
With the temperature below 10 ° C. the upper layer
solidified very rapidly. Colorless, transparent crystals
of cymene sulfonic acid, isolated from the upper part
of the lower layer, melted at 50 ° to 51° C. This
was the melting point found by Spica1 and later by
Eaton and McKee2 for a cymene sulfonic acid of the
composition C10H13SO3H.2H2O, which the latter two
made from spruce turpentine. All'of the constituents
of the upper layer were found to be soluble in water
with the exception of a small amount of a very finely
divided white substance which settled out after stand-
ing for a number of days. Examination of this white
precipitate showed it to be sulfur. Evidently it came
from the complete reduction of a small portion of the
sulfuric acid.
disposal of sulfonation products — The formation
of two distinct layers which could easily be separated
suggested that a recovery of the unused sulfuric acid
might be possible. The problem was to recover the
sulfuric acid without losing the cymene sulfonic acid
which was present in considerable quantity in the lower
layer. Inasmuch as it was necessary to add water
in the next operation, experiments were made to
determine whether the distribution of the substances
in the layers was affected by dilution.
1 Btr., 14 (1881), 653.
1 Unpublished thesis, University of Maine, 1911.
For these experiments 150 cc. of spruce turpentine
and 150 cc. of 66° B6. acid were used in the sulfona-
tion. When sulfonation was complete the hot prod-
ucts were poured into a 500 cc- graduate and allowed
to stand until the volumes of the layers became con-
stant. After reading the volumes a definite quantity
of water was added and the mass shaken until the
mixing was complete. The mixture was then allowed
to stand until the volumes became constant again.
10 cc. samples were taken with a pipette and analyzed.
The total acid content was determined by titrating
with standard sodium hydroxide. The free sulfuric
acid was determined by precipitation with BaClj.
Cc. Water Added
The difference between these gave the sulfonic acid
content which was calculated as sulfuric acid. The
results are given in Table III and are shown graphically
in Fig- 3-,
Table III
Combined
Combined
Free HjSO.
Free H,SOt
HiSO.
H1SO1
added
lower layer
upper layer
lower layer
upper layer
Cc.
G.
G.
G.
108.16
49.22
19.94
85.19
30
124.88
40.73
11.89
94.24
60
123.60
36.57
6.54
97.30
90
121.03
39.87
7.59
98.15
120
116.43
45.38
7.62
96.96
150
99.39
58.68
7.63
97.93
180
79.06
82.70
6.50
98.64
These results show that by the addition of a quantity
of water equivalent to one-fifth of the total volume
(approximately 300 cc.) the combined sulfuric acid,
which represents the cymene sulfonic acid, dropped
from 19.94 g. to 6.54 g. in the lower layer and in-
creased from 85.19 g. to 98.15 g. in the upper layer.
After this the values remained practically constant
with further dilution. The values given in the above
table for the combined sulfuric acid represent ap-
proximately the percent menc sulfonic acid
in the two layers.
The dilution experiments were carried out to the
point where the two layers merged; analyses at these
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 12
dilutions were not made for the reason that the acid
was not worth recovering. Although it was possible
to reduce the cymene sulfonic acid content in the
lower layer 60 per cent, the amount which still re-
mained was such that its loss probably more than
balanced the value of the acid recovered and the
amount of ground limestone saved. Market and plant
conditions will be the deciding factors. If the acid
is recovered the conditions that will give the lowest
cymene sulfonic acid loss should be used. At that
dilution the acid would have a concentration of about
6o° Be\ and could be used to neutralize the fusion
mixture in a later operation. The separation of the
layers could be made in the sulfonation kettle after
the products were cooled, if the kettle was made with a
bottom discharge as is usually the case.
NEUTRALIZATION OF THE SULFONATION PRODUCTS
This is a standard operation in many processes and the
conditions controlling it are well understood. The
neutralizing agents may be a good grade of finely
divided limestone or lime. Limestone is the cheaper
and is efficient, although the operation does not go
quite as smoothly as with lime on account of the
evolution of a large amount of carbon dioxide. A
lead-lined tank with a stirrer and foam breaker should
be used unless care is taken to discharge the sulfonation
products into a slurry of limestone in which case the
lead lining is not necessary. The calcium sulfate
formed may be removed without difficulty by using a
filter press. The filter cake has no value.
FORMATION OF SODIUM CYMENE SULFONATE Sodium
carbonate or sodium hydroxide may be used. Under
normal conditions soda ash would be the material to
use on account of its cheapness and the greater ease of
filtering the precipitated calcium carbonate as com-
pared to calcium hydroxide. A standard, mechani-
cally stirred wooden tank should be used.
SIMULTANEOUS NEUTRALIZATION OF SULFONATION
PRODUCTS AND FORMATION OF SODIUM CYMENE SUL-
FONATE solution — This may be done by neutralizing
partially or completely the sulfonation products with
limestone and then adding the requisite amount of
soda ash. By this method the calcium sulfate and
calcium carbonate can be removed by a single filtra-
tion. This procedure requires closer chemical control
than when the two operations are separated for the
reason that it is much more difficult to tell when the
reaction with the soda ash is complete. Unless close
watch is kept on this operation under plant conditions
an excess of soda ash will often be used by the work-
men. It is doubtful if this combined procedure will
work out as well as the former in plant practice as the
resulting saving in limestone and labor will be small.
EVAPORATION 0} I III SODIUM CYMENE SULFONATE
solution — It is obvious that the use of as little water
as possible in the preceding steps will save time and
expense in the production of dry sodium cymene
sulfonate. This salt is very soluble in water and its
water solutions are difficult to evaporate to dryness
at atmospheric pressure. The presence of a small
amount of water causes the salt to form a thick pasty
mass which becomes liquid above 700 C. This last
portion of solvent may be removed, in plant practice,
by either drying in vacuum or by use of a film dryer
such as the drum dryers (atmospheric pressure or
vacuum) which have lately come into such wide use in
drying concentrated or pasty substances in chemical
plants.
FUSION OF THE SODIUM CYMENE SULFONATE The
problem was to determine (a) the best fusion reagent,
(6) the proper fusion temperature, (c) the most suitable
type of fusion kettle, (d) the time required for com-
pletion of the reactions, and (e) the minimum amount
of fusion reagent for maximum yield.
The apparatus used for the preliminary fusion
experiments consisted of a cylindrical steel vessel 4,/«
in. in diameter and 5 in. deep. The steel was 3, ](
of an inch thick. The cover was a steel plate with
openings for a stirrer shaft and thermometer and could
be closed tightly by means of stove bolts and winged
nuts. It was necessary to have the stirrer work
through the whole mass of the liquid in order to break
up surface crusts and prevent the material from stick-
ing to the bottom and sides of the kettle. The vessel
was heated with a Fletcher burner. After making a
number of fusions with this apparatus it was obvious
that it was not possible to control the temperatures
closely enough. To overcome this difficulty the fusion
vessel, equipped as described, was placed in an insulated
bath containing about 20 lbs. of a eutectic mixture
of sodium and potassium nitrates. This bath, pro-
vided with a propeller type stirrer, was heated with a
Fletcher burner. With this arrangement there .was no
difficulty in keeping the temperature constant within
one degree. The difference between the temperature
of the bath and that inside of the fusion chamber was
less than one-half degree when the stirrers were run-
ning.
fusion reagent — Heretofore, those who have pre-
pared carvacrol by a fusion method have used potas-
sium hydroxide in large excess. Although scientific
literature favors the use of this reagent for the fusion
of sodium cymene sulfonate and similar salts, such as
sodium benzene sulfonate, modern commercial practice
on the latter has demonstrated that caustic soda can
be used with equal efficiency and at much less expense.
For this reason a good grade of commercial caustic
soda was used in all of the fusion experiments.
fusion temperature — To determine what effect
temperature has upon the efficiency of the fusion
operation, fusions were made at different temperatures.
The charges consisted of 150 g. of dry sodium cymene
sulfonate and 450 g. of caustic soda. The fusion
period was 6 hrs. The caustic soda which melted at
319° C. was fused first. To this the sodium cymene
sulfonate (in granular form) was slowly added. At j
the end of the fusion period the products were poured
gradually into 2 liters of cold water, forming a strongly
alkaline solution which was neutralized by adding
dilute sulfuric acid (400 Be.). The carvacrol set free
in this operation was extracted with benzene. After
separation of the benzene solution from the neutral
Dec, 191S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
liquors, the benzene was distilled off and recovered.
The residue was distilled yielding carvacrol and a tarry
residue. The carvacrol was weighed, and the yield
thus obtained was used as the criterion by which the
efficiency of the fusion operation was determined.
As the sodium cymene sulfonate dissolved in the
molten caustic the temperature at which the mass re-
mained molten rapidly fell. The average time re-
quired to get a smooth fusion was one-half hour. It
was possible to lower the fusion temperature to 255° C.
and still have the mass molten enough to stir well. If a
quantity of water equal to 10 per cent of the weight
of the caustic was added, the fusion took place much
more smoothly and the mixture was kept molten at a
still lower temperature. However, the addition of
water was of no advantage for the reason that its rapid
evolution as steam at higher temperatures made it
difficult to keep the molten material in the fusion
chamber until it was all given off. When 280 ° C.
Table IV
'hamber Uncove
X
t^*~
>
1
4
/
t
X
ft
Appr
ox/rn
a+e-Mean Fusion
T
>mperofure >
'feld
Cur
ye
215 215 ?9f 305 315 323 335 345 3S5 365 375 385
Degrees C.
Fig. 4.
was reached (fusion vessel uncovered) a bluish white
fume was observed. This increased in amount rapidly
with the rise of temperature until at 3250 C. it was
quite dense. The mass thickened under these condi-
tions and at the end of the fifth hour it was granular
and would not pour. If the temperature was kept
below 300 ° C, although some fume was evolved, the
material remained liquid until the end of the fusion
period and poured well. At 280° C. when a flame
was held in the upper part of the fusion chamber a
flash was observed. As the temperature was raised
the flash became more pronounced and at 3000 C.
the gas burned for a number of seconds. At 325° C.
it burned longer. With the fusion chamber open at
temperatures from 2750 to 3000 C. the yield of carva-
crol varied from 8.25 to 43.19 g. Above 3000 C. the
yields varied from 35.30 to 45.27 g. and, though higher
than for temperatures below 300° C, were very
'■i> iii' and difficult: to duplicate These fai
revealed by the data in Tabic IV.
Sfo
G.
G.
1
3
4
150
ISO
150
150
450
450
4 50
450
5
150
4511
6
150
4^11
7
150
450
8
150
450
0 C.
G. Per cent
Remarks
267
15.75
16.53
No fume.
275
15.10
15.80
No fume
nflammable gas.
275
8.25
8.66
No fume.
nflammable gas.
285
23.45
24.62
Slight fume
Small amount
of inflammable gas.
295
35.00
36.74
More fume.
More gas.
300
43.19
45 . 34
More fume.
More gas.
300
45.27
48.57
More fume.
More gas.
325
35.30
37.06
Rapid evolution of fume-
Solidified
before end of
period.
345
36.15
37.85
Rapid evolution of fume.
Solidified
before end of
period.
9 150 450 3.75
From 150 g. of sodium cymene sulfonate a yield of
95.25 g. of carvacrol should have been produced.
The percentage yields in this table and those following
were calculated on this basis.
Above 3000 C. there was less variation in the yields.
This and the fact that the yields were higher led to the
belief that still higher temperatures might give better
results. It was also noted that when the fusion
chamber was covered no fume was evolved, but as
soon as the cover was removed it appeared, showing
that there was a reaction with the oxygen of the air.
To determine whether this reaction was in any way
responsible for the great variation in yields, a series of
fusions was made at different temperatures with the
fusion chamber closed. The cover with an opening
and connections for a condenser was screwed down
tightly after each charge was inserted. A Liebig
condenser provided with an air-tight receiver was at-
tached. From one opening in the receiver a tube ran
to a gas holder. With the exception of the cover and
the accessories mentioned, the conditions for this series
were the same as for the previous one. The data and
results are given in Table V and shown graphically in
Fig. 4-
Table V
(Fusion Chamber Covered)
Charges consisted of 150 g. sodium cymene sulfonate and 450 g. caustic
soda. Fusion period. 6 hrs.
Remarks
Temp
° C.
crol
G.
Yield
Per cent
275
29.65
31.13
300
35.71
37.41
325
37.16
39.01
325
38.20
40.10
340
43.57
45.74
342
44.81
47.04
355
360
49.36
48.33
51.71
50.14
360
49.91
52.31
360
49.14
51.60
370
48.26
50.65
375
47.92
50.31
375
46.97
49.31
385
46.10
48.39
! of yellow oil distilled otT,
nflammable gas.
amber colored oil. Oil
6.5 bc. HiO and tra<
Small amount of
6 cc. HiO, 15 cc.
fluorescent.
6.5 cc. HjO, 21 cc. amber colored oil. Oil
fluorescent. About 3 liters gas.
8 cc. water, 22 cc. amber colored oil. Fluores-
cent. Passed gas through bromine. No re-
9 cc. water, 25 cc. amber colored oil. About
•1 liters gu. Oil less fluorescent.
7.5 cc. water, 23.5 cc. oil. Oil amber colored
and fluorescent.
Lost distillate.
9 cc. water, 22 cc. amber colored oil. Fluores-
cent.
9.5 cc. water, 23 cc. oil darker colored and more
fluorescent.
1 1 cc. water, 22 cc. amber colored oil. Fluores-
cent. When cover was removed, mass
flashed.
11 cc. water, 22 cc. lighter colored oil. Not
quite as fluorescent.
lift v. iii her oil. Oil fluorescent.
When rover was removed, mass ignited.
11 cc. water. 22.5 CC. nmbcr colored oil.
Fluorescent When cover was removed,
mass ignited.
10.5 cc. water, 22 cc. amber colored oil oil
fluorescent '■ did not ignite when
cover r
THE JOURNAL OF INDUSTRIAL AM) ENGINEERING I HEMISTRY Vol. 10, Xo.
The data of Table V show that the yields of carva-
crol increase and become more uniform with the rise of
temperature. Also that the range for maximum uni-
form yield is from 350° to 3700 C. Schorger1 states
that the fusion temperatures should not be above
300 ° C. That this is not correct is demonstrated by
the results of these experiments. Neither could he get
uniform yields'at temperatures below 3000 C. Above
370" C. decomposition becomes noticeable and' the
yields decreased. Between 3600 C. and 370° C. the
fusion mass had a tendency to ignite when exposed
to the air. This was much more marked at higher
temperatures. A comparison of the data obtained from
this series of fusions and that of the previous one shows
plainly that it is necessary to use a covered fusion
vessel. Without a cover the fusion mass thickens, due
to reaction with oxygen of the air, and the volatile
oil which distils off is lost.
It was noted that in all of the fusions an amber
colored, fluorescent oil came off. The quantity
distilled from the different fusions was quite constant.
It varied somewhat in color and in the degree of
fluorescence with different fusions. As a rule it became
darker on standing. In some instances it became more
fluorescent, and in others less, when exposed to the air
for some time. A quantity of this oil was carefully
fractionated; 75 per cent of it boiled between 1720 C.
and 1780 C. This fraction was water- white and had
the odor and characteristics of cymene. The higher
boiling fraction varied in color from light straw to very
dark brown and was relatively small in amount. All
of the fluorescent material boiled above 210° C.
To verify the belief that the oil was principally
cymene, the fraction boiling between 172 ° C. and
1780 C. was sulfonated in the usual manner. The
sodium salt was made and fused with caustic soda.
Fifty grams of the sodium yielded 10 g. of carvacrol
and 3.5 cc. of an amber colored, fluorescent oil similar
to that described. This proved that the oil which
distilled from the cymene sulfonate was essentially
cymene. Inspection of the results of this series of
fusions shows that the cymene recovered in the distil-
late from the fusions represents a decomposition of
from 18 to 20 per cent of the sodium cymene sulfonate
fused. Experiments showed that this cymene could
be easily recovered and re-used. On a factory scale its
recovery would be profitable. The presence of sodium
sulfate in considerable quantity as one of the fusion
products along with cymene seemed to indicate that
two reactions took place between the sodium benzene
sulfonate and the caustic soda, one of which formed
sodium carvacrolate and sodium sulfite, the other
cymene and sodium sulfate. However, the evolution
of hydrogen and methane and the formation of a con-
siderable quantity of tarry matter indicated that other
reactions took place.
The gas evolved during the fusions varied in quantity
from 2 to 4.5 liters. Samples from two fusions were
analyzed and were found to contain hydrogen and
methane. There were no traces of carbon monoxide,
oxygen, or unsaturated hydrocarbons.
1 This Journal, 10 (1918), 2.S9.
: from Fusioi
(Table V)
Table VI
Hydrogen
Per cent
Methane
Per cent
20:00 J fay vo1
To get some idea of the stability of sodium cymene
sulfonate 150 g. (containing 0.57 per cent moisture)
were placed in the fusion kettle alone and heated.
Between 345° and 3500 C. it melted and showed no
signs of decomposition. The temperature was gradu-
ally raised to 375° C. and at this temperature a dis-
tillate consisting of 13V2 cc. water and 7 cc. of a dark
.oil came over during the first hour. The heating was
continued for 3 hrs. During the entire period hydrogen
sulfide came off in large quantities. The mass gradu-
ally thickened and was sticky and black when poured.
The oil from this salt was somewhat similar to that
obtained from the fusions with caustic soda except
that it was smaller in amount, very much darker in
color, and was saturated with hydrogen sulfide. The
hydrogen sulfide formed showed that the reaction
without caustic soda was not the same as that with it.
If it were, sodium sulfide would have formed during
the fusion. This, in turn, would have reacted with the
sulfuric acid in the neutralization operation and hy-
drogen sulfide would have been evolved. Such was '
not the case.
M
^~
\
V
■ k
I 1
\
\
<3
.V
\
30
5
44
:c
f
J*
^~~
xl
Appt
ox/rrn
ite-M
°an ft
JSion
-Peru
« 1
id Yield Cume.
.'
/ 2 1 ■*■ i a
Hours
Fie. 5
time required for fusion was determined by
making a number of fusions with the temperature
and the composition of the charges constant using the
quantities of carvacrol as the criteria. The results
appear in Table VII and Fig. 5.
Fusion periods of from 4 to 6 hrs. gave the best
results. With longer periods the yields gradually
fell off and were more or less erratic. The same was
true for the shorter periods. The curve in Fig. S
shows the relation between the length of fusion period
and the yield of carvacrol. The products of the
IS, 20, and 24 hr. periods were dry, granular masses
Dec, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
989
when removed from the fusion chamber. On exposure
to air they gradually became hard and stony. In the
cases of the 20 and 24 hr. fusions the products were
liquid up to within 2 hrs. of the end of the periods.
The amount of distillate was practically the same for
all of the fusions of more than 2 hrs. duration, showing
that the consistency of the products at the end of the
period was in no way related to it.
during fusion, would be experienced, thus over-balanc-
ing the advantage of the process.
Temperature, 360° C.
Table VII
150 g. sodium eymene
jlfonate, 450 g. caustic
s. G.
15.15
13.71
5 17.21
31.15
31.43
39.78
41.14
47.12
49.36
49.81
49.91
49.33
49. 14
46.31
35.41
15.41
20.01
20.10
nd of period.
Percentage
Yield of
Carvacrol
15.90
13.39
18.07
32.59
32.99
41.76
43.19
49.47
51.82
52.29
52.31
50.14
51.60
48.69
37.17
16.18
21.01
21.10
Remarks
Liquid when poured.
Liquid when poured.
Liquid when poured.
Liquid when poured.
Liquid when poured.
Liquid when poured.
Liquid when poured.
Liquid when poured.
Liquid when poured.
Liquid when poured.
Liquid when poured.
Liquid when poured.
Liquid when poured.
Liquid when poured.
Remelted after 5 hours.
Remelted after 5 hours.1
Remelted after 5 hours.1
Remelted after 5 hours.1
QUANTITY OF FUSION REAGENT REQUIRED In all
of the fusions made in the previous experiments a
large excess of caustic soda was used. To ascertain
the minimum amount required for the highest carva-
crol yields and the best working conditions, fusions
were made with different quantities. The results are
given in Table VIII and Fig. 6.
Table VIII
Temperature, 360° C. 150 g. sodium eymene £
re.
Percentage
Caustic Car- Yield
Soda vacrol Carvacrol
ilfonate. Fusion period,
49.91
48.12
48.95
48.50
49.50
18.97
00.00
52.31
50.52
51.39
50.92
51.96
19.91
00.00
Remarks
Distillate 9.5 cc. water. 23 i
Distillate 9 cc. water, 22 c
Distillate 9 cc. water, 23 cc. oil.
Distillate 11.5 cc. water, 22 cc. oil.
Distillate 1 1 cc. water, 22 cc. oil.
Distillate 7 cc. watet. 17.5 cc. oil.
Distillate 13.5 cc. water, 7.5 cc. black oil.
It is interesting to note that the quantity of the
fusion reagents could be reduced almost to the theoreti-
cal amount required without much effect upon the
carvacrol yields. With less than 100 g. the mass could
not be poured from the kettle. With smaller amounts
the products were of a pasty consistency and had to
be scraped out. It is quite necessary that the contents
of the kettle be discharged rapidly in order to prevent
excessive loss due to reactions which take place on
exposure to the air. These reactions were so rapid
that ignition took place on two occasions. This was
especially true when the fusion products were semi-
solid. The results of the fusion in which no caustic
soda was used have been discussed previously.
FUSION OF CALCIUM CYMENE SULPONATI I IS
possible to fuse calcium eymene sulfonate with caustic
alkali and obtain carvacrol. Schorger1 obtained his
highest yield by using this salt. Although one filtra-
tion and the soda ash required for the making of the
sodium salt, would be saved, more caustic wo
necessary for the fusion; and mechanical difficulties,
resulting from the insoluble calcium sulfite
' Lot. cit.
,
I
«
0
s
;■
«5i
1l
x
/
100 300
Grams Caustic Soda
Fig. 6
Two fusions using calcium eymene sulfonate were
made with the following results. The charge con-
sisted of 8o g. of caustic soda and 80 g. of calcium
eymene sulfonate. The temperature was 3600 C.
Per cent of
Carvacrol Theoretical
No. G. Yield Remarks
1 14.82 28.80 16.5 cc. of fluorescent oil and 11 cc. of water
distilled during fusion. Fusion was thick
when poured.
2 17.70 34.41 14 cc. of fluorescent oil and 13 cc. of water
came off during fusion. Fusion quite
thick when poured.
The oil which distilled from the fusion was identical
with that obtained from the fusions of the sodium
salt. Although the two fusions were made under the
same conditions, there was quite a perceptible difference
in the yield of carvacrol.
NEUTRALIZATION OF THE FUSION PRODUCTS The
fusions were poured into 2 liters of water and allowed
to dissolve. To this solution dilute sulfuric acid
(40° Be\) was added in sufficient quantity to neutralize
the excess caustic soda and fri 1 > rol from the
sodium carvacrolate. \\ <lded in
excess it reacted with the sodium sulfite formed during
the fusion, and sulfur dioxide was evolved. Mm
served as a means of determining when the neutraliza-
tion was complete. It was necessary to add i;
to the solution by leading it through a tube to the
bottom of the vessel. If this was not done an excess
of acid on the surface reacted with the sodium sulfite
in that part of the solution before neutralization
throughout <■ te. The appearance of sulfur
dioxide under such a condition was not evidence that
neutralization was complete. If the excess sulfuric
acid were recovered at the end of the sulfonation
99©
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 12
operation it could be diluted and used for this purpose.
If concentrated acid is used, the time required for
neutralization will be greatly lengthened, due to the
great amount of heat produced. If concentrated acid
is added rapidly, the heat evolved will cause foaming
and loss of much carvacrol.
separation of the carvacrol — The specific gravity
of carvacrol lies so near to that of water that it does
not separate readily from water and dilute water
solutions of salts. While some of it collects on the
surface and forms an oily layer a great deal of it stays
in the body of the solution in the form of an emulsion.
For this reason it was necessary to remove the carvacrol
either by means of a solvent or by steam distilla-
tion. When extracted by means of a solvent, one-
half liter of benzene was used. It was well shaken
with the neutyral fusion liquors until it had dissolved
all of the carvacrol. The benzene layer was then
removed by means of a separatory funnel.
The removal of the carvacrol from the fusion liquors
by steam distillation had the advantage that a con-
siderable portion of the solid and suspended tarry
matter was left behind. A great deal of this went into
the benzene layer and caused trouble when the solvent
was applied directly. The yields of ' carvacrol were
the same by both methods. It was necessary to use a
solvent to completely remove the carvacrol from the
steam distillate. The benzene was recovered in all
cases and it was found that an average of 4 per cent
was lost in the extraction and distillation. When an
excess of acid was used in neutralization a large amount
of sulfur dioxide formed was taken up by the benzene.
After the removal of the benzene the residue con-
taining the carvacrol was distilled. The carvacrol
came over in the form of a clear, light yellow oil be-
tween 2270 C. and 2450 C, leaving a tarry residue
which averaged 0.25 g. for each gram of carvacrol.
It was noted that when the yields of carvacrol were
low the quantity of tar extracted was also low. The
amount of the residue depended upon the method used
for removing the carvacrol from the fusion liquors.
When the steam distillation method was used the
quantity of tar was much smaller. If the carvacrol
is extracted directly by means of a solvent, a still with
a bottom discharge should be used for the distillation
of the extract. This would provide for the removal
of the tarry residue when it was hot. If allowed to
cool it formed a hard, brittle mass.
purifk \ n<i\ of the carvacrol — This was done by
redistilling the product obtained from the fusion
liquor by either of the two methods mentioned. No
difficulty was experienced in getting a product with a
fairly constant boiling poinl .
LARG1 SCAL] EXP1 RIMENTS
Having determined the optimum conditions for the
several operations involved in the production of
carva on a laboratory scale,
it was desirable to tesl them by using larger quantities
of materials. \ this was done with ap-
paratus of semi
sulfonaik'n Fiftj three pound urpen-
tine were treated with 114 lbs. of 66° Be. sulfuric acid
for 6 hrs. at 98 ° C. in a cast iron sulfonation kettle.
The time was longer than would have been necessary
had the kettle been equipped with a thoroughly
efficient stirring apparatus.
REMOVAL Of THE EXCESS SULFURIC ACID — Xo at-
tempt was made to recover the excess acid. The
sulfonation products were slowly poured into a 150
gal. wooden tank containing a slurry of limestone
(95 per cent passed 100 mesh). On the basis of the
spruce turpentine containing 80 per cent cymene the
calculated amount of limestone required was 95.2 lbs.
The quantity needed for complete neutralization was
102 lbs. The neutral solution was filtered with a
12 in., 12-plate Sperry press.
PRODUCTION OF SODIUM CYMENE SULFONATE To the
filtrate from the liming operation 16.5 lbs. of 58 per
cent soda ash (58 per cent Xa20) were added. The
calculated amount was 17.1 lbs. The calcium car-
bonate formed was removed by filtration and the clear
solution was evaporated in a 50 gal., steam jacketed,
open iron kettle to a thick, sticky consistency. The
salt was dried in a steam-jacketed shelf vacuum dryer
to a moisture content of 0.7 per cent.
The yield was 70.5 lbs. of dry sodium cymene sul-
fonate. The calculated yield was 74.8 lbs. In factory
practice the sodium cymene sulfonate solution should
be evaporated to saturation with a vacuum and then
finished with a film drum dryer.
fusion of the sodium salt — Forty pounds of 76 per
cent caustic soda (76 per cent Na20) were fused in a
30 in. cast iron fusion kettle heated with gas. To the
fused caustic 70.5 lbs. (calculated to dry basis) of
sodium cymene sulfonate were slowly added. The
kettle was tightly covered, the condenser connected,
and the temperature gradually raised to 350° C.
The temperature was kept between 350° and 3600 C.
during the 6 hr. fusion period. At 2700 C. the fluores-
cent oil began to distill. The rate at which it came
over increased as the temperature was raised. The
fusion went smoothly and poured readily. Less
caustic could have been used without the substance
solidifying during fusion. The salt was poured into
an iron tank containing 30 gal. of water.
neutralization of the fusion liquor — Dilute
sulfuric acid (400 Be.) was slowly added until the
fusion liquor was neutral. 67.5 lbs. of acid were re-
quired. The calculated amount was 70.32 lbs. The
operation was carried out in a steel tank.
separation 01 1111 CARVACROL- Forty-live pounds of
benzene were thoroughly agitated with the neutral
fusion liquors. The benzene solution was separated
by drawing off the water solution from below. The
benzene (43.75 lbs.) was recovered by distillation with
a steam-jacketed still. The benzene loss was 2.7 per
cent.
There being no direct heated still of sufficient size
available, 1 liter of the extract was distilled in a dis-
tilling flask. The product obtained was slightly
fluorescent and contained a little finely divided carbon
which came from the cracking of the tarry sul
Dec, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
991
Quan- Per
tity cent
Yield Recov- Re-
Per ered cov-
When redistilled a clear, yellowish oil that boiled at
232° C. was obtained. From the quantity of carva-
crol obtained the total yield was calculated. The data
and results of the large scale experiments are given in
Table IX.
Table IX — Data and Results of Large Scale Experiments
Theo-
retical
Quan-
Quan- tity
tity Re-
Materials Used quired Y
and Products Lbs. Lbs. Lbs. cent Lbs. ered
Spruce Turpentine S3 ...
Sulfuric Acid (66° Be.) 114 32.2
Limestone 102 95.2
Soda Ash 16.5 17.1
Sodium Cymene Sulfonate
Caustic Soda 40.0 23.9
Sulfuric Acid (40° Be\) 67.5 70.32
Benzene 45 ...
Fluorescent Oil (recovered for re-use)
Sp. Gr. = 0.8890 Carvacrol
Tar
DISCUSSION OF RESULTS AND OBSERVATIONS
The most favorable conditions for the various
operations as determined in the laboratory when ap-
plied on a larger scale gave similar results. With the
greater quantities of materials the conditions were more
easily controlled. This was especially true of the
fusion operation which was the most difficult one in
the process to handle. The quantity of the cymene-
bearing oil obtained from the fusion, per unit of
sodium cymene sulfonate fused, was smaller than that
obtained from laboratory experiments. From the
latter it amounted to about 20 per cent of the original
cymene used and from the former to 13.7 per cent.
The apparatus required to collect this oil is simple and
inexpensive and the quantity of the oil given off is
such as to make its recovery imperative.
When the caustic soda was fused first and the sodium
salt added afterwards, trouble was experienced with
foaming unless the salt was added very slowly. How-
ever, this procedure may be used if the cover of the
kettle is such that it can be opened and closed quickly
so as to prevent oxidation and loss of the distillate.
When the sodium salt and the caustic were well mixed
together previous to charging, no trouble with boiling
over during the fusion was experienced. The stability
of the sodium cymene sulfonate permitted this to be
done. The fusion kettle, however, should be of ample
size to take care of the temporary swelling of the fusion
mass.
When dry sodium cymene sulfonate was exposed to
the air it took up moisture rapidly and became sticky.
This property would prevent it from being stored in an
open bin.
The time required for each operation was such that
it could be completed within 8 hrs., the ordinary
working day. This would be an important factor in
plant operation.
The yield of carvacrol from the operations with the
larger quantities of materials was about 5 per cent
greater than with the quantities used in the small
scale experiments. If the cymene recovered from the
fusion operation is taken into consideration, as should
be done, the carvacrol yield will be increased. The
difference this makes is shown in the followin
The cymene content of the original spruce turpentine
and of the oil recovered was taken as 80 per cent in
each case. The cymene content of the recovered oil
was subtracted from that originally taken. From this
the theoretical yield and the percentage yields were
calculated.
Per cent
Yield Not Per cent Yield
Taking Recov- Taking Recov-
No. ered Oil into ered Oil into Increase
(Table V) Consideration Consideration Per cent
7 51.71 63.94 12.23
8 50.14 62.60 12.46
9 52.31 64.65 12.34
10 51.60 63.65 12.05
11 50.65 62.51 11.86
Large scale experiment 57.2 66.4 9.2
Carvacrol can be produced by the process outlined
with the same equipment as that used in a plant for
the manufacture of phenol or beta-naphthol, with but
few changes. A fusion kettle equipped with a close
fitting, easily opened cover and a water-cooled coil
condenser would be necessary. In addition to this a
direct heated still for the distillation of the carvacrol
would be essential. Otherwise the phenol or beta-
naphthol plant could be used as it is.
Inasmuch as practically the same plant can be used,
the cost of production of carvacrol can be compared
with that of phenol. The United States Government
has fixed the price of phenol at 38 cents per lb. This is
commonly known to give the manufacturer an average
net profit of 7 cents per lb., thus making the total
average cost 31 cents per lb. The total material cost
per pound of carvacrol produced on the basis of 60 per
cent yield would be about 35 cents per lb. The labor
and overhead costs would be higher than those of
phenol due to the lower yield obtained. The overhead
cost would also be somewhat higher on account of the
extra equipment required. The total cost per pound
of carvacrol produced would be close to 60 cents, a
cost well within the limits of commercial possibility.
SUMMARY
A process for the manufacture of carvacrol from
cymene has been outlined and studied in detail.
The process depends upon the use of spruce turpen-
tine as the source of cymene.
The optimum conditions for the necessary operations
have been determined.
Briefly stated, the process consists of:
1 — Making cymene sulfonic acid by thoroughly
agitating spruce turpentine with an equal volume of
66° Be\ sulfuric acid at a temperature of 900 to 100° C.
for 4 hrs. in a cast iron sulfonating kettle.
2 — Neutralization of the excess sulfuric acid, forma-
tion of calcium cymene sulfonate in solution by adding
ground limestone to the sulfonation products and re-
moval of the calcium sulfate formed by filtration.
3 — Formation of sodium cymene sulfonate by adding
soda ash to the hot calcium cymene sulfonate solution
and removal of the precipitated calcium carbonate by
filtration.
4 — Concentration of the sodium cymene sulfonate
solution in a vacuum evaporator to the point of satura-
tion.
5 — Precipitation and drying of the calcium cymene
sulfonate by means of a rotary steam heated film dryer,
or other suitable n
992
THE JOURNAL OF INDUSTRIAL AND ENGINEERING I HEMISTRY Vol. 10. No. 12
6 — Fusion of the dry sodium cymene sulfonate with
approximately one-half of its weight of 76 per cent
caustic soda in a cast iron or steel fusion kettle pro-
vided with a cover and water-cooled condenser at a
temperature of 3SO° to 3700 C. for 6 hrs.
7 — Pouring the fusion products into a minimum
amount of cold water and neutralization of the solu-
tion so formed by adding just enough 40 ° Be\ sulfuric
acid to neutralize the excess caustic soda and set free
the carvacrol from the sodium carvacrolate.
8 — Separation of the carvacrol from the neutral
fusion liquid by steam distillation or by agitating with
a solvent such as benzene.
9 — Recovering the solvent by distillation.
10 — Distillation of the carvacrol from the benzene
extract with a direct heated still.
n — Purification of the carvacrol by redistillation
with the same still.
This process was tested on a large scale which gave
even better results than those obtained with the smaller
quantities.
Chemical Engineering Laboratory
Columbia University
New York City
THE SEEDING METHOD OF GRAINING SUGAR
By H. E. ZlTKOWSKl1
Received June 17, 1918
There is a disposition in some quarters to deny to
the sugar industry its claim as a member of the chemical
industrial family. That the beet sugar industry, the
direct descendant of scientific research and probably
the oldest member of magnitude of the chemical
industry family, should find it necessary to establish
any claim in this direction is anomalous. Someone,
sometime, as a labor of love, will bring this out as a
matter of record.
Here I desire merely to state that nowhere else in
industry has technical accounting been carried to the
point that it has in the beet sugar industry. The
beet sugar industry has taken laboratory manipulations
or processes such as dialysis or diffusion, precipitation,
filtration, evaporation, and crystallization and adopted
them to factory scale, handling millions of pounds of
material daily, and with a refinement which taxes the
ingenuity of the most expert manipulator to now
duplicate on a laboratory scale.
It is even held that the beet sugar industry, which
established itself in Europe during the Napoleonic
wars, deserves to a very large degree the credit for the
rapid development of the chemical industry of Ger-
many. It was the beet sugar industry which fur-
nished the technically trained and experienced men,
capable of transferring laboratory reactions and pro-
cesses to a factory scale and keep the commercial
requirements in mind, when the modern chemical
industry sprang into being.
Men go so far as to state that it was the beet sugar
industry of Germany which made possible the terrible
war that Germany is waging, not only because it was
the foundation stone for the chemical industry but
also because the cultivation of the beet brought with
1 Paper rend before the American Institute of Chemical Engineers,
Berlin, N. H.. June 19, 1918.
it scientific agriculture which doubled the agricultural
yields, thereby making Germany largely self-sustain-
ing and eliminating the threat of being starved to
submission by blockade. There is much that can
be said in defense of such a view-point.
However, at this time here it is desired to discuss
briefly the large scale practical application of the well
known "seeding" method of inducing crystallization.
The oldest, and for many years the only method of
producing sugar crystals was to concentrate the
properly purified sugar-bearing syrups to the required
density or supersaturation and set them away. In the
course of days, or weeks, or even months, as the solu-
tion cooled, sugar would crystallize out. Even after
the introduction of the vacuum pan method of "boil-
ing" sugar, for many years this was the only method
and was known as "boiling blanks." Sometime
during the fifties of the last century the art or rather
the "trick of the trade" of "graining" sugar while yet
in the vacuum pan was acquired, though this was not
generally adopted till 20 years later, and even up to
this day frequently, for reasons which need not be
discussed here, blanks ar^ boiled. The general pro-
cedure at present is as follows:
A quantity of the properly prepared sugar-bearing
syrup with a water content of from 30 to 40 per cent
is introduced into a vacuum evaporator or "pan"
and is concentrated till saturated. At this point the
boiling mass will be at a temperature from 700 to
8o° C., and under a vacuum of from 20 to 25 in.
Under certain conditions aqueous sugar solutions
have the property of forming supersaturated solutions
and in the presence of the non-sugars or impurities,
such as occur even in purified juices, this tendency is
greatly increased, so that in factory practice it is al-
ways necessary to carry the concentration to some
degree of supersaturation before crystallization occurs.
Now it is not to be inferred that in all cases simple
supersaturation will bring about crystallization, for,
if the content of non-sugars or impurities in the solu-
tion is great enough, crystallization will not occur
even though evaporation be carried to the point of
dryness.
Under the normal conditions of sugar manufacture,
however, that degree of supersaturation is finally
reached at which crystal formation begins. Sometimes
a sudden shock applied to the boiling, supersaturated
mass is resorted to in order to induce crystallization,
such as a sudden raising of the vacuum bringing with
it violent ebullition, or the introduction of a hot
syrup of a lower density which has the same effect, or
the injection of steam or air into the mass. Xo matter
how produced, at the moment of their formation the
crystals are infinitely small and some time is required
to attain a visible size, though this may be only a few
moments. Eventually the crystals formed do become
visible and then the critical moment of the "boiling"
of the "pan" arrives.
It becomes the attendant's business to allow the
formation of crystals to proceed till, in his judgment,
the proper number of nuclei for the apparatus in ques-
Dec, io i S
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
tion have formed, then to arrest the formation of
further crystals by lowering the supersaturation
coefficient, which is done by lowering the vacuum,
raising the temperature and diluting with syrup of a
lower density. From then on it becomes his business
so to regulate the temperature, the rate of evapora-
tion, and the introduction of syrup that the minute
crystals will grow, and, when the pan is full, be of
the size to supply the market's demand.
Not much time for deliberation is available when it'
is realized that often a pan holding 200,000 lbs. of
mass and yielding 80,000 lbs. of granulated sugar is
boiled complete in less than 2 hours. If the operator's
judgment at the time of "graining" is at fault, and he
allows the formation of too many crystals, the final
product will be too small, may cause great difficulties
in separation from the mother liquor and decrease the
yield; if the number of crystals formed is too small
the resulting end-product will be too large, the time for
crystallization will be longer, and again the yield will
be reduced. In both instances the cost of production
is increased.
But even at best the crystal formation at the time of
graining is not instantaneous, and by the time that
some have reached a visible size others are at the
point of formation, therefore infinitely small, with the
result that the final end-product is not uniform in
size. This is objectionable, not only on economical
ground, as the difficulty of separating the sugar crystals
from the adhering mother liquor is greatly increased
by uneven grains, but also a fastidious consuming public
demands not only a pure, white, sparkling crystal of a
certain size (varying somewhat in different parts of the
country) but the crystals must also be fairly uniform
in size.
The above points out briefly some of the problems
in connection with producing the "granulated" crystals
usually found on our markets. Not all of the sugar
produced is, however, so directly obtained as granu-
lated. Much of the final output is first obtained as a
"raw" or impure sugar, which is melted, reprocessed
and recrystallized. The liquors from which these
raws are obtained are of a lower purity and therefore
present greater difficulty to crystal formation or
"graining." The impurities present, however, must
not be above a certain ratio to the sugar present or
crystallization in the pan will be entirely prevented
and the mass will be blank, or if crystals form they will
remain so small as to be separated from the surround-
ing mother liquor only with great difficulty, if at all.
Eventually a final liquor, molasses, remains, which
in beet sugar manufacture may contain 50 per cent
of sucrose but also sufficient of impurities to prevent
further crystallization. Any procedure, therefore,
which increases the quantity of sugar recoverable by
direct crystallization, or which increases the yield with
each crystallization, or reduces the time elemetr
even merely simplifies the procedure, may be very
valuable. The saving may amount to only one
hundredth of a cent per pound of sugar, and yet,
on the quantity of sugar produced, run into astonish-
ing totals.
A very valuable recent development in the art of
boiling sugar is the "seeding" of the saturated mass
in the vacuum pan with sugar dust to serve as nuclei
for the sugar crystals, instead of the method above
described of bringing about spontaneous crystal
formation or "graining" by high supersaturation.
Considering the simplicity of the use of sugar dust for
this purpose and that it can be used without an expense
or alteration of any kind in the equipment, this method
is likely to prove to be one of the most valuable de-
velopments introduced into the industry in recent
years.
While the method of "seeding" herein considered is a
recent development, yet the principle underlying it is
not at all new.
In U. S. Patent No. 489,879 dated January 10,
1893, covering a Process of Obtaining Sugar, is found
the following:
"It has, however, long been known that if such-
impure solutions are brought in contact with a suffi-
ciently large number of crystals, a very effective
crystallization can be brought about in the vacuum
pan; and this knowledge has been made practical
use of in sugar factories by the addition of raw sugar
crystals to juices which could otherwise only be boiled
with great difficulty. Similarly it is sometimes
customary in sugar refineries, when very small crystals
are desired, to bring the liquor to the crystallization
point, and then by the introduction of a quantity of
finely pulverized sugar to start energetic crystalliza-
tion, thus insuring the formation of small crystals by
shortening the time of boiling and consequently that
given to the crystals in which to grow."
Similar references to "seeding" sugar can be found
at even earlier dates, and yet it appears very doubtful
that this method was ever successfully used in pro-
ducing marketable sugar until less than two years
ago.
To Mr. John C. Bourne, now somewhere with the
Canadian forces, belongs the credit of having called
attention to this subject, which led to the present
development. Mr. Bourne was not familiar with the
literature on the subject and was not aware that the
idea had ever been suggested — to him it was entirely
new.
The method as at present used very successfully, is
as follows:
The sugar-bearing syrup properly prepared is intro-
duced into the vacuum pans and under the usual
conditions of vacuum and temperature is concentrated
till the point of saturation has been passed, that is,
till the solution is slightly supersaturated or, in the
language of the industry, till it reaches a light "string
proof." At this point a quantity of sugar dust or
powdered sugar, varying from Vi qt- to 2 qts. for
each 1000 cu. ft. of vacuum pan capacity, is intro-
duced by aspiration, through suitable connection,
beneath the surface of the boiling mass, care being
taken to prevent the inrush of any considerable
quantity of air, as otherwise a portion of the sugar
dust introduced is likely to rush up with the air and on
This operation requires not more
994
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10 -No
than half a minute. One or two minutes are re-
quired for the sugar particles introduced to mix
through the boiling mass. For several minutes after
the introduction or "seeding" the usual "proof"
appears blank or at best simply shows a cloud, the
sugar particles introduced being too small to be visible
to the naked eye.
The solution, however, is supersaturated and is
boiling vigorously and the crystals or fragments of
crystals introduced immediately begin to grow and
soon show up on the "proof." Evaporation is con-
tinued till about that density is reached usually ob-
tained by the older methods of "graining." From here
on the procedure is as usual except that experience
has shown that less difficulty will be experienced to
keep out false grain or "smear" in a "seeded" pan
than one "grained" by the older method.
The essential difference between the two methods
is that in the one case the crystallizing nuclei are intro-
duced ready made, in the other are formed spontane-
ously by highly supersaturating the liquor which
carries with it certain objectionable features as pre-
viously pointed out.
The quantity of sugar dust to be used per unit
volume of pan capacity is dependent on the size of the
dust particles and on the size of crystals required in
the finished product.
In the writer's experience the "seed" used was such
sugar dust as accumulates in the usual dust collectors
of the sugar drying equipment. In size the dust
particles ranged from an impalpably fine powder to
particles just passing through a standard Tyler sieve
of ioo mesh. Particles larger than this were screened
out. In some instances powdered sugar as found on
the market was used with success.
As a great difference in size or volume exists be-
tween particles or crystals just passing through a ioo-
mesh sieve and particles impalpably fine, it was con-
sidered that perhaps superior results would be ob-
tained if the dust or "seed" used was more uniform
in size. With this thought in mind trials were made
with dust from which both the coarser and finer
materials had been removed; improved results were
obtained only if the seed did not contain too many
particles larger than So mesh.
While at the time of seeding a vast difference in
size and weight exists between a powder particle and a
particle of ioo mesh, when these nuclei have reached
the market size little difference exists. In all prob-
ability the rate at which the crystallizing sugar de-
posits on the nuclei is in direct proportion to their
surface areas. The surface area of an impalpably
fine particle in proportion to its volume is so im-
mensely greater than that of a particle of ioo mesh
that as the two particles grow, the smaller growing at a
relatively faster rate than the larger, the difference
in size will become negligible.
Then, also, possibly the tendency of crystal splinters
to regenerate the original shape of the crystals from
which they have been produced may play a role, as
the finer particles especially are largely crystal splinters.
io,
This describes briefly the new method of "graining"
sugars in the vacuum pans as practiced for the first
time during the past campaign in a dozen or more beet
sugar factories of the Western States. It deserves
further study before all the factors are determined.
However, the results obtained during the past cam-
paign in the factories coming under the writer's ob-
servation, especially on the lower products, were
uniformly superior to the normal results.
Rocky Ford, Colorado
A STUDY OF SOURCES OF ERROR INCIDENT TO THE
LINDO-GLADDING METHOD FOR
DETERMINING POTASH
By T. E. Keitt and H. E. Shiver
Received June 19, 1918
Prior to our study1 of the DeRoode method for the
determination of potash in fertilizer materials, much
data had been accumulated in this laboratory rela-
tive to sources of error incident to the Lindo-Gladding
method for determining potash. In the interest of
furthering the adoption of the modified DeRoode
method we deem it advisable to present the results
of these studies. In fact, the work on the DeRoode
method was undertaken, primarily, because of the
inaccuracies of the Lindo-Gladding method.
The determination of water-soluble potash in all
samples reported in Table I was done by the official
Lindo-Gladding method.2 Another set of determina-
tions was made exactly as outlined under the modified
official method.3 Still another set of determinations
was made on these samples by the modified official
method,4 except that hydrochloric acid was not added
to the filtrate nor was the ammonia and ammonium
oxalate added after the solution had been made to
volume and an aliquot of ioo cc. (equivalent to one
gram) had been taken.
This was done in order that the ammonia precipi-
tate and the lime might be separately estimated. The
aliquots were brought to boiling and ammonia was
added until alkaline, the boiling continued a few min-
utes to expel any considerable excess of ammonia,
then the precipitate was separated by filtering hot
and washing with hot water. The combined filtrate
and washings from each determination was then
evaporated to a volume of about 200 cc, made alka-
line with ammonia, and precipitated with ammonium
oxalate; the calcium oxalate precipitate was filtered
after standing over night, and thoroughly washed
with hot water. The combined filtrate and washings
from each of these precipitations was then used for
the determination of potash. In evaporating these
filtrates, as well as all other large filtrates that have
much salts of ammonia present, there is a decided
tendency to crawl. This can be controlled by acidi-
fying with 1 : 1 sulfuric acid, and filling the dishes
only to within a quarter of an inch of the top. The
volatilization of the ammonium salts was also accom-
1 This Journal. 10 (191S). 219.
' A. O. A. C, U. S. Dept. of Art.. Bureau of Chem., Bull. 107 re-
l Pept. of AKr., l!u
' Ibid
o( Chemistry, Bull. 16*.
Dec, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
995
panied with difficulties on account of the large amount
of residue and the danger of spurting. After we began
adding the sulfuric acid before evaporation was com-
plete, this trouble was greatly lessened.
J3 ' "0 J3T3 «
01 O 0 "SUB
•B*° 6*°
4
s
a tci3
5 a "B
5 4i"=
0
Pota
Li nd
[ Meth
Pota
Modifi
Gladdi
0 >.£^,
2 „
°"3
1 32
^0'
ill*
z
s
03
Per cent
(KjO).
Gladding
Per cent
(KsO),
Lindo -
Method
P
B 'S-g
HIS
5 '=. S IB
Difference
Modified
Gladding
vised
Method
1214
3.89 4.04
4.00
0.77
0.13
—0.15
—0.11
0.04
1216
2.63 2.60
2.60
1.05
0.34
0.03
0.03
0.00
1218
1.69 1.62
1.71
1.55
0.95
0.07
0.07
—0.09
1220
4.16 4.30
4.55
2.43
0.15
— 0.14
— 0.39
—0.25
Table I shows that in comparing three methods for
determining water-soluble potash, the essential fea-
ture of difference in the methods being the bulk and
method of handling of the ammonia precipitate and
the lime, the only large difference in results is
correlated with the amount of ammonia precipitate,
which consists mainly of hydrates of iron and of
aluminum. These hydrates constitute a bulky, sticky,
gelatinous precipitate, the influence of which will be
proved later.
From the data already outlined, we were led to be-
lieve that some of the potash is occluded by the bulky
precipitate formed on the addition of ammonia and
ammonium oxalate. To test this point we procured
ten samples that had been found deficient in potash
by the Fertilizer Control.
The method of procedure was as follows: 10 grams
of each sample were boiled with 300 cc. of distilled
water for 30 min., then filtered into a 500 cc. volu-
metric flask to separate from the insoluble material.
The residue was washed with hot water, and the com-
bined filtrate and washings, about 350 cc, were brought
to boiling, and ammonia and ammonium oxalate
added as directed for the Lindo-Gladding method.1
The solutions were cooled, made to a volume of 500
cc, and filtered rapidly by means of a suction pump
to separate the ammonia and ammonium oxalate
precipitate, the nitrate being used for the determina-
tion of potash.
Table II — Volume of Filtrate, Amount op Potash Recovered in
Filtrate, Amount of Potash Washed Out of Residue, Total
Potash Determined, and the Effect of Dilution before Pre-
cipitation on Potash Content
Modified
Official
Methods
,
.a s
JS V
- J V U
- u —
i-S- i
2
3 a
nJZ
alga
w - B 3
2.BU
|3QI
0
£ 'z
^0
£31
J5>
"•= ■
o*b u 0
Um
"*Z 0
z
1
<
0°
is
o*~
>
-
ioi
Per cent
Calc.onI
Between
and 500
-
Per cent
(K.O)
before
tation
Per cent
Soluble
(KjO)
luted bi
cipitati
38
478
3.15
0.13
2.95
3.28
3.13
3.05
160
463
2.71
0.18
2 . 69
2.89
2.72
2.64
547
48*
5.98
0.24
5.92
5.91
850
478
2.68
0.17
3.86
2.71
2.72
1229
475
2.93
0.29
5.80
3.22
2.84
2.76
1387
470
1.87
1.85
1 .82
1389
4X1
3.13
3 . 1 5
3.06
1991
Ml
3.04
2.74
2.68
2170
465
3.05
V 12
2473
482
4.09
4.28
4.16
which has already been discussed in detail. In mak-
ing these determinations, two aliquots were taken
from each flask, one of which was precipitated with
ammonia and ammonium oxalate in the volume of
the aliquot, 100 cc, while the other was diluted be-
fore precipitation. All were filtered and thoroughly
washed, potash being determined in the combined
filtrate and washings in each case.
Table III clearly brings out the compensation
effects of decreased volume and of occluded pot-
ash. It also shows the relation of the volume in
which the precipitation with ammonia and ammonium
oxalate takes place, to the occlusion of potash.
The ammonia and ammonium oxalate precipitates
on the filters which had been thoroughly washed
to remove potash, were each placed in a soil digestion
flask with 100 cc. hydrochloric acid (sp. gr. 1.115) and
digested at the temperature of boiling water until
solution was complete. The solutions were trans-
ferred to 500 cc. flasks, cooled, and made to volume.
An aliquot was taken, diluted to 400 cc, reprecipi-
tated, brought to boiling, and filtered. This opera-
tion was repeated twice, making three precipitations
in all. The potash from each precipitation was de-
termined separately, in order that we might determine
when the separation was nearing completion. The
results were so surprising that we had all of the work
duplicated. Due to the large amount of work en-
tailed, we used only five samples.
Table II!
— Occlusion
of Potash in
Addition
->f Ammonia ani
Ammonium Oxalate
Per cent Potash (K2O)
~ 5
j -
— ■4
-i*B w"
— 0 0
in Three Reprecipi-
-a E
= a
*o"o
i'i i_
tations of
the Am-
Ammo-
lS
"3*?
li a
<i fa's .,
.n-BH
Jo-'o
n Oxalate Pre-
u-=
cipitate. in
Volume.
400 cc.
^!l
- - :
z
a
1'^
C S E
B<\§l
s
B
£
t - 'r~
£X2<
SjSfl
Sjiu
33S0
w
<
<
<
-
6.
P.
ft
ft
58
0.91
0.89
0.90
3.28
4.18
3.15
3.99
0.84
160
0.59
0.61
0.60
2.89
3.49
2.71
3.23
0.52
547
0.67
0 . 62
0.65
6.22
6.87
5.98
6.64
0.66
850
0.58
0.64
0.61
2.85
3.46
2.68
3.31
0.63
1229
0.64
0.74
0.69
3 . 22
3.91
3.10
3.71
0.61
Other determination! '» were
made by thi i odified Lindo Gladding •■
Table III shows that in each case more than 0.5
per cent of potash was occluded by the ammonia and
ammonium oxalate precipitate, showing that there
are grounds for the manipulators' contention that the
Lindo-Gladding method of analysis does not account
for all of the potash added in the water-soluble form.
It further shows thai the Lindo-Gladding method
does not account for all • h soluble in water
at the time of the analysis.
To secure additional information regarding the
errors due to the occlusion of potasb and diminution
in \ olume incii 0 the Lindo- ( iladding 1 u
pure salt, solutions were prepared as follows:
Solution 1 contained potassium chloride and ferric sulfate
equivalent to 5.99 per cent K:<> and IO.31 per cent FeiOj.
Solution 2 contained potassium chloride and triealciinii phos
phate equivalent to 3 99 percent ECaOand 10 per cent Caj(PO«)2.
Solution 1 emit. mik-i I potatthun eliloridc, iron, and tricalcium
• alent to 5 .99 per cent KjO, 10.31 |
FesOi, an t Ca»(P0
996 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 12
Tadle IV — Errors Due to Diminished Volume and to Occluded Potash when Pure Salts Are Used
g I 1 1M ©I °i o|2 ©Is °ii 1" 11a HI 1! O o£tt
S-o „ - .? |o.S W-2 MS~ M4.& Mia t?ia 35 £ g| g g-s ? "= h3-e
*= i s 5 ^ ^ 1*1 i-sl «g S-S "I -Ji *.s| ^ i
■j t ° ° *ji 11 ii< m m w si-Es^s h h
3S E E S O -o »•< "££ c- g 0 t. g eg B -c.2 - : < 0 ■a5<j -: -- --■=
Is III tfffia 5i sfjJ tftatftapb g$g*»3 - glgjlS
Cc. Cc. Cc. Gram Gram Gram Gram Gram Gram Gram Gram Gram Gram Gram Gram
25 cc. KC1 500 500 50 0.0304 0.0304 0.0304 0.0304 0.0311 0.07 0.07
50 cc. KC1 500 500 50 0.0611 0.0611 0.0611 0.0611 0.0621 0.10 0.10
25 cc. KC1, 25 cc. FeCU 500 485 50 0.0279 0.0288 0.0006 0.0002 0.0001 0.0004 0.0285 0.0007 0.0292 0.0311 0.19 0.26
25 cc.'KCl, 50.ee. FeCU 500 475 50 0.0537 0.0565 0.0020 0.0009 0.0001 0.0007 0.0557 0.0017 0.0574 0.0621 0.47 0.64
25 cc. KCI, 50 cc. Cai(PO.)j.... 500 478 50 0.0279 0.0292 0.0009 0.0006 0.0002 0.0004 0.0288 0.0012 0.0300 0.0311 0.11 0.23
50 cc. KC1, 100 cc. Ca,(PO.)!... 500 475 50 0.0549 0.0578 0.0022 0.0008 0.0003 0.0005 0.0571 0.0016 0.0587 0.0621 0.34 0.50
25 cc. KC1, 50 cc. Cai(PO<)>, 25
cc. FeClj 500 475 50 0.0263 0.0277 0.0006 0.0019 0 0003 0.0005 0.0269 0.0027 0.0296 0.0311 0.15 0.42
50 cc. KC1, 100 cc. Caj(P04)2,
50 cc. FeCli 500 468 50 0.0521 0.0557 0.0006 0.0008 0.0002 0.0005 0.1529 0.0015 0.0544 0.0621 0.77 0.92
Solution 4 contained potassium chloride, iron, tricalcium ing, and determining potash in the filtrates and wash-
phosphate, and aluminum sulfate equivalent to s .99 per cent ings.
K20, 10.31 per cent Fe20,, 10 per cent Ca3(P04)2, and 10 per The use of pure salts for mak;ng known strength
cent Al2Oa. solutions shows that both iron and calcium phosphate,
These solutions were intentionally exaggerated as when precipitated with ammonia, occlude potash,
to content of impurities and were analyzed in the and that a combination of the two is even more effec-
same manner as already described for the mixed fer- tive in producing occlusion.
tilizers. The determinations shown are the first Laboratory of the South Carolina
and only results obtained, emphasizing the ease and Experiment station
J . . Clemson College, S. C.
accuracy of the method of determination.
Table IV shows that the precipitate formed by the
addition of ammonia and ammonium oxalate in the DETERMINATION OF THE VALUE OF AGRICULTURAL
flask considerably diminishes the volume when tri- LIME
calcium phosphate, ferric hydroxide, or a combina- B? s- D- Conner
tion of the two are present. It further shows that Received May 23, 191 8
some of the retained potash may be washed out with Three analytical methods are commonly used for
hot water, but that a considerable amount cannot be determining the value of agricultural limes and lime-
removed in this manner. Three successive repre- stones.
cipitations in large volumes, dissolving the precipi- 1— The making of an analysis and calculating the
tate each time in hydrochloric acid and reprecipitating value of the material from the percentages of calcium
with ammonia, show a small amount of potash re- and magnesium found.
covered. In the case of the potash, a larger amount was 2— The determination of carbon dioxide and calculat-
recovered in the third reprecipitation than in the sec- inS the value oi the limestone from this alone. Quite
ond, indicating that a continuation of these repre- a number of devices have been introduced in late
cipitations might have shown a greater recovery. A years to make it possible to carry out this estimation
comparison of the theoretical potash content with quickly and easily.
the amount determined shows slightly more occlusion 3— The determination of the acid-neutralizing power
by the amount of iron used than by the tricalcium of the material by digesting in a slight excess of stand-
phosphate, although the latter showed marked proper- ard acid, then titrating the excess acid with standard
ties in this respect; a combination of the two in- alkali. The titration method has been used during
creases the occlusion. t^ie Past ^ve years on many samples of limestone,
burned lime, hydrated lime, gas lime, marl, shells,
conclusions various by-products from beet sugar factories, acetylene
This work proves that there are two sources of generators, refuse from water-softening plants, etc. It
error in the Lindo-Gladding method for determining has in all cases been found very accurate and rapid,
potash: (1) the volume of the solution is decreased „.„.„.,.,«„ „^^„„^
f , . ,, . . . . , .... TITRATION METHOD
by the bulk of the precipitate formed on addition ot
ammonia and ammonium oxalate, which makes a plus The procedure used by the author follows:
error, and (2) the potash in solution is decreased by Pulverize a sample of the stone in an iron mortar until it
occlusion of potash by the heavy gelatinous precipi- feels free from grit. Weigh out exactly one gram and place
tate formed. These two sources of error are partially il in a -i° cc- beaker- cover with a watch Slass and introduce,
compensating at tlle llp' Wltll0ut removing the cover, 6 cc. of 4 A hydro-
chloric acid. When the effervescence nearly ceases add 75 cc.
hi. impossible to wash out with hot water the pot- tlistillod water and boU gently iu the covered beaker for 10 or
ash occluded within the precipitate. ,5 mnl ._ -m „hich time the reaction is completed and the carbon
The occluded potash may be separated to a certain dioxide driven off. Cool and titrate to faint pink with N/2
extent by repeatedly dissolving the precipitate in sodium hydroxide, using phenolphthalein as indicator,
hydrochloric acid, diluting to a large volume, precipi- The results are calculated to the equivalent of
tating with ammonia and ammonium oxalate, filter- calcium carbonate and the acid-neutralizing power
Dec, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
of the limestone is reported in terms of per cent of
calcium carbonate. With pure calcium carbonate
at one hundred, some magnesites and dolomites
will show a calcium carbonate equivalent of over one
hundred.
precautions to be observed — It is best to cool the
solution before titrating, as phenolphthalein is more
sensitive in the cold and also because some limestones
contain enough soluble iron to destroy the indicator.
This destructive action is very much greater in a hot
solution than it is in a cold one. Solutions which
give much ferrous hydroxide on neutralization should
be titrated slowly and with the addition of new portions
of indicator when nearing the end-point.
With materials high in magnesium, such as mag-
nesite, it is advisable to titrate slowly, as the color
change of the indicator is slow. If the end-point is
passed the solution can be titrated back with a standard
acid.
By running a blank determination on the acid it
will be found that boiling does not cause appreciable
loss of acid and does not materially affect the de-
termination.
pot tests
Pot tests on two types of acid soil with several
calcium and magnesium stones have been conducted.
The crops grown were wheat and red clover. Each
treatment was conducted in duplicate in paraffined
galvanized iron pots 9V4 in. in diameter and 11 in.
deep. The pots were subwatered by means of a tube
connected to an arch at the bottom of the pot.
Both the wheat and clover were sown February 27,
1917. After germination the seedlings were thinned
so that only three plants of wheat and three of clover
were left per pot. The pots were weighed at regular
intervals and kept at one-half the water holding
capacity of the soils throughout the experiment. The
wheat was harvested September 1, 191 7, and the
clover January 15, 1918.
Fig. 1— Pot Tests with Wheat and Clover on Acjd Black Sandy
Son. Treated with Various Minerals. See Table II
Two radically different types of acid soils were used
in the tests. Soil W is a peaty sand high in organic
matter, containing 5.72 Per cent ammonia-soluble
humus before extracting with dilute HC1 and 4.96
per cent humus after extracting with acid. Soil D
is a yellow silty clay very low in organic matter,
containing 0.73 per cent humus before and 0.70 per
cent humus after extraction with acid. These soils
were selected because Soil W represents a type pre-
dominating in organic acidity and Soil D represents a
typical inorganic acid soil with very little organic
acidity. In view of the fact that the results obtained
on the two types of soil agree very closely it seems
logical to conclude that like results would be obtained
on other soMs of an equal degree of acidity. Both
soils used are very acid and it is quite probable that
somewhat different relative results would be obtained
if similar tests were conducted with soils of slight or
medium acidity.
Fie 2— Pot Tests with Wheat
Clay Soil Treated with Va
Minerals. See Table II
In addition to pure cleavable calcite (calcium car-
bonate) the following high-grade minerals, pulverized
to pass a one-half millimeter sieve, were used to test
their values in neutralizing soil acidity and increasing
crop growth: Wollastonite (calcium silicate), raw
rock phosphate (commercial), gypsum (calcium sul-
fate), dolomite (calcium magnesium carbonate), mag-
nesite (magnesium carbonate), enstatite (magnesium
silicate), serpentine (magnesium silicate).
The comparative test of the different minerals was
made in addition to a basic application of nitrogen,
phosphate, and potash fertilizer. This basic fertilizer
was applied at the following rates per million pounds
soil: 91 lbs. ammonium nitrate, one-third applied
at the start and the remainder at intervals of two
months; 73 lbs. di-ammonium phosphate all a1 the
start; 100 lbs. di-potassium phosphate all at the start.
The basic fertilizer was prepared from neutral chemi-
cals of the highest purity free from calcium oi
nesium. It is approximately equivalent to a field
application of 1000 lbs. per acre of a formula con-
taining 6 per cent N, 8 per cent P2O5.. and 8 per cent
K2O. All treatments were thoroughly mixed with the
proper weight of soil before the pots were filled. At
I of the experiment soil samples from each pot
were taken the full depth of the pots by means of a soil
tube and tested for acidity.
Table I shows the CaO, MgO, and CO2 in the minerals
used, also the calculated calcium carbonate equivalent
as determined by three methods.
998
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 12-
th
formula
Calcite CaCOi
Wollastonite CaSiO
Rock Phosphate Ca PO
Gypsum CaSOi !HjO
Dolomite CaMg(COj)i
Magnesite Mg( ' »
Enstatite M
Serpentine MgtSiiOT.2HiO
e t— A-NAI.Y
i — Per cent
CaO
sis of Minerals 1 rd
Soluble in Dildtb HC1 — .
MgO CO:
By CaO and
MgO By CO.
By Titration
Per cent
Per cent
Per cent
Per cen
Per cent
Per cent
38.65
0.10
43.65
100.1
99.2
99.5
0.12
0.13
68.8
0.3
68.6
25.65
0.20
1.20
46.3
12.3
.53.25
0.22
0.22
59.3
0.5
0.0
30.40
20.50
47.04
105.6
. 106.9
106.0
0.12
46.20
51.00
115.6
115.9
116.2
0.08
0.28
0.16
0.8
0.4
0.3
0.05
19. 11
0.25
47.9
0.6
45.4
Table II — Sun. Acidity a*id Crop Returns with Dipferknt Treatments in Pot Test
Acidity of Soil after Cropping* Average Yields Pbr Pot
Wanatah soil Dupont soil Wanatah soil Dupont soil
Pot H» }' H J Wheat Clover Wheat Clover
No. Treatment1 Lbs. Lbs. Lbs. Lbs. Grams Grams Grams Grams
1 None 1800 6750 2460 4000 0.5 0.0 0.7 0.0
2 Calcite 80 3500 20 750 17.0 9.5 10.5 11.0
3 No Mineral IN P K) 171.0 6750 2800 412S 1.5 3.5 44.0 2.0
4 'A Calcite (NPE 520 4500 400 1750 27.5 8.0 54.5 12.5
5 Calcite (N P K i 411 1000 20 750 35.0 12.5 65.5 18.5
6 Wollastonite (N P K) 180 3250 260 1625 33.5 S.5 65.5 3.0
7 Rock Phosphate IX P K) 1160 5250 1780 3500 18.5 54.5
8 Gypsum (N P K) 1420 5500 1980 3500 1.5 0.5 50.5 0.5
9 Dolomite (N P K ) 80 2750 40 750 35.0 11.5 62.5 20.0
10 Magnesite INPK) 60 2500 20 625 34.0 8.5 64.0 16.0
11 Enstatite INPK) 1780 6000 2260 3500 3.5 3.0 49.5 2.0
12 Serpentine (XPKi 1160 5250 1700 2750 21.5 8.5 54.5 3.0
I (N P K) = 91 lbs. ammonium nitrate. 73 lbs. di-ammonium phosphate, and 100 lbs. di-potassium phosphate per million pounds soil. All minerals were
used at rate of 2 tons per million pounds soil, except Pot 4 which had one-half quantity of calcite.
J All acidity figures are in terms of CaCOs requirement per million pounds soil.
' H = By Hopkins potassium nitrate method, U. S. Dept. Agr., Bur. of Chem., Bull. 107 (revised). J = C. H. Jones calcium acetate method, Proc.
Off. Agr. Chem., 1914.
Table III — Soil Acidity Decreases and Crop Increases by Treatments and Soils
Decrease in Acidity per 1,000.000 Lbs. Soil -■ Average Crop Increases per Pot
Treatment Wanatah soil Dupont soil Average soils Wanatah soil Dupont soil Average soils Wheat and
Pot in addition Hi Ji H J H J Wheat Clover Wheat Clover Wheat Clover Clover
No. to N P K Lbs. Lbs. Lbs. Lbs. Lbs. Lbs. Grams Grams Grams Grams Grams Grams Grams
4 Vi Calcite 1240 2250 2400 2375 1320 2312 26.0 4.5 10.5 10.5 18.2 7.5 25.7
5 Calcite 1720 3750 2780 3375 2250 3562 33.5 9.0 21.5 16.5 27.5 12.7 40.2
6 Wollastonite 1580 3500 2540 2500 2060 3000 32.0 5.0 21.0 1.0 26.5 3.0 29.5
7 Rock Phosphate 600 1 sun 1020 625 810 1062 17.0 5.0 10.5 6.0 13.7 5.5 19.2
8 Gypsum 340 1250 820 625 580 937 0.0 —3.0 6.5 — 1.5 3.2 —2.2 1.0
9 Dolomite 1680 4000 2760 3375 2220 3687 33.5 8.0 18.5 18.0 26.0 13.0 39.0
10 Magnesite 1700 4250 2780 3500 2240 3875 32.5 5.0 20.0 14.0 26.2 9.5
II Enstatite — 20 750 540 625 260 687 2.0 — 0.5 5.5 0.0 3.7 —0.2 3.5
12 Serpentine 600 1500 1100 1375 850 1437 20.0 5.0 10.5 1.0 15.2 3.0 18.2
» H = Hopkins potassium nitrate method. J = C. H. Jones calcium acetate method.
Table II gives the arrangement and treatment of tralizing power of the minerals used, as determined by
the pots, together with the soil acidities found at the titration, correlates with the crop increases and acidity
end of the test, also the yields in grams of air-dry wheat decreases except in two cases. The high crop yield in
(grain and straw) and of clover hay. The widely the case of the rock phosphate may be partly due to a
divergent figures obtained in determining the acidity phosphate action in addition to that of the neutralizing
of the two soils with the various treatments illustrates value of the calcium. The relatively lower crop in-
the fact that the acidity of Soil W is largely organic in crease with magnesite is probably due to the fact that
nature while the acidity of Soil D is almost all in- magnesia has an injurious action under certain condi-
organic. The results obtained with the potassium tions.
nitrate method are not affected to any great degree by When calcium and magnesium were determined by-
organic acidity, while the results obtained with the means of dilute hydrochloric acid the calculated
calcium acetate method are very largely affected by CaCOs equivalent is a good indicator of the value oi
organic acidity.1 , carbonates and silicates of either calcium or mag-
Figs, i and 2 show the appearance of the wheat and nesium and of raw rock phosphate. This method
clover crops on each soil series just before harvesting, fails entirely in the case of calcium sulfate. It should
Table III gives the relative decreases in soil acidity be noted here that if an analysis of the total calcium
for each treatment as shown by the Hopkins potas- and magnesium is made, by fusion or otherwise, the
sium nitrate method and by the C. H. Jones calcium results obtained for enstatite or other more or less
acetate method. The relative crop increases over the insoluble silicates will be too high.
basic fertilizer treatment, as well as the average wheat The results obtained by means of the CO; method
increases, the average clover increases, and the total are in accordance with the crop results only in the case
increases of wheat and clover, are shown for each of the carbonates and gypsum. This method fails
treatment. entirely with silicates and raw rock phosphate. It
Fig- 3 gives the calcium carbonate equivalents of the is only with boiling acid that the C0» method will
different minerals used by the titration method in indicate the value of magnesite and some dolomitic
comparison with the relative crop increases and the limestones, as such minerals are not completely dis-
soil acidity decreases as shown by the Hopkins and solved by cold hydrochloric acid. The COs method,
Jones methods. The full application of calcite was of course, would not indicate the value of burned or
taken as one hundred in each case. The acid-neu- hydrated lime or of many waste products which might
■ S. D. Conner, J. Assoc. Off. Agr. Chan., 3 (1917), 139. be used for correcting soil acidity.
Doc.
iqiS THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
999
Fig. 3 — Relative Effect of Different Minerals as Shown by
Average Increase of Wheat and Clover and Decrease in Soil Acid-
ity by the Hopkins and Jones Methods Compared with Acid-Neutral-
izing Power of the Minerals Determined by Titration. Full
Calcite Application Taken as 100
It is a well-established fact that certain silicates of
calcium and magnesium compare favorably with
calcium and magnesium carbonates in neutralizing
acidity and in their beneficial action upon soils.1
Dana2 states that gypsum occurs intermingled with
limestone. Clarke3 says, "Wollastonite is commonly
found as a product of contact metamorphism, espe-
cially in limestones;" also, "In many localities
serpentine is associated with dolomite or dolomitic
limestones."
Taking all these factors into consideration it would
appear that the acid-neutralizing power of the lime-
stone as determined by titration is the best method
to use for determining the value of agricultural limes
and limestones.
SUMMARY
I — The value of agricultural limes was determined
by means of the acid-soluble calcium and magnesium,
by means of C02 determination with boiling hydro-
chloric acid, and by digesting in standard acid and
titrating the excess acid.
II — Pot cultures on two very acid soils were con-
ducted using calcite, wollastonite, raw rock phosphate,
gypsum, dolomite, magnesite, enstatite, and serpentine
as correctors of soil acidity.
Ill — Wheat and clover were grown in each soil
and the crop increases reported.
IV — Soil acidity was determined after cropp
means of the Hopkins potassium nitrate method and
the C. H. Jones calcium acetate method.
V — Crop increases due to various treatments were
obtained in the following order, the highest being
placed first: Calcite, dolomite, magnesite, wollas-
tonite, rock phosphate, serpentine, enstatite, and
gypsum.
■ Mclntin ud Willis, This Journal. 6 (1914), 1005; Ames and
SchollcnhcrKcr. Ohio F.xpt. Sta., Bull. S06 (1916), 385; Cowies. Mel. fr
Chem. Ent., 17 (1917), 664.
■ Dana. "Manual of Geology," 234.
» Clarke, U. S. Geol. Surv., Hull. *1«, 37S and 603.
VI — -The treatments decreased the soil acidity in
the following order: Magnesite, dolomite, calcite,
wollastonite, serpentine, rock phosphate, gypsum, and
enstatite.
VII — The results obtained in these experiments
indicate that the value of agricultural lime is in ac-
cordance with its acid-neutralizing power, rather than
with the CaO, MgO, or C02 contained, and that the
titration method is the most accurate and reliable
method for determining the value of agricultural
limes.
Soils and Crops Department
Purdue University Agriculture Experiment Station
Lafayette. Indiana
THE DETERMINATION OF THE HEXABROMIDE AND
IODINE NUMBERS OF SALMON OIL AS A MEANS
OF LDENTIFYING.THE SPECIES OF
CANNED 'SALMON
By H. S. Bailey and J. M. Johnson
Received June 21, 1918
At the suggestion of Mr. H. M. Loomis, formerly
of the Bureau of Chemistry, an examination of salmon
oils for their chemical and physical characteristics was
made in 191 5 by L. B. Burnett in this laboratory. His
preliminary experiments seemed to indicate that the
iodine numbers and hexabromide values would furnish
a method of distinguishing between the various salmon
species.
We have this year made a further study of oils ex-
pressed from canned salmon and believe that the
results we have obtained justify the assumption that
the oil from different species of salmon have charac-
teristic iodine numbers and hexabromide values.
In order to get a good working method for determining
the so-called hexabromide value of an oil, we carried
out a series of experiments using the different pro-
cedures suggested by previous investigators.
METHODS OF ANALYSIS
The precipitation of insoluble hexabromides from the
ether solution of oils and fatty acids was first accom-
plished in a qualitative way by K. Hazura.1 A
quantitative method for the determination of the hexa-
bromide value was afterwards worked out by Hehner
and Mitchell.2 This method depends upon the low
solubility of the hexabromides in a solution of ether
and glacial acetic acid. In their method, the precip-
itate of hexabromides was brought upon a filter
paper, washed with ether, dried and weighed. Procter
and Bennett3 found difficulty with Hehner and
Mitchell's method especially with tho filtration of the
precipitate. They changed the solvent and used
carbon tetrachlorM of ether, finally pre-
cipitating with alcohol. However, they did not
succeed in getting good results when brominating the
glycerides and recommended working with the fatty
acids. L. M. Tolman4 modified Hehner and Mitchell's
method, using a centrifuge for separating and washing
' Monalsh., 7 (1886). 637: * (1887), 148.
1 The Analyil.it (189S
■ J. Soc. Chtm. Ind., 2S (1906), 798.
< This Journal, 1 (1909
THE JOURNAL OF IXDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 12
the hexabromides, instead of carrying out these
operations on a filter. He also weighed in the same
flask in which precipitation took place. Tolman
allowed the mixture to stand only 30 min. after precip-
itation, but Sutcliffe,1 as a result of his investiga-
tions, recommended that after bromination, the
mixture stand over night at 11° before filtering and
washing the precipitate. He found that it was also
necessary to add enough bromine to give a good red
color instead of merely a yellowish brown as recom-
mended by previous investigators. Sutcliffe's method
was later called in question by Gemmell,2 but he in
reply3 demonstrated that if his directions were care-
fully followed his method could be used with satis-
faction.
The procedure finally adopted by us is a combination
of the methods of Tolman and Sutcliffe, as follows:
About 1 g. of oil is weighed into a tared weighing tube 1 in.
in diameter and 6 in. long, 25 cc. of absolute ether are added, and
the mixture cooled in ice water. Next there is added very slowly
drop by drop from a small burette a mixture composed of 5 cc.
of bromine and 25 cc. of glacial acetic acid. This reagent makes
an excellent brominating agent and allows the bromine to be
added more uniformly and gradually than when pure bromine
is used. Besides, it gives the acetic acid necessary for a proper
precipitation of the hexabromides. For most oils about 2 or 3
cc. of the solution are required to produce a deep red color,
which is considered indicative of a proper excess of bromine.
After the addition of bromine, the weighing tube is allowed to
stand in a refrigerator, temperature under 20 ° C, over night.
Next morning it is cooled in ice water and centrifuged from 2 to
4 min., the solvent is then decanted from the precipitate, 10 cc.
of ice-cold absolute ether added, the precipitate stirred up with
the ether, cooled in ice water, again centrifuged 2 to 4 min.
and the ether decanted off. This washing is repeated twice
more and after decanting the final wash ether, the weighing
tube is dried in an oven at 100° C. to constant weight, V* hr.
usually being sufficient. In the case of salmon oils which gave
a very large percentage of hexabromides, a weighed quantity
of the oil was mixed with a weighed quantity of a cottonseed
oil, which by test had shown no hexabromide precipitate, and
the hexabromide value was then determined upon the mixed
oil and calculated back to the original salmon oil. This was
found necessary as a very bulky hexabromide precipitate could
not be readily centrifuged and washed rapidly enough to prevent
the solution warming up and dissolving some of the hexabromides.
In order to get concordant results with an empirical method of
this kind of course every precaution must be taken to work
always under exactly the same conditions. After a little ex-
perience in the manipulation of this method, it is possible to
obtain duplicate determinations which agree within 0.2 per
cent with oils having a hexabromide value of 25 to 50.
The iodine number was determined upon a separate
portion of each sample by the regular official Hanus
method.4
ANALYSIS OF SALMON OILS
The salmon oils which we examined were obtained
from canned salmon furnished us by Dr. E. D. Clark
of the Food Research Laboratory and were collected
by him from various typical districts on the Pacific
Coast in 19 16. Enough cans to furnish the necessary
' The Analyst, 39 (1914), 28.
• Ibid., 39 (1914), 297.
' Ibid., 39 (1914), 388.
< J. A. 0. A. C, [3] J, Part II, 305.
amount of oil were opened, the contents ground in a
meat chopper and rqueezed in a cloth bag in a small
screw press. The oil and water mixture thus obtained
was centrifuged, the water layer removed with a
siphon, the oil dried with anhydrous sodium sulfate
and filtered through paper. The determination of!
iodine number and hexabromide value was made as
quickly as possible after the sample had been prepared)
as a precaution against any oxidation which might
take place upon standing. Table I gives the results
obtained upon these samples.
Table I Hexa-
bromide
O. F. W. Variety Iodine Value
No. Salmon Source Number Per cent
611 Sockeye Puget Sound 141.55 33.36
584 Alaska Red So. Eastern Alaska 140.72 32.61
586 Alaska Red Central Alaska 148.10 37.35
587 Chinook Bristol Bay. Alaska 126.62 24.90
573 Chinook Columbia River 128.03 24.58
577 Chinook Rogue River (fall) 134.48 31.06
579 Chinook Columbia River 129.13 26.45
583 Chinook Rogue River (spring) 130.40 29.52
588 Chinook Washington Coast 129.06 23.86
575 Silverside Rogue River 166.30 59.31
576 Silverside Columbia River 161.05 47.82
585 Medium Red So. Eastern Alaska 166.40 50.91
590 Coho Washington Coast 155.61 45.98
574 Chum Columbia River 133.10 27.62
589 Chum Central Alaska 136.19 30.12
595 Chum Bristol Bay, Alaska 133. 2S 27.59
581 Steelhead Columbia River 141.90 36.22
In the following table are given the figures found for
oils extracted with ether from single cans of Puget
Sound salmon packed under direction of Mr. R. W.
Hilts in IQI2— 13.
Table II
Hexabromide
O. F. W. Variety Iodine Value
No. Salmon Number Per cent
613 Coho 152.51 43.07
615 Pink 153.58 40.17
616 Chum 147.75 35.33
The ether in these oils was removed by evaporation
on steam bath in a current of carbon dioxide. That
ether extracted oils do not differ appreciably in their
constants from cold pressed oils is shown by the
analyses of two samples given in Table III.
Table III
Hexabromide
O. F. W. Iodine Value
No. Variety Number Per cent
574 Chum (cold pressed) 133.10 27.62
574 Chum (ether extracted) 135.43 27.91
589 Chum (cold pressed) 136.19 30.12
589 Chum (ether extracted) 141.28 30.23
The original scheme for this study of the salmon oils
contemplated the analysis of fresh salmon as well as
the canned product. Dr. Clark had individual fish of
several different species extracted with ether during the
1 9 16 season and these ether extracts were later sent to
Washington. Although the ether was only partially
removed from the oils, and they were kept in well-
stoppered bottles in the dark until they could be
analyzed, there appears to have been a marked change
in their composition. It is plainly evident that the
figures obtained upon these samples, as shown in Table-
IV, do not agree with those from the canned fish of the:
same species.
Table IV
Hexabromide
O F. W. Iodine Value
No. Variety Number Per cent
598 King 139.49 26.83
602 King 67.08
605 Silver 75.99 0.44
603 Chum 112.22 2.36
604 Chum 71.68
Dec, iojS THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
It might be assumed that there was a change in the
constants of the oil during the cooking incident to the
canning operations and that the values for the oil from
the fresh fish were the more nearly normal, if the latter
were not much lower than the corresponding values
for the canned samples. An increase in the hexa-
bromide and iodine values could hardly have been
caused by canning as so far as we know any alteration
in fish oils due to heat or oxidation always results in a
decrease in these constants.
DISCUSSION OF RESULTS
Five species of salmon (Oncorhynckus)1 are found in
the waters of the north Pacific: (i) Oncorhyncus
tschawytscha quinnat, tyee, chinook, spring or king
salmon; (2) Oncorkyncus nerka, blueback, red, sukkegh,
or sockeye salmon; (3) Oncorhyncus kisutch, silver, coho,
white or medium red salmon; (4) Oncorhyncus keta,
dog, keta or chum salmon; (5) Oncorhyncus gorbuscha,
humpback or pink salmon. With them the fisher-
men also incorrectly class the steelhead trout, which
really belongs to the closely related genus Salmo.
In Table I we have arranged the salmon oils
according to these classifications. It is readily seen
by reference to that table that the iodine numbers and
hexabromide values run fairly close together for the
same variety of salmon. 0. F. W. 587 was labeled
Alaska Red. Our analysis, however, indicated that
this was Chinook. After this sample was analyzed,
we submitted additional cans of the same lot to Drs.
W. C. Kendall and W. T. Bower, of the Bureau of
Fisheries, for identification. They, independently of
each other and without knowledge of our results,
pronounced the sample as Chinook. Therefore, we
have classified it accordingly.
A digest of Tables I and II show the following
variations:
Table V
Iodine Numbers Hexabromides
Lowest Highest Lowest Highest
Red. Sockeye, or Blueback 140.72 148.10 32.61 37.35
Chinook, King, or Spring 126.62 134.48 23.86 31.06
Medium Red, Coho, or Silverside. . . 152.51 166.40 43.07 59.31
Humpback or Pink 153.58 .. 40.17
Chum or Dog 133.10 147.75 27.59 35.33
The oils, therefore, show a little more characteristic
difference in their hexabromide values than in the
iodine numbers. In their iodine numbers, chums
and reds overlap, and pinks and medium reds overlap,
the highest value in the chums being nearly tho same as
that in the reds. As only one sample of pink salmon was
available for analysis, no sharp conclusion can be
drawn as to the limits of the values for the oil of this
species. Its iodine value would place it with the
medium reds, but its hexabromide value is lower than
the lowest found for any medium red sample.
If the coho oils are classified separately, and 0. F.
W. 616, chum salmon, omitted, we have the following
limits in these particular samples.
'John N. Cobb, "Pacific Salmon Fisheries," Bureau of Fisheries.
U. S. Department of Commerce, 1917, Document No. 839.
TABLE VI
Iodine Hexabromide
Number Value
Chinook 127-134 23-31
Chum 133-136 28-30
£e£ 141-148 33-37
Coho 153-156 43-46
Pink.... is4 40
Medium Red 161-166 48-59
This arrangement gives a much cleaner-cut distinc-
tion between the various species, both with reference
to the iodine numbers and hexabromide values. The
■ only case of over-lapping of the constants is between
the chums and chinooks.
CONCLUSIONS
i — A new method or perhaps more properly a
modification and combination of several methods for
the determination of the so-called hexabromide value
of fish oils has been worked out, using an acetic acid
solution of bromine as the precipitating reagent.
2 — Oils expressed from canned salmon, and dried
by the addition to them of anhydrous sodium sulfate,
after the major portion of the water has been me-
chanically removed, have practically the same iodine
and hexabromide value as the oils extracted with
ether, provided proper precautions are taken to prevent
oxidation in the extraction.
3 — In so far as a definite conclusion can be drawn
from the analysis of comparatively few samples,
the results obtained seem to indicate that it may be
possible to distinguish the variety of canned salmon
by a determination of the hexabromide and iodine
values of the oil.
On., Fat and Wax Laboratory
Bureau op Chemistry
U. S. Department op Agriculture
Washington, D. C.
COMPOSITION OF THE WATERS OF THE INTER-
MOUNTAIN REGION
By J. E. Greaves and C. T. Hirst
Received April 1, 1918
During the years 1916 and 191 7 the chemical de-
partment of the Utah Agricultural Experiment Sta-
tion made several hundred analyses of waters repre-
senting 58 streams, the majority of which were exten-
sively used for irrigation purposes. The results ob-
tained are of exceptional interest, for they indicate
the great quantitative and qualitative difference in
the composition of the irrigation waters. Moreover,
they clearly portray the enormous quantities of solu-
ble salts which at times may be carried to soil by
water and the great part which waters play in the
formation of alkali soil.
From the majority of streams monthly samples
were taken during the irrigation seasons. These
were collected according to standard methods in care-
fully cleaned containers and shipped to the labora-
tory where the analyses were made as soon as possi-
ble and according to the following methods.
METHODS OF ANALYSIS
total solids — Fifty cc. of water were evaporated
to dryness on an electric hot plate in 100 cc. beakers,
cooled in desiccators, and weighed accurately to the
fourth decimal place.
CARBo-, DIOXIDE Fifty cc. of water were titrated
THE JOURNAL OF INDUSTRIAL A.XD ENGINEERING CHEMISTRY Vol. 10, Xo. 12
Fig. I
against iV/30 H2S04, using methyl orange as an indi-
cator.
chlorine — Determined by Volhard's method,
using N/50 AgN03.
calcium — Twice precipitated as calcium oxalate,
each time washed, and finally titrated against N/10
KMnO,.
magnesium — The filtrate from the calcium was
concentrated, the magnesium precipitated by micro-
cosmic salt and weighed as magnesium pyrophos-
phate.
nitric nitrogen — Fifty cc. of water were evaporated
to dryness, the residue treated with 2 cc. phenoldisul-
fonic acid, allowed to stand ten minutes, and then
diluted with water.- The solution thus obtained was
made alkaline with ammonia, and the color compared
with a standard solution of potassium nitrate in a
Kennicot colorimeter.
The analysis of the water would give the basic and
acidic ions in the water, but in reporting the results
conventional combinations have been made according
to the calculations recommended1 by the Association
of Official Agricultural Chemists. These results are
reported as parts per million of water. That is, ac-
cording to the recommendation the hypothetical
combinations are made by calculating, the calcium
,and magnesium to the acid ions in the following order:
bicarbonate, sulfate, and chloride. Any remaining
acid ions are calculated to sodium.
The results, which are the average of from three to
seven analyses made on samples of water taken at
different times, are given in Figs. I to IV. The results
so presented give us at a glance the total and relative
quantities of total soluble salts, non-toxic bicarbonates
and calcium sulfate, and toxic chlorides and sulfates.
In so grouping the various streams into the four
divisions we do not wish to convey the idea that all
in the first group may prove injurious or that all in
the second or third group may be used with impunity,
but it has been used merely as a convenient method
of dividing, although a glance at the tables shows
quite a marked qualitative and quantitative difference
in the various groups.
1 /. A. 0. A. C. [4] 1, Part II, 51.
All of the waters, the analyses of which are listed in
Fig. I, are high in soluble salts.
It is, however, questionable whether any of them
are high enough in saline constituents to destroy
plants at the present concentration. But the magni-
tude of the problems which confront the users of
such waters is made clear by the following considera-
tion: one acre-foot of the Sevier River water would
carry to the soil 3581 lbs. of soluble salts which in 20
such irrigations would reach the enormous sum of
71,628 lbs., 75 per cent of which consists of toxic
salts. This in itself, if it be allowed to concentrate
in the surface foot, would be sufficient to render the
soil sterile. White River, which is lower in soluble
salts than any of the others in this group, would carry
to the soil in every acre-foot 1502 lbs. of salts, or in
20 such applications there would be added to the soil
over 1 5 tons of soluble salts.
Moreover, the water of the Sevier contains compara-
tively small quantities of calcium and magnesium bi-
carbonates and enormous quantities of the chlorides
and sulfates. The unbalanced condition of the salts
in Beaver River water makes it even more dangerous
than are the Sevier or Price River waters. It is im-
portant to note that in all of these streams, with the
exception of the White River, the toxic chlorides and
sulfates greatly predominate over the bicarbonates.
While the composition of these waters do not vary
greatly from year to year, there is a great variation
within one season. As a general rule, the concen-
tration of the salts in the water increases with the
season. The Sevier water is only two-thirds as con-
centrated during June as it is during September.
The fourteen streams listed in Fig. II are quite
different in composition from those previously con-
sidered.
With the exception of Ferron, Uinta, and Green
Rivers, the non-toxic bicarbonates predominate, and
even in these three streams there are large quantities
of calcium and magnesium bicarbonates which would
tend to neutralize the toxicity of the other salts, al-
though the problem confronting the users of these
waters is not nearly so complex as is the problem
Dec. 191S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
which confronts the users of the waters listed in Fig.
I. None of these waters contain sufficient salts to
be of injury to plant life, but the tendency to accumu-
late in the soil is impressed upon the individual in
passing over districts in which the waters have been
injudiciously used.
The streams which are listed in Fig. Ill contain
between 340 and 380 p. p. m. of soluble salts and in
every case the non-toxic bicarbonate greatly predomi-
nates. In not one case do the toxic salts reach 150
p. p. m. and in most cases the quantity present is far
below this amount.
These waters, if intelligently used on land, with even
fair drainage and not already filled with alkali, should
give no trouble. On the contrary, the quantity and
quality of the soluble constituents act as plant stimu-
lants. In short, this condition is found to occur with
many of even the high alkaline waters and the injury
comes only after there is a concentration of the solu-
ble salts within the soil.
All of the waters which are listed in Fig. IV contain
less than 180 p. p. m. of soluble salts and in every case
the toxic salts make up only a small fraction of the
total salts.
Sevier River and its tributary, Clear Creek, present
an interesting study. Clear Creek is a stream con-
taining only a small amount of soluble salts and over
76 per cent of this in the form of the non-toxic bi-
carbonates. But after flowing about 50 miles through
a district rich in soluble salts, receiving seepage and
being concentrated by evaporation, its nature has
been so changed that by the time it reaches Sigurd
Bridge, at Sigurd, it is a strongly saline water. In
flowing from Sigurd to the out-take of the Delta
Land and Water Company's canal there is a decrease
in common salt, but an increase of over 100 per cent
in the equally noxious sulfates. In flowing from
Clear Creek to Sigurd Bridge this stream has gained
over 400 per cent in soluble salts and the per cent of
non-toxic bicarbonates in the water ha di
from 76 per cent to less than 35 per ceni
Moreover, by the time the water reaches the Delta
Land and Water Company's canal the sail : h
creased over 600 per cent, with only 25 per cent of
them in the form of the calcium and magnesium bi-
carbonate. We therefore have the transformation
from a good carbonated water to a strongly saline
sulfate water which presents a tremendous problem
to the water user.
It is hard to place a limit upon the quantity of
alkali which may be in a water and the water still
be used for irrigation purposes, for it varies greatly
with a number of factors, chief among which are
the kind and quantity of alkali and the soil; the method
of irrigation and the quantity of water applied; the
physical nature of the soil as to whether sandy or
clayey and whether drained or water-logged.
It is generally conceded that sodium carbonate is
more injurious than the chlorides or sulfates. Prac-
tically all of the waters examined are very low in
sodium carbonate, but we must not lose sight of the
fact that sodium sulfate or sodium chloride, in the
presence of large quantities of decaying organic mat-
ter which liberates carbon dioxide, may be readily
transformed in the soil into the more harmful car-
bonate. Moreover, water which contains sodium
carbonate, if used on soils containing large quantities
of gypsum, will be no more detrimental than if it con-
tained an equal amount of sulfate; for the gypsum
would readily convert the carbonate into the less toxic
sulfate.
Moreover, as we have seen from the given results,
a stream may be comparatively free from alkali at
one season while at another it may be heavily charged
with alkali. The melting of snow in the mountainous
regions usually has the effect of freshening the water,
while local rains often have the opposite effecl . 1 (rain-
especially from alkali soils, greatly in-
creases the iii oi thi water. Many of
the cases in which large increases of alkali are noted
in the water during thi latei irrigation season must
be attributed to I
h good natural drainage a mon highl) concen-
trated water 1 i tere drainagi
For instance, in the Algerian I ilkaline
waters are used, the conditions are as follows: "The
ioo4
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 12
Arabs' gardens are divided into small plots about 20
ft. square, between which run drainage ditches dug
to a depth of about 3 ft. The soil being very light
and sandy, this ditching at short intervals insures
the most rapid and 1 borough drainage. Irrigation is
carried on by the check method and application is
made at least once a week, although two wettings
are often deemed necessary. A large quantity of
water is used at each irrigation. Thus a continuous
movement of water downward is maintained. There
is little opportunity for the soil water to become more
concentrated than the water as applied, and the in-
terval between irrigations being so short but little
accumulation of salt from evaporation at the surface
takes place."
The difficulty here is added to by the fact that the
soil is heavily charged with alkali. Under these con-
ditions such plants as melons, tomatoes, cabbage,
pepper, figs, and pomegranates do well. In this work
by Means1 the water used was all artesian water.
Where the soil is a clay loam, heavy adobe or soils
with hard pan or poor sub-drainage, entirely different
methods must be employed, for the salt would tend
to accumulate near the surface and soon become
injurious to plants. In soils such as named, every
effort must be made to conserve the soil moisture
and in this way cut down on the quantity of water
added to the soil and with it the alkali salt. It is a
fact that often better crops can be produced with
15 in. of irrigation water than with more.
Furthermore, there may be cases in which, because
of the physical and chemical composition of the soil,
together with the alkali content of the water, the crop
must be selected with this fact in view. For instance,
sweet or Egyptian clover may be irrigated with water
of such a high saline content that it would be fatal
to other crops. Old alfalfa is much more resistant
to alkali than is young alfalfa.
A soil which is heavily charged with soluble salts
may often be tilled if care be exercised in the use of
the irrigation water, but when we have such a soil
and have to use on it a highly saline water, the problem
becomes complex.
Although the use of a saline water on any soil is a
problem which must be solved independently in each
locality, taking into consideration the saline content
of 'In. water, the quantity and nature of alkali in the
soil, and the physical conditions of the soil, yet there
are certain standards which have been laid down
which are valuable guides. Hilgard2 considers that
the extreme limits of mineral content usually assigned
for potable watei ., 40 grains per gal. (571.2
p. p. m.), also applies to irrigation waters. Should it
happen that all or almost all of this were gypsum
and Epsom salt, only alarge excess of the latter would
constitute a bar to irrigation, while, on the contrary,
if a large proportion of the solids consists of sodium
carbonate or common salt, even a much smaller pro-
portion of salt might preclude its regular use, de-
1 U. S. Department of Agriculture, Bureau of Soils, Circular 10.
1 California Experiment Station, Bulletin 128.
pending upon the nature of the soil to be irri-
gated.
Forbes1 feels that 0.25 per cent of salts in the soil
is a more or less dangerous quantity of alkali, even
when composed of the less harmful salts. Any ad-
dition of alkali in the irrigation waters should be care-
fully controlled. He states further that water con-
taining 1000 to 1500 p. p. m. of salts as sulfates and
chlorides has often embarrassed the agriculture
of the farmer and in some cases it has led to the aban-
donment of farms. Forbes therefore considers "that
under the conditions of water supply, drainage, and
climate found in the principal irrigated districts of
Arizona and with prevailing agricultural practice,
waters containing 1000 p. p. m. of salts of average
composition are liable to cause in a few years harm-
ful accumulations of alkali."
The Bureau of Soils2 states that 5000 p. p. m. of
soluble salts when added to the Pecos Valley soils
may be taken as the extreme limit of endurance by
plants, while 250 to 300 marks the danger zone; how-
ever, in this case about 50 per cent of these salts are
harmful. At Carlsbad about 300 p. p. m. marks the
limit of safety.
Means,3 however, claims that the amount of alkali
salts permissible in irrigation water has been under-
estimated by American writers, and calls attention
to the fact that the Arabs in Sahara, Africa, use irriga-
tion water containing over 800 parts per 100,000,
more than one-half of which is sodium chloride. He
also quotes from an earlier publication: "The limit
of endurance for most cultivated plants in a water
solution is about 1 per cent, or 1000 parts of the readily
soluble salts in 100,000 parts of water."
There is considerable truth in Means' contentions,
for many of the early workers on soil alkali failed to
take into consideration the effect of balanced solu-
tions on plants and the antagonistic action of one
salt to the other.
Viewed in the light of Hilgard's interpretation, we
find only thirteen streams the alkali content of which
is dangerous, or, if interpreted in the light of Forbes'
experience, only two, but according to the work of
the Bureau of Soils none should be condemned.
But the fact which must be borne in mind is that
even though plants may tolerate large quantities
of alkalies in solution if they be in a balanced condi-
tion, the great danger comes from the accumulation
of the salts in the soil from their continual applica-
tion. Many saline waters when first applied to a
soil may furnish nutrient to the plant and actually
stimulate plant growth, but later, due to their ac-
cumulation within the soil, have an opposite effect.
Hence, users of saline waters must never lose sight
of the fact that these waters, if injudiciously used,
may be a very potent factor in ruining valuable land.
Utah Agricultural Collece
Logan. Utah
Arizona Experiment Station, Bulletin 44.
1 Report. 64, page 19.
1 U. S. Department of Agriculture, Bureau
of Soils, Circular 10.
Dec, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
1005
ON CONSTITUENTS OF OIL OF CASSIA— II
By Francis D. Dodge
Received June 13, 1918
The examination by the writer and A. E. Sherndal1
of the alkali-soluble portion of oil of cassia showed the
presence of several compounds not hitherto recognized
as constituents of the oil. More recently the writer
has had occasion to make a further study of this oil,
and especially of the aldehyde constituents.
Two samples were examined: one, A, a redistilled oil '
made in this laboratory from apparently pure com-
mercial oil; the other, B, a commercial U. S. P. oil.
The results of the preliminary tests were as follows:
A B
Sp.gr. at 25° 1.0528 1.0514
Aldehyde (by vol.) 88 per cent 80 per cent
Rotation Slightly + Slightly +
Rosin test Negative Negative
One pound of each of the samples was shaken with
sufficiently strong sodium bisulfite solution to ensure
complete extraction of the aldehydes, the reagent being
added in portions of about one pound, waiting after
each addition until the crystalline compound had com-
pletely redissolved. About 5 lbs. of bisulfite were re-
quired for each lot, and when the supernatant oil was
found to be free from aldehyde the aqueous solution
was separated, and heated on the water bath for several
hours to ensure the conversion of the bisulfite compound
into the more stable sulfonate. On cooling, the solu-
tion was filtered to remove traces of oil. This solu-
tion had a slight acid reaction; a portion made alkaline
with sodium carbonate became slightly turbid, and
showed by odor the presence of aldehyde other than
cinnamic, the latter not being liberated by soda.
The entire solution was accordingly made strongly
alkaline with sodium carbonate, and extracted with
ether. The ether solution was washed with N sodium
hydroxide to remove salicylic aldehyde, and then with
strong bisulfite to separate other aldehydes. From
the alkaline solution the salicylic aldehyde was ob-
tained by acidifying and extraction with ether, and the
other aldehydes similarly by neutralizing the bisulfite,
and treating with ether. The first ether solution,
after treatment with bisulfite, left a small residue
of the non-aldehyde portion of the oil, which had re-
mained dissolved in the original bisulfite solution.
The results on the two samples were:
A B
Original 453 g. 453 g.
Non-aldehyde About 50 g. About 80 g.
Salicylic aldehyde 0.985 g. 1.110 k.
Other aldehydes 3.850 g. 4.860 g.
Cinnamic aldehyde Not recovered
The small portion of saturated aldehydes thus ob-
tained was, in each case, a heavy, slightly yellow liquid
with strong odor of benzaldehyde. That it was not
entirely the latter was shown by the behavior with
bisulfite solution, in which the aldehyde mixture was
completely soluble with evolution of heat, but with
only a slight formation of crystals on standing.
Benzaldehyde under similar conditions is immediately
converted into a crystalline mass. • In exposure to the
air, the aldehyde mixture oxidize! readily, but not
' This Journai, 7 (1915), 1055.
completely to a crystalline acid, melting at 91-93°,
which was found by the usual tests to be impure
benzoic acid.
A small portion oxidized by permanganate gave an
acid which, after crystallization from benzene, melted
at 120°, and was evidently benzoic acid. This sug-
gested the possibility of the presence of hydrocinnamic
aldehyde, and with the view of limiting the oxidation
to the aldehyde group, another portion was oxidized
with hydrogen peroxide as follows:
3 g. aldehyde mixture were treated with 30 cc. official peroxide,
with a few drops of ferric chloride solution, keeping the mixture
slightly alkaline with sodium hydroxide, and adding peroxide
until all the aldehyde was in solution. The temperature was
kept at 30 to 50 °, with frequent agitation. At the end a distinct
odor of anisol was noted, which proved significant. Finally
the alkaline solution was filtered and concentrated to about
20 g. On acidifying, a crystalline acid mixture, melting below
ioo°, was precipitated. The characteristic odor of hydro-
cinnamic acid was not observed, and a separation of the acids
by recrystallization from water was not successful.
For further information as to the nature of the
aldehydes present, ■ a portion was converted into
oxime. One gram aldehyde with one gram hydroxyl-
amine hydrochloride and 33 cc. N/2 alcoholic potas-
sium hydroxide was allowed to stand 3 days, heated
to 70° for 3 hrs., neutralized with HC1, diluted
to 100 cc, and extracted with ether. On evaporation
of the ether solution, long white needles were de-
posited, which, after pressing and drying, amounted
to 0.35 g., and melted at 90° (corr.).
It seemed probable that this oxime might be the
oxime of hydrocinnamic aldehyde (m. p. 93-94°), or,
more likely, the oxime of methyl salicylic aldehyde
(m. p. 92°). The occurrence of the latter could in
fact almost be assumed as an oxidation product of the
methyl ortho-coumaric aldehyde already noted as a
constituent of the oil by Bertram.1 A similar re-
action would explain the occurrence of benzaldehyde.
C,H6 — CH = CH — COH
Cinnamic aldehyde
/OCHi
c,h/
nch = ch — coh
Methyl coumaric aldehyde
C,H8 — COH
Benzaldehyde
OCH,
-> C«H4/
XCOH
Methyl salicylaldehyde
The occurrence of anisol as an oxidation product
would also find an obvious explanation:
/OCH,
C6h/ + O = C.H, — OCH, + CO,
^COH
Methyl salicylaldehyde Anisol
To identify the oxime, a portion was converted into
nitrile by treatment with acetic anhydride, and the
nitrite saponified with alcoholic potassium hydroxide.
The reaction, however, did not appear to be smooth;
an oily acid was obtained and the result was incon-
clusive. The conversion into the corresponding acid
was, however, attained by the direct oxidation of the
oxime with permanganate, a method apparently not
previously suggested for this purpose, but which seems
>./. prakl. Chtm., [2] »1, 316.
ioo6
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMIS1 'AT Vol. 10. No. 12
to be applicable in cases in which the acid formed is
comparatively stable toward the reagent.
0.231 g. oxime, dissolved in a few drops of methyl alcohol,
was mixed with 2 cc. N/2 potassium hydroxide, and 5 per cent
permanganate added gradually until no further oxidation took
place. The manganese oxide was then dissolved by sufficient
sulfurous acid, the mixture strongly acidified, and the acid taken
out with ether. 0.145 g. acid was obtained, which, as it was
still contaminated with an oily impurity, was again treated in
the same way with permanganate. The acid solution was not
extracted with ether, but was allowed to evaporate. After a
few days, the greater part of the acid had separated in two
large, well-formed prismatic crystals, apparently monoclinic,
melting at 89° (corr.), and evidently methyl salicylic acid.
A careful comparison with the synthetic acid showed the identity
of the preparations, both crystallizing from alcohol in distinct
characteristic prisms, showing under the microscope oblique
extinction, and a 0-angle of about 49°, as described by Graebe.1
EXAMINATION OF THE NON-ALDEHYDE SECTION
The portions of the oil insoluble in bisulfite showed
the following properties:
A B
Sp. gr. at 25° 1.020 0.9966
Rotation +0.50° +0.75°
Acid value 4.0 6.0
Saponification value 170.0 110.0
Calc. as cinnamyl acetate 53.4 per cent 34.5 per cent
For further light on the composition of this section,
38 g. of non-aldehyde A were saponified and distilled
with steam. About 12 cc. of light oil were obtained,
the greater part of the alcoholic product remaining
dissolved in the aqueous distillate. To remove
alcohols, the oil was washed with 50 per cent resorcin
solution, which left a residue of 6.25 cc. light oil, very
insoluble in alcohol, and almost unattacked by per-
manganate. This, in fact, appeared to be a petroleum
section, evidently due to an adulteration of the crude
oil.
The aqueous distillate, on ether extraction, yielded
a small amount of heavy oil, which gave benzaldehyde
on oxidation with permanganate, and was probably,
in part at least, cinnamyl alcohol. The alkaline
residue from the distillation was found to contain
acetic and cinnamic acids, and the liquid acid with
fruity odor, previously noted.
A comparatively large amount of resin was formed
in the saponification, the cause of which remains un-
explained.
To conclude, oil of cassia has been found to contain
the following compounds:
Previously known: Cinnamic aldehyde, 75 to 90 per cent
Cinnamyl acetate
Phenyl propyl acetate (?)
Methyl ortho-coumaric aldehyde
Found by the writer
and Sherndal: .Salicylic aldehyde, 0.1 to 0.2 per cent
Coumarin
Benzoic acid
Salicylic acid
Liquid acid of fruity odor
Found by the writer: Benzaldehyde
Methyl salicylaldehyde
Laboratory of the Dodge and Olcott Company
Bayonne, New Jersey
LABORATORY AND PLANT
METHODS OF ANALYSIS USED IN THE COAL-TAR
INDUSTRY. IV— BENZOLS AND LIGHT OIL
By J. M. Weiss
Received October 24, 1918
BENZOLS
TEST E2 — SPECIFIC GRAVITY (SPINDLE)
apparatus — Hydrometer.2 The necessary ranges
for this class of compounds are 0.79 to 0.87, 0.86 to
0.94, and 0.93 to 1. 01.
method — See B4.3 Benzols shall always be taken
at 15.5° C. (6o° F.) and no correction shall be made of
a reading taken at a different temperature.
note — As under B4.
test E3 — specific gravity (westphal)
All matter as to apparatus, method, precautions,
and notes as given under H44 apply to this test on these
materials.
special note — This method is the reference method
for benzols and must be used in all cases where accu-
racy is required as in cases of dispute or check testing.
TEST E4— DISTILLATION OF PURE PRODUCTS
wm'aratus — Flask: The distillation flask shall be
a 200 cc. side neck distilling flask having the following
dimensions:
1 Ann., 139, 137.
< II. Paper I. This Journal, 10 (1918), 735.
1 Tins Journal, 10 (1918), 735.
< Ibid., 10 (1918). 911.
Diameter of bulb 73 mm. (2.881 in.)
Outside diameter of neck 24 mm. (0.945 in.)
Inside diameter of neck 21 mm. (0.826 in.)
Length of neck 105 mm. (4. 134 in.)
Inside diameter of side tube 5 mm. (0. 197 in.)
Length of side tube 127 mm. (5.000 in.)
Side tube joined to neck above the base of
the neck 52 mm. (2.047 in.)
The side tube shall be set so that the smaller angle
where it joins the neck is 750.
The allowable variation from the above dimensions
shall be not more than 5 per cent. See Fig. XVI.
Thermometer: This shall be graduated from 70°
to 120° C. at intervals of 0.20 C. It shall be made of
a suitable quality of glass so as not to change its read-
ing under conditions of use. It shall be provided with
an expansion chamber, and a ring at the top for at-
taching tags. It shall conform to the following dimen-
sions:
Total length Not over 305 mm.
Bulb length Not over 20 mm.
70" mark to bottom of bulb 80 to 100 mm.
Graduations per inch Not over 35 mm.
Stem diameter 5 to 7 mm.
Bulb diameter 5 to 7 mm.
The thermometer shall be accurate to 0.20 C. at
total immersion and shall be compared before use with
a similar thermometer calibrated at full immersion by
the Bureau of Standards, and proper correction ap-
plied.
It is preferable that this instrument shall not have
Dec, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
a supplementary bulb situated between the lowest
graduation and the main mercury reservoir. How-
ever, if such a chamber is present, its lowest point
shall be not more than 1 mm. above the top of the
main reservoir.
Condenser: The distillate shall be condensed in a
straight tube of V2 in. internal diameter and 24 in.
in length, set at an inclination of 75 ° to the vertical.
At least 15 in. of tube shall be cooled with cold water
in a trough condenser.
Burner: The heating flame shall be derived from
a Bunsen burner and the entire flame shall be blue.
Cylinder: An ordinary 100 cc. cylinder, graduated
at intervals of 1 cc, shall be used for the re-
ceiver. Graduations must be clear cut and distinct.
The graduate shall be approximately 1 in. in diam-
eter. The mark for each 10 cc. shall be longer than
the intermediate markings and shall be plainly num-
bered.
Fig. XVI — Assembly op Benzol Distillation Test
Assembly of Apparatus: Shown in Fig XVI. The
flask shall be supported on a sheet of l/«-in. asbestos
board, 6 in. X 6 in., with a hole in the center
1 in. in diameter. The asbestos board shall be sup-
ported on a circular metal shield enclosing the Bunsen
flame. The flask shall be so placed that the vapor
tube will extend at least 2 in. into the condenser
tube.
The thermometer shall be held in the neck of the
distillation flask by means of a cork stopper in such a
position that the top of the bulb shall be opposite the
lower side of the side tube and central in the neck of
the flask.
method — The sample to be tested shall be poured
into a 100 cc. graduated cylinder and 100 cc. of the
material shall be carefully measured and transferred
to the distilling flask. The flask shall be put in con-
nection with the condenser and the thermometer in-
troduced through a tightly fitting cork. The grad-
uated cylinder which was used to measure the oil
shall not be rinsed out but shall be placed under the
lower end of the condenser tube to catch the distillate.
The flask shall be heated up slowly, especially after
ebullition has begun, so as to allow the mercury col-
umn of the thermometer to become fully expanded
before the first drop distils off.
The flame shall then be turned up and the distilla-
tion conducted at the rate of 5 cc. per min. (2 drops
per sec). This rate must be exact. The distillation
shall be continued to dryness. The total yield of dis-
tillate shall not be less than 95 per cent.
A temperature reading shall be taken when the first
drop of distillate falls into the receiving cylinder. Ad-
ditional temperature readings shall be taken when 5
per cent and 95 per cent of distillate have distilled
1 over. A final reading shall be taken of the "dry" point,
which is the point at which liquid just disappears from
the bottom of the flask.
precautions — Care must be taken to quickly re-
move the burner as the last bubble is evaporated,
otherwise, too high a dry point may be produced by
superheating.
notes — The method given applies to pure benzol
and pure toluol.
The specifications for pure benzol and pure toluol
require that distillation from first drop to dry shall be
complete within a 2° C. range and, further, that the
true boiling point of the product in question shall lie
within that range.
To be sure that the true boiling point is strictly
within this range it will be necessary, of course, to
correct the observed temperature readings for varia-
tions from the standard thermometer, both for inac-
curacy and for stem immersion; also correction should
be made for differences in barometric pressure.
The barometric correction factors for each mm. of
difference are as follows, these factors being applied
directly as the difference in the barometric pressure
may be greater or less than 760 mm.
Benzol 0.043°
Toluol 0.047°
Xylol 0.053°
It is not necessary in ordinary works practice to
require the chemist to apply these corrections to each
test. For instance, if the material is one which boils
entirely within a 2° range, around, say, from 77 ° to
81 ° C, when the corrections are applied the results
will all fall within a similar 2° range. The same
applies to a 2° range between 108 ° and 11 2° C.
It is recommended, however, that such corrections
be applied when the sample is to be checked against
results obtained by another investigator, and in re-
porting results in such a case, a notation should be
made to the effect that these results have been cor-
rected for the variations mentioned.
An examination of all available literature on such
subjects will show that the authorities vary materially
in their report of findings of the true boiling points of
benzol, toluol and the three xylol isomers. Tl
lowing figures, however, arc considered sufficiently ac-
11 commercial practice.
Benzol 80.2° C.
Toluol HO .4°C.
Para-»ylol '•''•5» Xs
Meta-xylol 138.5° C.
(irtho-xylol 142.3 C.
The < mergi n1 tem corrections i hould
iws:
ioo8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 12
., the difference
ry and glass.
Let C = Number of degrees centigrade to be added to the observed
temperature.
N = Number of degrees of the stem exposed.
T «= Average temperature of the bulb.
t =» Average temperature of the stem.
K = Correction factor for the thermometer,
between the coefficients of expansion of i
Then C = KN (T — /).
Example.
Observed temperature = I
Stem temperature
Degrees emerging (from top of flask to 80° C.) = 1
Thermometer coefficient
80° C. — 25° C.
15" X 55° X 0.000154
Temperature corrected for emergent stem
= 0.000154
= 0.12787 = 0.13°
= 80.13° C.
TEST E5 DISTILLATION OF COMMERCIAL BENZOLS
apparatus — Exactly as given for E4 with the fol-
lowing exceptions: (1) The thermometer shall be a
standard o° to 400 ° C. thermometer (see C9)1;
(2) For materials boiling substantially below 145 ° C.
a 1 -in. hole shall be used in the asbestos board on
which the flask is supported. For materials boiling
substantially above 145° C. a 2-in. hole shall be used.
method — The distillation shall be conducted exactly
as given under E4.
"Special Specification Xylol" shall be read first
drop, s per cent off, 50 per cent off, 95 per cent off,
and dry, as under E4.
All other materials, except "Pure Xylol," shall be
read at first drop, and then volume readings taken at
every even 50 C. up to the dry point, thus:
Deg. C. Per cent
77 1st drop
100 90
105 98
108 Dry
"Pure Xylol" shall be read, first drop, every 1° C,
and dry.
precautions — Same as under E4.
notes — In light fractions it is well also to deter-
mine loss by pouring the liquid that recondenses in
the flask into the graduated cylinder and noting the
total volume. The difference between the reading and
100 gives the approximate result for "loss."
In some cases on the xylols where special accuracy
is required a thermometer graduated from 110° to
1600 C. in 0.2° C. intervals is used. This is not neces-
sary for ordinary practice. The specification, except
for scale range, is the same as for the 70 ° to 1200
thermometer given under E4.
This test, as well as E4, has been compiled from our
experience and also from matter given in the Gas
Chemists' Handbook, page 1S0, the standard method
for distillation of paint thinners (A. S. T. M., D-28-17),
and the article2 by F. W. Sperr, Jr., of the H. Koppers
Co.
TEST Ef5 SULFURIC ACID WASH
apparatus — Standards: The set of color stand-
ards against which wash tests shall be compared shall
consist of fifteen bottles (French square flint glass,
glass stoppered, one ounce capacity) each containing
; This Journal, 10 (1918), 819.
' Mel. &• Chem. Eng., Nov. 15, 1917, p. 586.
one of the colored solutions made up as given below,
the bottle being sealed.
For making up the standards the following basic
solutions shall be used:
A — 59.4965 g. C0CI2.6H2O (nickel-free) made up to
1000 cc. with a mixture of 25 cc. 31 per cent
HC1 and 975 cc. H20.
B — 45-054 g. FeCi3.6H20 made up to 1000 cc. with
a mixture of 25 cc. 31 per cent HC1 and 975
cc. H20.
C — 3.5 volumes of Solution A + 36.5 vol. Solution
B + 90 vol. of H20.
D — 3.5 volumes of Solution A + 36.5 volumes of
Solution B. (No water is added.)
E — Solution of K2CrO< saturated at 21 ° C.
F — One volume of a solution of K2Cr207 saturated
at 210 C. -+- one volume of H20.
As standard color solutions to be used for compar-
ison the following shall be made up and numbered
from o to 14:
No. o — Pure water.
No. 1 — One volume of Solution C + 1 volume of
H20.
2 — 51/2 volumes of Solution C + 2 volumes
of H20.
3 — Solution C as such.
4 — One volume of Solution D 4- one volume
of H20.
5 — 5V2 volumes of Solution D + two volumes
of H20.
6 — Solution D as such.
7 — 5 volumes of Solution E + 2 volumes of
water.
8 — Solution E as such.
9 — 7 volumes of Solution E -f- '/j volume of
Solution F.
10 — 6V2 volumes of Solution E + one volume
of Solution F.
No. 11 — 5V2 volumes of Solution E + two volumes
of Solution F.
12 — One volume of Solution E + one volume
of Solution F.
13 — Two volumes of Solution E + 5 volumes
of Solution F.
14 — Solution F as such.
These standard solutions shall, in all cases, remain
stoppered and sealed to prevent evaporation.
Test Bottles: These shall be one-ounce, French
square, glass-stoppered, flint glass bottles identical
in every respect with those containing the standard
solutions. (A suitable bottle is shown in the Whitall
Tatum 1910 catalogue, p. 21.)
method — 7 cc. of 96 per cent C. P. sulfuric acid
shall first be placed in a test bottle and approximately
21 cc. of the material to be tested shall be added. The
bottle after being stoppered shall be thoroughly and
vigorously shaken for 15 to 20 sec. and allowed to stand
for the specified time. (See Notes.)
The resulting color of the acid layer shall be com-
pared with the set of standards and the number of the
bottle in the standard set corresponding to the test
bottle shall be noted.
No.
No.
No.
Xo.
No.
No.
No.
No.
Xo.
No.
No.
Xo.
Dec, 1918
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
1009
precautions — If the color of the acid layer is not
uniform, it should be carefully mixed by slowly in-
verting bottle once or twice.
96 per cent sulfuric acid must be used. Some C. P.
I acid obtained is only 94 per cent and care must be
i taken to see that the strength is of the proper degree.
notes — In pure benzol and pure toluol testing the
benzol or toluol layer must remain white, and the color
of the acid layer, after standing 15 min., must not be
darker than No. 4.
For 90 per cent benzol and all grades of benzol and
toluol other than pure, the benzol or toluol layer
must remain white, and the color of the acid layer
after standing 15 min. must not be darker than No. 6.
For solvent naphtha the acid layer color only is
noted, and after standing 5 min. it must not be darker
than No. 14.
It is well to note that the above schedule shows the
limit of color allowable in the sales specifications, and
it is to be expected that to consistently pass the test,
works practice should call for a limit of at least one
number lighter in each case.
This test is not used on crude benzols. The color
standards are a modification of the old Barrett Com-
pany standard practice made by the Semet-Solvay
Company.
special note — In making the wash test upon an
agitator charge, this being recommended as a guide in
determining whether material in question has been
sufficiently washed to warrant making final distilla-
tion, it is necessary to first make the sample alkaline
by shaking with some of the caustic soda solution
which will be used in the factory upon the wash.
This is best carried out in a separatory funnel. After
shaking, the mixture is allowed to settle and the soda
solution drawn off as thoroughly as possible. 100 cc.
of the neutralized oil are then measured in a graduated
cylinder and transferred to a 200 cc. distilling flask.
No thermometer need be used in this distillation,
but care should be taken to make the distillation
through a condenser which has been used for pure
products, so that the distillate may not be contaminated
in the condenser.
The first 5 cc. distilled off are rejected. Then 70
cc. are distilled off and caught in a clean graduated
cylinder. The cylinder which was used to measure
the material into the flask should not be used for this,
as it would tend to contaminate the distillate. The
70 cc. of distillate thus caught are filtered through a
clean, dry, white filter, and tested for wash as de-
scribed.
If the resulting test is entirely satisfactory, the
factory alkali wash and result in distillation may be
safely relied on.
TEST E7 — CARBON BISULFIDE
apparatus — Erlenmeyer flask, rough balance, bu-
rette, separatory funnel 250 cc. capacity.
reagents — Solution of alcoholic caustic potash, pre-
pared by dissolving no g. of potassium hydroxide in
900 g. of absolute alcohol. Standard solution of cop-
per sulfate (1 cc. equi vrtbnt to 0.00; .vepared
by dissolving 12.475 S- °£ CuS04.sH20 in one liter of
distilled water. Potassium ferrocyanide solution.
Acetic acid solution.
method — Exactly 50 g. of the benzol to be tested
shall be weighed into an Erlenmeyer flask, mixed well
with 50 g. of alcoholic potassium hydroxide solution,
the flask stoppered and the mixture allowed to stand
for 5 or 6 hrs. at the ordinary temperature. The
carbon bisulfide by this treatment is converted to
potassium xanthate. The mixture shall then be
shaken up with about 100 cc. of water and the aqueous
layer separated from the benzol. This washing shall
be repeated several times with 30 cc. portions of
water, adding the washings to the original water
solution. The solution shall then be diluted to 250
cc. and an aliquot portion removed, neutralized with
acetic acid, and titrated with copper sulfate solution.
The end-point shall be determined by placing a drop
of the solution on a filter paper next to a drop of potas-
sium ferrocyanide solution. The completion of the
titration is indicated by a reddish brown zone of cop-
per ferrocyanide.
Cc. CuSO4Soln.X3.7s ir,e
calculations — — ; ; : : — =per cent CS>.
Cc. taken for titration
note — tThe above quantity of alcoholic caustic pot-
ash is sufficient if the benzol contains less than 5 per
cent of carbon bisulfide. If it contains more, a smaller
sample should be taken. In this case, the formula for
calculation must be modified accordingly.
test e8 — paraffins
apparatus — Babcock milk bottles. Centrifuge.
Pipette, 10 cc. funnel, with capillary stem.
reagents — Fuming sulfuric acid, 20 per cent free
S03.
method — 10 cc. of the benzol to be tested shall be
measured into the Babcock bottle, and 10 cc. of the
fuming sulfuric acid slowly added to it, cooling the
bottle in a bath of ice water during the addition of the
acid, and shaking the bottle vigorously after each
addition in order to thoroughly mix the contents.
After the addition of the acid is complete, the bottle
shall be removed from the ice bath, shaken until the
temperature rises to about 40° C, and then alter-
nately cooled and shaken for a period of 15 min., keeping
the temperature below 400 C. Then the mixture shall
be cooled again, 10 cc. more of the fuming sulfuric
acid added, the whole mixed thoroughly and shaken
and cooled as above, keeping the temperature below
400 C. Finally the mixture shall be allowed to stand
for 30 min. at a temperature of about 35° C. Then
the bottle shall be cooled in ice water and water added
through the capillary stem of the funnel so that it
enters below the surface of the acid. The water shall
be added in small portions very cautiously an
bottle thoroughly shaken and cooled after tin- addi-
tion of each portion. When sufficient water lias been
added to bring the level "I the liquid we
i e bottle shall be
1 fur 5 min.
The paraffins present will rise to the surf;
their volume shall read off -in terms of the
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. i>
graduations on the neck of the bottle. This reading
(in major divisions) multiplied by 2 gives directly the
volume per cent of paraffins in the original material.
precautions — The graduated portion of the bottle
should be 2 cc. divided into 10 major divisions. These
are further subdivided into 5 or 10 divisions each.
The readings should be taken in terms of the major
divisions (0.2 cc. each).
notes — On diluting the sulfonation mixture with
water it will frequently happen that a small quantity
of solid sulfone will be formed, which, on centrifuging,
will form a layer between the paraffins and the acid
layer. This sulfone should not be mistaken for paraffins.
In benzol work we have found it necessary to carry
on the dilution with water rather than concentrated
sulfuric acid in order to prevent solution of paraffins
in the mixture.
TEST E9 HYDROGEN SULFIDE
apparatus — Balance. Separatory funnel, 250 cc.
Beakers, funnels, desiccator, crucibles, etc.
reagents — Sodium hydroxide C. P., 10 per cent
solution. Bromine water, sulfur free, saturated solu-
tion. Barium chloride, 5 per cent solution.
method — 100 g. of the benzol shall be shaken thor-
oughly in a separatory funnel with 25 cc. of sodium
hydroxide solution, the liquids allowed to settle and
the lower layer drawn off into a beaker. The water
layer shall be diluted to 400 cc, about 20 cc. of
the bromine water added, the mixture acidulated
with hydrochloric acid, the excess bromine boiled off
and the sulfuric acid in the solution precipitated in the
usual manner with barium chloride. The barium sul-
fate shall be filtered and weighed. A blank determina-
tion shall be made on the same amounts of the mate-
rials used in the analysis and the weight of barium sul-
fate deducted from that obtained from the benzol.
calculations — Weight of barium sulfate X 0.1460
= per cent of H2S.
notes — Before proceeding with determinations of
H2S and SO. a qualitative test should first be made in
order to determine which of the two is present. This
can best be done at the time of performing the distil-
lation test, E4 or E5, by hanging strips of moistened
lead acetate paper and starch iodate paper on the end
of the condenser tube. If the lead acetate paper shows
discoloration, H2S is present, but not SO?. In this case
both papers will usually be discolored. If the lead
acetate paper shows no discoloration but the starch
iodate paper develops a blue color, S02 is present but not
H2S. If neither paper shows discoloration, neither is
present. As H2S and S02 mutually react both cannot
be present simultaneously.
TEST EIO SULFUR DIOXIDE
Apparatus, reagents, and method of analysis are
precisely the same as Eg.
calculations — Weight of barium sulfate X 0.2744 =
per cent SO2.
TEST EII SOLIDIFYING POINT OF PURE BENZOL
apparatus — Test-tube 5 in. long by 1 in. inside
diameter. Thermometer, o° to 8o° (see D6).1 Beaker,
400 cc. capacity.
' This JOURNAL, 10 (1918), 820.
METHOD — About 2o cc. of the benzol to be tested
shall be poured into the test-tube and cooled in a bath
of ice and water contained in a beaker, stirring continu-
ously with a thermometer. When the solid benzol
begins to separate the temperature will remain con-
stant for some time. This temperature shall be taken
as the solidifying point.
accuracy — =»= 0.05 °.
light oil
This material is tested for water, specific gravity,
tar acids, and tar bases as described under heavy oil
tests.1 Other special tests are made as follows:
TEST F5 BULB DISTILLATION
All matter as to apparatus, method, precautions and
notes as given under E5 for materials boiling substan-
tially above 135° C. apply to this test on these mate-
rials.
special note — With light oil, a dry point is ordi-
narily not taken, the distillation being continued only
until about 95 per cent of the material has distilled
over. Readings should be taken at first drop and every
even 10° C.
TESTS F6 AND F7 TAR ACIDS (CONTRACTION AND LIB-
ERATION METHODS)
These should be carried out exactly as given under
Hi 1 and H12.
TEST F8 HEMPEL DISTILLATION
apparatus — Flask, short ring neck, 200 cc. Hem-
pel tube. Condenser and stand. Thermometer, o° to
400 ° (specifications as under Cc.).2
The assembly of the apparatus is shown in Fig.
XVII.
Fig. XVII— Assembly of Hempel Evaluation Test for Licbt Oil
METHOD — After the extraction of tar acids from 100
cc. of oil the residual oil shall be placed in the 200 cc.
bulb and the apparatus assembled as in Fig. XVII.
Heat shall be applied and the distillation conducted
at the rate of 1 to 2 drops per sec. The volume which
has distilled at 130° C, 1700 C, and 2000 C, shall be
noted and recorded. The flame shall be removed when
the thermometer reaches 200 ° C.
■This Journal, 10 (1918) 911.
'Ibid., 10 U918), 819.
Dec. 19 1 S
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
notes — This test is a very rough evaluation test
•used for comparison purposes between oils. The 1300
fraction roughly represents crude benzol and toluol;
the 130° to 1700 fraction, crude solvent; and the 170°
to 200° fraction, heavy naphtha. If more exact in-
formation is desired, the test given under Fio should
be used. The residue in the bulb should be preserved
for Test Fo if this is desired.
TEST FQ CRUDE NAPHTHALENE
apparatus — Same as used under H17.1
method — The residue above 200° C. obtained in
Test F8 shall be transferred to the copper beaker,
cooled to 15.5° C, and held at this temperature for
30 min. It shall then be filtered and pressed as de-
scribed under Hi 7. The weight of dry solids divided
by the specific gravity of the original oil gives the per
cent by weight of crude naphthalene.
TEST FIO DETERMINATION OF BENZOL AND TOLUOL
apparatus — Distillation apparatus shown in Fig.
XVI. Partial condenser distillation apparatus shown
in Fig. XVIII. We shall be glad to furnish a detailed
drawing of this apparatus to any who desire to pro-
cure the outfit. Three thermometers, o° to 200°. pre-
viously standardized, and accurate to at least 0.5°.
One thermometer, 700 to 120°, graduated in 0.2° inter-
vals. One thermometer, 110° to 1600, graduated in
0.2° intervals. Three graduated cylinders, capacity
100 cc. One separatory funnel, capacity 2 liters.
Westphal balance. Hempel distillation apparatus
shown in Fig. XVII. Steam distillation apparatus.
reagents — Sulfuric acid, 60° Be\, commercial. Sul-
furic acid, 66° Be., commercial. Caustic soda solu-
tion, 10 per cent. Pure toluol, boiling within 1V20
C, sp. gr. at 15.5° C. not less than 0.870.
method: Preparation of Sample — 100 cc. of the sam-
ple to be analyzed shall be distilled following the pro-
cedure of E5. A larger sample of the oil, accurately
measured at 25 ° C, shall now be distilled, using a
Hempel column and collecting the fraction boiling be-
low 1600 C. The difference between this fraction and
the original sample shall be noted as "heavy oil."
The size of sample taken shall be so regulated by the
results obtained in the preliminary boiling test that
about 1000 cc. are obtained in this distillation. If the
preliminary distillation shows 90 per cent or more at
1600 C, the Hempel distillation may be omitted.
Acid Wash — The fraction up to 160° C. shall now be
washed in a separatory funnel with 1 per cent by vol-
ume of 6o° Be. sulfuric acid, care being taken that the
oil is kept cool during the washing. The acid sludge
shall be drawn off and the oil washed with three suc-
cessive portions of 2 volumes each of 66° Be\ sulfuric
acid, the acid sludge being drawn off after each wash-
ing. The oil shall finally be washed with a dilute
solution of caustic soda and this drained off. The
washed oil shall be put into a steam distillation appa-
ratus and distilled with steam until no further oil
comes over. The upper oil layer shall be carefully
separated from the water in a separatory funnel and
■This JOUUTU., 10 (1918), 916.
measured at 25° C. The difference between this vol-
ume and the volume before washing is noted as "loss
in washing" and represents unsaturated hydrocarbons.
The refined fractions so obtained should consist en-
tirely of benzol, toluol, solvent, and possibly saturated
paraffin hj'drocarbons.
Elevation
Fig. XVIII — Assembly op Partial Condenser
If the preliminary distillation showed less than 40 per
cent distilling between ioo° C. and 120° C, this refined
fraction should be mixed with an equal volume of pure
toluol before being subjected to analysis. In this case
the quantity of material originally taken for analysis
need be only about half that normally necessary, since
the volume of the total oil to be fractionated should
be 700 to 1000 cc.
Fractionation of Material — The refined fraction,
which should approximate one liter, shall now be
introduced into the 1V2 liter bulb of the partial con-
denser apparatus. The tank of the partial condenser
shall be filled with a high boiling oil agitated by means
of a small motor-driven agitator. The oil in the tank
shall be heated up to 70° C. and the distillation of refined
oil begun. The material in the flask shall be kept
boiling vigorously so that the flame under the partial
condenser may be turned off and the temperature con-
tinue to rise from condensation of vapors. The dis-
tillate shall be collected in 100 cc. cylinders, these
being changed when nearly full, brought to a temper-
ature of 25° C, and measured. As the temperature of
the oil approaches 8o° C. the distillation will very nearly
stop and when very near the temperature of 80 ° C.
a sudden increase in the rate of distillation will he
noticed. This is when the benzol begins to come over
in large quantities. The receiver shall now be changed
and all fractions up to this point combined. This shall
be called Fraction A.
The distillation shall be continued, allowing the
temperature of the oil in the oil hath to gradually
rise. The rate of distillation will gradually slacken
until just below no'C, when it is again practically
stopped. At about this temperature the rate will
again suddenly increase, the toluol coming over.
When about 50 cc. of n ' itled beyond
this point, the receiver shall be again changed and the
fractions between the benzol cut and the toluol cut
combined into Fraction B.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. u
As the temperature of the oil bath continues to rise
the rate of distillation will again decrease and will
suddenly increase when the xylol boiling range is reached
at about 13 7 ° C. The third cut shall be made when
about 50 cc. of this material have distilled over. The
distillation shall be stopped at this point, this com-
bined fraction being Fraction C. It is generally neces-
sary during the latter part of the distillation to place
a small flame under the oil bath to take care of loss
of heat by radiation. The entire time for the frac-
tional distillation should be about 2 hrs.
Pa etur Ton/a.
Curve I — Test F10. Distillation of Benzol-Toluol Mixtures
Interpretation of Results — 100 cc. portions of Frac-
tions B and C shall be submitted to distillation follow-
ing the procedure of E4, temperatures being observed
at start, 50 per cent off, and dry. The distillation of
Fraction B shall be made using a 700 C. to 1200 C. ther-
mometer, and the distillation of Fraction C using a 1 io°
C to 1600 C thermometer. All temperatures shall be
corrected for barometric reading; the correction factors
for one millimeter of difference being as follows:
Fraction B — 0.0450 C; Fraction C — 0.0500 C.
Fraction A should contain no toluol and shall be
regarded as benzol.
Fraction B is a mixture of pure benzol and toluol
with a very small amount of xylol. Its composition
shall be estimated by reading on Curve i, giving the
boiling tests of benzol-toluol mixtures, the percentage
of toluol corresponding to the temperature at which
50 per cent of the material was distilled off. The dry
point of the distillation shall then be compared with
the dry point curve of Curve 2 and the per cent xylol
estimated. This percentage shall be deducted from
the toluol. (This fraction should not contain more
than 2 per cent of xylol.) From the percentage com-
position of the fraction so obtained and from its vol-
ume the actual amount of benzol, toluol, and xylol in
it are figured.
Fraction C shall be similarly distilled and the per-
centage of toluol in it obtained from Curve 2 by the tem-
perature at which 50 per cent was distilled off. This
fraction should contain nothing but toluol and xylol.
The actual amount of toluol is calculated from this
figure and the volume of the fraction. From these
figures the total volume of benzol and toluol in the
original oil are determined. The toluol figure so
tained must of course be corrected for any pure toluol
added before the fractionation.
Correction for Paraffin Hydrocarbons — If paraffin hy-
drocarbons are present in the original oil they will of
course appear along with the benzol and toluol and
their presence here can be corrected for. This cor-
rection is made by determining the gravities of the
three fractions, B, C and D, accurately at 15.5° C. by
means of the Mohr-Westphal balance following the
procedure of H4.1 Assuming a specific gravity of
0.884 tor pure benzol. 0.871 for pure toluol, and 0.860
for pure xylol, the theoretical gravity of the three frac-
tions can be calculated as follows:
0.884 X per cent benzol 4- 0 .871 X per cent toluol
100 theoretical gravity of fraction
The specific gravity of the aliphatic hydrocarbons
corresponding to the three fractions would be, respec-
tively, 0.720, 0.730, and 0.740. The percentage par-
affin in the fraction can now be calculated as follows:
Theoretical sp. gr. of the fraction = a
Actual sp. gr. of fraction ' = b
Sp. gr. of corresponding aliphatic hydrocarbons = c
Per cent aliphatic hydrocarbons in fraction =
The per cent paraffin so obtained must of course be
corrected for in the benzol and toluol figures.
gjtesf — , , i 1 i ■ ' 1 ; i H~~H -H
/
/
/ '$' /
/ s*y /
l iV U
y >]
/ <«5-
/ >
' y ^"
/ x ^
tT JJ-ttT
""! , iM
PtGCetT TOLUOL
Curve 2— Test Flo. Distillation cfl? Toluol-Xylol Mixtures
precautions— Care should be taken throughout all
the operations that proper precautions are taken to
prevent loss both in distillation and in handling.
Corks should be tight and the distillate kept cool and
covered as much as possible. For making cork con-
nections, shellac is recommended.
reporting results — All results obtained are fig-
ured back to the original oil as follows:
Volume of constituent X 100
il volume of oil
= per cent constituent
The Barrett Company
17 Battery Place. New York City
This Journal, 10 (1918). 911.
Dec, i 918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
1013
A NEW ILLUMINATOR FOR MICROSCOPES1
SECOND PAPER
By Alexander Silverman
Received September 25, 1918
Since the publication of the first paper2 about one
year ago, a number of important improvements have
been made in the illuminator3 for microscopes therein
described.
tor also reduces the heat traveling towards the objec-
tive. Both lamps yielded a light of much greater
intensity than any hitherto employed. Results obtained
will be discussed later.
The lamp reflector is placed at an angle of 45 ° to
the plane surface of the stage. Low power objectives
may be an inch or more above the stage, so a tube
has been designed which may be clamped to the
stage. The lower end of the tube will support the
, lamp at a constant distance from the object under ex-
amination and the objective may be raised or lowered
inside the tube. The inner surface of the tube is dull
black.
A shutter may at times prove desirable to cut the
light off from one-half of the circular source. The
experimental shutter employed for this purpose is a
dull black disk which covers half of the lamp and is
attached by prongs which are held by the lamp. De-
tails are sometimes visible by this method which are
obscured when the entire lamp is bare.
The illuminator may be attached to a microscope
together with a vertical illuminator, thus affording a
comparison of the separate effects of oblique and \ er-
tical light on an object. There is a marked difference
in the appearance of metallurgical specimens under the
two illuminators, the new one facilitating the study of
depressions and showing details not hitherto re-
vealed. In blow-holes and pits the slag content, etc.,
may be seen. The pits appear black by vertical light.
In the first paper the lamp holder was attached to
the tube of the microscope by a clamp. In the newer
form (Fig. 1) three fingers fasten the holder directly to
the objective (Fig. 2). The fingers are iris-like in
operation and are controlled by springs, so that it is
possible to attach the illuminator to any objective.
The lamp described in the earlier paper was a 6 volt,
0.7 ampere unit operated by dry or storage cells. The
new lamp is a 9 volt, 0.7 ampere unit of blue (day-
light) glass and gives about 50 per cent more light.
A rheostat has been devised which screws into an
ordinary lighting socket. The rheostat has three taps,
107 volt, 112 volt, and 118 volt. A rheostat for 220
volt circuits is in preparation. If a greater light inten-
sity is desired one can connect with a lower voltage
tap. This is of advantage in photography. The nor-
mal voltage connection suffices for visual work.
Recent experiments with a colorless, one ampere i,;
volt lamp show that it can be employed safely. The
lamp was placed in the holder, clamped to
objectives, and allowed to run continuously for half an
hour, a period of time far exceeding any employed in
actual operation. The objectives were not af
although the lamp carried an overvoltagc of
cent. Further, a colorless 0.7 ampere, 20 voll
was silvered instead of enameled. The sil
tor reduces the amount of heat radiated towards tin-
objective. Blackening the outer surface of the
1 Presented at flic Cleveland Meeting of the
Society, September II, 1918.
! This Journal, 9 (1917), 971.
•U.S. Pet. 1,267,287. Van. Pat. 185,283. nd lor. iK
patents pending.
Fio. 2
us, etc., with light-absorbing surt
or none of i
ili . I ii.l.T i hi new lamp a weall h
seen which a
Should one wish to employ the new illuminator alone,
and remove the vertical illuminator, ii is necessary to
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 12
extend the draw-tube of the microscope to about the
176 mm. point for clear images, as most microscopes at
present on the market are corrected for the normally
interposed vertical illuminator.
Questions have arisen repeatedly regarding the use
of a lamp of such low wattage for photomicrography.
Experiments conducted in the writer's laboratory prove
that good results are obtainable with the 0.7 ampere,
q volt daylight lamp with 8 and 16 mm. objectives
and those of lower power, when the eyepiece is removed.
With the colorless 0.7 ampere, 20 volt silvered lamp or
the one ampere. 13 volt lamp it >s unnecessary to
remove the eyepiece, as the light intensity is ample to
yield clear images on the ground glass.
Focusing may be facilitated by greasing the ground
:^lass with a little vaseline, subsequently rubbing it
is dry as possible with a cloth. Bronzes, highly
polished ball bearings, enamel, paper, etc., have been
photographed in this way. The best results were
obtained with Hammer Ortho extra fast and Hammer
Ortho nonhalation plates.
Figs. 3, 4, s, 6, 7 and 8 show results obtained with
the 0.7 ampere, 20 volt silvered lamp with exposures
of from 15 to 30 seconds, using a 16 mm. objective and
10X eyepiece. Fig. 3 is a blue enameled steel;
4, a steel casting, 0.37 carbon, not pressed or heat
treated; 5, an iron-zinc alloy obtained in zinc manu-
facture; 6, a piece of blue cover paper; 7, a piece of
cloth; 8, a cast iron specimen.
In conclusion, the writer wishes to express his appre-
ciation to the scientists in various fields who have
experimented with the new device and made sugges-
tions which have resulted in valuable improvements in
methods of application.
School of Chemistry
Univbrsity op Pittsburgh
Pittsburgh. Pa.
A SPECIAL STOPCOCK FOR DROPPING LIQUIDS AR-
RANGED FOR EQUALIZING THE PRESSURE ABOVE
AND BELOW THE OUTLET IN THE STOPCOCK1
By Harry L. Fisher
Received June 4. 1918
The stopcock described herein was designed in con-
nection with a generator for carbon dioxide which was
to be ussd alternately with pressures below and above
atmospheric in the final preparation of cupric oxide and
for the determination of nitrogen by the Dumas
method according to the modification of Fieldner and
Taylor.5
Ordinarily an outside tube connecting the top of the
reservoir of acid with the upper part of the container
of the carbonate is used. In this new apparatus the
connection is made by means of an annular groove in
the key of the stopcock so that no matter which i
position the key occupies there is always communica-
1 Presented at the Boston Meeting of the American Chemical So-
ciety, September 10-13. 1917
' Fieldner and Taylor. This Journal. 7 (1915), 106.
Dec, 1 9 1 8 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
1015
tion between the atmosphere in the lower flask and the
atmosphere in the upper flask. One arm of the stop-
cock is extended until it opens above the liquid in the
upper container. The liquid enters at an aperture
in the lower part of this extended arm and is de-
livered through a small glass tube sealed in at this
opening. The entire arrangement is more clearly-
understood by a glance at the accompanying diagram.
Two different styles were made, using the same
principle in each.
Fig. 1 — Longitudinal Section
Fig. la — Cross Section at Centsr
Fig. 2 — Longitudinal Section
Additional Dimensions
Fig. 1
Mm.
Length of stopcock barrel 35
Outside diameter of inner tube 5
Inside diameter of inner tube 3
Outiide diameter of outer tube 10
Inside diameter of outer tube 7
I wish to acknowledge my thanks to Mr. W. Wiegand
of the firm of Eimer and Amend, New York City, for
his interest and skill in making these two stopcocks.
Laboratory op Organic Chemistry
Columbia University, Ngw Yore City
A NEW TIMING DEVICE FOR SIMPLIFYING THE THER-
MOMETRIC READING OF CALORIMETRIC
DETERMINATIONS
By Cbas. A. Myers, Jr.
Received May 18, 1918
At the beginning of the war the chemical laboratory
of the New York Navy Yard was called upon to do all
the chemical analyses of coal used by the fleet and its
auxiliaries in the northern district. This wrought a
tremendous increase in the work which the laboratory
in normal times was expected to do; but notwith-
standing the increase in the number of analyses it was
essential that there should not be any sacrifice in the
accuracy to which these operations were ordinarily
accustomed. The writer, who has for some time
been engaged in the work in question, has developed
an electrical timing device for calorimeters which he
believes would be of great assistance to anyone called
upon to determine calorific values under such circum-
stances, where radiation factors are involved.
One of the chief advantages of this timing device is
its absolute accuracy in giving the operator the exact
second at which to read the thermometer. The in-
strument, moreover, relieves to an almost unbelievable
If the flasks arc used as shown they must be securely
fastened by clamps close to the lips. The upper flask
can be filled through a funnel attached by means of a
piece of rubber tubing. The liquid will flow down
the inside walls and not drop into the extended tuba.
The arrangement and kind of flasks can be changed as
desired, and it is bi at the- apparatus will be
of service elsewln
ratOT who may be called
upon to make constant readings over an extended
period of time. With this device it is no longer
necessary to divide attention between the stop watch
thermometer, first looking at one and then
the other, as an audible warning signal is given 5
before the time to read, and a second signal
moment at which the readin taken.
ioi6
THE JOl RNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 12
A further advantage is that almost any number of
calorimeters may be operated at one time by this
device, it being simply necessary to have the signals
loud enough to be heard by all of the operators.
The device consists of a clock put out by one of the
large photographic supply houses which has a large
second hand making one complete revolution every
minute. On the face of this clock are cemented four
platinum-foil squares arranged so that contact will
be made 5 seconds before the minute and half-minute,
and again exactly on the minute and half-minute.
Contact is made by a fine platinum wire soldered to the
second hand of the clock. Two buzzers are used to
give the signals, one of high pitch and the other low.
The writer selected the high-pitch buzzer to give the
warning signal 5 seconds before the time to read
and the low-pitch buzzer for the signal to read. As
the buzzers consume a relatively large amount of
current it is impossible to make contact for them
directly through the platinum wire and the contacts
really operate two relays and these in turn pass the
A -clock
B - DouBLt-THRow switch
C-Relat for Buzzer "j."
D- — ■• - -F-
E- S- SECOND WAB«|BSlBujZtR
F-READIN& BUZ.ZE.R
&- CUT -OFF Switch
Fig. Ill
current through the buzzers. The relays are made
from common nails about i'/j in- long turned down
in a lathe and wound with eight layers of No. 36 double
silk covered copper wire. A small piece of platinum
is soldered to the end of one of the magnets of each
relay ( the one furthest from the hinge) and this makes
contact with another piece of platinum soldered to the
armature, thus closing the circuit to the proper buzzer.
The relay magnets and their supports are mounted
on a hard rubber base which insulates the armature
from the magnets when current is not flowing through
the latter. A double switch is provided to cut out the
half-minute readings when these are not desired and a
single point switch to shut off all readings. The de-
tails of the wiring are shown clearly in Fig. III.
Chemical Laboratory
Navy Yard
Brooklyn, N. Y.
ADDRL55E.5
SOME APPLICATIONS OF PHYSICAL CHEMISTRY IN THE
COAL-TAR INDUSTRY
By Wilbert J. Huff
This paper will be divided into two distinct parts, the first
of which deals with volume relations in solidifying creosotes,
while the second applies to the vapor densities of coal-tar frac-
tions.
I — VOLUME RELATIONS OF SOLIDIFYING CREOSOTES
Since liquid coal-tar products are regularly sold by volume,
the exact determination of the variation of volume with tem-
perature is of great economic importance to both distiller and
consumer. The standard temperature for oil measurements
is usually 6o° F., although in the case of creosote oil ioo° F.
has been somewhat generally adopted. Since it is obviously
' Read before- the New York Section of the Society of Chemical In-
dustry. May 24, 1918.
impossible to bring tank car quantities to the standard tem-
perature before gauging their volume, the shipper determines
the volume at the shipping temperature and calculates the vol-
ume at 6o° F. by means of a coefficient of cubical expansion;
the receiver invoices at the temperature at which he happens
to get the car and calculates by means of the same coefficient
to the same temperature.
Now the trade has found it difficult to obtain concordant re-
sults between measurements taken at shipping and receiving
points on creosote oil in tank cars and tank vessels. The dis-
crepancies have in some instances amounted to as much as
5 per cent of the volume of oil handled.
Adjustments, however, were necessary not only in company-
consumer shipments, but also in inter-plant shipments and
even in inventory calculations at the same plant. Clearly,
something was wrong.
Some earlier work on volume relations in creosote oil was car-
Dec, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
1017
ried on by Mr. H. E. Lloyd, of The Barrett Co., and the results
obtained by him, although not conclusive, fully indicated the
need for a more searching investigation into the problem.
One of the first things that attracted my attention while con-
sidering this problem was the mental haze of the practical em-
ployee when dealing with the simple mathematical relations
involved in calculating coefficients of cubical expansion. I have
found by personal observation and experience that very many
chemists (strange to relate) do not relish the mental gyrations
of the mathematician. Even engineers had been somewhat
lax, for the trade had been making no correction for the coeffi-
cient of cubical expansion of the container and in consequence
did not calibrate the container at any definite temperature.
Although it is a repeating of very elementary matter, I will
give here the formulas which are used in determining and ap-
plying coefficients of cubical expansion.
The change in volume per unit volume per degree change in
temperature is called the coefficient of cubical expansion.
Thus:
V, = V,(i + at)
in which a is the coefficient of cubical expansion.
Since in practice the container is always an expanding ma-
terial, the apparent expansion is less than the real. The con-
tainer expands, partly compensating for the expansion of the
material.
The relations are generally expressed by the equation
A + C = T
in which A is the apparent coefficient of cubical expansion of
the liquid, C is the coefficient of cubical expansion of the con-
tainer, while T is the true coefficient of cubical expansion of the
liquid.
This relation is strictly true only for the case where the con-
tainer is always kept full, as in most specific gravity determina-
tions with a pycnometer. When the liquid rises and falls in
a steel container the deviation in the apparent coefficient from
this relation can be shown mathematically to be about 3 parts
in 100,000 per degree Centigrade.
This is of course much smaller than the errors of measure-
ment in practice. Consequently the form given above (which
is exceedingly simple) may be regarded as correct for all cases.
One of the first points considered was the relative effects of
the variations in conditions in a large container, as for instance:
stratification, sedimentation, inequalities of temperature, etc.,
which would not be pronounced in the small volume of a specific
gravity bottle in which the previously used coefficient of cubical
expansion of creosote oil had been determined. Accordingly,
a hollow iron container with a capacity of about 2V2 gal- was
fitted with a screw cap carrying a glass tube to serve as the
neck of a pycnometer, and with three thermometers placed at
different distances from the center. This was placed in a 50-
gal. water bath provided with an agitator, and suitable burners,
etc., for applying heat. A glass pycnometer was placed in the
same bath in order to duplicate the work in a small volume.
No essential difference in results was obtained, showing that
the difficulty lay somewhere else.
The iron container was twice calibrated with water and the
apparent coefficients of expansion of water in iron calculated
over the ranges: 15.5-25° C, 25-38° C, 38-60 C, 60-80° C.
These observed values were then subtracted from the true
zero ones, giving by difference the coefficient of cubical expan-
sion of iron. The mean of one set of experiments gave 0.000037
for this, while the mean of another set gave 0.000036. These
results were considered very satisfactory, for the accuracy of
0.00001 to 0.00002 is from 5 to 10 times more than tin pre-
viously accepted coefficient of cubical expansion of creosote oil
(0.00079 Per degree C). The subsequent work with oils, how-
ever, was probably not quite so accurate, for the oils were much
harder to bring to a constant volume, probably because of a
lower heat conductivity.
In the work with oils the container was filled at 80° C. and
later made to the mark at about 60 °, 38°, 25°, 15.5°, with
weighed water. The pycnometer was made to mark with the
oil when used with liquid oils. With solid oils it was filled at
80 °, made to mark with oil at 60 °, and then with water at
temperatures below 60 °.
Two creosote oils were examined: A refined liquid creosote
oil, hereafter referred to as No. 1 , which does not solidify in
' the range covered, and an oil representing a commercial grade
of creosote oil according to the standard specifications of the
American Railway Engineering Association, hereafter desig-
nated as No. 2, which gave a small amount of crystals at 15 .5°
C. The coefficients found for these oils checked very satisfac-
torily in duplicate experiments both in the large container and
the small specific gravity bottle. The mean true coefficients
found (0.000703 for No. 1 and 0.000724 for No. 2) were slightly
lower than the previously accepted value (0.00079). The
apparent coefficients in steel tank cars would be even lower.
These findings, however, did not explain the discrepancies en-
countered in practice.
The thing which was especially interesting to me was the
absence of variation in the coefficients with temperatures.
The coefficient of cubical expansion of water shows a huge
variation over the interval in question (i5°-8o° C). This
variation amounts to from 200 to 300 per cent.
The influence of salts upon the coefficients of cubical expan-
sion of these oils was next studied by salting the same oils with
pure naphthalene for a limpid point of about 40° C.
This mixture consisted of No. 1 oil 71.5 per cent and naph-
thalene 28.5 per cent by weight. A little more than 30 per
cent distilled below 235° C. In the upper ranges this mix-
ture contracted regularly with descending temperature and
gave the coefficients found for the original No. 1 oil. At tem-
peratures below 38° C, however, the crystallization caused an
enormous shrinkage. In one experiment the average coefficient
between 38° and 25° was from 4 to 5 times as great as that for
liquid creosotes. In a duplicate experiment the value was
from 3 to 4 times as great. This abnormal behavior was always
exhibited below 38°, that is, below the temperature at which
crystallization became important. The expansion and con-
traction observed was of course the resultant of three factors:
(1) The mechanical expansion or contraction of the liquid
phase. (2) The mechanical expansion or contraction of the
solid phase. (3) The volume change due to the solution or
crystallization of the solid phase. Now it is very probable
that the coefficient of cubical expansion of solid naphthalene
is much less than that of the liquid creosotes. (Beilstein re-
ports the density at 40 and 15° C. to have practically the same
value.) Undoubtedly these huge and irregular coefficients are
caused by the crystallization.
Naphthalene dissolves in creosote oil with an increase in
volume; 1 qt. of naphthalene and 3 qts. of a salt-free creo-
sote oil will make more than 1 gal. of mucttlM
The magnitude of the volume change accompanying the solu-
tion or crystallization is unfortunately very large. Some of
the experimental results obtained showed that an error of as
much as 404 gals, per 10,000 gals, in a temperature interval
from 110° to 70° C. might easily be possible, using the old
coefficient of cubical expansion.
The word "unfortunately" is used advisedly. The process
of crystallization and solution is very slow when contrasted with
the mechanical expansion or contraction of the solid and liquid
phases. In consequence, with varying temperatures there
may be, and probably often will be, incomplete equilibrium be-
tween the two phases. Accordingly, the observed volume of
the total will vary a great (leal with the Immediate past history
ioi8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No.
of the mixture. It is only to be expected, therefore, that the
results obtained in measuring the coefficient of expansion of a
partially solid oil will not check unless great care and a suffi-
ciently long time is allowed to elapse at each temperature to
insure that the crystallization or solution has attained equi-
librium. Since in actual practice it is very often not desira-
ble or even possible to maintain a tank or tank car at exactly
the same temperature for a sufficiently long time to insure
equilibrium between the solid and liquid phases before deter-
mining the volume, the practical value of such a coefficient,
even when obtained with the greatest care, is very doubtful.
Variations in the amount of crystallizable substances from time
to time in the same grade of oil will seriously affect the coeffi-
cient.
Another possible complication is the variation in the charac-
ter of the crystallizing solid. Suppose anthracene crystals ap-
peared instead of naphthalene crystals, what would happen then?
This point was investigated by dissolving crude anthracene
in the No i oil. The work was abandoned, however, because
of the extremely slight solubility of this compound in this oil;
less than 5 per cent of the solid gave a limpid point of 400 C,
while it took more than 28 per cent of naphthalene to give the
same limpid point With less than 5 per cent of anthracene
present, it was not deemed worth while to examine the volume
relations of the mixture.
Naphthalene is, of course, the most important solid. More-
over, its similarity in physical properties composition, and
structure to other coal-tar compounds leads one to believe
that an analogous effect occurs when most of the other solids
crystallize or dissolve.
The magnitude of the error, and the inherent insurmount-
able obstacles encountered when one attempts to predict the
volume of an oil at a temperature at which it may be partly
solid, may ultimately revolutionize the present practice of
buying and selling oils by volume.
The simplest expedient, of course, is to buy and sell by weight.
At present, however, such a departure is so radical that it
is practically impossible.
It is probable that a temperature of too" F. will be widely
adopted as the standard, displacing the 6o° F. of the present,
since at ioo° F. the creosotes are liquid. The trade situation
was somewhat amusing — we had been buying and selling
gallons at 6o° F without knowing the volume relations which
relate 60° F to the customary temperatures of trade.
II — THE VAPOR DENSITIES OF COAL-TAR FRACTIONS
Although the composition of the higher fractions from the
distillation of coal tar has long been a subject for study and
speculation, and many of the compounds present have been iso-
lated and identified, the quantitative composition of these in-
teresting mixtures still remains a matter of mystery. It is
probable, however, that the number of compounds present is
very great.
This question was of especial concern to the engineering de-
partment of The Barrett Company in the design of large capacity
condensing systems, since a knowledge of the exact composition
would give by a simple calculation the vapor density of any
fraction, and in turn a key to a design for a condenser em-
bodying economical construction ami efficient fractionation.
It fell to the lot of Mr. Gainey and myself to investigate
these vapor densities which, of course, could be ascertained
only by experiment.
Of all the methods for determining vapor densities, the
Victor Meyer is the lust suited for a problem of this kind,
since it is applicable over a wry wide range of temperatures
and pressures and is equally useful for pure compounds and
mixtures < ther methods afford souk- of these advantages
but not all. Thus the 1 mums could In- used at the tempera-
tures and pressures desired but, unfortunately, is inapplicable
to mixtures whose components have different boiling points.
The Dumas, you will remember, calls for a light glass bulb
drawn to a point and weighed. The substance under examina-
tion is introduced and the bulb is then placed in a constant
temperature bath while a certain pressure is applied (generally
atmospheric) until the bulb is completely filled with vapor
and the excess vapor has been removed. The bulb is then
sealed off and weighed. In this procedure, the lower boiling
components would probably be removed from the bulb before
the higher were completely vaporized, so we could not employ
this to determine the vapor densities of fractions of the coal-
tar distillate. The Gay-Lussac-Hofmann method, which
consists in the introduction of the substance into the vacuum
above an upright barometer, can be employed equally well for
pure compounds or mixtures, but is unfortunately limited to
temperatures where mercury exerts no appreciable vapor ten-
sion, that is, below 1500 or 1750 C, and could not be used for
coal-tar fractions whose boiling points in some cases are higher
than 4000 C.
For the sake of a clear understanding of what follows, I will
recall the principles which are involved in the Victor Meyer
method of determining vapor densities by air displacement.
In its simplest form the apparatus for this method consists
of a long "pear-shaped" glass tube provided with two side-
tubes near the upper end. One of these side tubes is connected
through a rubber tube to a gas burette. The lower portion of
the glass pear is brought to a temperature which is sufficiently
high to insure complete volatilization of the test material. This
material is then introduced through the stoppered opening in
the top of the tube and dropped at the proper moment by with-
drawing a glass rod thrust through one of the side tubes. Upon
reaching the hot portion of the pear, the material vaporizes,
driving up ahead of it and over into the gas burette, air, which,
of course, does not condense and can be measured as soon as
the system reaches equilibrium. From a knowledge of the
weight of the material, the volume of the air driven over into
the gas burette, and its temperature and pressure, it is possi-
ble to calculate the density of the test material in the vapor
form.
A modification of the method consists in attaching the pear
to a manometer and measuring the increase in pressure at
constant volume caused by the volatilization of the test ma-
terial. This modification is particularly useful when it is neces-
sary to employ a diminished pressure to insure complete vola-
tilization, since it is very difficult to measure an increase in
volume in a system maintained at a very low pressure.
Such considerations are so preliminary and general that I
feel compelled to apologize for presenting them to you.
The first consideration peculiar to the vaporization of these
coal-tar distillates was the question of coking. To throw sud-
denly these hydrocarbon-containing mixtures upon glass sur-
faces heated to several hundred degrees Centigrade without
cracking and coking them was indeed a problem, especially when
the boiling point ranges ran above 350° and 4000 C. De-
composition by cracking and coking had to be guarded against
in the distillation which gave the test fractions also.
A composite oil typical of the distillate from coal tar. be-
tween first runnings and hard pitch, was distilled in the labora-
tory and cut to 500 C. fractions. This oil began boiling at 200'
C. under atmospheric pressure, and the distillation was continued
under atmospheric pressure for two fractions until the vapor
temperatures reached 3000 C. In order to forestall cracking,
the distilling bulb was then allowed to cool and an absolute
pressure of 50 mm. of mercury was then applied. The oil be-
gan to distill once more at 1 75 ° C. and continued to distill until
a temperature of 370° C was attained. Further heating only
produced decomposition into non-condensing vapors. In all, S7
per cent of the oil distilled and five 500 fractions were obtained. I
Dec, 191S TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Vapor Density Results
Compound Formula
Naphthalene di-hydride C10H10
Naphthalene CioHs
Methyl naphthalenes C11H10
Diphenyl CuH.o
Aeenaphthene C.2H10
B.
P
at 760
mm
200-210'
C,
218° C.
240-243'
C
254° C.
278° C.
Anthracene C14H10
Methyl anthracene CuHh Ai.ove 360° C.
Chrysene CuHio 436° C.
A number of preliminary experiments were made to fix a
method of procedure. It was found advisable to confine the
test fractions in Woods metal bottles which melted immediately
and threw the entire contents in contact with the hot glass
surface. Glass containers were unsatisfactory; the lower boil-
ing material passed into the vapor form, reached the cool por-
tion of the tube and condensed, before the higher boiling ma-
terial was completely volatilized. Considerable time was
spent investigating the possible coking of the fractions in the
Victor Meyer pear. The criterion for coking was the appear-
ance of the glass pear, which became badly discolored with
carbon when the pear was heated much above 360° C. In a
mercury vapor bath (giving a temperature of 357 ° C), how-
ever, no coking occurred. This was extremely fortunate, for
it permitted the use of this vapor bath as the heating agency,
giving a temperature which remained constant without atten-
tion and was easily reproduced.
The discovery that coking became serious above some 360 °
or 370° C, coupled with the fact that two of the fractions had
boiling point ranges higher than this when under atmospheric
pressure, rendered it imperative that an apparatus capable of
measuring vapor densities under diminished pressure be fitted
up.
Accordingly a flexible mercury manometer made from two
glass tubes, a rubber hose, and an upright meter stick was
attached to the Victor Meyer tube and the tube evacuated
to a low pressure by means of a vacuum pump, the fraction
volatilized and the change in pressure noted. The calculations
for this low pressure work involved a factor known as the tube
constant. This constant depended upon the size of the tube;
thus, when a tube of a certain size is used half as much pressure
is developed by a given amount of vapor as is developed when
a tube of only half that certain size is used, i. e., in a tube twice
as large, only half the pressure is developed.
The constant was determined by volatilizing in the tube at
the temperature of the experiment a known amount of a com-
pound possessing a known vapor density. The determina-
tion of this constant proved quite a bugbear to Mr. Gainey and
myself. The slow deliveries on special glassware due to war
conditions compelled us to blow our fragile tubes at the blast
lamp. We would often carefully standardize a tube in dupli-
cate (consuming several days in the operations) only to break
it by some accident before we could use it for a determination.
You can then imagine us sweating over the blast lamp in the
heat of last August while we blew another tube, hoping for
better luck the next time.
In the above table are given our vapor density results, com-
pared with the calculated vapor densities of a few well-known
hydrocarbons whose boiling points place them in the range of
the appropriate fraction.
The vapor densities of the first two fractions were obtained
by determining the volumes of air driven into a gas burette
in the standard Victor Meyer method, the third was obtained
by packing the tubes with hydrogen whose rapid rate of diffu-
sion into the volatilizing oil insured complete vapoi
the last two were obtained by the use of the manometer and
the low pressure system. Mercury vapor was used as the heat-
ing medium for all the experiments.
Vapor density
at 0° C. and 760 mm.
per cc.
Obtained
Calculated
0 00179 I
0 00572 }
0.00634 J
0.00688 i
0.00688 I
0 00794
0.00858
0.00902
0.00579
0.00667
0.00691
0.00S67
0.1047
Coal-Tar Fractions
Boiling Point Ranyes
199-249° C. under 755 1
249-296" C. under 755 mm. Hg
180-229° C. under 50 mm. Hg
229-276° C. under 50 mm. Hg
276-322° C. under 50 mm. Hg
ACKNOWLEDGMENT
The experimental material presented in this paper was ob-
tained while I was engaged in physical chemistry research for
The Barrett Company and is the product not only of my own
efforts but also of the efforts of Mr. John Gainey, who so ably
assisted me in the latter part of the work and who is now still
engaged in extending it. My debt, however, is not limited to
Mr. Gainey. It is owed to the administrative officers of the
Research Department of The Barrett Company, to whom I
extend my thanks for direction and advice.
It is my belief that physical chemistry is afforded no richer
field for research and development than the coal-tar industry,
so economically important to the country in peace and so promi-
nent in the scheme of modern warfare. My short connection
with this industry has led me to believe that it is only in its
infancy and that many of its latent possibilities will be real-
ized by the aid of physical chemistry.
Research Department
The Barrett Company
New York City
A MANUFACTURER'S EXPERIENCE WITH GRADUATE
CHEMICAL ENGINEERS1
By S. R. Church
Received July 15, 1918
The writer has often objected to the term "Chemical Engi-
neer." It seems to place chemical engineering alongside of
civil, mechanical, and electrical engineering as one of the natural
divisions of the engineering profession. We would define
chemistry as the science of the composition of materials, and
engineering as the science of works. Chemistry is therefore
the fundamental science, as without some knowledge of the
composition of materials an engineer will fail.
For the purpose of this paper the writer will consider that a
chemical engineer means a graduate in engineering who has had
at least four years of college training at an institution recognizing
the engineer's need for knowledge of the composition of ma-
terials
During the past two years we have employed in our General
Manufacturing Department 100 student engineers. These men
were employed, not to occupy at first a definite position, but to
undergo a course of study in the Company's business and to
fit themselves for positions in the engineering, operating or
experimental departments of manufacturing, after a period of
at least 6 months' training. In this training period the men
receive instruction in the form of lectures on various products
and processes by heads of the manufacturing and technical staff
and are given special assignments for personal study of a prod-
uct, process, manufacturing unit, laboratory, or works experi-
ment, etc.
It is our purpose to have at all times about 10 to 20 men in the
training period and at the end of about 6 months to assign a
student to a definite position, or release him. or under certain
conditions to continue Ins probationary period.
The men are in general selei te I with a view to their apparent
fitness to become assistant superintendents or foremen, but In R
■Paper submitted for the Proceeding of the Aiihm
for the Advancement of Science.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. Xo. 12
few cases men have been employed because of special ability
in line of designing apparatus, etc. These men ranged from 21
to 40 years of age and from newly graduated students to men
having 10 years' industrial experience. Among them are civil
and mechanical engineers, but a majority are graduates from
chemical engineering courses. In the number are graduates
from most of the engineering colleges and universities east of the
Mississippi.
While the results have of course been almost as varied as the
number of men engaged, yet certain observations have been
made which may reflect the influence of the institutional training
received by these men. It seems especially true of the chemical
engineers that they lack ability to correctly evaluate measure-
ments. They seem to have been taught that a result must be
accurate to a certain decimal fraction, and attempt to apply
this without reasonable sense of proportion.
They are usually careful and fairly good in the technique of
experimental work but lack ability to discern from an unsuccess-
ful experiment the suggestive feature that should point the way
to further experiments. They appear not to have been im-
pressed with the importance of qualitative results. They often
fail to discern the value of an indicative result in an experiment
that has partly or wholly failed in its primary object and lack
the imagination which enables the exceptional student to see
his way through an accumulation of data that to another is only
material for a progress report.
At this point we might note that ability to write a really good
comprehensive report is not possessed to a satisfactory degree
by the majority. In some cases this is so serious that men
entirely capable of doing good work have utterly failed to make
good. Instructors do not perhaps realize to what a large extent
the graduate will, during his first 6 months or year in com-
mercial life, be judged by his written reports.
Another common failing of many of our chemical engineers
is poor training in the graphic presentation of experimental
data. The superiority of a well-planned chart over a series
of tables, both in facility of interpretation and suggestiveness,
does not appear to be well grounded in them. Many lack a
good sense of relative values, such as enables the exceptional
man to consider a sample of material, the report of a day's
run on a still or mixer, only for what it is worth; and to avoid
the loss of time and effort that the average student would ex-
pend on carrying out elaborate analysis or calculations on a
premise having obvious limitations. A greater familiarity on the
student's part with the general principles common to works
practice might seem to be reasonably expected. As for in-
stance that the value of accuracy in laboratory analysis depends
absolutely on the accuracy with which the sample represents a
given lot of material, and that knowledge of the limitations of
accurate measurements or sampling outside the laboratory
may save much time in eliminating refinement of procedure
and calculation.
The writer is of the opinion that a comprehensive course in
Chemical Engineering should cover at least 5 years and pref-
erably six He realizes that for various reasons, not the least
of these being the tremendously increased demand for chemical
engineers, many colleges will not extend their courses to a 5 or
6 year basis. He urges that especially in the shorter courses
every effort be made to give the student a sense of values, a
better touch with the work, and to develop his imagination so
that he will see in the problem assigned to him not the possi-
bility of solving the value of X and writing Q. E. D., but of
coming to his employer with a suggestion that by raising the
temperature of this reaction we may obtain an increased yield of
5 per cent; or by putting a worm conveyor here we can eliminate
the work of two men.
The writer is a firm believer in long and thorough schooling,
in painstaking, and in accuracy; but the man who has not been
taught at school to eliminate the unnecessary in his work and
way of thinking will be slow to perceive the value of the short
cut in manufacturing.
It is too much to expect that all of the defects herein noted.
which are in some degree common imperfections in all of us,
can be cured in a 4, 5, or 6 year college course. The writer felt
that criticism rather than commendation would be more help-
ful and has purposely omitted reference to the many good
qualities possessed by the men we have employed.
The Barrett Company
17 Battery Place
New York City
CURRENT INDUSTRIAL NLW5
By A. McMillan, 24 Wettend Park St., Glalgow, Scotland
BURMESE MONAZITE SANDS
The Geological Survey of India reports that an analysis made
of the monazite sands of Mergui and Tavoy in Tenasserim,
Lower Burma, taken from 28 locations, shows but 0.18 per
cent of thoria in the heavy concentrates, which is equivalent
to 0.00216 lb. of thorium oxide per cubic yard of the ground
sampled and adds that such minute fraction is, of course, of
no practical utility.
INCANDESCENT LAMPS
A new edition of their "Incandescent Lamp Handbook,
No. ia" has been sent out by the British Thomson-Houston
Co., London, and contains particulars and prices of lamps
of both the vacuum and the half watt types, for standard light-
ing service. In addition, there is a great deal of information
about the terms and definitions used in the lamp trade and the
photometric units and standards employed in illuminating
engineering. The lumen, which has been adopted as the unit
of light rating for electric lamps by the engineering societies
and lamp manufacturers of the United States and Canada and
by the leading British lamp makers, is explained at considera-
ble length and examples are given showing how lighting calcula-
tions are simplified by its use.
ALUMINUM AND ITS ALLOYS
Dr. W. Rosenhain, lecturing recently in London on aluminum
and its alloys, said that the possibilities pf aluminum and its
alloys depended primarily on the lightness of aluminum. Light-
ness of itself, however, was of little value. What was required
was a combination of great strength and lightness. This had
been attained to an astonishing degree in the modern aluminum
alloys. There were many moving parts in light machinery,
such as cycles and sewing machines, in which the extensive use
of light alloys would appear to offer a great field for real ad-
vance. For air craft and other purposes, it has the impor-
tance of a "key" industry.
PEAT FUEL
A method of treating peat for fuel purposes proposed by-
Mr. S. C. Davidson, Belfast, consists in disintegrating it, mix-
ing it with 15 per cent of pitch and submitting it to a pressure
of at least two tons per square inch in a hydraulic press. In
this way its bulk is reduced to about one-third and it comes
out of the press in a solid block looking like polished hardwood
which burns with a steady yellow flame. From his experi-
ments, Mr. Davidson believes that the peat will require only
a short period of air-drying before treatment by this process.
Dec, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
OILS FROM COAL TAR
Prof. Carl Goldschmidt, of Essen, and R. Friedlaender, of
Berlin, both members of the recently formed Kohlchemie Kon-
sortium, have recently issued a pamphlet, says the Oil and Color
Trade Journal, 54 (1918), 962, calling attention to the advan-
tages and possibilities of their so-called coal Liquefaction
Process, i. e., the synthetic manufacture of benzolenes, lighting,
engine, and lubricating oil from lignite, generator tar, crude
oil, and crude oil derivatives. They mention the cracking
and separating processes of Zern, Walther, and Graele, whereby
the constituent parts of tar boiling at higher temperatures are
transformed into benzolenes. They also deal largely with the
somewhat related Bergin process whereby with the aid of heat
and hydrogen, both benzolene and lighting oils are obtained
of a quality equal to those obtained from natural sources.
The chief primary raw material, lignite-tar, can be obtained
from the heating of generators, for instance, in lignite briquette
factories in which some 20,000,000 tons of lignite are worked
up, glass kilns, paper mills, and the like, in which some 12,000,-
000 tons are used to fire boilers instead of being gasified. In
this way alone, 1,500,000 tons of tar are obtained for distilla-
tion, etc., and the gasification of lignite alone would suffice to
supply Germany with all her requirements in enriched oil prod-
ucts. Until such gasification plant has been established every-
where steps should be taken to secure a steady importation of
raw oil and more especially of raw materials for the synthetic
manufacture of benzolene and oil. Such a raw material is a
by-product in Russian, Roumanian, and Galician distilleries,
which use large quantities of it as an inferior kind of fuel.
SODA AND SULFITE PULP
The Paper Maker, quoting from a German contemporary, states
that in the sulfite process certain residues of the wood substance
survive and are found in the paper, whereas by the alkaline
process the purification is far more complete. These residues
of cell content which are particularly to be found in the cells
of the medullary rays, may be made visible by staining, and
serve for the differentiation of soda and sulfite pulps. The
residues are found even in bleached sulfite pulps and exist as
aggregates or chains of small spherical elements. Their stain-
ing capacities depend on the presence of resin. With an aqueous
alcoholic solution of Soudan III, with a little glycerin added,
they are stained red; with zinc chloride-iodine solution, sulfur-
yellow. In preparing the pulp for microscopic examination
care must be taken to avoid dissolving the resin by the caustic
soda. Medullary ray cells are so numerous that the presence
of even 5 to 10 per cent of sulfite pulp in a mixture can thus be
detected. For quantitative estimation of mixtures of sulfite
and soda pulps a solution of rosaniline sulfate with a little
alcohol and sulfuric acid is of service. The contents of the
pitted pores are strongly stained in the cum of the sulfite pulps,
but not with soda pulps. The inner side of the fiber wall of
sulfite pulp is more strongly dyed than the outer. In zinc
chloride-iodine solution the sulfite fibers show a characteristic
variation.
FERROMANGANESE MANUFACTURE IN SPAIN
There is a note in the Bolelin Oficial de Minus by the engineer
of the district of Vizcaya saying that for the refining of the 294,000
tons of steel produced, 3,000 tons of ferromanganese are re-
quired. The article formerly was imported from abroad, but
the extraordinary rise in the price of this product from 312
pesetas per ton in the year 1913 to over 2,000 pesetas at present
and the almost insuperable sea transport difficulties have made
it indispensable to have it produced in Spain and the necessary
furnaces and engineering plants have been provided for the
purpose.
ELECTRIC LAMP INDUSTRY IN FRANCE
In a recent communication to the Bulletin of the Societe In-
ter aalionale des Electriciens, Mr. A. Larnande remarks that the
present capacity of French glow-lamp factories amounts to 15-20
million lamps per annum, but this figure may be doubled in
the near future. The tonnage required for the transport of
material in this industry is small, as one ton of ore will provide
sufficient material for 3,000,000 lamps. An important element
in the manufacture of gas-filled lamps has been the production
of argon required for the smaller types. This gas is now being
made in considerable quantity by the process of Mr. Claude.
GERMAN ENTERPRISE IN THE UKRAINE
The firm of Krupp, says Engineering, is usually ready to step
in where there appears to be a chance of a business worth doing.
Its latest move is the formation of a concern with a capital of
$5,000,000 and an additional guar?nteed capital of $16,000,000
for the purpose of exploiting Ukraine industrially. A number
of undertakings in the iron and steel industry in the machinery
and electrical branch are also interested in the venture. At
the same time, a number of banks and financiers have formed a
syndicate for the exploitation of Ukraine financially and, it is
added, in the matter of railway construction. The latter con-
cern has so far a capital of only $1,000,000 and its works will, in
the first instance, be confined to a close study of the country
and the possibilities it offers. The fact that the two concerns
have not joined hands has caused some surprise, but the reason
is stated to be that the banks wanted a concern which com-
prised all industries and did not find it expedient to cooperate
with one which only represented a limited number. The two
undertakings are understood not to clash in their Ukraine ven-
tures.
ANNEALING ALUMINUM
At a recent meeting of the Institute of Metals held in London,
Mr. R. J. Anderson, in a paper on the above subject, urged con-
sideration of the possibility of abbreviated exposure at various
temperatures being able to confer workable properties upon
cold-rolled aluminum sheet, with less fuel, in a shorter time,
and with a smaller percentage of defectives in subsequent draw-
ing. He gave particulars of a number of experiments in which
various gauges of cold-rolled aluminum sheet were exposed for
three minutes at a series of temperatures varying from 4000 to
5000 C. He concluded that exposure to 3700 C. for 24 hrs.,
as is usual in commercial mill practice, is unnecessary, and that
the lighter gauges can be softened by such an abbreviated ex-
posure as three minutes at 400° C. He stated that tests in the
mill have demonstrated that aluminum softened by short ex-
posures to heal fulfils the draw-press requirements and that
the percentage of defective shapes is smaller than with similar
metal annealed for. say, 24 hrs. at 3700 C. In the manipulation
of certain shapes by the draw-press the sheet is ordinarily cut
into circles or other geometric patterns and annealed before
being drawn and. in 011c instance, the number of defective
shapes was observed to be 30 per cent out of 4,400 blanks drawn,
1 In 111. lal having been annealed by long exposure. As a test
of the effectiveness of long annealing, 200 cold-rolled No. 22-
gauge circles were annealed for three minutes at 475° and drawn
by a typical draw-press operation into a given shape; only one
defective Ited from rupture in the press, or a scrap loss
of 0 s per cent, Other tests on sheets of various gauges vrhlCD
hail been annealed for relatively short times, ranging from 5
to (in mill . gave sera)) losses of less than one per cent in all cases
He pointed out, that, if the annealing can be effected by rela-
tivelv short exposures, a continuous annealing furnace for alum-
inum becomes possible, provided certain minor details can be
overcome
THE JOURNAL OF INDUSTRIAL ANDmENGINEERING CHEMISTRY Vol. io, No.
TANNING MATERIAL IN GERMANY
The German Government, according to the Chemical Trade
Journal, is offering prizes for the solution of the following three
problems:
(i) A method for the currying and dressing of leather with-
out the use of cod oil and other fish oils, as these oils are almost
unobtainable.
(2) A substitute for chrome salts for the production of leather
of the nature of chrome-tanned leather, also a substitute for
the production of leather by means of other mineral salts or
mineral salts combined with vegetable material which will pro-
duce a leather similar to combination-tanned leather.
(3) A method that can be used during the war which will
result in a saving of vegetable tanning material without affecting
the quality of the leather so produced.
A first prize of $5,000 and a second prize of $1,250 are offered
in these cases. JThe offer is an indication that Germany is
badly suffering from a lack of fish oils and grease for stuffing
leather and from a shortage of chrome salts and vegetable
tanning materials. The judges include Prof. E. Fischer, Dr.
Fahrion, the oil chemist, Prof. Paeffler, a leather trade chemist,
and five tanners.
JAPANESE CAMPHOR
The manufacture of camphor in Japan proper and Formosa
during the fiscal year ending March 31, 1918, amounted to
10,678,800 lbs., of which 10,362,000 lbs. were sold by the
camphor monopoly office. The latter figure shows a decrease
of 4,989,600 lbs., as compared with the preceding year. The
monopoly office has received many offers from Europe and
America, but is unable to execute all because of the growing
demand for camphor on the domestic market. Of 10,362,000
lbs. sold by the monopoly office, 4,276,800 lbs. were supplied to
camphor manufacturing companies, 831,600 lbs. to celluloid
companies, while 343,200 lbs. were placed on the market.
The remainder, 4,910,400 lbs., were shipped abroad. The
authorities, says the Chemical Trade Journal, are now en-
couraging the export of manufactured goods and preventing
the shipment of camphor as far as possible.
NICKEL STEEL
In a recent issue of the Eleklrotechnische Zeitschrifl it is stated
that the magnetic properties of nickel steel caused it to be
used by the German navy for the construction of parts of ships
near to the compass in order to prevent variable effects on the
compass field. It has, however, recently been stated in the
same journal that this use of nickel steel is by no means new and,
in fact, is a very costly method of obtaining good compass
fields. On this account the method has been almost completely
discontinued. The compasses are now almost entirely gyro-
scopic. The use of this type of compass has the further advan-
tage of saving large quantities of nickel which is so expensive
and difficult to obtain.
GAS-FIRED BRAZING TABLE
A self contained, gas-fired brazing table designed by the
Davis Furnace Company, Luton. England, especially for the
aeroplane industry and certain toolmakers' work, has a fire-
brick table 3 ft. 10 in. by 1 ft. 6 in., mounted on a strong cast
iron stand. There are two blowpipes, 19 in. long with 7/i» 'n-
nozzles and 1 in. heads, each swivel-mounted on a vertical pillar
with suitable adjustment for height. For lateral adjustment the
pillars slide along a machined bar of square section fixed hori-
zontally along the front of the table. The air-blast is provided
by a high pressure blower mounted on a shelf below the table
and driven by belt or by electric motor. The gas and air are
conveyed to the blowpipe by flexible metallic tubes, each with
its separate main control cock.
A CHINESE PERFUME PLANT
The plant locally known as Lang-rhoa (Cymbruiium end-
folium), one of the finest orchids known, is regarded in China
as the queen of flowers. An account of its cultivation has
recently been published by Yang-Tsen Kia, as its scent is so
exquisite that it holds great possibilities for the perfume indus-
try. So valued is this plant that the greatest care and atten-
tion are devoted to its cultivation. Each plant is grown in a
separate pot, the temperature during the day being maintained
at i7ct020°C. and during the night at 12° to 140 C. Ventila-
tion must be abundant and only rain water used for watering.
The perfume is very powerful and very sweet and it is possi-
ble that the essential oil may be distilled from the plant, when
it would become available to European perfumers.
THE SCHOOP METAL-SPRAYING PROCESS
From Zurich comes the news of considerable improvement in
the Schoop spraying process, says Engineering. Instead of
melting the metal, which is generally applied in the shape of
wire by the oxyhydrogen flame or the blow-pipe, electric fusion
is now used and is said to be both simpler and cheaper. The
pistol apparatus is used as before, but two ends of the wire are
placed in the pistol instead of one and they are approached to
one another as electrodes of an electric circuit. When the
arc strikes, the wire fuses and the air current tears the fine
metallic particles away. Zinc sprays in particular have been
produced in this way, according to an article in Z. angeic.
Chcm. The electric heating may be simple, but the preven-
tion of the oxidation of the sprayed metal will probably be as
difficult as before.
NEW SOURCE OF ALCOHOL
Among the substitutes for fibrous material to which German
manufacturers have been compelled to have resource is the
black millet (Sorghum vulgure). It has found a place in paper
making and it is now suggested as a material for the production
of alcohol. The food value of the grain is high, between that of
peas and lentils, so that its cultivation, which costs no more
than that of wheat or rye, is recommended to the farmer on
the ground of its being a paying crop. If the straw be used as
a source of cellulose or of alcohol, the crop becomes doubly-
valuable.
BICHROMATE MANUFACTURE IN SWEDEN
The British Commissioner at Stockholm reports that a large
new factory has just been started at Malmo for the production
of bichromate, chrome alum, and other chromium salts. The
undertaking has been financed by Swedish and Danish inter-
ests and the proposed scale of operation is sufficiently great
to render importation of these materials unnecessary. Hitherto
these have been imported from Germany and the United King-
dom to the value of $1,220,000 per annum.
BEECHNUT OH. IN THE NETHERLANDS
The Dutch Minister of Agriculture, Industry and Commerce .
plans to increase the supply of edible oils in the Netherlands by
using the domestic beechnut crop. He estimates that between
2000 and 2500 metric tons of these nuts can be collected and
that this amount of raw nuts will yield 300.000 to 400,000 kilos
of oil, a valuable addition to the dwindling stocks of edible oib {■
in the Netherlands. The Zulphen Gazelle reports that school
children are to be used to gather the nuts. Owners of private
lands on which beechnuts are gathered will receive 5 per cent (.
of the sums paid to the gatherers and will have the right to pur-
chase cattle cake prepared from the pulp of the nuts from their
own property.
Dec, 1018 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
SCIENTIFIC SOCIETIES
FRENCH SECTION, AMERICAN CHEMICAL SOCIETY
Chemical Warfare Service
A. P. 0. No. 717, American E. F.
October 21, 1918
Dear Doctor Herty:
I know that the members of the American Chemical Society
will be interested in the following communication from Prof.
V. Grignard. The letter is self-explanatory.
Ministere de l'Armement
et des Fabrications de Guerre
Inspection des Etudes
et Experiences Chimiques
Paris, September 28, 1918
My dear Colonel:
Allow mp to acknowledge with thanks the receipt of the docu-
ments which you sent to my laboratory: Doctor Parsons' letter
to you, including membership blanks for the American Chemi-
cal Society, and the charter which was granted by that Society
for the formation of a French Section.
I can assure you that French chemists will welcome the op-
portunity to cultivate advantageous relations with their American
colleagues, and I am convinced that the French Section of the
A. C. S. will shortly become a worthy complement to the Ameri-
can Section of the Societe de Chimie Industrielle.
I feel deeply honored by the privilege of transmitting the char-
ter to the new Section, and I shall do everything in my power
to further this matter.
With sincere regards, believe me to be,
Most cordially yours,
V. Gric.nard, Directeur
I.ABORATOIRB CHIMIQUE MlUTAIRB DB LA SoRBONNB 1
We are all extremely busy just now, but arrangements have
been made whereby the French Section of the American Chemi-
cal Society will be formally organized.
Our colleagues at home will also appreciate this note from
M. Landowski, President of the Societe des Chimistes Francais,
of which the General Secretary is M. Arpin, and the Treasurer,
G. Sellicr.
Societe des Chimistes Francais
Paris, July 4, 19 18
Colonel:
At this solemn hour, when all France, as a single soul, pro-
claims her eternal gratitude to the Sister Republic whose citizens
have unanimously responded to the call of their immortal
President by coming to the aid of Right and Liberty, the Societe
des Chimistes Francais, recognizing the importance of the r61e
played by chemists in the liberation of the world, wishes to trans-
mit, through the Chief of the Chemical Warfare Service of the
American Army, fraternal greetings and an expression of its
admiration for all American chemists who have placed their
learning and their lives at the service of liberty
Receive, Colonel, the assurance of my very highest regards,
The President,
H. Landowski
With kindest regards from Major Hamor and myself,
Cordially yours,
R. P. Bacon, Colonel, C. W. S.
Chief of Technical Division
IOTA SIGMA PI
The object of the Society is not to take the place of Sigma
Xi, American Chemical Society, or any other organization,
but is to foster and stimulate interest in chemistry among
college women and to advance the standard of personal accom-
plishment in chemical fields, thus making the work of women in
science more effective.
The spirit, of the society may perhaps be best illustrated by
quoting a few suggestions made by the National Convention:
1 — In view of the present emergency, the Convention recom-
mends that every member of Iota Sigma Pi encourage all young
women to train themselves for scientific work.
2 — In order to further the ideals of this organization the
Convention recommends that every member, as soon as she is
able, join the American Chemical Society.
The national officers elected were as follows:
President: Mary L. Fossler, Nitrogen Chapter. University of Nebraska.
Vice-President: Miriam E. Simpson, Hydrogen Chapter, University
of California
Secretary: Edith Hindman, Oxygen Chapter, University of Wash-
ington.
Treasurer: Icie Macey, Tungsten Chapter, University of Colorado.
Editor: Helen Keith. Iodine Chapter. University of Illinois.
A directory of the Society is in the process of preparation and
will be sent out to each Chapter when completed. Bulletins will
also be sent out from time to time by the Editor.
The first national convention of the lota Sigma Pi, an honorary
•chemical society for women, was held at the University of
Nebraska, Lincoln, Nebraska, in the new Chemistry Hall, just
•opened. Five of the eight chapters which constitute the frater-
nity at present were represented by delegates.
SOCIETY OF CHEMICAL INDUSTRY
NEW YORK SECTION
At the meeting held in Rumford Hall on Friday evening,
October 25, 1918, Major W. H. Dudley of the British-American
Anti-Gas Liaison Office spoke on "Gas Warfare both Offensive
and Defensive." Having already printed the address of S. J.
M. Auld on "Methods of Gas Warfare,"1 covering more or less
the same ground, we do not give Major Dudley's address in full;
but because of the interest of the explanations they contain,
his introductory remarks are given here..
It is now a matter of common knowledge that the Germans
introduced the use of asphyxiating gases in warfare by launching
clouds of chlorine gas against the unsuspecting and unprepared
Allies in the neighborhood of Ypres on April 22, 1915. In spite
of this well-established fact they have from time to time at-
tempted to saddle the Allies with the responsibility of having
started this latest horror of modern warfare. On July 17,
1918, their official wireless sent out a communique to this end.
This wireless message stated that "the idea of using poison
gas originated with the British Admiral Dundonald."
The Admiral Dundonald to whom reference is here made is
probably an Admiral of that name who was born in 1775 and
died in i860. He was a man of considerable chemical knowledge
and warned the British Government of that date that it might
be possible to employ asphyxiating gases in warfare. This
possibility has, of course, been known to all the Great Powers,
and because of this knowledge the Hague Convention of 1899
expressly forbade the use of gas. It remained for Germany
deliberately to violate this stipulation in the early stages of the
present war.
The German wireless message further states that "poison
gases were first used in the war on March I, 1915, by the British
and French, whereas the French and British Army could not
announce a German attack with poison gas until April 24,
1915." (The attack actually took place on April 22, 1915.)
This statement is a deliberate lie and will not bear examination.
It would mean that in a period of about eight weeks the Germans
developed sufficient material in organization to carry out an
ive uas attack. This is an absolute impossibility.
The best an WB to this typical German falsehood is given in
tin- words c >f Lord French, who, as Commander in Chief of the
British Army at the time, in his report of May \. i<>i5, stated
:is follows: "A week before the Germans used this method
(gas attack) they announced in their official communique thai
wc win- making use of asphyxiating gases. At that time there
appeared to be no reason for this astounding falsehood but
1 Tmn fOtlBHAt, 10 (1918), 297.
1024
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 12
now, of course, it is obvious that it was part of the scheme.
It shows that they recognized its illegality and were anxious to
forestall neutral and possibly domestic criticism."
It is interesting to realize that as late as July of this year the
Germans should still be attempting in a most unscrupulous way
to place the responsibility of initiating gas warfare to the account
of the British and French.
At this meeting the Section unanimously adopted the fol-
lowing resolution :
Whereas, for many years the German Government has
fostered the chemical and other "key industries" with the
object of reducing other nations to dependency upon her, and
at the same time rendering herself independent of others, and
establishing industries which in time of war would give her an
enormous advantage over those she was planning to attack and
rob; and
Whereas, from the very beginning of her outrageous attack
upon the civilized nations of the world, Germany has pursued
a deliberately organized course, having for its object the per-
manent economic injury or destruction of other countries who
had been her competitors in the world markets; and
Whereas, in pursuance of this course Germany has delib-
erately
First: Stolen and carried away whatever machinery she
could;
Second: Destroyed whatever machinery and property she
could not steal or carry away;
Third: Deported or destroyed communities of skilled
artisans;
Fourth: Murdered or by studied brutal ill treatment per-
manently injured prisoners of war and innocent civilians, so as
to deprive their countries of their skill and labor; and
Whereas, it is essential that the allied civilized nations must,
as a matter of self- protection, render Germany impotent to do
further harm from a commercial as well as from a military
standpoint, and prevent her, although defeated on the field of
battle, from reaping a commercial triumph as the result of her
deliberate wickedness above referred to;
Therefore be it Resolved, that the Xe%v York Section of the
Society of Chemical Industry requests that the proper authorities
of the various allied governments take special note of the above
facts, and insist that Germany, where possible, be compelled to
restore the stolen machinery and other property, or replace the
stolen property and also whatever machinery or property has
been destroyed by equivalent machinery or property taken from
German factories; and that they furthermore see to it that all
allied industries are fairly and justly safeguarded under the
ultimate terms of peace, against the machinations of an insidious
and conscienceless enemy, whose express intention is to reduce
other nations to industrial subservience and dependence.
NOTES AND CORRESPONDENCE
AN OPPORTUNITY TO HELP THE FRENCH
A communication has been received from the chairman of
the American Ouvroir Funds, 681 Fifth Avenue, New York
City, asking the American Chemical Society to interest itself
in securing among our members the "adoption" of children
whose fathers were technical men and who have been orphaned
by the death of their fathers, graduates of l'Ecole Polytechnique
who have fallen at the front.
In using the word "adoption" it is not, of course, intended
to bring the children to this country and immediately adopt
them, but to help the officers' widows educate their children
and bring them up as nearly as possible as would have been
done had their fathers lived. L'Ecole Polytechnique has among
its graduates some of the most illustrious, brilliant, and educated
men in the French Army. Many of them were poor and are
among those whose families now most need help. Although
America has lost many men on the French front, they have,
with few exceptions, been young men without dependents;
so that we shall not realize in our own country the great need
which has come to France where the families in many cases have
been left entirely dependent.
The American Ouvroir Funds will be glad to submit to any
responsible man or woman who requests it, a selection of histories
. of these technical graduates, with photographs of the war or-
phans, the citations of their fathers, their addresses, and all the
facts which may be of interest to anyone who may "adopt"
them. "Adoption" means an annual expenditure of from $100
to $250 a year, according to the circumstances of the family
whose child is "adopted." Such expenditure will insure board,
lodging, and education for a child whose father has been killed
in the war.
The following is taken from a communication sent to the
Secretary by the American Ouvroir Funds:
SAVING CHILDREN FOR THE FRANCE OF TO-MORROW
In the midst of the overtaxing burdens of war, men and
women of France, with international reputations for achievement
and character, have found a way, in spite of the thousands of
orphaned children, to give a personal accounting of individual
cases. These men and women are associated with various
French Societies long established for the care of orphans.
The American Ouvroir Funds as the chosen link with Amer-
ica of these well-established organizations in Prance, stands for
the French idea of personal service and contact. It asks for
a definite sum for an individual orphan, whose story one may
have, whose photograph may be seen, to whom one may write,
from whom letters will be received. No personal gift contributed
as an individual fund through the American Ouvroir Funds is
lost in the great melting pot of war benevolence. It goes
straight from you, bearing your message of sympathy, and brings
directly back to you a warm response from the heart of a child
or its mother. What a glorious privilege for us to be able to
help preserve to these children their precious heritage; to give
as nearly as possible to them the same chance for environment
and education that would have been theirs had their fathers
lived. We give with some understanding of the varying in-
dividualities and circumstances of the orphaned children.
Our aim is not just to clothe and feed a quantity, but to pre-
serve to France, the children of the men who in even.' rank of
life represented what was most noble, most worthy, and most
high-minded in their country.
We reward a brave soldier who has died fighting for the
cause of individual liberty, of America as well as of France, by
giving the aid that is necessary to keep his child out of an insti-
tution and under the protection of the mother or some loving
guardian; to be brought up in his own faith and to the same
opportunities that would have been his had the free life of France
been uninterrupted by war.
France asks nothing of the world. She fights, has fought
from the beginning of this war, with her eyes to the front, her
head lifted proudly in the assurance of the righteousness of her
cause. She says nothing of what she has endured, utters no
outcry for the needs of her people. France is proud. But we
who look on must see those scars, must see the needs of her
orphaned children, and, since she is fighting for America's
cause also, they should be as our orphans.
We owe it to her that her children at least should not suffer,
should not lose, as the result of their father's sacrifice, one jot of
that individuality, that freedom, which is the priceless heritage
of their country.
The above was brought before the Advisory Board of the
American Chemical Society at its recent meeting in New York.
The Secretary was instructed to inform the members through
This Journal. "Adoption" can be made by a number of indi-
viduals as well as by one individual, if necessary.
President and Mrs. Nichols have "adopted" the first two,
a boy and a girl. Four others are promised. You will be put
in personal touch with the child you "adopt."
Many American citizens, both men and women, have welcomed
the opportunity thus offered to relieve in some measure the bur-
den of the war that has fallen on the women and children of
France. The informal "adoption" of one or more of these little
children entails no obligation other than a contribution to
the child's maintenance for one year.
It puts the adopter into immediate personal relations with
Dec, iqtS THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
1025
a French family, and brings the joy of helping a little child to
become a worthy citizen of France.
The several French Societies transmit the full amount received
for the children, without deduction for expenses or cost of any
kind.
Local sections will please take up this matter. Members
may send to the Secretary, who will either choose for them or
seem l- the photographs of the children and history of the family
helped.
Charles L. Parsons, Secretary
NEW AFTER- WAR PREPARATIONS IN THE CHEMICAL
INDUSTRY OF GERMANY1
THE AGEEEMENT BETWEEN THE DYESTUFF TRUST AND
THE CARTEL OF EXPLOSIVES. REDUCTION OF THE TAX
ON WAR PROFITS IN FAVOR OF PRODUCTS MANU-
FACTURED FOR EXPORT. THE NEED FOR AN
INTERALLIED TECHNICAL ORGANIZATION.
The organization which has been called the German Dyestuff
Trust is already old; but recently its development has been
completed by an agreement with the Cartel of Powders and Ex-
plosives. This latter, before the war, was controlled by the
Nobel Trust Co. of London, but at the end of 1915 elimination
of the English company was effected by an exchange of the
German shares which it owned for English stock held by German
firms. The Cartel of Powders and Explosives then comprised
only houses of German nationality whose nominal capital repre-
sented a total of about 100 million marks. At the present
moment, however, the financial strength of the group is con-
siderably greater; the profits made, the reserves established,
and the enlargement of plants are all proofs. In fact, during
the war, such factories as the Bayer and Badische have produced
almost exclusively explosives, gases, and acids, and thesehavebeen
furnished as raw materials to companies manufacturing powders
and explosives. Hence the two cartels which have concluded
an agreement have an output of very similar products. There
is no doubt that the installations made and developed for the
manufacture of explosives, gases, and munitions will be main-
tained as they are, ready to function from the start of the next
war. Therein lies an urgent counsel of M . Rathenau, and German
technicians declare on every occasion that never before did they
begin a war with such an inferior industrial organization, that
it is necessary to be better prepared for the next one — a provision
for the future which will not prevent them from employing,
in the meantime, the factories and materials in the manufacture
of chemical and pharmaceutical products, synthetic perfumes,
etc. Thus, the aim and object of the organization of the Dye-
stuff Trust is to give its directors the mastery of trade, domestic
and foreign; it is to preserve this that the Trust has concluded
an agreement with the Cartel of Explosives.
Accordingly there is now in Germany a single concern selling
dyestuffs, chemical and pharmaceutical products, a single
purchaser of prime materials for these industries, and this Trust
is already assured of the ownership or control of several lignite
mines of importance. This concentration should permit the
reduction to a minimum of the cost price and the fixing of export
sales prices at a figure which will enable products to pass over
tariff barriers. Preparations for beginning exports when hos-
tilities have ceased are complete, reaching the point where the
merchandise is already packed and labelled, either in French or
English, while catalogues in both languages have already been
printed.
But the efforts made in Great Britain and France to establish
and develop the dye industry and manufacture of organic prod-
ucts, the rapid and unexpected development of this industry
in the United States and in Switzerland, have caused a feeling
of uneasiness in the Trust, and also, in the Imperial Govern-
ment, which considers dyes to be one of its best economic weap-
' Translation of an article in Chimie el Industrie for June I. 1918.
ons. Even those who rely on a free trade restocking Germany
with raw materials, in view even of guarantees in this respect
in the future treaty of peace, even these men cannot be ignorant
of the fact that in many foreign countries German products
will meet with hostility which no text of treaty will be able to
prevent. Hence they proclaim the necessity of still greater
production and at a lower price. The particular interest which
the Imperial Government takes in the dye industry has probably
still another cause due to the knowledge that it has become
the stockholder and associate of the great companies such as
the Bayer, the Badische, etc.
When it became necessary to enlarge the existing works and
to establish new factories equal to the task of making munition
of war, the State made the considerable advances of money
required, because the times were pressing, and it was impossible
to think of increasing the capital of the companies. At the end
of 1917, the majority of the firms belonging to the Trust had
increased the capital of their concerns 150 million marks in
round figures, the flotation of the new stock to take effect Jan-
uary 1, 1918. It is to be noted, however, that the Bayer and
Badische companies each asked for the listing on the Berlin
stock exchange of 18 millions of new stock and not 36 millions,
the amount actually issued. Similarly, the Gesellschaft fur
Anilinfabriken issued 12 millions and asked for the listing of
only 5.8 million marks. In view of the debt contracted by
these companies with the State and the zeal of the latter for the
interests of the public treasury, the natural conclusion is that
the repaying of the sums advanced by the Empire was effected
by remittance of new stock, which, of course, was not admitted
to dealings on the Bourse. The result is that the Empire has
made an excellent investment (the last dividend of the Badische
was 25 per cent), it will be represented on the boards of directors,
and becomes directly interested in the prosperity of these com-
panies. They are now certain that all the powers of the govern-
ment will be exerted in their favor.
The first result of this association is that, from this moment
the Imperial Government will grant the remittance of a large
part of the tax on war profits to the manufacturers of dyestuffs
and chemical and pharmaceutical products which are actually
being made for export as soon as hostilities have ceased.
Under such conditions the chemical industry of the enemy will
be in a position to produce merchandise of various kinds at a
price which costs the manufacturers nothing. From the first
day of peace they will export this merchandise and will be able
to deliver it in Great Britain, France, Switzerland, Italy, and
the United States at a price which will not represent even the
customs duties, however high, imposed by these different coun-
tries. The budding industries of the Entente nations will thus
be placed in a position in which it is impossible to live, and their
competition so much feared by the enemy will be killed in the
germ. The Germany monopoly once reconstituted and become
definite in aim, cost prices which are remunerative will be fixed,
and the products of its chemical industry will again serve as
excellent articles of "compensation" to obtain favorable treat-
ment for other merchandise.
We must nut deceive ourselves as to the grave danger pr
by this Machiavellian con pecially for Prance,
Croat Britain, and Italy, for in Switzerland and in the United
States the dyestuff indu
States possesses m\\ material! as compensation, such a-
and cotton, which will ins "f an economic struggle.
But in France ami Great Britain it is Bcarci ly likely thai manu-
facturers will be in a pc
utical products when peace is made. Industries which
utilize dyestuffs will find themselves in the presence of German
offers, ready for delivery at an extremely low price, whereas
British and French firmi will have, in tin- case of many articles
of manufacture, only promises or very high prices It is more
1026
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 12
than doubtful whether a considerable number of these con-
sumers will postpone business activity until the moment when
they will be able to obtain the products of national industry.
In every way all possibility of exportation will be extinguished,
Germany having recaptured her clientele in every country
where chemical industry has not been solidly established.
In France and Great Britain men are strongly individualistic
and opposed to concentrations of industry; wc talk readily of
good relations between commercial houses or the laboratories,
but the bonds between factories remain loose for the most part,
and those between companies belonging to different countries
are far more relaxed. In face of the German Trust which, thanks
to its organization, can sell at any price whatever, it is to be
feared that there are concerns of more or less financial strength,
several of which will manufacture the same article and will
perhaps compete with each other while other articles of mer-
chandise will be lacking. In this case tariffs are not a remedy,
for duties, however high, will be powerless to prevent the pene-
tration of articles which the Germans will be able to sell at an
iusignificant price and which cannot be supplied by other coun-
tries. We wish to point out that, in relying on high tariffs,
we may be mistaken, while their establishment against neutrals
will raise grave difficulties. It is well known that, for this
reason, the intervention of neutrals is part of the German pro-
gram.
Does this mean that we must be resigned, or expect everything
from the prohibition of imports of enemy chemical products?
Certainly not, but it is necessary to resort to energetic measures,
however rigorous they may appear to our habits of independence
and liberty.
The first thing to realize is the methodical re-allotment of
labor and the specialization of manufactures in the countries
of the Entente. For this purpose it would suffice if, in these
countries, the entire group of corporations which manufacture
dyestuffs, pharmaceutical products and derivatives were in
agreement to accept a central committee of technical directors.
This committee, knowing the needs of each country and versed
in the material and technical resources of its works and factories,
would introduce a special organization into each, of such a kind
that each product would be manufactured by one or two works,
which would permit the most economical production and an
output nearest to the centers of demand. The same technical
committee would effect likewise a specialization of the munition
factories before they are used for after-war purposes. Under
these conditions the business and administrative freedom of
all these companies would remain untouched, but the technical
direction would be the work of one board — a system which im-
plies the minimum of interference with the life of the most
individualistic of concerns. The technical committee would
all be experts trained to receive the communication of researches
made in the laboratories and to indicate those which appear to
them useful. It would seem that with such an organization
our manufacturers might arrive at a point where they could
make themselves independent of Germany in the matter of nearly
all the products which she counts upon supplying at the end of
hostilities, either directly or by the intermediary of a borrowed
neutral name. Then custom duties might be raised until they
reached a prohibitive level.
Measures of this order certainly constitute an assault on the
independence of corporations, but it must not be forgotten that
it is a question of life or death for our infant chemical industry;
it was permissible, in a rigorous sense, to hope for success in
face of the German trust, but before the perspective of a combine
which will permit the enemy to make a pretense of renouncing
dumping, under the guise of selling for almost nothing, the strug-
gle of isolated industries becomes impossible, and hence a tech-
nical organization is a necessity, we may even say, a duty.
R. Pi-tit
Professor of the Facility of Sciences of Nancy
THE AMERICAN DYESTUFF INDUSTRY AND ITS
PROSPECTS1
With the advent of 1918 the American chemical works, and
especially the dyestuff factories, were confronted with numerous
problems. Owing to the requirements of home and Allied
industries they found themselves in a difficult position, for,
despite all promises, they were not able to command a sufficient,
nor even a moderately satisfactory supply of the most im-
portant fundamental materials. Americans, induced by the
promises of company promoters, and with an eye to great ex-
pansion of the markets, have invested, since the outbreak of
the war, about 225 million dollars in dye works, and yet, as they
expressly give out, have produced only dyes which hitherto
have been made only in Germany. How much of this vast
sum has been actually paid in, it is not possible to judge, but it
may be admitted that the companies are very much "watered."
In order to provide security for this capital, those interested
clamor for a protective tariff, by which, after the war, they are
to be preserved from a destroying competition. The interested
circles point out that war requirements have diminished stocks
of raw materials throughout the world, so that the prices of
dyestuffs and technical chemicals even after the war will hold
at an abnormal figure. The same circles trot out the old fable
according to which Germany has accumulated important quan-
tities of dyestuffs and chemicals with which to inundate the
world's markets after the war. Experts, however, with keener
insight, do not support this view, suspecting that Germany
herself has experienced a certain shortage of raw materials for
this purpose. The greatest concern of the American producer
is the fear that, after the war, Germany will purchase large
quantities of raw materials in the United States. Although the
industry has a specious appearance, as if some of the leading
factories had achieved a fair amount of success in making some
products, the position of a portion of the industry is regarded
as insecure, and even as distinctly a hazard. A feeling of de-
cided irritation was observable when the Government in 1917
commandeered all supplies of methyl alcohol at a fixed price,
since methyl alcohol forms the basis of many dyestuffs. At
the same time the Government took over the entire output
of toluol, and all gas companies were required to set up ovens
for the preparation of tar products. In spite of the efforts of
the dye manufacturers, consumers complain that the prices of
dyes are still very unfairly differentiated from those existing
before the war. In addition to this, the quality of the dyes,
in the judgment of the textile industry', leaves much to be de-
sired; the textile products, especially for military purposes,
are not satisfactory, as their fastness to light and water is un-
certain.
The general opinion is that, so long as no foreign competition
breaks down its development, the American dye industry may
well he in a position to satisfy a demand restricted by defects
of quality and fastness. But in its present proportions the Ameri-
can industry has not grown up to the demands of fashion and
of other individual consumers, so that its development in 1918
will run in the grooves of the past year, and this means that
only staple dyes without much variety will be produced.
THE JOURNALS OF THE AMERICAN CHEMICAL SOCIETY
Editor of the Journal of Industrial and Engineering Chemistry:
It has often occurred to the writer that the journals of the
American Chemical Society show a peculiar dissimilarity in
the headings of the solid pages of reading matter, and might
possibly with slight changes be made a little more convenient
for one usitrg them in reference. Presumably the present
arrangement follows custom or precedent and is designed to
I Translation of an article reprinted in the Zcilschnfl fir antrxattiU
Chtmic. March 19. 1918. from the Norddeutsche Mlgemrint Zrilunr.
Dec, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
1027
give a balanced and neat appearance to the page, but probably
none of us will mind sacrificing a little in this respect, if neces-
sary, if there is a compensating advantage in using the journals.
The Journal of Industrial and Engineering Chemistry carries
on the left-hand page of reading matter its own name, the
volume, and number; 011 the right, the date and its name again.
The Journal of the American Chemical Society has on the left
the name of the author, and on the right the subject of the
article. Chemical Abstracts has the name of the journal on the
left and the branch of chemistry on the right.
Without going too far into specific suggestions, the writer
would like to see the headings of the pages arranged so that
one can get as far as possible the references without, for exam-
ple, turning back to the front cover to find the volume number
each time, and then perhaps having to translate a Roman
numeral. There is little difference in looking up one or two
references, but for a larger number it is distinctly easier to use
the Journal of Industrial and Engineering Chemistry than either
of the others. Even the addition of the volume number to the
pages of the other two journals would be a real convenience.
Without expanding too far, the point to be emphasized is the
rather strange dissimilarity of headings, each of which has a
part, but only a part, of the essential data used in index or
reference work. Could we not with little effort modify our
headings to fall in with the present spirit of efficiency and at
the same time answer all the practical and esthetic requirements
of the printed page?
Chas. F. Goldthwait
West Duluth, Minn.
October, 28, 1918
THEFT OF PLATINUM
The following notice has been sent us by Mr. G. D. Buckner,
chemist of the Kentucky Agricultural Experiment Station:
$100.00 REWARD
For the recovery of the platinum dishes and crucibles answer-
ing the following descriptions stolen from the Kentucky Agricul-
tural Experiment Station, Lexington, Kentucky, during the week
following October 17, 1918, or for information leading to the
conviction of the thief:
Platinum Platinum
Dish Weight Crucible Weight
No.
2 11.9750
3 11 .9703
10 16.0273
13 8.4319
18 15.8232
22 15.7905
26 15.7580
18.9421
No. Grams
1 46 4689
11 32.6709
12 33.0927
14 49 1097
15 48.6788
20 48.5347
22 48.3856
23 47.2223
The urgent need for this material at this time deserves your
earnest effort and cooperation in its recovery. Address
J. J. Reagan, Chief of Police, Lexington, Ky.
CHEMICALS FOR RESEARCH WORK
Editor of the Journal of Industrial and Engineering Chemistry:
In your issue of August 1 you were good enough to insert a
letter announcing that the Research Laboratory of the Eastman
Kodak Company were undertaking the preparation of chemicals
for research work, and asking the cooperation of the manufac-
turers of intermediate products and of organic chemists either
in the industries or the universities who were preparing materials
which might be of use to others or who had need of organic
reagents. As a result of that letter and of the endorsement of
the sections of organic and industrial chemistry at the Cleveland
meeting of the American Chemical Society we have received
a great deal of assistance and feel most grateful to the chemists
of the United States for the hearty response which they have
given to our request. The manufacturing concerns have proved
willing to supply us with the various raw materials and inter-
mediates which they produce, and a considerable number of
university and other research chemists have written to us offering
their assistance in preparations.
A special department of the Research Laboratory has now
been established under the name of the "Department of Synthetic
Chemistry," and has been staffed with women chemists, who
are proving most enthusiastic and capable in this work.
Up to the present time we have not found it possible to issi'e
a list of the chemicals which are available, though a considerable
number are now in stock on our shelves. The University of
Illinois has supplied us with the chemicals which it prepares.
We have already obtained a few from other sources. We have
prepared a number of new reagents ourselves, and we are engaged
in the purification of a number of intermediates, some of which
are purified with ease, while in the case of others the process of
purification is proving extremely difficult and expensive. We
hope to issue our Erst price list of chemicals by the first of Decem-
ber and shall be glad to receive applications for copies of thjp
price list when issued. At first it will probably be necessary
to issue new price lists monthly, adding reagents as they be-
come available.
It is our purpose to stock chemicals eventually of three grades
of purity. The first class will embrace chemicals only of the
highest purity which it is possible to obtain, and we propose
to distinguish these by the name of ''Eastman" chemicals.
In our first list we shall include chiefly these chemicals of the
highest purity, since the supply of these appears to be most
urgent. The second class will be prepared of the purity necessary
for the greater number of synthetic organic preparations. The
amount of purification which the technical product must undergo
will depend both on the technical product and on the reaction
for which it is generally used, and the greatest care will be taken
to see that the chemicals supplied under this class are really
suitable for the purposes for which they are likely to be employed .
We propose to state, as far as possible, their purity and the im
purities which they contain. We shall distinguish these chemicals
under the term of "Practical Synthetic" chemicals. The third
class will consist of crude technical intermediates should then-
prove to be a demand for these, as we expect will be the case
In Germany these technical intermediates have been supplied
by the firms who supply chemical reagents and for many purposes
it is advantageous for chemists to be able to obtain them in
small quantities. We find that the makers of intermediates
would prefer that we should retail them rather than fill orders
for small quantities of these materials themselves. We shall
designate these "Technical" chemicals. In some cases the
"Practical" and "Technical" products will naturally be identical.
Unless there is great objection shown to the course, we propose
to sell chemicals by metric weights only, listing them by the
hundred grams and kilogram. We believe that this will meet
with the approval of the majority of chemists, although up to
the present almost all orders have come in for pounds. We
have dealt with this by handling an order for 1 lb. as if it were
for 500 grams. If our action in this is not endorsed by our
prospective customers we shall be willing to alter it if necessary.
In this undertaking we regard ourselves primarily as serving
the chemists of the United States and especially the members
of the American Chemical Society, and we shall most heartily
welcome any criticisms or suggestions.
RliSltARCH I.AIIORATORY C. )'.. K. MBES
Eastman K<>i>ak Company
November II, 1918
COOPERATION BETWEEN MANUFACTURERS AND
UNIVERSITIES
£<it7or of the Journal of Industrial and Engineering Chemistry:
We are building up a collection of analyzed snniplos of raw
i and intermediate and finished products of our typical
I Industries, and expect to use these specimens as practical
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 12
material in our courses in quantitative and technical anal-
ysis.
It has been our experience that the work in analytical chemistry
is greatly strengthened by the use of such material, but at
present the time of most instructors is too occupied to devote
the time necessary to make the analyses required to check the
results of the students. The laboratories of many of our chemical
manufacturers make such analyses as a matter of routine,
and it would be a very helpful method of cooperation if they
could turn over to us and to other universities laboratory samples
together with their analytical data on the same. You have
advocated a closer cooperation between the manufacturers and
the universities and it appears to me that here is a chance for a
definite service involving little extra work on the part of the
works laboratory forces. Samples of one to two pounds are
sufficient for a year's supply, and different samples of the same
material are useful in diversifying the work of different students
of the same class.
We shall be glad to pay the transportation charges. The
standard samples issued by the Bureau of Standards are too
expensive for general use and their range is too limited.
We shall be grateful for any aid you can give us in this matter
and shall welcome any suggestions as to an efficient presentation
in the proper quarters.
R. E. Oesper
Associate Professor of Analytical Chemistry
University op Cincinnati
Cincinnati, Ohio
October 15, 1918
INVENTION PROBLEMS
The Invention Section of the General Staff of the United
States Army has submitted to the War Committee of Technical
Societies a list of seven problems requiring scientific and inven-
tive talent for solution. Problem V is of chemical interest and
is reprinted here.
PYROTECHNIC SMOKE SIGNALS
It is desired to secure, if possible, a suitable chemical substi-
tute for Red Saxony Arsenic now used for the manufacture of
Yellow Smoke Signals. The characteristics of such a chemical
are that it should produce the effect required, that it should be
procurable in large quantities, and that it should be perfectly
stable in combination with other chemicals, such as potassium
chlorate. The effect desired is a rather deep orange-yellow.
There is no objection to the use of dyes should these give the
effect required and be procurable in large quantities at a reason-
able price.
A suitable formula for a Red Smoke Signal is also a desid-
eratum. The effect required is a pronounced and positive
shade of red. As in the case of the Yellow Smoke Signal, chem-
icals composing it should be readily procurable and should be
stable. Since, however, the requirements for this signal are
considerably smaller than for the Yellow Smoke Signal a greater
latitude may be allowed in selecting slightly less readily avail-
able and higher priced material for this signal.
The smoke signals outlined above are displayed from rockets.
Very cartridges, Viven-Bessiere cartridges and 35 mm. cart-
ridges. The rockets now used by our forces weigh about 2
lbs. with an approximate length of 18 in. The V-B, Very cart-
ridges, and 35 mm. cartridges have an average length of about
6 in. with a diameter, respectively, of 2 in., 25 mm., and 35 mm.
The V-B cartridges are thrown from the rifle grenade discharger,
and the Very cartridges and 35 mm. cartridges from the 25 mm.
signal pistols.
Should any person accredited by the Inventions Board be-
come interested in the two pistols outlined above,. this office
would be very glad to give all the information in its possession.
It should be noted that Auramine has already been tried
as a dye for the Vellow Smoke Signal and that Paratoner has
been used in the Red Smoke Signal.
All communications regarding this matter should be addressed
to Inventions Section, General Stall, Army War College, Wash-
ington, D, C. Attention of Captain Scott.
SAFETY OF TNT AS AN EXPLOSIVE
Editor of the Journal of Industrial and Engineering Chemistry:
There have been quite a few cases in this country where tri-
nitrotoluol has exploded under conditions which would lead us
to believe that it is not the safe explosive that it is ordinarily
supposed to be in contradistinction to picric acid which is known
to form rather unstable compounds with metals.
I would like to call attention to the fact that it is perfectly
possible for trinitrotoluol to contain highly nitrated phenolic
derivatives which could form salts with metals, thereby render-
ing the trinitrotoluol very much more subject to outside in-
fluences than if it were absolutely pure. I remember in the
ordinary manufacture of nitrotoluol some ten years ago, we often
isolated from our sodium carbonate w ash liquors notable amounts
of a red crystalline body which, at that time, I identified as a
sodium salt of one of the nitrophenols.
In my reading, I recently came across a confirmation of this
in Berichte, 18, p. 2668, el seq., in an article by Nolting and Forel
on an investigation of the six isomeric xylidenes. In speaking
of the formation of the nitrophenolic bodies in the nitration of
xylols on page 2670, he says (free translation):
If one treats crude nitrotoluol, as obtained in the factory by
nitration with mixed acid, with soda, a similar solution is ob-
tained from which by sufficient concentration, a red and yellow
mass of crystals separates. I have investigated and found that
it consists of the sodium salts of the two dinitro cresols (the
1 -methyl, 3,5-nitro, 4-hydroxy; and the 1 -methyl, 3,5-nitro,
2-hydroxy derivatives), about */« being made up of the first
mentioned. The dinitro cresols are formed, according to my
idea, from cresol which can result during nitration by the oxida-
tion of toluol by nitric acid or oxides of nitrogen. From the
ordinarily formed 1,2,4- and 1,2,6-dinitro toluols, the above
isomers cannot be formed. It might be possible that small
amounts of 1,3,4,5- or 1,2,3, 5 -trinitrotoluols are formed which
could go over, under the influence of alkali, into the correspond-
ing dinitro cresols by replacement of the 2 or 4 nitro groups with
hydroxy 1, but this assumption seems to me to be improbable.
I am sending you this information for publication in the
Journal as I believe it will be of considerable interest to all those
manufacturing trinitrotoluol and that these facts will be certainly
worth taking into consideration in the manufacture and handling
of the material if they are not already clearly recognized.
Research Department t ^j \Veiss
The Barrett Company
New York City
Xovembei 7, 1918.
Oil Seed. Cake Feeding Waste Bleaching
Paper Making Also in the Electrical
Rubber Trades as Trades-
Salt men's Laborers on
Soap General Laboring
Tar Distilling Miscdla
WOMEN IN THE CHEMICAL INDUSTRIES OF ENGLAND
The British Ministry of Munitions has issued a circular con-
taining a list of processes in which women are successfully era-
ployed in connection with the following industries:
Charcoal
Chemical
Distilling
Explosives
Gas
Miner.il Oil Refining
NOTE — The possibility of employing female labor on some of the opera-
tions scheduled herein depends on local circumstances such as lay-out of
plant, locality, type of labor available, etc.
The operations here scheduled may. in general terms, be
classified as follows:
A — -Simple laboring operations.
B— Operations requiring care, intelligence, and, or, resourceful-
ness.
C — Skilled operations.
D — Dangerous operations or operations requiring resistance
to unpleasant conditions, t. g., heat, dust, fumes, odor, etc.
The different sections of the chemical industry in which
women are successfully employed, and the departments of each
section, are as follows
Dec. 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
1029
ACETONE
B — Tankhouse: Charging tanks with mash
B — Tankhouse: Blowing steam through vats
B — Tankhouse: Noting temperature of fermenting mash
A — Tankhouse: General laboring
B — Cooking house: Charging cookers with maize meal
A — General laboring
ALUM
A — General laboring
ALUMINUM SULFATE
A — General laboring
ammonia (concentrated) at Gas Works
B — All operations
ANILINE SALTS
A — General laboring
BARIUM CHLORATE
A — Assisting in concentration and crystallization
A — Chipping out crystals with chisel and hammer
A — Crushing, drying, and packing
BLEACH
B — Making up lute, making cell heads, cleaning up, oiling bearings in
electrolysis house
BUTYL ALCOHOL
B — -Attending mixer
B — Adding salt to alcohol
A — General laboring
CAUSTIC SODA
BD — Fusing caustic soda
BD — Ladling fused caustic soda from melting pots and casting into
stick form
A — "Detaching," i, e., breaking up caustic in cooling trays with ham-
BD — Packing powdered caustic; labelling tins
A — General laboring
ELECTROLYTIC PROCESSES
A — Making up lute
B — Making cell heads
B — Preparing cell diaphragms
B — Assisting in dismantling, repair, and assembly of cells
B — Attending cells
B — Attending switchboards
B — Regulating voltages
B — Recording switchboard readings
ETHER CAMPHOR
B — Final dressing and preparing of camphor tubes
FERTILIZERS
BD — Grinding slag in cake mill
BD— Grinding phosphate in Kent mill
AD — Mixing guano
A — General laboring
IODINE
A — Screening salt in extraction of iodine from kelp
LABORATORY
C — Research chemists
C — Routine testing
B — Laboratory attendants
C — Controlling chemical laboratory
C — Acting as chemist-in-charge
B — Assisting in making up culture-tubes
C — Mounting organisms on slides and noting their condition
MAGNESIUM SULFATE
B — Crushing magnesite
B — Charging dissolvers
B — Attending evaporators and crystallizing vats
B — Whizzing
MAGNESIUM CARBONATE
A — Discharging filter presses 1
B — Packing presses for moulding
MISCELLANEOUS
A — Helping on press for compressed sal ammoniac
B — Operating machine for tableting ammonium chloride
B — Control of acid circulation pumps
B — Assembling parts in drum-making shop
C — Control testing on plant
A — Feeding and attending dissolvers
B — Charging and discharging drying ovens
A — Assisting in repacking condensers and towers (ground work only)
It— Assisting in repairs to decomposers
B — Controlling valves for blowing liquids from vats
NITRIC ACID
A — Charging nitrate, attending and emptying rotary drier
B — Weighing charges of nitrate for stills
BD — Charging stills, luting manhole and pipe joints
B — Running on acid
BD — Firing still and controlling temperature
it Attending and greasing acid pumps
nitric acid (concluded)
A — Breaking dumped niter cake, harrowing, and tipping into barge
A — Breaking up niter cake in cooling pans
C — Sampling and testing
AD — Filling, sealing, and packing carboys
BD — Working on Valentiner nitric acid still
A — General laboring
OLEUM
AB — Unloading pyrites, attending breaking machine
AB — Hauling broken pyrites, weighing charges of pyrites on sulfur
B — Charging and attending sulfur burners
C — Sampling and testing
AD — Grinding and calcining magnesium sulfate
B — Impregnating granulated anhydrous magnesium sulfate with plat-
inum chloride
AD — Filling, sealing, and packing carboys
A — General laboring
PHENOL
A — Washing and stencilling drums
A — Unloading empty drums, testing, and stacking
A — General laboring
PHOSPHORUS
AD — Finishing
AD — Packing amorphous phosphorus
REFINED BICARBONATE OF SODA
A — General laboring
REFINED SODA CRYSTALS
A — Tipping soda ash into dissolvers
B — Cleaning filter presses
B — Filling, operating, and emptying centrifugal driers
A — Grading crystals
A — General laboring
RESPIRATORS
B— "-Operating press tools for stamping out frames on plates
B — Mechanically cleaning same
B — Dipping in acid
B — Nickel plating
B — Cleaning and polishing
B — Mounting with tapes and elastic bands
A — Packing
SILICA
A — Drying on open floors
A — Crushing and bagging
SILICATE OF SODA
A — General laboring
SODA ASH
A — Charging vats with black ash
A — General laboring
B — Taking distiller temperatures
SODIUM BISULFITE
BD — Dissolving sulfur dioxide in caustic soda
BD — Concentrating sodium bisulfite solution
SODIUM (METALLIC)
BD — Charging and dipping from electric furnaces
SODIUM SULFIDE
A — Stripping and breaking from detaching beds
A — General laboring
sulfur
A — Melting crude sulfur
A — Breaking out sulfur from sulfur beds
A — Emptying sublimers, dressing flowers of sulfur
B — Preparing moulds for roll sulfur
A — Removing from moulds after casting
A — General laboring
sulfuric ACID
A — Feeding and attending pyrites breaking machine
A — Sieving pyrites
B — Weighing out charges
B — Charging furnace (or burners)
C— Controlling valves on dc-arsenicatinn plant
AD — Filling and sealing and packing carboys
C — Sampling and testing
BD Coking Kcssler concentrators
HD 'Helping on cascade concentrators
lili 1 )|m ntiiu: Gaillard tower concentrators
producers, including winding and wheeling ma-
terial
It Pumping vitriol over Gay Lussac and Glover towers
It Working iron oxide briquette plant
A — General laboring
TUNOSTBN
,\ Crushing, sieving) end packing
CfDS
BD I Operating dtoltrmtlofl plant , til opt
: 1 ATJON
it MsJdng Bra* laj moulds snd condi
i°3°
TEE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMIS1 R V Vol. 10. No. 12
TWO LETTERS ON EFFECT OF COAL ASH ON THE
NATURE OF CEMENT MILL POTASH
Editor of the Journal of Industrial and Engineering Chemistry:
In a recent article by Messrs. Potter and Cheesman,1 at-
tention has been called to the fact that in some cases the coal
used as fuel for the burning of cement carries sufficient potash
to affect both the total amount of potash driven from the kiln
and the nature or condition of the potash occurring in the re-
sulting flue dust. The statement is made that the so-called
"recombincd potash," which has previously been assumed to be
the result of a combination of the potash vapor and the floating
coal-ash particles,2 is only that potash held in the ash and
originally contained in the coal, together with the undecom-
posed and insoluble potash contained in the dust or raw mix
mechanically blown out of the kiln.
Investigations conducted in this laboratory by the writers,
and at the factory of the Security Cement and Lime Company,
in cooperation with Mr. Haff, chief chemist for that company,
have led to conclusions which are at variance with those above
set forth. As these questions may in some instances become
very important in the future the following data are submitted
so that they may form a part of the printed literature available
to the cement mill chemist and engineer.
Coals from nine different cement plants, both in this and
foreign countries, have been analyzed at this laboratory for ash
and potash, with the following results:
Ash in K2O in KzO in
No. Coal Ash Coal
of riant Location Per cent Per cent Per cent
1 Ohio 10.45 0 66 0.069
2 Maryland 9.23 1 43 0.132
3 Michigan 10.60 1.96 0.208
4 Michigan 14.55 1.90 0.276
5 Michigan 10.38 2.08 0.216
6 Michigan 17.75 4.64 0.824
7 Michigan 12.07 1.73 0.209
8 South America 19 65 0.71 0.140
9 New Zealand 11.02 0.89 0.098
Average 12.85 1.77 0.241
It will be noted that the highest potash content of the coals,
represented by these nine samples, is equivalent to 0.82 per cent
K2O, while the average is equivalent to only 0.241 per cent K20.
Ignoring the abnormally high potash sample marked No. 6,
the average of the eight remaining samples becomes only 0.1687
per cent K20. On the other hand, the potash content of the
resulting ash of the full nine samples is equivalent only to 1.77
per cent K20, and should we ignore sample No. 6, the average
potash content of the ash becomes only 1.42 per cent KjO.
From this it would appear that the samples' investigated by
Messrs. Potter and Cheesman have an abnormally high potash
content, particularly as determined by analysis of the ash.
The amount of coal consumed per barrel of cement burned
varies greatly in the different mills throughout the country,
and it is very difficult to strike an average. As indicated in
Messrs. Potter and Cheesman's article, the coal consumption
varies possibly from 80 lbs. per barrel to 250 lbs. per ban el,
as the extreme limits. The average coal consumption for the
plants from which the above nine samples were taken is 135
lbs. of coal per barrel of clinker produced. This figure also holds
approximately for the remaining eight samples, should we ignore
the high potash Sample No. <i. Using these eight samples as
the basis for calculation, we find that there is introduced into the
kiln with the coal, an amount of potash equivalent to 0.23 lb.
of KjO for every barrel of clinker produced Since the average
potash content of the cement raw material used in these eight
plants is approximately 0.75 per cent KjO, there is introduced
into the kiln with the raw material, an amount of potash equiva-
lent to 4. .5 lbs. K;0 for every barrel of clinker produced. It
would seem from this that the potash introduced with the coal
1 This Journal, 10 (1918), 109.
' Ibid.. 9 (1917), 646.
is approximately only 5 per cent of the total potash entering the
kiln.
Meade, in his book on Portland cement, states that probably
half of the ash from the coal drops in the kiln, and is then carried
out with the clinker. It is difficult to determine, with accuracy,
the amount of coal ash that actually is carried out with the
clinker, or that which is blown out with the gases. Messrs.
Potter and Cheesman assume that only 25 per cent of the coal
ash is carried out with the clinker, even in a wet kiln, which is
probably a very low figure. However, should we assume this
minimum figure, as used by Potter and Cheesman, and also
assume only a 40 per cent volatilization of the potash carried
by the raw material, it follows that even then less than 10 per
cent of the total potash carried out with the gases can possibly
come from the coal. It is evident, therefore, that the coal ash
is of relatively minor importance, so far as the total potash blown
from the kiln is concerned. The relatively small amount of
potash introduced with the coal also makes it improbable that
this can effect any material change in the nature or condition
of the total potash material collected.
The authors referred to, state in their article "that taking
into consideration the K20 content of the ash, and the KjO in
the raw mix carried over mechanically, there is apparently
no recombination of the volatilized KjO with siliceous ash
particles." In connection herewith, the following figures taken
from a factory where potash is actually being collected com-
mercially, may be of interest, particularly as these figures are
representative of the nature of the material collected over a
period of several months. During the period of operation
represented by the samples, the coal burned in the kilns had a
potash content equivalent to 0.132 per cent KjO. Approximately
80 lbs. of this coal were burned per barrel of clinker produced.
There was thus introduced into the kiln with the coal, an amount
of potash equivalent to 0.11 lb. K20 per barrel of cement
burned, while about 6 lbs. of K20 per barrel were introduced
with the raw material. During this period the dust collected
from the stack gases carried, as insoluble and slowly soluble
potash, an amount of potash equivalent to 0.88 lb. K20 per
barrel of clinker produced in the kilns. The terms "insoluble"
and "slowly soluble" are used here in the sense that the so-called
insoluble portion is not affected by long boiling, and is only appre-
ciably soluble in weak hydrochloric acid, while the so-called slowly
soluble portion is completely dissolved by either method, both
insoluble and slowly soluble being differentiated, however,
from the soluble potash, which dissolves readily in hot water.
Of this total of 0.88 lb. of insoluble and slowly soluble potash,
approximately 0.30 lb. was in the insoluble form, and 0.58 lb.
in the slowly soluble form.
The insoluble potash, equivalent to approximately 0.30 lb.
of K20 per barrel, can be accounted for on the assumption that
it represents the potash in the dust or raw mix mechanically
blown out of the kiln. The total amount of dust recovered
during this period, per barrel of clinker produced, is equal to
approximately 20 lbs. The analysis of this dust indicated it
was 50 per cent calcined, which would give a potash content
of this dust of approximately 1.4, on the assumption that none
of its potash had been volatilized. This latter assumption can
unquestionably be made, as none of this dust had at any time
been subjected to a high temperature. This dust should,
therefore, contain 0.28 lb. of KjO in insoluble form, which
figure checks fairly accurately with the insoluble potash de-
termined by analysis.
This indicates that the slowly soluble potash present in an
amount equivalent to 0.5S lb. KjO per barrel of cement burned,
must have come from sources other than the dust mechanically
blown out of the kiln. Should we make the improbable and
extreme assumption that all of the coal ash was carried out
with the gases, and that noue settled in the kiln to be carried
Dec, ioiS
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
1031
out with the clinker, this would still account for an amount of
potash equivalent to only 0.11 lb. K20, as arising directly from
the coal ash. This extreme assumption that the total coal ash
is carried out of the kiln, therefore, still makes it necessary for
us to account for 0.47 lb. K20 per barrel of clinker produced.
It follows then that this must have come from sources other
than the dust blown out of the kiln or the coal ash carried out
with the gases. The only other source from which potash could
have been derived is the potash vapor resulting from the
volatilization of the potash from the kiln burden. The assump-
tion that the incandescent siliceous coal-ash particles react
with this potash vapor is not an unreasonable one, and from
the information at hand it appears that this is the explanation
of the cause or source of the greater part of the "slowly soluble"
potash occurring in the collected dust, as outlined in the former
paper above referred to.
Moreover, as was pointed out in that paper, such an ex-
planation is not new. Thus, Henry S. Spackman, in a patent
dated October 24, 1916, states that it is well known that the
considerable portion of the alkali in the collected dust from
cement kilns that is insoluble is due to the union of the volatilized
alkali with highly heated, finely divided, siliceous dust to form
glass.
From analyses made of dusts from several other cement
factories it appears that the figures given above for the plant
in question do not represent abnormal conditions, for some
flue dusts have even a much larger amount of "slowly soluble"
potash as compared with the amount of potash carried into the
kiln with the coal.
Considering further that for every barrel of cement burned
there is introduced into the kiln with the raw material an
amount of potash equivalent to 6.00 lbs. of K20, while only
0.11 lb. of K20 are added with the coal, it will be readily seen
that the potash introduced with the coal has a relatively small
bearing upon the question of by-product potash manufactured
in rotary kilns, where only the soluble potash comes into con-
sideration. In making accurate potash calculations, however,
where the total "potash" is of interest, the potash introduced
v ith the coal and carried by the coal ash should be carefully
considered, as pointed out by Messrs. Potter and Cheesman.
SUMMARY
I — The coal used in cement burning carries comparatively
small amounts of potash, the average being only 0.24 per cent
K2O for the nine plants investigated.
II — The amount of coal-ash poash introduced into the kiln is
ordinarily very small as compared with the amount of potash
entering the kiln with the raw material.
Ill— The sum of the insoluble and slowly soluble potash
collected from coal-burning kilns, exceeds the sum of the total
potash contained in the coal and in the raw material mechanically
blown from the kiln.
LaBORATORII> 1
Western Precipitation Company
I.os Angei.es, California, April t.S, 191 S
E. Anderson
R. J. Nestbll
Editor of the Journal of Industrial and Engineering Chemistry:
In February 1918, there appeared in This Journal, page 109,
.in article by N. S. Potter, Jr., and R. D, Cheesman, entitled
"Effect of Coal Ash on the Liberation and Nature of Cement
Mill Potash." In this paper, the authors make the following
statement: "The potash collected from the kiln stack gases
where coal is used for burning appears in practically two foims,
water-soluble potash and the insoluble or slowly soluble potash.
The insoluble potash ' ttributed to two cat]
potash in the unburned or partly calcined raw matcn t!
over mechanically in the gases and to a recombination of the
volatilized potash with the finely divided ash particl
coal." Potter and Cheesman refer to an article1 in which ap-
pears this statement: "In some plants where coal is used for
burning, the extent to which the potash occurs in the 'recom-
bined' form may be considerable, while in certain other plants
where oil is used for fuel this combination of the potash is present
in comparatively small amount." From this statement they
deduce, "It is evident that the potash content of the coal ash
has been quite neglected."
From the experimental data which are recorded in this article.
Potter and Cheesman arrive at the following conclusions:
"I — -KjO content of coal ash is considerable.
"II — K20 content of coal ash must not be disregarded in
calculating the liberation in kilns.
"III — K2O content of coal ash appears in 'treater dust' as
insoluble K20.
"IV — Taking into consideration the K2O content of ash and
the K2O in raw mix carried over mechanically there is ap-
parently no 'recombination' of the volatilized K20 with the
siliceous ash particles."
The above deductions do not agree entirely with observations
that have been made and experimental data that have been
collected at the plant of the Security Cement and I.ime Com-
pany, Hagerstown, Md. Therefore, these observations and data
are discussed in connection with the conclusions derived by
Potter and Cheesman.
"/ — KiO content of coal ash is considerable," In support
of this contention Potter and Cheesman analyzed four samples
of coal ash (each representing the average for one week) and
found that "the average potash content figures close to 5 per
cent" from which they conclude that the amount of potash
introduced by the coal per barrel of clinker produced lies be-
tween 0.4 lb. and 1.25 lbs., depending upon the type of plant.
In Table I are given the results obtained by the analysis of six
samples of Fairmont gas coal used by the Security Cement and
Lime Company.
Table I
Average Sample for Ash in Coal KjO in Ash
24 hours ending Per cent Per cent
10-29-17 8.50 1.77
10-30-17 8.85 1.68
10-31-17 9.00 1.23
11-1-17 9.25 1.95
11-2-17 9.25 1.84
11-3-17 9 01 1.65
Average 8.98 1.68
Numerous determinations of the K20 in coal ash have been made
at the laboratory of the Security Cement and Lime Company since
the above table was prepared, and in no case did the result
exceed 2 per cent.
If the coal consumption at different plants ranges from 80 to
250 lbs. per barrel of clinker, the average of the results given
above would show the possibility of the introduction of only
0.12 to 0.37 lb. of K2O per barrel of clinker as contrasted with
0.4 to 1.25 lbs., according to the calculations of Potter and
Cheesman.
The following data were secured from information furnished
by the Bureau of Mines.
Table II — Alkalies in Ash o* P78S1 \ iroinia Coals
K,() in foal Ash
County Town Per cent
;r Century 1.91
Fuyctte Dunloop and Prudence I .92
Favcitc Dunloop and Prudenet 1.33
Dunloop and Prudence 2.72
McDowell \i 0.69
.veil Hit Four 0.34
McDowell North Fork 0.82
Freeman 1.89
Mcrrcr Fr.-cmun 2.09
MoiiouKahclu Morxantown I 00
Table III, in which are given the per cent ash and per cent
KjO in ash for ten Mmptea of Fairmont gas coal as they art
presented on pages .334 and 333. Bulletin .-. V. ■ 1 Virginia
Geological Survey, 191 1, is also of Interest in tin . onm 1 Hon
■ W H Ro« and A R Men "The Recovery of Water-Soluhle Potash
as a By-Product in the Cement Industry," This Journal, » (1917), 1035.
1032
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 12
Sample No.
Table hi
Ash
Per cent
5.72
6.64
7.42
8.22
6.42
6.04
8.14
7.22
7.11
7.50
. 6.94
KiO in Ash
Per cent
0.94
The figures presented in Tables II and III substantiate the re-
sults of the analyses made at the laboratory of the Security
Cement and Lime Company.
"II — K20 content of coal ash must not be disregarded in
calculating the liberation in kilns." By percentage liberation
is meant the per cent of K20 contained in the raw material which
is volatilized in the kiln during the process of burning. At
the plant of the Security Cement and Lime Company it is
calculated as follows:
Percentage liberation =
580 X per cent K20 in raw mix — ■ 380 X per cent K20 in clinker
580 X per cent K20 in raw mix
It is considered that 580 lbs. of raw material must be actually
burned in the kiln to make 380 lbs. of clinker.
Potter and Cheesman assume that in a dry process plant
90 per cent of the coal ash passes up the flue with the gases.
If, in addition to this, we were to assume that (1) go lbs. of
coal are burned per barrel of clinker, (2) the coal contains 10
per cent ash, and (3) the potash content of the ash is 2 percent,
then the amount of K20 deposited in the kiln by the ash would
be 0.018 lb. per barrel of clinker, or 0.0047 per cent of the weight
of the clinker. If it were found by analysis that the raw ma-
terial contained 1.2 per cent K2O and the resulting clinker 0.60
per cent, as ordinarily calculated, the percentage liberation
would be
580 X 1.2 —380 X 0.6
, or 67.2 per cent.
380 X 1.2
If from the per cent K20 determined to be present in the clinker
0.0047 per cent be subtracted (assuming that all of the potash
deposited by the coal ash in the kiln emerged with the clinker),
the percentage liberation would become
580 X 1.2 —380 X 0.5953
— — , or 67.5 per cent.
580 X i.a
Even though the K20 content of the coal ash were 5 per cent,
the percentage liberation would be only 67.7. Therefore it
would seem that the effect on percentage liberation of the KjO
in the coal ash, in dry process plants at least, is negligible.
"Ill — KzO content of coal ash appears in 'treater dust' as
insoluble Kt0." At this point, attention is directed to the fact
that instead of two there are in reality three forms of potash
present in treater dust.1 They are designated as water-soluble,
acid-soluble or slowly water-soluble, and acid-insoluble. In
speaking of insoluble potash, a distinction should be made be-
tween that which is acid-insoluble and that which is often
referred to as insoluble in water, for the latter includes both the
acid-soluble or slowly water-soluble and acid-insoluble portions.
It is evident that Conclusion III refers to water-insoluble potash,
since in an earlier portion of their paper Potter and Cheesman
state, "the potash collected from the kiln stack gases where
coal is used for burning appears in practically two forms, water-
soluble potash and the insoluble or slowly soluble potash."
"IV — Taking into consideration the A'«0 content of ash and
the K*0 in raw mix carried over mechanically there is ap-
parently no 'recombination' of the volatilised A',0 with tlte
siliceous ash particles." In order to determine the accuracy
of this statement, several tests were conducted at the plant
1 \V n Ross and A R Men, This Journal. 9 (1917), 1035.
of the Security Cement and Lime Company, using a kiln and
treater that comprise one of the units of the plant. In each
case the duration of the test was 24 hours. Necessary pre-
cautions were taken to determine as accurately as possible the
weights of clinker, stack-, base-, and treater-dust produced,
and to obtain an average sample of each. A sample of coal
representing the average for the entire period of each test was
secured by an automatic coal sampler.
In Table IV are given the data that were obtained from the
analysis of the various samples collected in three of the tests;
in Table V are the results of calculations based on the data in
Table IV.
Table IV
22.44
6.95
0.42
6.75
8.82
1.80
0.48
11.10
553.94
24.93
7.77
1.51
7.75
10.18
0.64
0.84
11.66
Test number
Barrels of clinker made 498
Coal:
Tons used
Per cent ash
Per cent KjO in ash
Treater dust:
Tons drawn
Per cent water-soluble K2O.
Per cent acid-soluble KiO. .
Per cent acid-insoluble KiO
Per cent total KsO
Stack-base dust:
Tons drawn 2.15 3.30
Per cent water-soluble KjO 3.06 4.58
Per cent acid-soluble KiO 1.09 1.17
Per cent acid-insoluble KiO 0.43 0.22
Per cent total K-O 4.58 4.97
Table V — Pounds KiO per Barrel or Clinker
Test number 1 2
In treater dust -f- stack-base dust:
Water-soluble 2.651 3.275
Acid-soluble 0.581 0.318
Acid-insoluble 0.167 0.261
Total 3.399 3.854
In coal ash entering kilns 0.026 0.105
24.81
8.97
1.38
6.8
8.42
1.30
1.38
11.10
0.90
3 . 53
1.36
0.43
5.32
2.192
0.365
0.354
2.911
According to Potter and Cheesman, the K20 content of the
coal ash and the K20 in the raw mix carried over mechanically
should account for all the water-insoluble potash collected.
In this connection the figures presented in Table VI are of
interest.
Table VI — Pounds KiO Collected per Barrel op Clinker
Test number 1 2 3 4
Water-soluble potash (KiO) 2.651 3.275 2.192 7.706
Water-insoluble potash:
Acid-insoluble (raw mis blown over) 0.167 0.261 0.354 0.26O
Acid-soluble (slowly water-soluble) :
Coal ash blown over (90 per cent) 0.023 0.094 0.099 0.072
Partially burned material 0.558 0.224 0.266 0.349
Recombined ... ... ...
TotalRO 3.399 3.854 2.911 3.387
It will be observed that, after deducting from the total KjO
the water-soluble potash and the sum of the potash content
of the raw mix and of the coal ash carried over by the flue gases,
there still remains a portion, the average of which for the three-
tests amounts to 0.349 lb. per barrel of clinker, or 10.31 per cent
of the total potash collected. Moreover, the sum of the potash
content of the raw mix carried over mechanically and of the
coal ash blown over (which amounts to 0.332 lb. per barrel of
clinker) is sufficient to account for only one-half of the water-
insoluble portion. As indicated in Table VI, the other half
may not all be recombined potash; it is reasonable to suppose
that it may be made up, in part at least, of raw material that
has been only partially burned, thus making the potash com-
pounds which it contains acid- or slowly water-soluble. That
such partial decomposition does take place is clearly shown
by an analysis, given in Table VII, of a sample of treater dust
obtained by W. H. Ross and A. R. Merz' from the plant of the-
Riverside Portland Cement Company.
Tablk vii
KjO i
Combination
Water soluble..
Slowly soluble.
Acid-insoluble..
Treater Dust
Per cent
9.8
Total KjO
in Dust
Per cent
91.59
'. 54
1.87
Total
H Ross and
(1917), 10.
A R. Men. U. S. Dept.
100.00
Agriculture, Bull.
Dec, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
1033
At the Riverside plant, oil is used as fuel. Since in such a
plant no coal ash is present with which the volatilized potash
may recombine, the small amount of slowly-soluble potash
that is found in the treater dust must be due either to partially
burned material or to a recombination of some of the volatilized
potash with siliceous material in the raw mix.
At the plant of the Security Cement and Lime Company
(where powdered coal is used for fuel) it is now customary to
add a small proportion of sodium chloride to the raw mix for the
purpose of decreasing recombination. A patent covering this
process has been applied for by R. C. Haff, Chief Chemist, and
R. D. Cheesman/'l^formerly assistant chief chemist of the
Security Cement and Lime Company. Before this practice was
started, the treater dust produced contained a high percentage
of water-insoluble potash, and yet at that time the operation
of the kilns was practically the same as at present, approxi-
mately the same quantity of coal was consumed per barrel of
clinker, and probably about the same quantities of raw and
partially burned materials were carried out of the kilns. There-
fore the sum of the quantities of K20 in the coal ash and in the
raw and partially burned material carried over in the kiln gases
must have been approximately the same as now, but the amount
of recombined potash was considerably higher and the water-
soluble portion correspondingly lower.
In Table VIII are given the analyses of two samples of
Security treater dust. The first was obtained by Ross and
Merz before the practice of adding sodium chloride to the raw
mix was started; the second is the sample from Test No. 1, the
data for which are given in Tables IV, V, and VI. These
particular samples were chosen because they are almost identical
in their respective percentages of total and acid-insoluble potash,
therefore making it possible to compare accurately the per-
centages of recombined and water-soluble potash which they
contain.
TABLE VIII
Before Addition of After Addition of
Sodium Chloride Sodium Chloride
Water-soluble KiO, per cent 6 . 80 8 . 82
Acid-soluble K2O, per cent 4.10 1.80
Acid-insoluble K2O. per cent 0.50 0.48
Total KjO, per cent 11.40 11.10
It will be noted that (1) the potash content of the treater dust
due to raw material carried over by the flue gases (indicated
by the amount of acid-insoluble K2<0 determined) is approxi-
mately the same in each case, (2) there has been a decrease of
approximately 2.3 per cent in the amount of acid-soluble potash,
with a corresponding increase in the amount of water-soluble K20.
Assuming that the amount of partially burned material carried
over with the flue gases is approximately the same at the Security
and Riverside plants, and that this amount of the Riverside
plant as shown in Table VII is approximately 6.54 per cent
of the total potash recovered, the percentages of this material
present in the treater dust must have been about 0.74 before and
0.73 after the addition of salt to the raw mix. Subtracting
these amounts from the percentages of slowly-soluble K20 given
in Table VIII, the recombined K20 present in the treater dust
collected at the Security plant must have been approximately
3.37 per cent before and 1.07 per cent after the addition of
sodium chloride, showing a reduction in recombination of ap-
proximately 2.3 per cent of the weight of the dust or 20.3 per cent
of the total potash collected. In other words, by the intro-
duction of sodium chloride vapors into the zone of combustion,
thereby causing the preferential formation of potassium com-
pounds which answer the official requirements as to "soluble
potash," the Security Cement and Lime Company has de-
creased recombination approximately 68.0 per cent and at the
same time has obtained an increase of 32 per cent in the per-
centage of water-soluble K20 present in the treater dust which
amounts to 20.3 per cent of the total potash collected.
Results obtained at the Security Cement and Lime Company
do not substantiate the conclusions regarding potash liberation
reached by Potter and Cheesman.
The effect on potash liberation as here calculated is not
greatly influenced by the low percentages of K2O present in the
coals used.
When salt is added to raw mix the percentage of water-soluble
K20 in the treater dust increases at the expense of acid-soluble
K30.
This is explained satisfactorily only on the assumption that
recombination to the extent of about 68 per cent has been
prevented .
Grateful acknowledgment is made to Mr. H. S. Bair who
assisted in the experimental work, and to C. H. Miller, H. C.
Mackenzie, and J. E. Baker who made the analyses reported,
under the direction of Mr. R. C. Haff.
E. O. Rhodes and J. J. Porter
The Mellon Institute op Industrial Research
University or Pittsburgh, Pa.
The Security Cement and Lime Company
Hagerstown, Md.
May 1, 1918
WASHINGTON LLTTLR
3
By Paul Wooton, Union Trust Building, Washington, D. C.
So unexpected was the collapse' of the enemy, just at a time
when the Government's war machine was most intent on quan-
tity production, that the armistice caught the authorities with-
out a reconstruction policy. In fact, there was nol
definite plan for the conversion of the war machine to a peace
basis.
Strenuous efforts are in progress to evolve definite rft
tion policies but nothing comprehensive has come out during
the week following the signature of the armistice Individual
ideas, however, are beginning to become available which indi
catc the general trend of thought. The 0 in1 single
development is that there is to be no BCelung of
contracts. The curtailment is to be allocated in much the
same manner as that in which ll '" '« ' ' '"
work is to be engineered by the War I
special cooperating agencies within the departmi
Due recognition is being taken of the laboi lituation, both in
the curtailing of contracts for raw
ing out of the Army Befon canci llin «J ""'
tract, reports mi I to the Wai 1 11-I11 1 1 1. . Board show
ing the following :
(a) The effect of the proposed cancellation on the Indl
(b) The effect on labor conditions.
(c) The effect 0 0 ility.
(d) The 1 8e< thi iven contractor.
By far the most comprehensive statement as to the industrial
in period has been nude by Benedict
Crowell, director of munitions for the War 1 lepartment, as
follows
With I h " cd with.
,„ intricati problem end les of the
country, which have re»| rtedl «11 of the Govern-
d pre*
attained, must be diverted from war-time production to their normal oc-
ni in times of I-
The first and primal \ 1 onsidt ration
possible,
and wit h a CO
- HI "' popul ition
both herr and rot hould be
i°34
THE JOURNAL OP INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 12
stopped as speedily as is consistent with the primary consideration of labor
.tnd the industries.
Instructions have therefore been issued to all Bureaus of the War
Department, governing the methods of slowing down of production, so
that as far as possible there should be a tapering off of war work, giving
time for industrial readjustment and for the industry' to take up civilian
work.
So that manufacturers might as rapidly as possible get into work
on civilian needs, at our request the War Industries Board have with-
drawn all priority ratings on army work.
No order is being suspended or cancelled by the War Department
without consideration of the nature of the work or the locality in which
the work is being perfoimed. labor, and the re-employment of labor at such
places in other industries, and without conference and consultation with
the War Industries Board which has been constantly in touch with the
industries of this country, and with the Department of Labor, which is in
intimate touch with the conditions of employment in all parts of the
United States.
Overtime, holiday, and Sunday work has been stopped, and as rapidly
as possible and as rapidly as the labor can be used in normal day shifts,
night shifts will be discontinued.
It is often the case that in a certain locality where labor is working
on a war project, this work may be stopped and the same labor utilized
on other work in the same locality.
During the war, production has been largely diverted from articles
called for in times of peace to war necessities, and civilian needs have been
curtailed and non-essentials largely eliminated With the assistance of
the War Industries Board the articles for war necessities are being rap-
idly curtailed and the industries proportionally freed to work on civilian
needs Industries which have been larcely concentrated in certain areas
with resultant congestion of transportation, with a great influx of labor
in this area, with inadequate facilities for housing, etc., are being taken
into consideration in this readjustment.
The two standards which the War Department has set up for itself
are that these contract readjustments must be made equitably, in regard
to the industry and labor, and promptly, to safeguard the financial ele-
ments of the problem.
Of no small interest to the chemical industries is the matter
of the future of the large number of women now engaged. Miss
Mary Van Kleeck, the director of the Women in Industry Ser-
vice of the Department of Labor, expresses the following thoughts
in this connection:
The question peculiar to women relates to those who have taken men's
places. It would seem fair to the returning soldiers that they be rein-
stated in their old positions, but in justice to the women who have taken
their places, sufficient notice should be given to enable thera to be trans-
ferred to other work. The number of women who have been drawn into
gainful employment for patriotic reasons is probably much smaller than
is generally supposed Large numbers of women in the war industries
have been transferred from other occupations and the problem of read-
justment is to return these woikeis to their normal occupations.
With the need for production to feed and clothe and shelter other na-
tions besides our own there is no reason to believe that the employment
of women in industry will not increase rather than decrease. In view of
the responsibility of women for their own support and often for the support
of dciyrndents they cannot be asked to withdraw entirely from gainful
employment.
That there is an important demand for the continuation of
government control in many industries is indicated by the
agreements which have been reached at a meeting of the War
Industries Board and the copper industry and of the War
Industries Board and the steel industry. The copper- producing
industry, represented by Daniel Guggenheim, C. P. Kelley,
1 C. Jaekling, and R. L. Aggassiz, made a hard-and-fast
agreement with the War Industries Board, in which the prin-
cipal points are:
(u) The present rate of pioduction is to be maintained in the mines,
smelters, and refineries, continuous employment being thus insured duting
the li( si period of the transition from a war to a peace basis.
(b) The present level of prices of the metal and the existing wage
scale of labor are to be preserved.
(r) The War Industries Board, or such other governmental agency
as may be designated, is to continue regulation of prices and allocation
of the material.
The agreement is subject to renewal or revision January 1.
Following the meeting, Bernard M. Baruch, the chairman of
the War Industries Board, commented significantly on the
copper situation. Practically the same situation exists with
regard to many chemical products. The remarks of Mr. Baruch
are substantially as follows:
One of the allied governments within the last twenty-four hours has
requested information on delivery of 200.000 tons of copper. This is
accepted as a sign that the European demand will not only be large but
immediate. Prospective requirements for civilian consumption, due to
the curtailment of the productivity of many American industries for toe
last eighteen months because of the needs of the war pro.ram. have
created a demand that is expected to prove a factor in stabilizing condi-
tions generally.
The civilian demands in Europe and elsewhere, held in check for
more than four years, will work to the same end.
The demand for copper will be heavy, and most of it must
be met by the United States, as between 75 and 85 per cent of
the copper production is in the hands of American industry.
With the refining facilities included it is probable that the
proportions controlled by American producers is nearly 90 per
cent.
After the conference with the heads of the steel industry, the
War Industries Board made a formal announcement of which
the following is a paragraph:
The Iron and Steel Institute Committee, in the course of its sugges-
tions, placed emphasis upon the point that a continuation of governmental
supervision of industry for the present was highly desirable. It was agreed
that many changes in operating conditions of the steel mills will be neces-
sary in the transition from a war to a peace basis. Some cancellations
and adjustments in war contracts will follow, but owing to the removal
of many restrictions imposed on non-war industries and the immediate
demands of such industries and a probable resumption of Federal. Mate,
and Municipal improvements which had been temporarily suspended, and
the demands from abroad for foreign construction which are already tak-
ing definite shape, it is believed that the transition can be accomplished
in an orderly and systematic way.
An announcement from the President with regard to use which
will be made of the powers conferred upon him by the War
Minerals Act is expected soon. He already has authorized the
use of Si 00,000 of the appropriation carried by the Act. for the
stimulation of the production of potash, arsenic, and zirconium.
This work already is under headway. It is being directed by
J. E. Spurr, in charge of the War Minerals Section of the
Bureau of Mines.
In addition, however, it has been suggested to the President
that a comprehensive effort be made looking to the development
of the potash industry to the point where the United States will
be independent of outside sources. It is contended that the
War Minerals Act gives a rare opportunity to get this industry
on its feet. Many are of the opinion that the German product
can be undersold in addition to reducing the price of cement
and pig iron, which would be possible when the potash by-
product is recovered.
The Department of Agriculture is interested equally with
the Bureau of Mines in the development of a domestic potash
industry Wallace W. Mein, the assistant secretary of agricul-
ture, is giving the matter a considerable portion of his personal
attention. Potash hunger has manifested itself in crops from
Maine to Florida This demonstrates, he believes, that pot-
ash is a necessary ingredient of fertilizers. He regards as very
dangerous the propaganda which has been conducted by certain
fertilizer interests to the effect that potash is not necv
proper fertilization of soil On the other hand, he regards it
as essential to discount the preaching of the German potash
industry which urged the use of excessive amounts of potash
and fertilizer. By finding the middle ground between these
extremes, the best interests of American agriculture wll be met,
Mr. Mein says. He deprecates the policy which has allowed
large quantities of domestic potash to go unused during the war.
Disbanding of the Chemical Warfare Service of the Army
began with the signing of the armistice. Whether the skeleton
of the organization will be retained is a matter of ques:ion.
Some contend that chemical warfare is a development of the
times and may be retained. Such a view is strengthened by
reference to the loud protest which went up when the British
army first made use of shrapnel. It was characterized as in-
human and barbaric. Any continuance of the use of gas in
warfare is condemned by the men who directed the service in
the American army. Should the international situation not be
adjusted stably, and should nations continue to compete in
armament, it is admitted that the Chemical Warfare Service
probably would become a permanent branch of the Army As
no such outcome is anticipated, present preparations are being
made largely on a basis of complete disbanding,
r At the date of this writing the entire staff of the Chemical
Warfare Service is continuing with the work. Maj S. W.
Avery is an exception. His resignation was given preference
that he might return to especially urgent work at the Ui
of Nebraska. Many other resignations, however, have been
submitted and prompt action on them is expected. The per-
Dec, 101S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
i°35
sonnel of the service is being released in compliance with the
War Department's general policy of not returning men from
the Army faster than they can be absorbed in the industries.
This does not affect chemists as importantly as men in other
industries. Most of the chemists who have been working with
the Chemical Warfare Service have positions awaiting them.
There is to be no uncertainty in this particular, however, as
Major Allen Rogers, the chief of the Industrial Relations Branch
of the Chemical Warfare Service, has sent to each man a series
of questions which will establish his status with regard to his
employment in civil life.
Major Rogers is of the opinion that the demand for chemists ,
will be very much greater as a result of the many practical
demonstrations during the war of their worth in many indus-
tries The presence of Army chemists in so many plants has
taught manufacturers many lessons in the handling of their
business.
The manufacture of toxic substances already has been stopped.
This portion of the chemical service had attained large pro-
portions with the end of the war The manufacturing capacity
of the United States of these substances was greater at that
time than those of England and France combined. Large
supplies of materials entering into gases are on hand. As they
cannot be stored for any great length of time, their disposition
is offering a problem.
It is not claimed at the offices of the Chemical Warfare Ser-
vice that gases superior to those in use by the Germans were pro-
duced. That the best German efforts were equalled is a claim
which it is practically certain will be established. In the devel-
opment of the gas mask, however, there is no question that the
best efforts of the enemy or of the Allies were outdone. Im-
portant announcements along these lines may be expected after
the conclusion of peace.
Over 13,000 replies have been received to the questionnaire
which was sent to chemists in September by the Chemical War-
fare Service. The number of questionnaires originally sent
was 18,000. Classification of the replies received has been
completed. There are more than 100 classes into which the
chemists are separated.
ganized. The war has resulted in the disorganization, it is
said, of the chemical departments at most of the institutions
for higher education. The remarkable advance made by the
chemical industries during the war, as well as the practical
experience which has been attained by so many of the chemical
instructors and pupils will result in a very material improve-
ment, it is believed.
In this connection it may be stated that a frequent criticism
heard in Washington of the Chemical Warfare Service, is that
the college professors had too much to say regarding its manage-
ment. Their inability in certain cases to apply practical meth-
ods is said to have delayed the program to some extent. Had
industrial chemists had a greater voice, some believe progress
would have been more rapid. At any rate, all admit that those
connected with the Service have had some very valuable prac-
tical training.
At the close of hostilities there were 1500 chemists on active
duty with the Chemical Warfare Service. This is in addition
to 3000 other men with chemical training, who also were on active
duty.
Chemists in Washington expect to see material improvement
when the chemical departments of schools and colleges are reor-
With reference to America's war system of economic control,
Chairman Baruch, of the War Industries Board, has called
attention to an editorial published in the Frankfurter Zeitung,
not long before Germany laid down her arms, lamenting the fact
that Germany had not adopted the far-sighted methods of the
United States to check abnormal rises in the prices for raw ma-
terials needed in the war program. Opposed at first to the
price-fixing regulations of the Government, observed Mr. Bar-
uch, the industrial leaders of America have themselves come
around to appreciate the wisdom of the President in insisting
upon a check on the prices for the basic materials where scarcity
stimulated the tendency towards extraordinarily high levels.
Had a different policy been pursued, said Mr. Baruch, the steel
and iron industry, for example, would be facing a return to
peace conditions with the price for pig iron boosted up to $150
a ton or more, and other items of their production similarly
scaled. It is in appreciation of the value of a restraining influ-
ence, he said, that the steel industry and others are asking that
government control be extended over the period of transition
from a war to a peace basis.
PERSONAL NOTL5
First Lieutenant Elbert C. Baker, son of Mr. and Mrs. J. T.
Baker, of Easton, Pa., was killed in action in France on Sep-
tember 30. Lieutenant Baker graduated from Cornell Uni-
versity in 19 1 5 and then took an extra year of special work in
chemistry", receiving the degree of Bachelor of Chemistry.
After leaving Cornell he was associated with his father at the
J. T. Baker Chemical Works in Phillipsburg, N. J.
Professor William Main, scientist and engineer, and formerly
professor of chemistry in the University of South Carolina, died
recently at his home in Piermont, N. Y. Professor Main was
one of the pioneers of the copper and lead mining industries of
this country. He was the inventor of the lead-zinc storage
battery, and the first to apply the storage battery to the propul-
sion of street cars.
Mr. William E. Garrigue, a member of the Chicago Section of
the American Chemical Society and for many years prominently
identified with the chemical industry of this country, died at
Toronto, Canada, on October 2, 1918.
Mr. H. M. Barkesdale, vice president of E. I. du Pont de
Nemours & Co.. Inc., died of influenza at Wilmington, Del.,
on October 18, 1918.
Mr. Roy O. Fitch, of the Bureau of Standards, died on Octo-
ber 13, 1918. His work with the Bureau of Standards was
chiefly on bituminous materials of construction.
Mr. Thomas Bartlett Ford, associate physicist of the Bureau
of Standards, died on October 1, 1918. He had been foi
years in charge of the low-temperature laboratory of the Bureau,
including the liquid air and liquid hydrogen apparatus and had
devoted considerable attention to the separation <>f rare gases.
Mr Milton Birch, mi and treasurer ••( th
morcland Chemical and Color Company died in Octobi •
brief ill'
Miss Elizabeth S. Weirick, for the past eight years instructor
in chemistry at Pratt Institute, Brooklyn, N. Y., has resigned
her position there to take up the work, on January 1, of
textile chemist in the chemical laboratories of Scars Roebuck and
Company, Chicago.
At the request of the Board of Regents of the University of
Nebraska, the War Department has permitted Major Samuel
Avery, chief of the University Relations Branch, Chemical
Warfare Service, to resign his commission, in order to resume
his duties as Chancellor of the University, on December 1.
Major Victor I.enher, in addition to his other duties in the
Relations Section, now takes charge of the work relinquished
by Major Avery.
At the meeting of the New York Section of the Societe de
Chimie Industriclle on November 19, addresses were made by
George Maoussa, Docteur des Sciences, Member of the French
High Commission, and C. O. Mailloux. E.Ii , MS., D.Sc, Past
President of the American Institute of Electrical F'ngincers,
Member of the American Industrial Committee to France.
Dr. W. M. Burton was recently elected president of the
Standard Oil Co. of Indiana, to succeed the late Lauren J.
Drake. Dr. Burton has been connected with the company for
many years, having been chief chemist, superintendent, general
manager, and vice pre
Mr. G. D. Cain, chief chemist of the fertilizer control labora-
tory .it tlf Louisiana Agricultural Station, lias been appointed
irth Louisiana Station at Calhoun,
Mr I ned as directoi ami chemist of the
perimenl Station and professor of agri-
, ultural chemistry
charge of tin laboratory "f 01 '' plants
uii.iii 1 ' 'i% 1 i' 1 tin- w •'■ I '< portment
i°3°
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. i;
Captain W. G. Gribbel, of the First Gas Regiment, has re-
turn* d from active service in France to act as instructor in gas
offense.
Dr. Robert P. Fischelis, director of the control department of
the H. K. Mulford Co., has entered the Chemical Warfare
Service and is now stationed at the control laboratory of the
Gas Defense Plant, Long Island City, N. Y.
Dr. A. D. Hirschfelder, of the University of Minnesota, is
now with the Research Division of the Chemical Warfare Section
and is stationed in Baltimore.
Mr. G. W. Gray, of the Midland Refining Company, El
Dorado, Kansas, has been appointed a director of the Bureau of
Refining, Oil Division, U. S. Fuel Administration.
Mr. Charles D. Test, formerly chemist for the Western
Potash Works of Antioch, Nebraska, has accepted a position
on the staff of the United States Tariff Commission.
Mr. Otto Kress, formerly in charge of the research work in
pulp and paper at the U. S. Forest Products Laboratory, Madi-
son, Wis., is now director of the new technical dyestuffs labora-
tory in the dyestuffs sales department of the E. I. du Pont de
Nemours & Co., Wilmington, Del.
Major Henry S. Spackman, of the Spackman Engineering
Co., Philadelphia, has been promoted to the rank of Lieutenant
Colonel in the Engineers Corps, U. S. A.
Mr. John E. Schott, formerly an Industrial Fellow at Mellon
Institute, has accepted a position with the Experimental Division
of the Hercules Powder Co., Kenvil, N. J.
Mr. Phillip Wealey has been appointed manager in charge
of the oxyhydrogen plant and sales office of the International
Oxygen Co., Pittsburgh, Pa.
Professor E. C. Franklin, of Stanford University, California,
is on leave of absence and is engaged in research work for the
Nitrate Division, Ordnance Department of the Army. This
Division has taken over the experimental ammonia plant and
laboratory which has been conducted near Washington by the
Department of Agriculture. The work is in charge of R. O. E.
Davis and L. H. Greathouse.
Mr. George Quelch, one of the staff engineers of the Inter-
national Oxygen Co., New York, sailed recently for England to
supervise the installation of a 460 cell plant of the I. O. C. Unit
Oxyhydrogen Generators for the British Admiralty.
Dr. Alfred J. Larson, assistant professor of chemistry, Carleton
College, Northfield, Minn., has been in the chemical service
of the Government for a year and was recently commissioned
Captain.
Mr. F. K. Bezzenberger, of Harvard University, has been
commissioned Captain, and is stationed at Cleveland as gas
chemist in the Chemical Warfare Service.
INDUSTRIAL NOTL5
The editorial office of Paper and the office of the Secretary of
the Technical Association of the Pulp and Paper Industry have
moved to 131 East 23rd St., New York City.
The Director of Munitions, Washington, has stopped the
construction work at the government air nitrate plant at Ancor,
near Cincinnati Col. Joyes, who was in charge of the work,
states that a study is being made to determine the best way to
utilize these plants to meet the changed needs of the country.
A contact sulfuric acid plant will be located at Grand Rapids,
Mich. The plant is to be situated upon a tract of land which
is the property of the United States Government and upon
which a picric acid plant is now being erected. When in opera-
tion this plant will produce approximately 75,000 net tons per
year.
Arrangements have been made by the Subsistence Division
of the Quartermaster's Corps whereby the laboratories of the
Bureau of Chemistry, Department of Agriculture, throughout
the United States are to be more fully utilized by the Army.
The British Board of Trade Journal announces that as potash
salts form an essential ingredient in glass making, the very great
development which has taken place in the production of Brit-
ish glass would not have been possible had not a parallel devel-
opment in potash production also taken place.
In view of the need of a permanent exposition of textile and
allied industries, a site at San Gines, in the suburbs of Barce-
lona, Spain, near Catalonia, the center of the textile industries,
has been chosen for an imposing edifice for the exposition. The
scope of the exposition as planned is both practical and theo-
retical.
Work has recently been commenced at the salt mines at
Buurse, Holland, which is near the German frontier. Pre-
viously all the salt for household and industrial needs in the
Netherlands was imported from Germany and when these im-
portations stopped there was a great shortage of the commodity.
At a conference on the American potash situation, held
October 15 in the office of William Wallace Mein, assistant to
the Secretary of Agriculture, in charge of fertilizer control, it
was stated that the view of the Department of Agriculture is
that the Government should do all that is possible to encourage
the production of potash from the cheapest sources in this
country in order to enable the farmers to obtain it at a low
price, because foreign supplies are now unavailable.
Predictions made a year ago that the deposits of tungsten ore
or wolframite in South China would prove to be one of the most
important additions to the world's supply of this ore, have
been amply fulfilled in the development of the industry-. Ship-
ments of the ore from Hongkong alone have totaled $1,831,590
gold in value so far for the current year
Arrangements have been made by the Conservation and
Reclamation Division of the Quartermaster's Corps to take over
the disposition and reclamation of waste materials at ordnance
depots and arsenals which were heretofore handled by the
Ordnance Department. An order has been issued by the Chief
of Ordnance directing that all waste products at ordnance
stations be turned over to the Conservation and Reclamation
officers. Kquipment will be installed at the Picatinney Arsenal
for the reclamation of empty cast iron and steel shells.
A very fine deposit of kaolin, the fusion point of which is
about 35000 F., has been discovered in northeastern Oklahoma
by W. T. Croslin, president and chief engineer of the South-
western Light and Power Transport Co., Miami, Okla.
The first concrete ship built in China, a small ferro-concrete
vessel named Concrete, was taken out on trial recently and
proved very satisfactory in every way, especially as it was
found to be easy to handle.
Due to the difficulties in the shipping situation, England is
now utilizing domestic waste material such as fen grass, reed,
lumber trimmings, and straw in the manufacture of paper.
Dr. Charles S. Venable, formerly gas chemist at the American
University, Washington, is now a captain in the Development
Division of the Chemical Warfare Service doing gas offense work
in Cleveland.
The largest plant in the world for the manufacture of ammon-
ium nitrate with which to fill high explosive shells is located at
Perryville, Md. This government plant which is of concrete
construction has all been built since March 4, 1918, and began
operations on July 26. It consists of two distinct operating
units with a capacity of 300 tons of ammonium nitrate daily.
A special commission spent a month studying ammonium nitrate
production in England and planned a plant closely resembling
the British works.
Proctor & Gamble, soap manufacturers of Cincinnati, have
offered to run the New York City garbage plant on Staten
Island in order to obtain the 1,000,000 lbs. of glycerin which can
be produced there.
Artificial rubber has been made in an experimental way for
many years, but it is now reported that the great dye and color
works at Elberfeld, Germany, are erecting a large factory- for the
production of synthetic methyl rubber on a large scale.
Secretary' Lane of the Department of the Interior says: "The
United States does not need German potash. Germany has
thought that she had a whip-hand over America because of her
supply of this material, but America can in two years become
entirely independent of Germany by the development of her
own deposits and the use of the process devised by Dr Cottrell
of this department."
Dec, 191S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
i°37
GOVERNMENT PUBLICATIONS
By R. S. McBridb. Bureau
KOTICK— Publications for which price is indicated can be
purchased from the Superintendent of Documents, Government
Printing Office, Washington, D. C. Other publications can
usually be supplied from the Bureau or Department from which
they originate. Commerce Reports are received by all large
libraries and may be consulted there, or single numbers can be
secured by application to the Bureau of Foreign and Domestic ■
Commerce, Department of Commerce, Washington. The regu-
lar subscription rate for these Commerce Reports mailed daily is
$2.50 per year, payable in advance, to the Superintendent of
Documents.
COUNCIL OF NATIONAL DEFENSE
X-Ray Apparatus and Supplies, Part IV. Revised edition
of the War Industries Board's list of staple medical and surgical
supplies selected to meet war conditions by Committee on
Standardization. 20 pp. Issued September 1918.
PUBLIC HEALTH SERVICE
An Experimental Investigation of the Toxicity of Certain
Organic Arsenic Compounds. G. B. Roth. Hygienic Labora-
tory Bulletin 113. Issued July 1918.
On the Toxicity of Emetine Hydrochloride, With Special
Reference to the Comparative Toxicity of Various Market
Preparations. G. C. Lake. Hygienic Laboratory Bulletin
113, Part II. Issued July 1918.
BUREAU OF CENSUS
Textiles. Report from the Census of Manufacturers. 1914.
165 pp. Paper, 30 cents. This includes a report on pro-
duction and other data relative to wool manufactures, cotton
goods, hosiery, knit goods, silk, textiles, and miscellaneous
materials.
COMMERCE REPORTS SEPTEMBER 1018
Owing to increased demands for vegetable oils in the United
States, this industry has increased greatly in Japan. The principal
oils produced there are soy bean, coconut, rapeseed, cotton-
seed, and peanut. Of the twenty-five largest plants, all but
three use the pressure system ; these three use the benzene
extraction method. (P. 867)
Efforts are being made to develop the extraction of rubber
seed oil in the Malay states. It may be used as a substitute
for linseed oil in paint and varnish, and in soft soap. (P. 887)
Manufacture of calcium carbide has been started in South
Africa. (P. 915;
The British Scientific Products Exhibition, recently opened,
includes exhibits of chemical products and processes, glass,
quartz, refractories and porcelain, photographic materials,
paper and textiles, and substitutes for petroleum products.
Among the chemical products are dyes, laboratory reagents,
thymol, aspirin, .-(tropin, and other drugs (Pp. 936-8)
Among the substitutes for fuel oils and lubricating oils being
developed in Sweden are wood-tar oil, sulfite spirits, coal-tar
distillates, shale oils, peat-tar oi!. etc. (P. 970)
A new fertilizer in use in Italy, known as "tetraogisogate"
is made from low grade phosphate rock by heating the powdered
rock to 600° to 8oo° C. with 6 per cent of a mixture of calcium,
sodium and magnesium carbonate and a small amount of sodium
sulfate. After heating, the product is treated with phosphorous
acid, and mixed with sand or dry earth. (P. 1026)
Large phosphate deposits have been discovered on islands
near New Zealand. They have been furmed by the impregna-
tion of coral deposits by guano from rookeries of sea birds.
The phosphate is said to be 85 per cent available. These
islands formerly belonged to Germany, but havi recentlj been
taken over by Great Britain. (P. 1139)
of Standards, Washington
Large deposits of high grade chxomite have been discovered
in South Africa, and are being developed. (P. 1141)
Great efforts are being made in Germany to develop cellu-
lose yarn, made from wood fiber. The product when woven
into fabric is strong when dry, but it becomes very weak when
wet. (P. 1 142)
COMMERCE REPORTS— OCTOBER 1918
The manufacture and use of industrial alcohol is increasing
in South Africa. Alcohol to be used for motor fuel is to be
denatured with 2 per cent by volume of "wood naphtha" and
0.5 per cent of pyridine bases. (P. 59)
A large number of women are now studying chemistry at the
German technical schools. (P. 63)
Abandoned mines of Bohemia are now yielding large quanti-
ties of tungsten ore. (P. 63)
The petroleum industry of Mexico is described in detail,
giving the location of the fields, and the properties of the fuel
oil and other products. (Pp. 84-89)
Steps are being taken to develop nickel deposits in Santo
Domingo. (P. 99)
The rubber industry of Ceylon is increasing and areas formerly
devoted to cinnamon, rice, tea and citronella are being planted
in rubber. (P. 102)
Efforts are being made in Germany to increase the price of
potash. The domestic consumption has increased and made
up in some degree for loss of foreign trade. A large number
of prisoners of war and women are employed in the potash
mines. (P. 118)
A pure white fiber, obtained from nettles, is being used ex-
tensively for textiles in Germany and Denmark. Cloth is
being made from peat, with 25 per cent of wool waste. (P. 121)
The British paper industry is now in a serious condition owing
to the dependence on foreign sources for raw material. Supplies
of rags and esparto have been practically cut off and wood
pulp is greatly reduced. Local supplies of straw, grass, and
reeds have been utilized. Restrictions to save paper are more
drastic than in the United States. Thus, for example, envelopes
for official correspondence are used repeatedly by the use of a
detachable gummed label for the address. (Pp. 122-5)
Two plants are to be erected in Norway for extracting salt
from sea water by electricitv (presumably by electrical heating).
(P- 165)
It is pointed out in Dutch journals that the German potash
industry will, after the war, face severe competition from Cata-
loma (Spain), Holland, and the United States. (P. 186)
Extensive deposits of iron and nickel ore have been discovered
and arc being developed in Celebes, Dutch East Indies. It
is estimated that there are 350,000,000 tons of lateritic iron
lining considerable chromium and nickel, and a large
amount of ore containing 25 per cent of nickel. (P. 196)
It is expected that deposits of tungsten ore in Sweden will
supply all Sweden's needs for 20 yeai
A survey of the potash situation in Great Britain shows that
the following sources of supply are actually meeting tin- demands:
blast furnace dust, kelp, wool I cement. It is esti-
mated that 50,000 ton', of potash can be obtained annually
from the blast furnaces, with almost no additional cost, except
fur lln small amount 1
mpanyii inn- half controlled bythi
ment and one half by the- publii All bla: 1 furnace dust is under
Pp i'iX-200)
The manufacture of lithopone has been started in Italv
(P. 202)
1038
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol, 10, Xo. 12
Large amounts of tungsten ore are being exported from
Hongkong. (P. 216)
A marked increase is noted in the imports of American dye-
stuffs into Japan. (P. 247)
It is reported that synthetic rubber is being manufactured
successfully at Elberfeld, Germany. (P. 265)
By a new "cold" process paper pulp is being made in England
from straw yielding '65 per cent of pulp instead of 40 per cent
by the soda process. The new pulp will not bleach white,
but it may be used up to 10 per cent in newsprint paper, of
which it actually increases the strength. (P. 280)
A new explosive known as "sengite" is made in South Africa
by the addition of sodium nitrate to guncotton Consider-
able water may be left in the pressed mixture without decreas-
ing its blasting power, but increasing its stability on handling.
(P. 282)
The cellulose industry of Sweden shows a marked increase,
especially of sulfite pulp. (P. 326)
Manganese ores are now being produced in Chihuahua,
Mexico, in large quantities, and exported to the United States.
The manganese content is from 40 to 48 per cent. (P. 356)
Paper yarn for textiles is now being used extensively in Ger-
many where 88,000,000 lbs. per year are produced. Thread
is being made which is suitable for coarse sacks, etc., but no
fine threads. (P. 358)
Exports to tub United States
Samoa — Sup. 62a France — Sup. 5d Ceylon (P 213)
Copra Aluminum Citronelta oil
Hides Boues Crolon seeds
Rubber Carbon Papain
Saffron Graphite
Casein Rubber
Japan — Sup. 554 Glass Vanilla
§eanho,f Essential oils Dutch East Indies—
Potato starch °»« oil -, P' 53°
Vegetable wax Peanut oil Copra
Paper stock Damar
»T r. - . , Platinum Gambier
Honduras — Sup. 31* zinc ore Hides
Balsam Nicaragua — Sup. 34a Kapok
Liquid amber Balsam Coconut oil
Copra Copper Quinine
Hides Fustic Rubber
Indiuo Gold Tin
Antimony ore Hides Platinum
Gold Rubber Paraffin
Silver Silver Indigo
Sarsaparilla Sugar
BOOK RLV1LLW5
Organic Compounds of Arsenic and Antimony. By Gilbert
T. Morgan, D.Sc, Professor of Applied Chemistry, City
and Guilds Technical College, Finsbury. 8vo., 376 pp.
Longmans, Green & Company, London, England, 1918.
Price, $4.80 net.
In this monograph Dr. Morgan presents in a well systematized
manner the chemistry of the organic compounds of arsenic and
antimony. The work as a whole discusses the development of
this most complicated, but most interesting field of organic
chemistry from the earliest discoveries to the most modern,
including an account of all researches up to the end of 1917.
In the introduction the author gives a brief review of the more
important discoveries, in their historical order, which have
brought the chemistry of the arsenicals into its present important
position in relation to medical science and the theory of chemistry.
In Chapter IV the author, starting with the classic work of
Bechamp, develops the chemistry involved in the preparation
of atoxyl and its closely allied derivatives; in Chapters V, VI,
and VII he describes the developments which led to the discovery
and use of salvarsan and neosalvarsan, and the more modern
arsenicals, luargol, gallyl, etc. The detail of their preparation,
as well as the chemistry involved, and the discussion of their
use in the medical field are given.
In the later chapters the author treats of the preparation
and properties of the more important organic compounds of
antimony. In the appendix a discussion of the analytical
methods for the determination of arsenic and antimony in their
organic combinations is given, also a complete and accurate
bibliography of the publications on the organic arsenicals and
antimonials arranged in chronological order. The use of graphic
formulas throughout the work to illustrate the constitution of
these compounds and their relation one to another does a great
deal towards helping the reader to a clear understanding of the
subject.
The appearance of this book, the only complete and modern
treatise on this subject in the English language, should be most
welcome.
J. B. Churchill
The Chemical Engineering Catalog — 1018 Edition. 836 pp.
Illustrated. Price, $5.00. or obtained by special arrangement
with the Publishers, The Chemical Catalog Co., Inc., New
York City.
One of the features of the Fourth National Exposition of
Chemical Industries was a booth piled high with the volumes of
the 19 1 8 edition of the Chemical Engineering Catalog, ready for
distribution, as a loan without cost, "to any Chemical Engineer,
Chief Chemist, Industrial Plant Superintendent, Works Mana-
ger, Buyer, or Head of a Chemical Department in a University
or College." The piles rapidly disappeared. Congratulations
to the publishers upon the prompt appearance of this veritable
Exposition in itself, in type and cut!
That the Chemical Catalog has proved its usefulness to the
industry is attested by the following figures:
Catalog
Year Pages
1916 205
1917 347
1918 578
i. of Firms
Using
Space
132
247
439
N-o of
Copies
Printed
8500
8500
10200
As in previous years, the volume is published under the super-
vision of a committee appointed by the American Institute of
Chemical Engineers, the American Chemical Society, and the
Society of Chemical Industry. This committee for the 1918
volume consisted of Messrs. Charles F. McKenna, Chairman, L.
H. Baekeland, M. C. Whitaker, Raymond F. Bacon, William M.
Grosvenor, Gustave W. Thompson, and William H. Nichols.
The present volume shows a large increase in the Chemicals
and Materials Section, and a similar growth in the Equipment
Section, including "pumps, packing, valves, and fittings of all
kinds for the handling of steam, air, and liquids; belting, power
transmission equipment, conveying, hoisting, and transporting
machinery, etc."
For the first time a technical book department has been in-
cluded, and a book purchasing service is offered the users of the
Catalog.
The editors, with every reason to be proud of their achieve-
ment, waste no space in idle boasting, but frankly recognize
the possibilities of error in so comprehensive a publication, and
ask for friendly criticism and corrections.
Tin- Catalog is an exemplification of the growth of the chem-
ical industry and will be constantly consulted by those who
bear the responsibility for further development of that in-
dustry.
Chas. H. Herty
Dec, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
NEW PUBLICATIONS
By Clara M. Guppy. Librarinn, Mellon Institute of Industrial Re
eh, Pittsburgh
Butter: Book of Butter; A Text on the Nature, Manufacture and Market-
ing of the Product. E. S. Guthrie. 12mo. 270 pp. Price, $1.75.
The Macmillan Co., New York.
Chemical Directory: Annual Chemical Directory of the United States.
B. F. LovBLACB AND C C. Thomas. 2nd Ed. 8vo. 534 pp. Price,
$5 .00. Williams and Wilkins, Baltimore.
Chemistry: Calculations of Inorganic Chemistry and Qualitative Analysis.
Alexander Smith and W. C. Moore. 12mo. 106 pp. Price, $t.00.
The Century Co., New York.
Chemistry: Future of Pure and Applied Chemistry; Presidential Address
Delivered at the Annual General Meeting of the Chemical Society,
March 21, 1918. W. J. Pope. 8vo. 12 pp. Chemical Society, Lon-
don.
Chemistry: Outlines of Theoretical Chemistry. F. H. Getman. 2nd
Ed. Revised and enlarged. 8vo. 539 pp. Price, $3.50. John Wiley
and Sons, Inc , New York.
Chemistry: Precis de Chimie Industrielle. Pierre Carre. 976 pp.
Price. 16 fr 50. Bailliere et Fils. Paris.
Chemistry: Problems in Inorganic Chemistry. L. M. Dennis. 8vo.
41 pp. Price. $0.25. W. F. Humphrey. Geneva. N Y.
Chemistry: Treatise on Applied Analytical Chemistry. Volume 2-
Translated by T. H. Pope. Vittorio Villavecchia and Others. 8vo.
Price, $6.00. P. Blakiston's Son & Co . Philadelphia
Chemistry for Beginners. C. T. Kingzett. 3rd Ed. 8vo. Price,
2s 6d Bailliere et Fils, Paris.
Coal and Its Scientific Uses. W. A. Bone. 8vo. 491 pp. Price, $7.00.
Longmans. Green 81 Co., New York.
Dyke's Automobile and Gasoline Engine Encyclopedia. The Standard
Work on Motor Mechanism. 7th Ed. 8vo. Price, 21s. American
Book Supply Co.
Electric Welding. D. T. Hamilton and E. V. Oberg. 8vo. 294 pp.
Price. $'.50 Industrial Press, New York.
Fuel Economy in Boiler Rooms. A. R. Maujer and C. H. Bromley.
2nd Ed. 8vo. 308 pp. Price. $2.50. McGraw-Hill Co., New York.
Handbook of Mechanical and Electrical Cost Data. H. P. Gillette and
R. T. Dana. 12mo. 1734 pp. Price, $6.00. McGraw-Hill Co., New
York.
Metallurgy of Lead. H. O. Hofman. 8vo 664 pp. Price, $6.00.
McGraw Hill Co., New York.
Steam Wagon: Manual of the Steam Wagon. Maintenance, Over-
hauling, Garage, and Running Repairs. 8vo. 104 pp. Temple Press.
Temperature: Methods of Measuring Temperature. D. Griffiths.
8vo. 176 pp. Price, $2.75. J. B. Lippincott Co., Philadelphia.
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Dyeing: Application of Dyestuffs in Cotton Dyeing. J. M. Matthews.
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nal. 10 (1918). 794.)
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Silicic Acid Gels. II N IIi.i.mks. Journal of Physical Chemistry, Vol
22 (1918), No. 7, pp 110
Sodium Sulfide in Cyanidation. F. Waktknv.hii.hk Mining and
Vol 117 (1918), Mo, IX. pp, 591-593
Sugar in Chestnut Extract. C T. Galky and Oscar Kiktiiui- Journal
of the A met 1, .in Leather Chemists Association, Vol. 13 (1918). No. 10,
I'P ' 0
Terry Differential Flotation Process. J T, THOT \dining and SdmUJk
Vol 117 (1918). No. 16, I .
MARKET REPORT— NOVEMBER, 1918
WHOLESALE PRICES PREVAILING IN THE NEW YORK MARKET ON NOVEMBER l6, 1918
INORGANIC CHEMICALS
Acetate of Lime 100 Lbs.
Alum, ammonia, lump 100 Lbi.
Aluminum Sulfate, (iron free) Lb.
Ammonium Carbonate, domestic Lb.
Ammonium Chloride, white Lb.
Aqua Ammonia, 26*, drums Lb.
Arsenic, white Lb.
Barium Chloride -• .Ton
Barium Nitrate Lb.
Barytes, prime white, foreign Ton
Bleaching Powder, 35 per cent Lb.
Blue Vitriol Lb.
Borax, crystals, in bags Lb.
Boric Acid, powdered crystals Lb.
Brimstone, crude, domestic Long Ton
Bromine, technical, bulk Lb.
Calcium Chloride, lump, 70 to 75% fused Ton
Caustic Soda, 76 per cent 100 Lbs.
Chalk, light precipitated Lb.
China Clay, imported Ton
Feldspar Ton
Fuller's Earth, foreign, powdered Ton
Fuller's Earth, domestic Ton
Glauber's Salt, in bbls 100 Lbs.
Green Vitriol, bulk 100 Lbs.
Hydrochloric Acid, commercial, C. P Lb.
Iodine, resublimed Lb.
Lead Acetate, white crystals Lb.
Lead Nitrate, C. P Lb.
Litharge, American > Lb.
Lithium Carbonate Lb.
Magnesium Carbonate, U. S. P Lb.
Magnesite, "Calcined" Ton
Nitric Add, 40* Lb.
Nitric Acid, 42* Lb.
Phosphoric Acid, 48/50% Lb.
Phosphorus, yellow Lb.
Plaster of Paris Bbl.
Potassium Bichromate Lb.
Potassium Bromide, granular Lb.
Potassium Carbonate, calcined, 80 @ 85%.. -Lb.
Potassium Chlorate, crystals, spot Lb.
Potassium Cyanide, bulk, 98-99 per cent Lb.
Potassium Hydroxide, 88 @ 92% Lb.
Potassium Iodide, bulk Lb.
Potassium Nitrate Lb.
Potassium Permanganate, bulk, U. S. P Lb.
Quicksilver, flask 75 i.bi.
Red Lead, American, dry 100 Lbs.
Salt Cake, glass makers' Ton
Silver Nitrate Ox.
Soapstone, in bags Ton
Soda Ash, 58%, in bags 100 Lbs.
Sodium Acetate, broken lump Lb.
Sodium Bicarbonate, domestic 100 Lbs.
Sodium Bichromate Lb.
Sodium Chlorate Lb.
Sodium Cyanide Lb.
Sodium Fluoride, commercial Lb.
Sodium Hyposulfite 100 Lbs.
Sodium Nitrate, 95 per cent, spot 100 Lbs.
Sodium Silicate, liquid, 40* Be
Sodium Sulfide, 60%, fused in bbls Lb.
Sodium Bisulfite, powdered
Strontium Nitrate Lb.
Sulfar 100 Lbs.
Sulfuric Acid, chamber 66* Be Ton
Sulfuric Acid, oleum (fuming) Ton
Talc, American white Ton
Terra Alba, American, No. 1 100 Lbs.
Tin Bichloride, 50* Lb.
Tin Oxide Lb.
White Lead, American, dry Lb.
Zinc Carbonate Lb.
Zinc Chloride, commercial Lb.
ORGANIC CHEMICALS
Acetanilid, C. P., in bbls Lb. 65
Acetic Acid, 56 per cent, in bbls 100 Lbs. 9.30
Acetic Acid, glacial, 99'/i% 100 Lbs. 19.50
Acetone, drums Lb. 251
Alcohol, denatured, 180 proof Gal. 68
nominal
19 9
20
nominal
9 'A &
17
70.00 @
80.00
12 @
14
30.00 @
35.00
4'/t @
5
9'A @
9>/<
7'/. @
10'/<
7Vi @
8»/«
nominal
75 @
20.00 @
22.00
3.90 &
4.10
4'/< @
5
20.00 @
30.00
8.00 @
15.00
nominal
20.00 @
30.00
2.10 @
3.00
2.00 @
2.25
nomina
4.25 @
4.30
20
@
30
jO.OO
@
7»A
»'/■
65.00
7'A
@
9
1.10
@
1.15
2.00
@
2.50
1.75
<3>
1.95
125.00
a
130.00
11.25
a
11.50
17.50
a
22.00
63 '/«
&
65
10.00
9
12.50
2.60
9
2.70
2.60 @
3.60
4.42'A @
5.00
3'/« @
3 'A
18.00
32.00
15.00
1.1 7>A
30
1.00
10'A
20
U'A
9.55
19.70
Alcohol, sugar cane, 188 proof Gal.
Alcohol, wood, 95 per cent, refined Gal.
Amyl Acetate Gal.
Aniline Oil, drums extra Lb.
Benzoic Acid, ex-toluol Lb.
Benzene, pure Gal.
Camphor, refined in bulk, bbls Lb.
Carbolic Acid, U. S. P., crystals, drums Lb.
Carbon Bisulfide Lb.
Carbon Tetrachloride, drums, 100 gals Lb.
Chloroform Lb.
Citric Acid, domestic, crystals Lb.
Creosote, beech wood Lb.
Cresol, U. S. P Lb.
Dextrine, corn (carloads, bags) Lb.
Dextrine, imported potato Lb.
Ether. U. S. P. 1900 Lb.
Formaldehyde, 40 per cent Lb.
Glycerine, dynamite, drums extra Lb.
Oxalic Acid, in casks Lb.
Pyrogallic Acid, resublimed, bulk Lb.
Salicylic Acid, U. S. P Lb.
Starch, corn (carloads, bags) pearl 100 Lbs.
Starch, potato, Japanese Lb.
Starch, rice Lb.
Starch, sago flour Lb.
Starch, wheat Lb.
Tannic Acid, commercial Lb.
Tartaric Acid, crystals Lb.
OILS, WAXES, ETC.
Beeswax, pure, white Lb.
Black Mineral Oil, 29 gravity Gal.
Castor Oil, No. 3 Lb.
Ceresin, yellow Lb.
Corn Oil, crude 100 Lbs.
Cottonseed Oil, crude, f. o. b. mill Lb.
Cottonseed Oil, p. s. y 100 Lbs.
Menhaden Oil, crude (southern) Gal.
Neat's-foot Oil, 20* Gal.
Paraffin, crude, 118 to 120 m. p Lb.
Paraffin Oil, high viscosity Gal.
Rosin, "F" Grade, 280 lbs Bbl.
Rosin Oil, first run Gal.
Shellac, T.N Lb.
Spermaceti, cake Lb.
Sperm Oil, bleached winter, 38* Gal.
Spindle Oil, No. 200 Gal.
Stearic Acid, double-pressed Lb.
Tallow, acidless Gal.
Tar Oil, distilled Gal.
Turpentine, spirits of Gal.
4.90 •
4.95
91 'A 9
92
4.20 9
4.50
30 9
32
3.00 9
3.25
22 9
22 '/■
1.24'A @
1.25
42 9
45
9 9
10
nominal
63 9
70
1.12 9
1.20
2.00 9
2.10
19 9
20
8 •
9
nominal
27 9
30
16'A Gov't
price
3.25 @
85 9
6.00 9
13 9
I2'A 9
9>A 9
nominal
65 9
85 9
17
a
IB
16.75
a
17.75
17 'A
a
—
21.00
a
22.00
1.15
9
1.25
3.45
a
3.55
9»A
a
10
METALS
Aluminum, No. 1, ingots Lb.
Antimony, ordinary Lb.
Bismuth, N. Y Lb.
Copper, electrolytic Lb.
Copper, lake Lb.
Lead, N. Y Lb.
Nickel, electrolytic Lb.
Platinum, refined, soft Ox.
Silver Ox.
Tin, Straits Lb.
Tungsten (WO.) Per Unit
Zinc, N. Y
FERTILIZER MATERIALS
Ammonium Sulfate 100 Lbs.
Blood, dried, f. o. b. New York Unit
Bone, 3 and 50, ground, raw Ton
Calcium Cyanamide Unit of Ammonia
Calcium Nitrate, Norwegian 100 Lbs.
Castor Meal Unit
Fish Scrap, domestic, dried, f. o. b. works.. . -Unit
Phosphate, acid, 16 per cent Ton
Phosphate rock. f. o. b. mine: Ton
Florida land pebble, 68 per cent Ton
Tennessee, 78-80 per cent Ton
Potassium "muriate," basis 80 per cent Ton
Pyrites, furnace size, imported Unit
Tankage, high-grade, f . o. b. Chicago Unit
J.'
•
34
13
a a
14
3
.50
26
26
a
a
9
8.05
3
65
55
9
nominal
.•l'A
nominal
56
M
00
a
2 4
CHI
9
40
9
9
60
7
40
a
7
M
37
00
9
nominal
37
50
7
25
and
Mc
17
50
3
18.00
nominal
5
00
9
6
00
7
00
9
a
M
300
00
9 310
00
nominal
6
H
9
6
so
AUTHOR INDLX
THL JOURNAL OF INDUSTRIAL AND LNGINLLRING CHLMI5TRY
VOLUME X— 1918
ABEL. J. J. A National Institute of Therapeutics and Pharmacology 969
Adams, E. Q. and L. E. Wise. Photographic Sensitizing Dyes:
Their Synthesis and Absorption Spectra. Dyestuff Symposium,
Cleveland Meeting, A. C. S 801
Alexander, J. An Introduction to Theoretical and Applied Colloid
Chemistry, by W. Ostwald. Translated by M. H. Fischer.
(Book Review) 249
Introductory Address. Perkin Medal Award 138
The Chemistry of Colloids, by R. Zsigmondy. Translated by E. B.
Spear. (Book Review) 250
Alsberg, C. L. Drug Research and the Bureau of Chemistry 971
Anderson, E. and R. J. Nestell. Effect of Coal Ash on the Nature
of Cement Mill Potash, 1030; .Sec Potter and Cheesman 109
Anderson, R. P. Reagents for Use in Gas Analysis. VII — The
Determination of Benzene Vapor 25
and M. H. Katz. Reagents for Use in Gas Analysis. VI — The
Absorption of Hydrogen by Sodium Oleate 23
Andrews, C. E. Para Cvmene. 1 — Nitration. Mononitrocymene,
1-CHj, 2-NOj, 4-CHICa): 453
Arny, H. V. Annual Report of the Chemical Laboratory of the
American Medical Association. Vol. 10. Compiled by the
American Medical Association. (Book Review) 668
Auld, S. J. M. Methods of Gas Warfare. Address 297
BACHMANN. F. M. The Use of Microorganisms to Determine the
Preservative Value of Different Brands of Spices 121
Bacon, R. P. French Section American Chemical Society. Note. . 1023
Bailey, H. S. and J. M. Johnson. The Determination of the Hexa-
bromide and Iodine Numbers of Salmon Oil as a Means of
Identifying the Species of Canned Salmon 999
Baker, H. A. The Canning Industry — Some Accomplishmeuts^and
Opportunities along Technical Lines 69
Baker, J. T. Reagents and Reactions, by E. Tognoli. (Book Re-
view) 667
Baker, N. D. Transfer of the Experiment Station at American
University to the War Department, 654; See Wilson 654
BAKER, R. T. Platinum Wanted by the Government. Note 867
Bamman, F. C. Correspondence with C. L. Parsons on "Saving Fats
from Garbage." 320
Bancroft, W. D. Chemical Warfare Research. Address, Cleveland
Meeting, A. C. S 785
Barker, H. H. The Bisulfate Method of Determining Radium . . . 525
BASKERvrLLE, C. Sir Wm. Ramsay as a Scientist and Man, by T. C.
Chaudhuri. (Book Review) 962
Beckman. J. W. Chemistry for Soldiers in Training Camps Note 869
BELL, J. M. A Manual of Chemical Nomography, bv H. G. Deming.
(Book Review) 668
Benson, H. K. Chemistry of Materials, by R. B. Leighou. (Book
Review) 666
Bergeim, O. and J. O. HalvERSON. The Preparation of .V/100 Per-
manganate Solutions 119
BlESTERPELD, C. H. and O L. Evenson. A Study of the Estimation
of Fat in Condensed Milk and Milk Powders Correction 159
Blake, A. F. An Alinement Chart for the Evaluation of Coal, 627;
Correction 948
BlakelEY, A. G. and H. H. Geist. Some Results of Analysis of Airs
from Mine Fire 552
BlasdalE, W. C. Equilibria in Solutions Containing Mixtures of
Salts I — The System Water and the Sulfates and Chlorides of
Sodium and Potassium . 344
The Separation of the Chlorides and Sulfates of Sodium and Potas-
sium by Fractional Crystallization 347
Bleininger, A. V. Recent Developments in Ceramics. Address,
Chemical Exposition 844
Bogbrt, M. T. Collar Insignia for Chemical Warfare Service. ..... 655
Cooperation of American Chemical Society with the Chemical
Service Section . . 581
Message, Wm. H. Nichols Medal Award 312
Special Chemicals and Apparatus Available through the Chemistry
Committee of the National Research Council. Note 158
BOGGS, C. R. Vulcanization of Rubber bv Selenium 117
Boyi.es, F. M. The Determination of Essential < His in Non- Alcoholic
Flavoring Extracts 537
Bradley, L. Recovery of Potash from Iron Blast Furnaces and
Cement Kilns by Electrical Precipitation Address. Chemical
Exposition 834
Brand, C. J. The Bureau of Markets in its Relation to the Conserva-
tion of Foods 66
Brbckenridge, J. E. The American Fertilizer Handbook for 1918.
(Book Review) 9"
Brkitiii.-t, F. E. Census of Chemists, 946; S« Chemical Warfare
Service ■ ■ ■ °83
Brewster. J. F. Method of Enzyme Action, by J. Beatty. (Book
Review) 504
Brooks, B T., D. F Smith and II Manufacture of
Amy! Acetate and Similar Solvents (rem Petroleum Pentane. . . . 511
Brother. G II Suggestions on Some Common Pre atlotu 129
Brown, R P. The Automatic Com .rement of High
i ,< ures, . . 133
Browne, C. A The Deterioration ol I " * Problem
mi d Conservation , . . ■ * ' °
lation and the I — i "i in taternationai
Saccharimetric Scale - • • 916
Burton, W. M. Chemistry in the Petroleum Industry. Medal Ad-
dress. Willard Gibbs Medal Award 484
Bushnell. L. D. The Influence of Cold Shock in the Sterilization of
Canned Foods 432
CAIN, J. R. and L. C. Maxwell. Rapid Determination of Carbon
in Steel by the Barium Carbonate Titration Method 520
Campbell, E. DeM. II— On the Influence of the Temperature of
Burning on the Rate of Hydration of Magnesium Oxide 595
Capps, J. H. AND G. B. Taylor. Effect of Acetylene on Oxidation of
Ammonia to Nitric Acid 457
and A. S. CoolidgE. The Production of Nitric Acid from Nitrogen
Oxides 270
Carothers, J. N. Electric Furnace Smelting of Phosphate Rock and
Use of the Cottrell Precipitator in Collecting the Volatilized
Phosphoric Acid, 35; Correction 239
Chamot. E. M. Chemical Microscopy. Address 60
and H. I. Cole. The Use of Textile Fibers in Microscopic Qualita-
tive Chemical Analysis 48
Chandler, C. F. Arthur Henry Elliott. Obituary 498
Dr. Nichols — Leader in Chemical Industry 92
Chapin, E. S. Natural Dyestuffs — An Important Factor in the Dye-
stuff Situation. Dyestuff Symposium, Cleveland Meeting,
A. C. S 795
Chapin, R. M. The Preparation and Testing of Pure Arsenious
Oxide 522
Chapin, W. H. A Rapid Pressure Method for the Determination of
Carbon Dioxide in Carbonates 527
Charlton, H. W. Recovery of Potash from Greensand 6
Cheesman, R. D. and N. S. Potter, Jr. Effect of Coal Ash on the
Liberation and Nature of Cement Mill Potash, 109; See Letters. . 1030
Church, S. R. A Manufacturer's Experience with Graduate Chemical
Engineers 1019
Churchill, J. B. Organic Compounds of Arsenic and Antimony, by
Morgan. (Book Review) 1038
Clark, A. N. A Quick Method for Lime Cake Analysis 51
Clark, A. W and L. DuBois. Jelly Value of Gelatin and Glue 707
Clarke, H. T. Examination of Organic L^eveloping Agents 891
Classen, C. H. An Automatic Hvdrogen Sulfide Stopcock 131
Cloukey, H. and R. C. Palmer. The Influence of Moisture on the
Yield of Products in the Destructive Distillation of Hardwood. . . 262
Cole, H. I. and E. M. Chamot. The Use of Textile Fibers in Micro-
scopic Qualitative Chemical Analysis 48
Cole. \V. H. Conversion of Formulas 555
Collins, W. D. Arsenic in Sulfured Food Products 360
Conner, S. D. Determination of the Value of Agricultural Lime. . . 996
Cook, A. A. and A. G. Woodman. The Detection of Vegetable Gums
in Food Products 530
Cooke, R. D. Chemistry for the Public. Note 752
Coolidge, A. S., G. B Taylor and J. H. Capps. The Production of
Nitric Acid from Nitrogen Oxides 270
CornEHSON, R. W. On Reproducing Beilslein's Handbuch der
Organischen Chemic. Note, 867. See Editorial, Turn About is
Fair Play 672
Crane, E. J. Chemical Research in the Various Countries before the
War and in 1917. Note 236
The Indexes to Chemical Abstracts. Note 237
Cushman, A. S. Antimony Sulfide as a Constituent in Military and
Sporting Arms Primers 376
DAUGHTERS, M. R. The Loganberry and the Acid Content of its
Juice. 30; Correction 159
The Seeds of the Echinocystis Oregana 126
Davidson, J. G. The Formation of Aromatic Hydrocarbons from
Natural Gas Condensate 901
Davis, A l< The Distillation of Resins, by V. Schwcizcr. Translated
by II B. Stocks. (Book Review) 249
M. D. 1 I New Method for the Quantitative
Estimation of I A Differential Pressure Method. 709
on the Absorption of Light Oils from Gases 718
AND D. G. MacGi-' I'plication of the Differential
iho.l to ' lie Estimation of the Benzene and the
Total Light Oil Content of Gases 712
Davis, 1. D. and G. B. Tayi.uk Chemical Control of Ammonia
Oxidation N-. Pea 155
Davis, M. If ami II S DAVXB A New Method for the Quantitative
Examination ol Vapors in Gases A Differential Pressure Method 709
n the Absorption of Light Oils from G ai .718
and I). G MacGkHOOB The Application of the Differential '
sure 'lion of the Benzene and the Total
Light 0 ... 712
■ •,. B. S. Ammonia and Nitric Nitrogi L>i nil non in
Soil I ' Solutions 600
enienl Electric Heatei (or Use in the Analytical
823
I 'evelopments
of the Natui " • .lull Symposium, Cleveland Meet-
798
I New full'
89, 169. 251, 331. 415, SO
A In. Potash from Scarles Lake. Address, Chi -
. . 839
K Noltoi.itR. Recovery of Solvents from Air-
593
1042
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 12
Dodge, F. I). On Constituents of Oil of Cassia — II 1005
C. A An American Emblem for American Chemists . . 653
Dowei.i.. C T. and W. G. Fkibdkman. The Use of Sodium Sulfate
in the Kjeldahi-Gunning Method 599
Downs. C. R and J. M. Weiss. Notes on "Free Carbon" of Tar 400
and C G Stijpp. The Determination of Phthalic Anhydride in
Crude Fhthalic Acid 596
DoBois. L. and A. W. Clark. Jelly Value of Gelatin and Glue. . . . 70/
Durand. H. and R. Stevbnson. Research on the Detection of Added
Water in Milk 26
Duschak. I. H. Address. Dedication of Gilman Hall, University
of California 393
EARLE. R. B. Report of Committee on Organic Accelerators. Rub-
ber Section. A. C. S., 865. See Council Meeting, Cleveland Meet-
ing, A C. S 772
Edson. H. A. Effect of Frost and Decay upon the Starch in Fotatoes. 725
Eggs. W A. and E. P. Harding A Proximate Analysis of the Seed
of the Common Pigweed, Amaranthus Relroflezus L 529
Eglopp. G. Toluol by Cracking Solvent Naphtha in Presence of Blue
Gas 8
Eldrbd. F R. An Institute of Therapo-Chemical Research 973
Elliott. F. A. and S. E. Sheppard. The Reticulation of Gelatin. .. . 727
Embrv. W. O. and G. C. Spencer. Studies in Synthetic Drug Anal-
ysis. V — Estimation of Theobromine 605
and C. D Wright. Studies in Synthetic Drug Analysis. VI —
Evaluation or Hexamethylenetetramine Tablets 606
Encel, R. French Section. American Chemical Society 575
Erdahl. B. F. The Concentration of Potash from Raw Materials
Containing Only a Trace of this Element by Means of the Electric
Precipitation of Flue Dust and Fume Cement Kilns 356
Esselbn, G. J.. Jr Airplane Dopes 135
Bssbx, H . B. T. Brooks and D. F. Smith. The Manufacture of
Amy! Acetate and Similar Solvents from Petroleum Pentane. ... 511
Evans, W. L. Library for Edgewood Arsenal Laboratory. See
Letters 868
BVBHSON, O. L. and C. H. Biesterpeld. A Study of the Estimation
of Fat in Condensed Milk and Milk Powders. Correction 159
FALCONER. J. British Progress in Dyestuff Manufacture 145
Field. A. J. The Determination of Acetone 552
FlBLDNER. A. C. The Storage of Bituminous Coal, by H. H. Stoek.
(Book Review) 668
Fishek. H. L. A Special Stopcock for Dropping Liquids Arranged
for Equalizing the Pressures above and below the Outlet in the
Stopcock 1014
Fitzgerald, F. A. Mr. A. J. Rossi and His Work. Address. Perkin
Medal Award 138
FOLLETT. H. I... G. FoRMANEK. C. T. LINCOLN AND G W. KNIGHT.
Estimation of Phenol in the Presence of the Three Cresols, 9:
Correction 239
Foote, II W. A Summary of the Literature on the Solubility of
Systems Related to Niter Cake 896
Formanek. G. C. T Lincoln G. W. Knight and H. L. Follett.
Estimation of Phenol in the Presence of the Three Cresols, 9;
Correction 239
Fox. P. J. Chemical Control of Ammonia Oxidation. Note, 155.
See Taylor and Davis 156
Frear, W James Henry Shepard. Obituary 499
Frbbland. E. C. and F. W. Zerban. On the Preparation of an Active
Decolorizing Carbon from Kelp 812
Frerichs, F. W. Relation between Efficiency of Refrigerating Plants
and the Purity of their Ammonia Charge 202
FrEV, R W. and j. S Rogers. A Volumenometer 554
Friedeman W G. and C. T. Dowell. The Use of Sodium Sulfate
in the Kjeldahi-Gunning Method 599
Fuller, A. V. An Improved Automatic Pipette-Washing Device. . . 297
GEIST. II II. and A G. Blakelev. Some Results of Analysis of
Airs from a Mine Fire 552
George, J. Platinum Resolution by the State Council of Defense
for California 656
Gibds, H. I). The Color Laboratory of the Bureau of Chemistry.
Dyestuff Symposium, Cleveland Meeting. ACS 802
Gill. A H. Aids in the Commercial Analysis of Oils. Fats and their
Commercial Products. A Laboratory Handbook, by G. F.
Pickering. (Hook Review) 666
American Lubricants, by L. B. I.ockhart. (Book Review) 504
Lubricating Engineer's Handbook, by J. R. Battle. (Book Re-
view) 168
The Occurrence of Carotin in Oils and Vegetables 612
Gillrtt. 11. W. and A E. Rhoads. A Rocking Electric Brass
, Furnace. 459
Goldthwait. C. F. The Journals of the American Chemical Society.
Note 1026
Golbr. G. W. The Debt of Preventive Medicine to Chemistry.
Address 303
Goodwin. C. J. The Sulfuric Acid Indi . 751
Gray. G P. The Consumption and Cost of Economic Poisons in
California in 1916 Address 301
Grav, II LbB. A 'lest for Wool 633
Reduction of Waste See Letters 153
Gray. T .. G. I. Kbllby. M. G. Spencer and C H 'lungworts'.
Determination of Manganese in Steel in Presence of Chromium
madium by Blectrometric Titration 19
Greaves. J. E. and C. T. Hirst The Composition of the Water of
the I'llcriuountain Region . ... 1001
Grignard. V. The Collaboration of Science and Industry. Address.
Trann i . 1. ,7
Guppy, C. M. New Publications:
HAIGII I. D Variation in the Ether Extract of Silage 127
Hale. W. J Resolution Concern Nomenclature. Note. 944
IIai.i W T Standard Methods of Chemical Analysis Edited by
W W Scott (Book Review) 250
A II. On the Quantitative Analysis of Dyestuffs Dye-
stuff Symposium. Cleveland Meeting ' . .. 804
HALVBRSON I O. and <> BbROSIH. The Preparation of rV/100 Pcr-
1 |9
II vmok. W. A. A Letter from France 495
Harding, E. P. and H. Ringstrom. A Comparison of the Proximate
and Mineral Analysis of Desiccated Skim Milk with Normal
Cows' Milk 295
and W. A. Egge. A Proximate Analysis of the Seed of the Common
Pigweed. A maranlhui Relroftexus L 529
Hart. E. An Evaporator for Acid Liquids 555
The Utilization of Niter Cake Note 238
Hart. R. An Improved Distillation Method for the Determination
of Water in Soap 598
Healy. J R. Licenses Required for Explosives and their Ingredients.
Note 237
Hebdbn. J. C. Dyeing of Khaki in the United States. Address... 640
Heidenhain. H. Critical Elaboration of Quantitative Precipitation
Methods Exemplified by a Method for the Determination of
Phosphoric Acid 426
Hendrick. E. L. Address. Annual Meeting of Chemists' Club. 489
Hendrickson, N. and G. C. Swan. Determination of Loosely Bound
Nitrogen as Ammonia in Eggs 614
Herreshopf. J. B. F. Sulfuric Acid Handbook, by T. J. Sullivan.
(Book Review I 960
Herty, C. H. Introductory Address. Wm. H. Nichols Medal
Award 305
Chemical Engineering Catalog, 1918 Edition. (Book Review). . . 1038
Permanent Chemical Independence. Address, Chemical Exposi-
tion 826
Unsigned Editorials:
A Chemists' Club (or France
A Dyestuff Section of the American Chemical Society: 674
A French Local Section 510
A Golden Opportunity 967
A Long Step in the Right Direction, 172: See Somebody Please Cut
the Tape 94
A Patent Abuse 1 73
A Record of Achievement 879
A Regrettable Decision of the Directors 4
A Special Meeting of the Council 967
A Victory of Arms, Not Yet of Ideals 966
America in Safe Hands 418
An Appreciation and a Greeting 95
An Army without Reserves 508
An Embargo on Research Work 968
An Experiment in Publicity 967
An Inglorious Rout . 419
An International Courtesy 673
Another Idol Shatteled 880
By Order of the President 590
Camp Followers 255
Chemistry Insignia 95
Commissions for Baseball Players 879
Conservation Begins at Home 879
Developments in Ceramics 878
Facts for the Tariff Commission 1 73
Four Days More 336
Important Notice: Licenses Required for Explosives and their
Ingredients 256
Living from Hand to Mouth 591
National Sclf-Containedness 966
No Change in Exposition Plans 672
On With the Investigation 93
Organization within the Dyestuff Industry 256
Pernicious Activity 880
Platinum:
Platinum at White Heat 508
i Oscillations
Pla
Scraps.
The Great Ga
Political , but not Politics
Preparation for after the War
Progress in Selective Service
Prophecy and Fulfilment
Publicity Work to be Continued
Research and the Tar Bahy . . . :
Secretary Crowell at Cleveland
Somebody. Please Cut the Tape
Spruce Turpentine.
Spruce Turpentine to the Fore
Sugar and Soap
The Approaching Exposition
The Bull's Eye
The Chemical Alliance
The Chemical Service Section of the National Army.
The Chemistry Rainbow
The Chemists1 Club
The Cleveland Meeting
The Custodian in Action
The Demise of the "Garabed"
The Great Gamble
The Missing Five Thousand
The Modern Miracle
The \.i\ .il Consulting Board
The Parting of the Ways
Rtturn of the Chemists
tnan Pronouncements
is Pair Play
slry in the Alleviation of Suffering
Notes
Typical G
Turn Aboi
W^r Chen
Washingtc
W..sli
What's in a Name'
Where :tre the Leaders'
Wood Waste
reparation for After the War. Address, 881;
Set Editorial
Report on Census of Chemical Imports
Hicgins. C. A Recovery of Potash from Kelp. Address, Chemical
Exposition
Solvents from Kelp. Address. Chemical Exposition
Hilciehkami, I 11 The Extraction of Potash and Other Constituents
from Sea Water Bittern
Hill. C. W. College Courses for Industrial Chemists. Address. .
Hill. R. A. Importance of Chemists Recognized by Secretary of
336
419
590
878
3
419
338
420Vf
672
174
175
592
674
3
2
254
338
591
673
590
419
5
jot
175
968
420c
672
673
418
256
Hi;
W. P. Government Control of Platinum. Note
Dec, 1918 THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Hiltner, R. S. and C. E. Parker. An Improved Method for De-
termining Citral. A Modification of the Hiltner Method 608
Hirsch, A. The Pyrophoric Alloy Industry. Address. Chemical
Exposition g^o
Hirst. C. T. and J. E. Greaves. The Composition of the Water of
the Intermountain Region jOOl
HrxsoN, A. W. and R. II McKEE. Study of the Conditions Essential
for the Commercial Manufacture of. Carvacrol. . . . 982
Hopkins. O. P. Chemical Markets in the Union of South Africa' ".' 887
Chemical Markets of South America:
Argentina. Brazil, and Uruguay 701
Chile, Peru, and Bolivia '.....'. 805
Colombia, Ecuador, the Guianas, Venezuela, and Paraguay ' 977
Effect of the War on American Chemical Trade .'.'.'.'.'. 692
Our Publications and Their Bearing on the Chemieai Industry.
Symposium: Bureau of Foreign and Domestic Commerce and
Its Relations to American Chemical Industry 933
Horne W. D. Valuation of Raw Sugars ,....!!!! 809
Hornsey. J. W. Pot ish from Desert Lakes and Alunite. Address,
Chemical Exposition 838
Howe, H. E. Minutes of Sessions. Division of Industrial' Chemists
and Chemical Engineers, Cleveland Meeting, A. C. S. . . 865
Howe. J. L. As to Platinum. Note 159
Hudson, C. S. American Sources of Supply for the Various Sugars.
Address 1 75
and F. B. LaForge. The Preparation of Several Useful Substances
from Corn Cobs 925
Hufp. W. J. Some Applications of Physical Chemistry in the Coal-Tar
Industry 1016
Hurley, E. N. Communication from U. S. Shipping Board, 864;
See Council Meeting, Cleveland Meeting, A. C. S 772
ILLINGWORTH, C. B., G. L. Kblley. M. G. Spencer and T. Gray.
Determination of Manganese in Steel in the Presence of
Chromium and Vanadium by Electrometric Titration 19
JACOBSEN, J. Pipette Used in Titration of Oils for Acidity 633
Jambs, C. C. Reverted Phosphate 33
Jamieson, G. S. The Determination of Arsenic in Insecticides by
Potassium Iodate 290
Jayne, D W. Institute for Research on Synthetic Drugs 975
Johlin, J. M. An Aspirator 632
Johnson, J. M. and H. S. Bailey. The Determination of the Hexa-
bromide and Iodine Numbers of Salmon Oil as a Means of
Identifying the Species of Canned Salmon 999
Johnson. M. O. Reaction of Hawaiian Soils with Calcium Bi-
carbonate Solutions, Its Relation to the Determination of Lime
Requirements of Soils, and a Rapid Approximate Method for the
Determination of Lime Requirements of Soils 31
Johnson, T. B. Address of Acceptance. Wm. H. Nichols Medal
Award 306
The Development of Pyrimidine Chemistry. Medal Address.
Wm. H. Nichols Medal Award 306
Johnston, J. A Summary of the Proposals for the Utilization of
Niter Cake 468
Jones, G. The Tariff Commission and the Dye Industry. Ad-
dress 232
War Disturbances and Peace Readjustments in the Chemical In-
dustries. Address, Cleveland Meeting, A. C. S 783
KATZ, M. H. and R. P. Anderson. Reagents for Use in Gas
Analysis. VI — The Absorption of Hydrogen by Sodium Oleate. . 23
Keitt, T. E. and H. E. Shiver. A Study of Sources of Error Inci-
dent to the Lindo-Gladding Method for Determining Potash.. 994
A Study of the DeRoode Method for the Determination of r'otash
in Fertilizer Materials 219
Kellby, G. L., M. G. Spencer, C. B. Illincworth and T. Gray.
Determination of Manganese in Steel in the Presence of
Chromium and Vanadium by Electrometric titration 10
Kbrr. R. H. Chemical Tests for the Detection of Rancidity 471
Kiplinger, C. C. A Device to Insure Tight Connections between
Glass and Rubber Tubing 631
KnBCHT, M The Great Effort of the French Industries. Address.. 423
Knight. G. W.. C. T. Lincoln, G. Furmanek and H. L. Follbtt.
Estimation of Phenol in the Presence of the Three Cresols, 9;
Correction 239
JCnobdlbr, E. L. and C. A. Dodce. Recovery of Solvents from Air-
Vapor Mixtures 593
Kobbr, P. A. Technical Applications of Nephelometry. Address. . 556
KRBSS, O. and C. K. Textgr. Some Experiments on the Pulping of
Extracted Yellow Pine Chips by the Sulfate Process 268
Kunz, G. F. Platinum Resolutions. Note 159
LAFORGE. F. B. and C. S Hudson. The Preparation of Several Use-
ful Substances from Corn Cobs 925
Laird, C. N. The Potteries at Shek Waan, Near Canton, China.
Address 568
Langmuir A. C. The Chemist's Pocket Manual, by R. K. Meade.
( Hook Review) 960
Leech. P.N. Examination of American-Made Aectylsalieylic Acid. . 288
LbMaistre. F. J. Conditions of the French Chemical Industries
during 1916. Addresi 421
Leveni:. I'. A. An Institute for Chemotherapy 970
Lewis. II. F. The Quantitative Estimation of Anthraquinone 423
Liniiargkr. s. C Carborundum Refractories Address. Chi
.ion .847
Lincoln. C. T., G. W. Knight. G. Furmanek and H. L. Follbtt.
Estimation of Phenol in the Presence of the Three Cresols, 9;
Correction ■ 239
Little. A D. Cellulose— An Outline of Chemistry of Structural Ele-
ments of Plants, by Cross and Bevan. iliooli 1
Losveniiart, A. S. Institute for Research in Synth
Chemistry ..971
Lubs, H. A Detection oi Added Color in Buttei
MACDOWELL, C. II. The Work of the Chemical Section of the War
Industries Hoard. Address, Cli • ?80
MacGrbgok, I) G , II. s Davis ani> m n Davh The Applica-
tion of the Differential Pressure M ■' 'he
• • and the Total Light Oil I 7I2
Mains. G. II and II B. Path II The
nation of Distilled Watei 279
:ing. Dye-
of Carbon
Marshall, A. E. Avoidable Waste in the Production of Sulfuric
Acid by the Chamber Process Note
Mason, W. P. Chemical Engineering in our Universities, 753: Sa
Zoller
Matos. L. J. America's Progress in 'Dyestuffs ' Manufacturing.
Dyestuff Symposium. Cleveland Meeting, A. C. S
Matthews, J. M. Application of Dyestuffs in Cotton Dy
stuff Symposium, Cleveland Meeting, A. C. S.
Maxwell, L C. and J. R. Cain. Rapid Determinatior
in Steel by the Barium Carbonate Titration Method
McBride, R. S. Government Publications-
84, 165, 245. 331, 408. 503. 586. 662, 758. 873, 954,
Toluol Recovery and Standards for Gas Quality
McDowell, A. H. Some Methods of Analysis lor Nebraska Potash
Salts and Brines
McELROY, K. P. Chemical Patents and Allie.l Patent Problems, by
E. Thomas. (Book Review)
Product Patents
McGratii. S. J. On Reproducing Beilstein's Handbuch der
1 'rg.inischen Chemie. Note, 867; See Editorial, Turn About is
Fair Play
McHargue, J. S. Uniform Nitrogen Determination in Cottonseed
156
645
790
794
520
1037
111
128
Meal.
Fertilizing Value of
672
533
400
.'.so
982
Effect of Fertilizers on Hydrogen-Ion Concentration
962
1027
656
476
480
106
920
338
1015
McKay, G. P. and G. G. Nasmith.
Activated Sludge. 339; See Rudniek. . . .
McKee. R. H. Laboratory Guide of Industrial Chemistry, by A
Rogers. (Book Review)
and A. W. Hixson. Study of the Conditions Essential for the
Commercial Manufacture of Carvacrol
McMillan, A. Current Industrial News Items:
73. 150, 228, 312, 394, 487, 572, 648. 744, 861. 937,
Meade. R K. Valuation of Lime for Various Purposes
Van Nostrand's Chemical Annual, Edited by I. C. Olsen and M P
Matthias (Book Review)
Mbes. C. E K. Chemicals for Research Work. Note
Organic Reagents for Research and Industry
Planning a Research Lal-oratory for an Industry. Address
Merrill. C. W The Ammonia Program for 1918
Mbrz, A. R. Direct Heat Treatment of Cement Mill Dust to Increase
Its Water-Soluble Potash Content
Russia's Production o' Platinum
Metzger, F. J. The Chemists' Club. Communication and Ques-
tionnaire
Morsb. F. W.
in Soils...
Mount. G. The Association of British Chemical Manufacturers. . . .
Munn. W. F. Determination of Acetic Acid by Distillation with
Phosphoric Acid
New Portable Hydrogen Sulfide Generator ?
MunroB, C. E Explosives, by A. Marshall. (Book Review)
Myers, C. A., Jr. A New Timing Device for Simplifying the
Thermometric Reading of Calorimetric Determinations
NASMITH, G. G. and G. P. McKay. The Fertilizing Value of
Activated Sludge. 339; See Rudniek 400
Nestell. R. J. and E. Anderson. Effect of Coal Ash on Nature of
Cement Mill Potash. 1030; See Potter and Cheesman 109
Nichols, B. G. and W. D. Turner. An Inexpensive Ash Leaching
Plant 374
Nichols. W. H A Retrospect and an Application. President's Ad-
dress. Cleveland Meeting. ACS 768
Platinum Resolution bv the Argentine Chemical Society. Note,
323; See Schaefer '. 323
Presentation Address. Perkin Medal Award 140
Presentation Address. Wm. H. Nichols Medal Award 305
Ramsay Memorial Fund. Note 236
Northrup, Z. An Anaerobic Culture Volumeter 624
Noyes. H. A. Comparison of Percentages of Nitrogen in Tops and.
Roots of Head Lettuce Plants 621
OBI-RFELL, G. G. Testing Natural Gas for Gasoline 211
Oesper. R. E. CoSperation between Manufacturers and Uni-
versities. Note 1027
Olsen, J. C. Reports of American Institute of Chemical Engineers
Meetings:
10th Annual Meeting, St. Louis. December 5 to 8, 1917 77
10th Semi-Annual Meeting. Gorham and Berlin, N. II , June 19 to
22. 1918 651
O'NEILL. E. Dedication of Oilman Hall, University of California.
Introductory Address 391
PALKIN, S. The Identification and Determination of Potassium
Guaiacol Sulfonate 610
Palmer, A. M. Cooperation Requested by Alien Property Custodian.
Note 947
Palmer. R. C. The Effect of Catalyzers on the Yield of Products in
lestructive Distillation of Hardwoods 264
1 Incomplete Distillation on the Yield of Products in
estructive Distillation of I'.irch 260
AND H. CLOUXBY. The Influence of Moisture on the Yield of
ructive Distillation ol Hardwood 262
Parker. C. E. and R. S Hiltner. An Improved Method for De-
termining Citral A Modification of the Hiltner Method 608
ParKHI'RST. I. P. The BffeCl ol Annealing on I
ol Hardened Carbon Staeuj 515
Parr, s w. Methods lor the Coalmen I rid Analysis of
I Sub-
committee "f the I on under the
666
American Chemical Society Pin 80
portunity to Help the French. Note 1024
Cleveland Meeting A 1 . . . 653
I.etlcr I. vised State-
b) w 11 Walker .321
..I the American "ie 236
In Wari. Iddrest, 1 leveland Meeting,
776
Pattin II B. and G 1 I b«
I
1044
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 12
Pearl, K. Statistics of Garbage Collection and Garbage Grease Re-
covery in American Cities 927
Perry, R. P. Coal Gas Residuals, by P. H. Wagner. (Book Review) 667
Peterkin, A. G.. Jr. Synthetic Phenol 738
Petit, R. New After-War Preparations in the Chemical Industry of
Germany. Translation 1025
PlCKREM., E. R. The Method of Preparation of the Census of Ch
cal Imports. Symposium: Bureau of Foreign and Domestic
Commerce and its Relations to American Chemical Industry. . . 936
Pierce, E. W. Problems in Testing Dyes and Intermediates. Dye-
stuff Symposium, Cleveland Meeting. ACS 803
Porter, J. J and E. O. Rhodes. Effect of Coal Ash on Nature of
Cement Mill Potash, 1031; See Potter and Cheesman 109
Potter, N. S., Jr. and R. I). Cheesman. Effect of Coal Ash on the
Liberation and Nature of Cement Mill Potash L 09 ; Set Letters. . 1030
Pranke, E. J. Development in Nitric Acid Manufacture in the U. S.
since 1914. Address, Chemical Exposition 830
Pulsifer, H. B. A Standard Apparatus for the Determination of
Sulfur in Iron and Steel by the Evolution Method 545
RABAK, F. Influence of Time of Harvest, Drying and Freezing of
Spearmint upon the Yield and Odorous Constituents of the Oil. . 275
Randall. M. Oilman Hall: The Research Unit of the Chemistry
Group at the University of California. Address 634
Randall, W. W. Charles Caspari. Jr. Obituary 240
Note on the Use of the Dipping Refractometer 629
Rather, J. B. An Accurate Loss-on-Ignition Method for the De-
termination of Organic Matter in Soils 439
REED, E. O. A Method for Determining the Absorbency of Paper. . 44
AND F. P. VEITCH. A Constant Temperature and Humidity Room
for the Testing of Paper, Textiles, Etc 38
F. P. Veitch and C. F. Sammet. Blue and Brown Print Paper:
Characteristics, Tests, and Specifications 222
Rhoads, A. E. and Gillett, H. W. A Rocking Electric Brass
Furnace 459
Rhodes, E. O. and J. J. Porter. Effect of Coal Ash on Nature of
Cement Mill Potash, 1031; See Potter and Cheesman 109
Rhue, S. N. Improved Methods for the Estimation of Sodium and
Potassium 429
RICE, F. E. A Simple and Entirely Adjustable Rack for Kjeldahl
Digestion Flasks 63 1
Richards, J. W. Milwaukee Meeting American Institute of Mining
Engineers. Note 945
The Ferro- Alloys. Address, Chemical Exposition 851
Report, 34th Meeting American Electrochemical Society. Note. . 944
Richardson, W. D. Tentative Standard Methods for the Sampling
and Analysis of Commercial Fats and Oils 315
Ringstrom. H. and E. P. Harding. A Comparison of the Proximate
and Mineral Analysis of Desiccated Skim Milk with Normal
Cows' Milk 295
Rittenhouse, E. A Safety Valve 633
Robinson, W. O. A Proximate Quantitative Method for the De-
termination of Rubidium and Caesium in Plant Ash - 50
Rogers, A. Allen's Commercial Organic Analysis. (Book Review) . 250
Everyman's Chemistry, by E. Hendrtck. (Book Review) 168
The Leather Specimen Book, by F. W. I.aCroix. (Book Review) . . 88
Treatise on Applied Analytical Chemistry. (Book Review) 960
Rogers, J. S. and R. W. Frey. A Volumenometer 554
Ros&NGARTBsN, G. D. The Chemical Engineering Catalog — 1917
Edition. (Book Review) 88
Rossi, A. J. Address of Acceptance. Perkin Medal Award 141
Roth, C. F. Report of Southern Trip of American Electrochemical
Society 489
Rudnick, P. Report of Committee on Research and Analytical
Methods. Fertilizer Division, A. C. S 946
The Fertilizing Value of Activated Sludge. Note, 400; See Nasmith
and McKay 339
SADTI.ER, S. P. Advances in Industrial Organic Chemistry since
the Beginning of the War. Address. Chemical Exposition 854
Joseph Price Remington. Obituary. 240
Sammet, C. F. • Determining the Comparative Melting Points of
Glues as a Measure of the Jelly Strength 595
Relative Viscosity of Oils at Room Temperature 632
F. P. VEITCH and E. O. Reed. Blue and Brown Print Paper:
Characteristics, Tests, and Specifications 222
SaTTLER. L. A Hvdrogen Sulfide Generator 226
SaxTON, B. The Recrystallization of Niter Cake 897
Schaefer, G. F. Platinum Resolution by the Argentine Chemical
Society. Note, 32i\ See Nichols 323
SohoellkopF, J. F., Jr. The Development of the Dvestuff Industry
since 1914. Dvestuff Symposium. Cleveland Meeting, A. C. S. . 792
Scholes, S. R. Pcimancnce as an Ideal of Research. Address 390
SchorgEr. A W. Sulfite Turpentine 258
Seidenbekg, A a Method for the Detection of Foreign Fats in
Butter Fat 617
Sharwood, W J. Notes on Sodium Cyanide 292
Sheppard. S. E The Science and Practice of Photography. (Book
Review) '. 961
and F. A. ELLIOTT. The Reticulation of Gelatin 727
Sherman, II. C. Food Chemistry in the Service of Human Nutrition.
Address 383
Shiver. H. E. and T. E. Keitt. A Study of Sources of Error Inci-
dent to the Undo Cladding Method (or Determining Potash... 994
A Study of the DeRoodc Method for the Determination of Potash
in Fertilizer Materials 219
i',. A. A Differential Refractometer 553
Shrbvb. R. N. General Symposium on the Chemistry of Dyestuffs
Note
Introductory Remarks Dvestuff Symposium. Cleveland Meeting,
A. S. C ... 789
Silverman. A. A New Illuminator for Microscopes 1013
Smith, D. F, B. T. Brooks and II Essex. The Manufacture of
Amvl Acetate and Similar Solvents from Petroleum Pcntane. ... 511
Smith, E. Fuel for Manufacture of Chemicals. Note 159
Snow, C. D. Government Trade-Building Information. Sym-
posium: Bureau of Foreign and Domestic Commerce and Us
Relations to American Chemical Industry .... 931
SpBNCR, I). Catalysis in Vulcanization . 115
Spencer, G. C. and W. O. Emery. Studies in Synthetic Drug
Analysis. V — Estimation of Theobromine 60S
Spencer, M. G., G. L. Kelley, C. B. Ii.i.ingworth and T. Gray.
Determination of Manganese in Steel in the Presence of Chro-
mium and Vanadium by Electrometric Titration 19
Stebbins, J. H., Jr. I — Upon the Action of Tctrazodi-o-Tolyl-
methane Chloride upon Naphlhol and Naphthylamine Sulfo
Acids 445
Stevenson, R. and H. Durand. Research on the Detection of Added
Water in Milk 26
Stiegler, H. W. The Structure of Scarlet SiR(B) and Ponceau
3R(By) 600
Stieglitz, J. Reduction of Waste. Letters. See Gray 153
Stillman, J. M. Dedication of Gil man Hall, University of Cali-
fornia. Address 392
STOCKETT, A. W. The Potash Situation 918
Storm, C. G. Disinfection with Formaldehyde. A Substitute for
the Permanganate-Formalin Method 123
Stipp, C. G. and C. R. Downs. The Determination of Pbthalic
Anhydride in Crude Phthalic Acid 596
Suydam. J. R., Jr. and Whitaker, M. C. A Comparative Study of
the Thermal Decomposition of Coal and of Some of the Products
of Its Carbonization 431
Swan. G. C. and N. Hendrickson. Determination of Loosely Bound
Nitrogen as Ammonia in Eggs 614
SwETT, C. E. Distinguishing Manila from all Cither "Hard" Rope
Fibers ..227
TALBOT. H. P. A Short Manual of Analytical Chemistry, Qualita-
tive and Quantitative — Inorganic and Organic, by J. Muter.
(Book Review) 88
Taylor, G B. and J. H. Capps. Effect of Acetylene on Oxidation
of Ammonia to Nitric Acid 457
and A. S. Coolidge. The Production of Nitric Acid from Nitrogen
Oxides 270
and J. D. Davis. Chemical Control of Ammonia Oxidation.
Note. 156; See Fox 155
Textor, C. K. and O. Kress. Some Experiments on the Pulping of
Extracted Yellow Pine Chips by the Sulfate Process 268
Thompson. G. W. The Importance of Practical Chemistry. Ad-
dress. Chemical Exposition 829
Thornton, W. M., Jr. A Simple and Efficient Filtering Tube 132
Thuras. A. L. and E. E. Weibel. An Electrical Conductivity Re-
corder for Salinity Measurements 626
Tillisch, H. Decanting 63 1
Toch, M. The Pigments of the Tomb of Perneb 1 18
Tolman. I.. M. Introductory Address. Willard Gibbs Medal
Award 483
Tomlinson. G. H. Wood Waste as a Source of Ethyl Alcohol. Ad-
dress, Chemical Exposition 859
Tone, F. J. The Exposition in War and in Peace. Address, Chemical
Exposition 828
Torossian, G. The Emblem of the American Chemical Society.
Note, 869; See Doremus 653
Tucker, S. A. Standard Table of Electrochemical Equivalents and
Their Derivatives, by C. Hering and F. H. Getman. (Book Re-
view) 88
Turner, W. D. and B. G. Nichols. An Inexpensive Ash Leaching
Plant 374
UPTON, H. S. Volumetric Determination of Free Sulfur in Soft
Rubber Compounds 518
VAN ARSDALE, G. D. Tube Milling, by A. DelMar. (Book
Review) 168
Vbitch, F. P. and E. O. Reed. A Constant Temperature and
Humidity Room for the Testing of Paper. Textiles. Etc 38
and C. F. Sammet. Blue and Brown Print Paper: Characteristics,
Tests, and Specifications. . 222
Very, E. D. Municipal Contribution to Conservation through
Garbage Utilization. Address 563
WAGGAMAN, W. H. and C. R. Wagner. The Agricultural Avail-
ability of Raw Ground Phosphate Rock 442
The Use of "Mine Run" Phosphates in the Manufacture of Soluble
Phosphoric Acid 353
Wagner, C. R. and W. H. Waggaman. The Agricultural Avail-
ability of Raw Ground Phosphate Rock 442
The Use of "Mine Run" Phosphates in the Manufacture of Soluble
Phosphoric Acid 353
Walker. H. S. Notes on the Analysis of Molasses 198
Walker. W. H. Library for Edgewood Arsenal Laboratory. See
Letters 868
Revised Statement from the Chemical Service Section. 321; See
Parsons 234
Waller, C. E. Method of Calculating Comparative Strength and
Efficiency of High Explosives from Their Composition and Ap-
parent Densities 448
Washburn, E. W. The Place of the University in Chemical War
Work. Address. Cleveland Meeting. ACS 786
Wbbre, A. L. Theory and Practice in the Design of Multiple
Evaporators for Sugar Factories 191
Weibel, E. E. and A. I.. THURAS. An Electrical Conductivity Re-
corder for Salinity Measurements 626
Weidlein. E. R. Remarks Concerning Suggestions for Central
Medicinal Research Laboratory 976
Weill, L. S. Y. Conservation of Platinum. Letter 494
Weiss, J. M Safely of TNT as an Explosive. Note 1028
Methods of Analysis Used in the Coal-Tar Industry:
I— Crude Tars' 732
II— -Distilled Tars and Pitches 817
III — Heavy and Middle Oils 911
IV — Benzols and Light Oil 1006
and C. R. Downs. Notes on "Free Carbon" of Tar, 400; 5«
Monroe and Broderson, This Journal. 9 (1917). MOO.
Wells. R. American Garbage Disposal Industry and Its Chemical
Relation. Address 567
Wertz. F. A. Notes on the Color Designation of Oil Varnishes 475
Wesson, D. Cotton Oil Industry in the War 930
Edible Fats and Oils, by C. A. Mitchell. (Book Review) 668
Edible Fats, in War and Law 71
igiS
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Wheeler, A. S. Toluol from Spruce Turpentine 359
WiiiTAKKK. M. C. and J. R. Suydam, Jr. A Comparative Study of
the Thermal Decomposition of Coal and of Some of the Products
of Its Carbonization 43 \
White, K. C. Chemists and the Draft. Note ....'. 160
Wichmann, H. J. The Detection and Determination of Coumarin
in Factitious Vanilla Extracts 535
Willard, F. W. Andrew P. Peterson. Obituary 755
Wilson. W. Civil Service Rules Waived for War Gas Investigators
Executive Order " 753
Licensing of Fertilizer Industry Ordered. Proclamation 323
Transfer of the Experiment Station at American University to the
War Department, 654; See Baker 654
Winter, O. B. A Contribution to the Composition of Lime-Sulfur
Solutions
Wish:, L. E. and E. Q. Adams. Photographic Sensitizing Dyes:
Their Synthesis and Absorption Spectra. Dyestuff Symposium,
Cleveland Meeting. A. C. S SOI
Withers. W. A. The Chemistry of Farm Practice, by T. E. Keitt.
(Book Review) 249
Woodman, A. G. Th
poses, by J. Race
and A. A. Cook.
Products
Wooton, P. Washingt
Examination of Milk for Public Health Pur-
( Book Review)
'he Detection of Vegetable Gums in Food
>n Letter:
80, 160, 239, 325, 403, 496, 582, 656, 753, 870, 948,
Wright, C. D. and W. O. Emery. Studies in Synthetic Drug
Analysis. VI — Evaluation of Hexamethylcnetetramine Tablets.
I045
666
530
1033
606
ZERBAN, F. W. The R6Ie of Oxidase and of Iron in the Color
Changes of Sugar Cane Juice 814
and E. C. Freeland. On the Preparation of an Active Decolorizing
Carbon from Kelp 812
Zitkowski. H. E- The Seeding Method of Graining Sugar 992
Zoller, H. F. Some Constituents of the American Grapefruit
{Citrus decumana) 364
' The Status of Chemical Engineering in Our Universities and Col-
leges Immediately Prior to the Declaration of War. Address,
644 ; See Mason 753
SUBJECT INDLX
THL JOURNAL OF INDUSTRIAL AND LNGINLLRING CHEMISTRY
VOLUML X 1918
ABSTRACTORS and Assistant Editors, Directions (or
Accidents, Metal-Mine, in U. S. during 1916. Fay. Gov. Pub
Accidents. Quarry, in U. S. during 1916. Fay. Gov. Pub
Acetic Acid, Determination of, by Disillation with Phosphoric Acid.
W. F. Munn
Acetone, Determination of A. J. Field
Acetylene, Effect of, ou Oxidation of Ammonia to Nitric Acid. G. B.
Taylor and J. H. Capps
Acetylene, Reactions of. Note
Acetylsalicylic Acid, American- Made, Examination of. P. N. Leech.
Acetylsalicylic Acid. What's in a Name? Editorial
Acid, Liquids, An Evaporator for. E. Hart
Acid-Proof Alloys. Note
Acidity, Pipette Used in Titration of Oils for. J. Jacobsen
Acids, Fatty, in Putter Fat. Holland and Kuckley, Jr. Gov. Pub. . .
Addressbs 60, 133, 297, 383, 476, 556, 634, 918,
Aeronautic Construction, Fabrics for. Whalen. Gov. Pub
Aeronautic Power Plant Investigations. Dickinson. Gov. Pub. . . .
Aeronautics and Meteorology. Blair. Gov. Pub
Aeronautics, National Advisory Committee for
Aeroplane Construction. Note.
Agriculture, Courses in Secondary, for Southern Schools. Barrows.
Gov. Pub
Agriculture, Department of. Gov. Pub 332, 503, 763,
Air Propellers. Experimental Research on. Durand. Gov. Pub....
Air Raid Signals. Note
Airplane Dopes. G. J. Esselen, Jr. Address
Air Vapor Mixtures, Recovery of Solvents from. E. L. Knoedler and
C A. Dodge
Airs from Mine Fire, Some Results of Analysis of. A. G. Blakelev
and H. H. Geist
Alabama, Oil and Gas Possibilities of the Hatchetigbee Anticline.
Hopkins. Gov. Pub
Alabama Technical Association: Joint Meeting with Alabama
Section A. C. S., Birmingham, Ala., May 2, 1918. Program
Alcohol as Used in Medicines, Conservation of. Note
Alcohol, Industrial-, Chemistry, and Preservatives. Gov. Pub
Alcohol. New Source of. Notes 313,
Alcohol Production in Germany. Note
Alcoholic Medicinal Preparations
Alcohols and Bases in Vacuum Tar. Note
Alfalfa Hay, Corn Silage, and Velvet-Bean Meal when Fed Singly and
in Combinations, Digestibility of. Ewing and Smith. Gov. Pub. .
Alien Property Custodian, Cooperation Requested by the. A. M.
Palmer. Note
Alien Property Custodian: The Custodian in Action. Editorial. . . .
Alinement Chart for Evaluation of Coal. A. F. Blake
Alloy, A Deoxidizing. Note.
Alloy, New Aluminum. Note
Alloy, New Magnesium. Note
Alloys, Acid-Proof. Note
Alloys, Aluminum, Analysis of. Note
Aluminum. Hill. Gov. Pub. In 1916. 84; in 1917
Aluminum. Note
Aluminum Alloy. New. Note
Aluminum Alloys, Analysis of. Note
Aluminum and Copper in Germany. Note
Aluminum and Its Alloys. Note
Aluminum, Annealing. Note
Aluminum Goods for Brazil. Note
Amalgam. Copper, as Metal Cement. Note
American Association for the Advancement of Science: 75th
Annua! Meeting. Pittsburgh. December 28, 1917, to January 2,
238
958
958
457
488
288
255
555
649
633
763
1016
873
873
873
873
943
503
959
873
941
247
493
495
409
1022
650
245
650
673
627
398
650
75
649
747
860
862
650
747
649
1020
1021
229
74
I'm
American Ceramic Societv: Northern Ohio Secti
Toledo. April 6, 1918; Cleveland, June 10. 1918. . .
The Journal of. Editorial
American Chemical Society:
.Pin. C. L. Parsons..
for A
Chemists. C. A. Doremus, 653;
Note.
.American Ei
See Torossi
An Opportunity to Help the French. C. L. Parsons.
Chemistry for the Public. R. D. Cooke. Note
Communication from II S. Shipping Board E. N. Hurley
Cooperation with the Chemical Service Section Note
Dr. Nichols— Leader in Chemical Industry. C. F. Chandler
Editorials:
\ Dyestuff Section of tbo A. C. S
V French Local Section.
A Golden Opportunity
A Regrettable Decision of the Directors
A Spocial Meeting of the Council
America in Safe Hands
An Experiment in Publicity
Vn International Courtesy
\notlicr Idol Shattered
Preparation for After the War
Publicity Work to be Continued
rhe Missing I-', vi- Thousand
The Naval Consulting Hoard
Fertilizer Division: Report of. Committee on Research and Analyti-
cal Methods. 1'. Rudnick
56th (Annual) Meeting, Cleveland, September 10 to 13, 1918:
Announcements, 494. 6 191, 67J; Tentative Pro-
gram. 748; Symposium on Chemistry of Dyestuffs. Note. R
N. Shrcv
President's Address.
Nichols
A Retrospect and an Application. W. H
869
1024
752
864
967
418
967
673
SSI'
878
338
750
768
American Chemical Society (concluded):
Council Meeting
General Meeting
Symposium — Chemists in Warfare
Symposium — Chemistry of Dyestuffs
Program of Papers
Industrial Chemists and Chemical Engineers Division:
Minutes of Business Sessions at Cleveland Meeting. H.
II,
Tentative Standard Methods for the Sampling and Analysis of
Commercial Fats and Oils 315
Journals. Note 1 02^
Local Sections:
Alabama Section. Joint Meeting with Alabama Technical
Association, Birmingham, May 2, I91K. Program of Papers.
Etc 493
French Section 575, 1023
New York Section. Resolutions following suspension of L. P.
Brown as Director of Bureau of Food and Drug Inspection of
the City of New York 49?
North Carolina Section Joint Meeting with North Carolina
Academy of Science, Greensboro, N. C, April 26 and 27, 1918.
Program of Papers 492
Officers for 1918 92
Organic Chemistry Division: Resolution Concerning Organic
Nomenclature 944
Our Preparation for After the War. Address. B. C. Hesse 881
Rubber Section: Report of Committee on Organic Accelerators.
Cleveland Meeting 865
Spring Meeting. Announcement of Its Omission 236
American Chemical Trade, Effect of the War on. O. P. Hopkins 692
American Chemists Welcomed by the Cercle de la Chiniie. Transla-
tion. President of the Cercle de la Chimie 482
American Drug Manufacturers Association: Annual Meeting,
New York City, January 29 to 30. 1918 233
American Dyestuff Industry and Its Prospects. Translated from
German 1026
American Electrochemical Society:
Resolutions Concerning Alien Enemy Members " ^n
33rd General Meeting, Tour of South, April 28 to May 4, 1918:
Announcement, 321; Report bv C. F. Roth 489
34th General Meeting, Atlantic City, September 30 to October 2,
1918:
Announcement, 750, 866; Program of Papers ... 866
Report J. W. Richards 9+4
American Institute of Chemical Engineers:
10th Annual Meeting. St. Louis. December 5 to 8, 1917 77
10th Semi Annual Meeting. Gorham and Berlin, N. H., June 19 to
22, 1918:
Program of Papers 4V.i
Report. J. C Olsen
American Institute op Mining Engineers 116th Meeting, New
York City. February 18 to 21. 1918. Program of Paper 321
Report of Milwaukee Meeting, October 7 to 12, 1918. I W".
Richards 94J
American Leathbr Chemists' Association:
Annual Meeting. Atlantic City. N. J.. May 16 to 18, 1918:
Program of Papers 44.;
American Metric Association: Second Meeting 154
American Pharmaceutical Association:
Announcement of Annual Convention
Ammonia and Nitric Nitrogen Determination in Soils Extracts and
Physiological Solutions. B. S. Davisson 600
Ammonia Industry, License of. Presidential Proclamation. Gov.
Pub 40s
Ammonia in Eggs, Determination of Loosely Bound Nitrogen as. N.
Hendrickson and G. C. Swan I < I -J
Ammonia. Latent Heat of Vaporization of. Osborne and Van Dusen.
Gov. Pub 4 1 !
Ammonia, Liquid, Latent Heat of Pressure Variation of. Osborne
and Van Dusen. Gov. Pub Mf
Ammonia. Liquid, Speci6c Heat of Osborne and Van Dusen. Gov.
Pub 41.'
Ammonia. Oxidation of. Note 94 I
Ammonia Oxidation Process. Analytical Control of. P. J. Fox.
Note. 15.5; See Taylor and Davis 156
Ammonia Program for 1918. C. W. Merrill 4SC
Ammonia: Relation between Efficiency of Refrigerating Plants and
the Purity of their Ammonia Charge. F W. Frerichs 202
Ammonia to Nitric Acid. Effect of Acetylene on Oxidation of. G. B.
Taylor and J. H. Capps 45:
Amyl Acetate and Similar Solvents from Petroleum l'entane. Manu-
facture of. B. T. Brooks, D. F. Smith and H. Essex ill
Anaerobic Culture Volumeter. Z. Northrup 624
Andean Sulfur Deposits. Miller and Singewald, Jr. Gov. Pub 586
Anthelmintics. Efficacy of Some. Hall and Foster. Gov. Pub. . . 504
Anthraquinonc, Quantitative Estimation of. H. P. Lewis 425
Antimonial Silver-Lead Veins of the Arabia District. Nevada. Knopf.
Gov. Pub 331
Antimony in 1916. Bastin. Gov. Pub 761
Antimony Sulfide as a Constituent in Military and Sporting Anns
Primers. A. S Cnsliman
Antipneumococcic Serum. Phenols as Preservatives of. Pharma-
cological Study. Voegtlin. Gov. Pub
Apparatus (see under name of piece).
Apparatus and Special Chemicals Available through the Chemistry
Committee of the National Research Council. M. T. Bogert
Note 15*
Dec, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Argentina, Coal-Mining Machinery for. Note 228
Argentina, Jute Sacks for. Note ....'. 74
Argentine Chemical Society, Platinum Resolution by. See Letters
G. F. Schaefer and W. H. Nichols 322
Army, National, The Chemical Service Section of the. Editorial. . . '. 2
Army Ordnance, U. S., High-Grade Technical Men and Skilled
Operatives Wanted for. Note 495
Army Without Reserves. Editorial, 508; Symposium 685
Aromatic Hydrocarbons from Natural Gas Condensate, The Forma-
tion of. J. G. Davidson 90)
Arsenates, Calcium. Robinson. Gov. Pub 764
Arsenic. Umpleby. Gov. Pub In 1916, 409; in 191 7 761
Arsenic Compounds, An Experimental Investigation of the Toxicity
of Certain Organic. Roth. Gov. Pub 1037
Arsenic in Insecticides, Determination of, by Potassium Iodate. G
S. Jamieson 290
Arsenic in Sulfured Food Products. W. D. Collins 360
Arsenious Oxide. Pure. Preparation and Testing of. R. M Chapin, 522
Arsphenamine and Neo-Arsphenamine. Some Qualitative and Quanti-
tative Tests for. Meyers and DuMez. Gov Pub 758
Arsphenamine (Salvarsan) and Neo-Arsphenamine (Neo-Salvarsan).
Gov. Pub 586
Arsphenamine (Salvarsan): Licenses Ordered and Rules and Stand-
ards Prescribed for Its Manufacture. Gov. Pub 245
Asbestos Industry, Russian. Note 397
Ash Leaching Plant, Inexpensive. W. D. Turner and B. G. Nichois. . 374
Ash: Proximate Quantitative Method for the Determination of
Rubidium and Caesium in Plant Ash. W. O. Robinson 50
Asphalt and Coal Deposits. Gov Pub 408
Aspirator. J. M. Johlin 632
Aspirin: Examination of American-Made Acetvlsalicylic Acid. P
N. Leech, 288; See Editorial 255
Assistant Editors and Abstractors, Directions for 238
Association of British Chemical Manufacturers. Note 751
Atlantic Coast, The Menhaden Industry of the. Greer. Gov. Pub. . 166
Australia and New Zealand, Railway Materials, Equipment, and Sup-
plies in. Rhea. Gov. Pub 664
Australia, Goods in Demand in. Note 861
Australian Gelatin, Glue and Size. Note 487
Autoclaves and High Pressure Problems. Note 230
Automatic Control and Measurement of High Temperatures. R. P.
Brown. Address 133
Azotobacter, Soil Reaction and Growth of. Gainey. Gov. Pub. ... 959
BACTERIA, Effect of Nitrifying, on Solubility of Tricalcium Phos-
phate. Kelly. Gov. Pub 763
Bacteria, Nitrogen-Assimilating, Influence of Nitrates on. Hills.
Gov. Pub 504
Balloon Fabrics, Determination of Permeability of. Edwards. Gov.
Pub 762
Bank, National Metal and Chemical. Note 940
Baseball Players, Commissions for. Editorial 879
Bases and Alcohols in Vacuum Tar. Note 650
Batik Dyeing Process. Note 938
Bauxite. Hill. Gov. Pub. In 1916, 84; in 191 7 760
Bauxite, Refractory Material from. Note 862
Beilstein's Handbuch der Organischen Chemic. Turn About is Fair
Play. Editorial, 672; See Letters 867
Belting. Laminated. Note 314
Benzene: Application of the Differential Pressure Method to the
Estimation of the Benzene and the Total Light Oil Content of Gases.
H. S. Davis, M. D. Davis, and D. G. MacGregor 712
Benzene Vapor, The Determination of. VII — Reagents for Use in
Gas Analysis. R. P. Anderson 25
Benzols: Methods of Analysis Used in the Coat-Tar Industry. IV —
Benzols and Light Oils. J. M. Weiss 1006
Bichromate Manufacture in Sweden. Note 1022
Biological Products, Nature of Contaminations of. Bengston. Gov.
Pub 873
Biological Products. Studies in Preservatives of. Neill. Gov. Pub. . 873
Birch, The Effect of Incomplete Distillation on the Yield of Products
in the Destructive Distillation of. R. C. Palmer 260
Bismuth Umpleby. Gov. Pub. In 1916, 409; in 1917 873
Bismuth, Industrial Uses of. Note 573
Bismuth, Pure. Notes 229, 573
Bismuthinite, Photoelectric Sensitivity of. Coblentz. Gov. Pub.. 762
Bittern, Sea Water, The Extraction of Potash and Other Constituents
from. J. H. Hildebrand 96
Ulast-Furnace Breakouts, Explosions, and Slips, and Methods of
Prevention. Willcox. Gov. Pub 412
Blast-Furnace Plants, Occupational Hazards at, and Accident Preven-
tion Baaed on Records of Accidents at Blast Furnaces in Pennsyl-
vania in 1915. Willcox Gov. Pub 412
Blast-Furnace Practice. Note 746
Blast-Furnace Work. Slag Viscosity Tables for Keild and Roystcr.
Gov. Pub 959
Blue and Brown Print Paper: Characteristics, Tests, and Specifica-
tions. F. P. Veitch, C F Sammet, and E. O. Reed 222
Blue Gas. Toluol by Cracking Solvent Naphtha 111 the Presence of.
G. Egloff f
Boiler Scale, Graphite for Note 395
Boiler Scale, Prevention of. Note 151
Bolivia. Ecuador, and Peru, Textile Markets of. Tucker. Gov.
Pub 664
Bolivian Wolfram Industry Not* 940
Hook Rbvikws (see separate heading l«t
Borax and Boric Acid. Note
BOTU Production in 1916. Yale and Gall .,. Pub H"
Bordeaux Mixtures. Commercial Hon to Calculate Their Values.
Wallace and Evans Gov. Pub 959
Boric Acid and Borax. Note "
Boron Its Effect on Crops and Its Distribution in Plants and Soil
in Different Parts of the U S. Cook and Wilson. Gov. Pub... 764
Brake, Fan Dynamometer. Note . 744
Brass, Bronze, and Copper Products. Gov. Put) 332
Brass. Cadmium in. Note 939
rhcrmal Expansion of Alpha and ol Beta Brass between
0° and 600° C. in Relation to the Mechanic .1 Properties of Hetero-
geneous Brasses of the Muntz Metal Type. Merica and Schad.
Gov. Pub 762
Brass Tubes, Corrosion of. Note
Brazil. Aluminum Goods for. Note 229
Brazing Table, Gas-Fired. Note 1022
Brick, Sand-Lime, in 1917. Middleton. Gov. Pub 956
Brines and Potash Salts, Nebraska, Some Methods of Analysis for. A.
H. McDowell 128
Briquetting, Fuel, in 1917. Lesher. Gov. Pub 662
British Board of Trade. Notes:
76, 151, 230. 314. 398, 488, 574, 650, 747
British Chemical Manufacturers, Association of. G. Mount 495
British Dye, New. Note 75
British Dyes Limited. Account of Progress. J. Falconer.. . 145
British Empire, Petroleum in. Note 572
British Paper Exports. Note 76
British Progress in Dyestuff Manufacture. J. Falconer. 145
British Trade: Register of Overseas Buyers. Note 573
Bromine in 1917. Stone. Gov. Pub 957
Bromine Process Decision. Case of Dow Chemical Co. vs. American
Bromine Co. and A. E. Schaefer 157
Bronze, Brass, and Copper Products. Gov. Pub 332
Brown and Blue Print Paper: Characteristics, Tests, and Speci-
fications. F. P. Veitch, C. F. Sammet. and E. O. Reed 222
Buckwheat: Comparative Study of Salt Requirements for Young
and for Mature Buckwheat Plants in Solution Culture. Shive
and Martin. Gov. Pub 959
Bulletin, Official V. S. Note 654
Bureau of Census. Gov. Pub 331, 412, 958,1037
Bureau of Education. Gov. Pub 412
Bureau of Fisheries. Gov. Pub 166
Bureau of Foreign and Domestic Commerce. Gov. Pub 664, 764. 874
Bureau of Foreign and Domestic Commerce: Its Relations to
Chemical Industry:
Government Trade-Building Information. C D. Snow 931
Our Publications and Their Bearing on the Chemical Industry.
O. P. Hopkins 933
-Method of Preparation of the Census of Chemical Imports.
E. R. Pickrell 936
Bureau of Labor Statistics. Gov. Pub 412
Bureau of Markets in Its Relation to the Conservation of Foods.
C. J. Brand 66
Bureau of Mines: Director's Annual Report H2
Government Publications 85, 332,412, 958
Yearbook, 1916 85
Bureau of Ordnance. Gov. Pub H2
Bureau of Standards:
Government Publications 85, 166, 412, 503, 762, 959
Recovery of Light Oils and Refining of Toluol 51
Burmese Monazite Sands. Note 1020
Butter and Milk, Enzymes of. Thatcher and Dahlberg. Gov. Pub.. 503
Butter Fat, A Method for the Detection of Foreign Fats in. A.
Seidenberg- 617
Butter Fat and Income. McDowell. Gov. Pub 763
Butter Fat. Determination of Fatty Acids in. Holland and Buckley,
Jr. Gov. Pub 763
Butter or Oleomargarine. Detection of Added Color in. H. A. Lubs . 436
Butter Substitute from Fish Oils. Note 397
Butter Tree. Shea, Gutta-Percha from. Note 76
Buttons, Manufacture of. Gov. Pub . . 332
Book Reviews 88, 167, 249, 504, 666, 960, 1038
Analytical Chemistry, A Short Manual of, Qualitative and Quanti-
tative—Inorganic and Organic, by Muter. H.P.Talbot 88
Applied Analytical Chemistry, Treatise on, by Villaveechia, et at
Translated by Pope. A. Rogers 960
Cellulose. An Outline of the Chemistry of the Structural Elements
of Plants, by Cross and Bevan. A. D. Little 960
Chemical Analysis, Standard Methods of, edited by Scott. W. T. Hall 250
Chemical Annual, Van Nostrand's, edited by Olsen and Matthias.
R. K. Meade 962
Chemical Engineering, Catalog, issued bv The Chemical Catalog Co..
Inc., 1917 Edition, G. D. Roscngarten, 88; 1918 Edition, C. H.
Herty 1038
Chemical French, by Dolt. A. M. Patterson 961
Chemical Laboratory of the American Medical Association, Annual
Report of, by American Medical Association. H. V. Amy 66K
Chemical Patents and Allied Patent Problems, by Thomas. K. P
McElroy 167
Chemistry, Everyman's, by Hendrick. A. Rogers 168
Chemistry of Farm Practice, by Keitt. W. A. Withers 249
Chemistry of Materials of the Machine and Building Industries,
by Leighou. H. K. Benson '■<«'
Chemist's Pocket Manual, bv Mrade. A. C. Langmuir '>(><'
Coal, Bituminous, The Storage of, by II. 11. Stoek. A. C. Fieldner. . 668
Coal, Coke, and By-Products, Methods for Commercial Sampling and
Analysis, by J. M. Camp. S. W. Parr 666
Coal Gas Residuals, bv K. 11 Wagner. R. P. Perry '•<>
Colloid Chemistry, Theoretical and Applied, An Introduction to,
by Ostwald. J. Alexander '*"
Colloids, The Chemistry of. by Zsiginondy. J. Alexander
Commercial 1 rrganic Analysis, by Allen. A. Rogers 250
Electrochemical Equivalents and Their Derivatives, Standard Table
of, by Hexing and Getman. S. A. Tucker 88
Enzyme Action. The Method of, by Heatty. J. F. Brewster 504
Explosives, by Marshall. C. K. Munroc 167
Fats and Oils. Edible. 1>\ C A. Mitchell. D. Wesson 668
Fertilizer Handbook, American, by Ware Bros. Co., .JiUJ by Toll.
I. B. Breckenridge 962
Industrial Chemistry, Laboratory Guide of , by Rogers. Nil. McKec 250
Leather : i roix, A. Rogers 88
l.ul.iir.mr., \in.-iieaii. bv Lockhart. A.H.Gill 504
1. uiMu.it hi Handbook, by Battle. \ H. G1U l"x
Milk Examination of, f.ir Public Health Purposes, by J. Ruce. A
hii.i.i A<"'
Nomographv.Ch.-nin-.il. I Manual of, by H. G. Defiling. J.M.Bell 668
ami rii. 11 Commercial Products, Aids in the Commercial
Inalysii ,,t Handbook, by O, !•' Pickering, A.
ind \ntini.ini . hj Morgan. J. B,
kill '- . ,
Photography, ' no Practice of, by Roebuck, s B
ppard
by lognoli. J. I . Baker
1 he Distillation "f. by Schwdzer, A 11. Davis..
9i „„tist ami m Basker-
■ ill.-
1038
Ml
1048
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, Xo. 12
Book Reviews (concluded):
Sulfuric Acid Handbook, by Sullivan J P.. F Herrcshoff 960
Tube Milling, by DelMar c, d Van Arsdale 168
Cadmium in Brass: Note 939
Cadmium in 1917 Siebenthal. Gov. Pub 954
Cadmium Vapor. Resonance and Ionization Potentials for Electrons in.
Tate and Foote Gov Pub 762
Caesium and Rubidium in Plant Ash, A Proximal.- Quantitative
Method for the Determination of. W. O. Ro ... 50
Calcium and Magnesium, Influence of Carbonates of, on Bacteria of
Wisconsin Soils Fulmer Gov. Pub 763
Calcium Arsenates. Robinson. Gov. Pub 764
Calcium Chloride in 1917. • Stone Gov. Pub 957
CALENDAR OF Mektincs 121, 403, 494. 580, 653, 748
California, The Research Unit of the Chemistry Group at the Uni-
versity of. Oilman Hall. M Randall 634
California. University of, tuk Dedication of Gilman Hall 391
Calorimeter Installation. A Convenient Multiple Unit. Davis and
Wallace. Gov. Pub 959
Camphor. Japanese. Note 1022
Canada, Mineral Production in. Note 74
Canada's Export Trade. Note 572
Can. uli. in Lake, Recovery 0 "1 Potash from. Note 151
I anadian Nickel, Recovery of Platinum Metals from. Note 76
Cane Hy- Products in Natal Note . 745
Canning and Preserving. Gov Pub 332
Canning Industry: Some Accomplishments and opportunities Along
Technical Lines. Address. H A Baker 69
Carbon, Active Decolorizing, from Kelp. On the Preparation of. F.
W. Zerban and E. C. Freeland 812
Carbon Dioxide in Carbonates, A Rapid Pressure Method for De-
n, m of. W. H. Chapin 527
Carbon Dioxide, New Determinations of, in Water of Gulf of Mexico.
Well. Gov Pub 954
Dioxide, Relation of. to Soil Reaction as Measured by the
Hydrogen Electrode. Hoagland and Sharp Gov. Pub 504
Carbon in Steel. Rapid Determination of. by Barium Carbonate
Titration Method I. R Cain and I. C. Maxwell 520
ii-.ii Studies II- The Carbonation of Distilled Water. H.
i, and G H Mains 279
l anionic (ires Mining and Concentration of. Kithil and Davis.
Gov. Pub 958
Carotin in Oils and Vegetables, The Occurrence of. A. H. Gill 612
rol A Study of Conditions Essential for Commercial Manu-
facture of. A W. Hixson and R H. McKee 982
in Presence of Starch, Effect of Time of Digestion on Hydroly-
McHargue. Gov. Pub 504
Casein. Manufacture of. from Buttermilk or Skim Milk. Dahlberg.
Gov. Pub "63
Charles, [r Obituary WW Randall 240
lil of. Constituents of II F. D Dodge 1005
Cast Iron Pipe Gov Pub 331
from Metallic Salts. Note 747
Catalysts in Vulcanization. D. Spence 115
Processes in Germany. Note 939
ers Effect of, on Yield of Products in Destructive Distillation
ol Hardwoods R C Palmer. 264
Cell New Voltaic. Note 744
1 urpentine Note K2
Cement: Concentration of Potash from Raw Materials Containing
only a Trace of this Element bv Means of the Electric Precipitation
of Flue Dust and Fume Cement Kilns B F Erdahl 356
: . incut Draintile and Concrete in Alkali Soils. Durability of. (Con-
taining Results of Third Year's Tests Wig, rt of. Gov. Pub 85
Industry, The Recovery of Potash as a By-ProduCt in the.
I 0\ Pub 332
Cement, Metal. Copper Amalgam as Note .... 74
Cement Mill Dust, Direct Heat Treatment of, to Increase Its Water-
Soluble Potash Content. A R Merz 106
Cement Mill Potash. Effect of Coal Ash on the Liberation and Nature
of. N S. Potter, Jr., and R D Clue, man 109; Se< Letters 1030
Cement Mortars and Magnesium Note 746
Cement, Portland, Properties of. Having a High Magnesia Content.
Bates 413
I ortland, Standard Specifications and Tests for. Gov. Pub. . 874
Cement Production (1916). Burchard. Gov. Pub 110
Census ol Chemists F. E. Breithut. Note 946
Dyes and Coal-Tar Chemicals, 1917, A Record of Achieve-
ment Editorial 879
i eramici Developments in. Editorial . 878
imie Uncu, n i !i. mi ,t Welcomed by the Fransla-
Pr< sidi iit of the Cerch de la Chin . 482
with Reference to Their Content in " Antineuritic Vita-
mine, The Dietary Defici Voegtlin, el of, Gov, Pub . 586
irhotite Ores of Southern Oregon, Flotation of Clial-
.412
iidable Waste in the Production of Sulfuric Acid
by the A E Marshall Note 156
a A. F, Blake
ction 948
Cheese Ripening, Suulv ol the Streptococci Concerned in Evans,
763
Cheese, Varieties of, Doanc and Lawson ' .'^ Pub f63
Chemical I nnial Index Patrons .... 77
Chemical Abstract . The Indexes to E.J ,;
Chemical Alliance The Editorial, 2; Announcement 231
Chemical and Allied Indu Pub 958
Chemical and Dec Industry, Italian. Note 745
Chemical Hani, National Metal and. N..t. ...... 940
ities and Colleges Immediately
Pnoi to I ion ol Wat the St itu ol II F /oiler, r.44:
' P Mason 753
ilh Graduate.
. 1019
■ s of Walker ami Smithcr.
,. i'., i, . . 762
CHUMICAL I-."' OSITION Ol
N.v. \ i 1918 Editorials, 592, 672.
list ol Exhibitors, 749. Ad-
' 826
Chemical Industries, Fraudulent Promoters ol. Camp Followers.
Editorial -';^
ICh, During 1": ::. 4.'1
Chemical Industries of England. Women in the. Note 1028
Chemical Industries. 1 S Tariff Commission Inquiry in Regard to . 158
Chemical Industry, American and the Burbau of Porbign and
DoMEsi U '
Government Trade Building Information C. D. Snow . . . . 931
Our Publications and Their Bcarin.: on the Chemical Industry. O.
P. Hopkins 933
Method of Preparation of the Census of Chemical Imports E. R.
Pickrell 9t6
Chemical Industry in China Note . 649
Chemical Industry in the Netherlands Note 947
Chemical Industry of Germany. New After-War Preparations.
Translated from French 1025
1 Manufacturers. Association of British. G. Mount, 495;
See Note 751
Chemical Markets in the Union of Solth Africa OP Hopkins . 887
Chemical Markets of Soi-tii America o p Hopkins
Chemical Trade of Argentine, Brazil, and Uruguay 701
Chemical Trade of Chile, Peru, and Bolivia 805
Chemical Markets of Colombia, Ecuador, the Guianas, Venezuela,
and Paraguay 977
Chemical Microscopy E. M. Chamot. Address 60
Chemical Research in the Various Countries Before the War and in
1917. E.J.Crane. Note .236
Chemical Service Section of the National Army: Editorial. 2; Note
CI. Parsons, 234; Revised Statement. W H.Walker 321
Chemical Societies m New Vork City. Program for 1918-1919
Season 748
Chemical Society for Women. Iota Sigma Pi. Note 1023
Chemical Society (London). An International Courtesy. Editorial. 673
Chemical Tests for Detection of Rancidity. R H. Kerr 471
Chemical Trade, American, Effect of the War on. O. P. Hop-
kins 692
ChjSmical Warfare Service
Editorial Note, 675; General Orders. No. 62 675
Organization Plan of Chemical Warfare Service 677
Commissioned Personnel. 680; Correction 948
Census of Chemists 683
Chemists in Camp 684
Chemical Warfare Service. Collar Insignia for. Note 655
Chemical Warfare Service. Commission for Baseball Players.
Editorial 879
Chemicals and Explosives Divisions. War Industries Board. Note. . . 654
Chemicals Division of National War Savings Committee Organized.
Note 402
Chemicals, Explosive. Note 745
Chemicals for Research Work. C. E. K. Mees Notes 656, 1027
Chemicals. Fuel for Manufacture of. E Smith Note 159
Chemicals. Special, and Apparatus Available Through the Chemistry
Committee of the National Research Council. Note. M. T.
Bogert 158
Chemistry for Soldiers in Training Camps. J. W. Beckman 869
Chemistry for the Public. Note. R. D. Cooke 752
Chemistry. Industrial Alcohol, and Preservatives. Gov Pub 409
Chemistry of Cotton Plant with Special Reference to Upland Cotton.
Vierhoever, el al. Gov Pub 764
Chemistry of DyBSTUPPS, SYMPOSIUM on (Cleveland Meeting,
A C S
Introductory Remarks R N Shreve fU
America's Progress in DvestulTs Manufacturing I. J. Matos
The Development of the Dvestuff Industry Since 1914. J. F.
Schoellkopf. Jr .792
Ipplication of Dyestuffs in Cotton Dyeing. J M. Matthews
Natural DvestufTs — An Important Factor in the Dvestuff Situation.
K. S Chapin .795
The Manufacture. Use. and Newer Llevelopments of the Natural
Dyestuffs C. R Delaney .
Photographic - Their Synthesis and Absorption
Spectra. L. E Wise and E. Q Adams -. 801
The Color Laboratory of the Bureau of Chemistry H. D. Gibbs . 802
Problems in Testing Dyes and Intermediates E W Pierce 803
l m the Quantitative Analysis of Dyestuffs A H Halland 804
Chemistry, Physical, in Coal-Tar Industry. W .1 Huff 1016
Chemistry. The Debt of Preventive Medicine to G W Gol
Chemists, American, An American Emblem for. C. A. Doremus.
Note
Chemists, American Welcomed by the Cercle de la Chimie. Transla-
te la Chimie 482
Chemists ami Enemy-Owned Chemical Works
The Custodian in Action Editorial..
Chemists and the Draft. E. C. White
Chemists' Club: Annual Meeting.
Editorial gl
Portrait ol C M Hall Note 9K
The Parting of the Ways Editorial 2SJ
Chemist- club for France. Editorial..
Chemists Deferred Classification and Furloughs for Government and
Slate Chemists Note
Chemists in Warpari on I Cleveland Mi
The American Chemist in Warfare C I. Parsons
The Work of the Chemical Section of the War Industries Board.
C 11 MacDowcll '80
War I lis d Peace Read lustments in the Chemical Ill-
dust n, ■ " -S2
Chemical Warfare Research W D Bancro
The Place of the University in Chemical War Work. E W Wash-
burn
Chemists in War Service A Letter from France. W A llaiuor 495
A Long step in the Right Direction. Editorial 1
In Safe Hands Editorial 418
An Army Willi.
i of the President Editorial ■ ■ 654
v Insignia. Editorial ''■"
American Chemical Society with the Chemical ser-
NoK ■ - 581
I - the Importance of Chemistry in the War
C 1. vised Statement W II Walk.:
liied by Secretarj of War N.
but not Politics. Editorial
Prepared Note 3«
Prophecj and Fulfilment. Editorial **1^
Somebody Please Cut the Tape, Editorial '4
The Chemistry Rainbow Editorial
The Return of the Chemists 968
Dec, 1918
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Chemists in War Service (concluded):
Transfer of the Experiment Station at American University to the
War Department. W. Wilson, N. D Baker. Note. 654; See
Editorial
War Risk Insurance for Chemists in Military Service. Note. . .
Washington Notes. Editorial
Where are the Leaders' Editorial
Chemists, Industrial. College Courses for C. W. Hill
Chemists, The Census of. F. E. Breithut. Note
Chile, Potash Salts in. Note
China, Chemical Industry in. Note
China, Jute Production in. Note
China, Potteries at Shek Waan, Near Canton. C. N. Laird
Chinese Pencil Factory. Note
Chinese Perfume Plant. Note
Chlorides and .Sulfates of Sodium and Potassium, Separation of, by
Fractional Crystallization. W. C. Blasdale
Chlorides: Equilibria in Solutions Containing Mixtures of Salts.
I — The System Water and the Sulfates and Chlorides of Sodium and
Potassium. W. C. Blasdale
Chlorine, Tar-Still Corrosion by. Note
Chrome Ore and Magnesite. Transvaal Deposits of. Note
Chrome Tanning. Note
Chromite. Diller. Gov. Pub. In 1916, 84; in 1917
Citral, An Improved Method for Determining A Modification of the
Hiltner Method. C. E. Parker and R S Hiltner
Civil Service Rules Waived for War Gas Investigators. W. Wilson.
Clay-Working Industries and Building Operations in the Larger Cities
in 1916. Middleton. Gov Pub
Clays, Louisiana, Including Results of Tests Made in the Laboratory
of the Bureau of Standards at Pittsburgh Malson. Gov. Pub...
Cloves, Oil of. Note
Coal; A Comparative Study of Thermal Decomposition of Coal and
Some of the Products of Its Carbonization. M. C. Whitaker and
J. R. Suydam, Jr
Coal, An Alinement Chart for the Evaluation of. A. F. Blake. 627;
Correction
Coal: Analyses of Mine and Car Samples of Coal Collected in Fiscal
Years 1913-1916. Fieldner, el al. Gov Pub
Coal and Asphalt Deposits. Gov. Pub
Coal and Rock-Dust Mixtures in Mines, The Quick Determination of
Incombustible Matter in. Fieldner, el at Gov Pub
Coal Ash, Effect of, on the Liberation and Nature of Cement Mill
Potash, N S Potter. Jr. and R. D. Cheesman, 109; See Letters. .
Coal. Cancel, in the U. S. Ashley. Gov. Pub
Coal, Combustion of. Note
Coal, Combustion of, and Design of Furnaces. Kreisinger, el at.
Gov. Pub
Coal, Effect of Low Temperature Oxidation on the Hydrogen in. and
the Change in Weight of Coal on Drying. Katz and Porter. Gov.
Pub 1
Coal for Shipment or Delivery, Directions for Sampling. Pope.
Gov. Pub
Coal Mines of Illinois, Use of Permissible Explosives in. Fleming and
Koster. Gov. Pub
Coal-Mining Machinery for Argentina. Note
Coal. New Views of the Combustion of tin Volatile Matter in. Katz.
Gov. Pub
Coal Products, an Object Lesson in Resource Administration. Mineral
Industries of the U. S. Gilbert. Gov. Pub
Coal, Resource and its Full Utilization: Mineral Industries of the
United States. Gilbert and Pogue. Gov I'uh
Coal Saving. Note
Coal. Stored, Effects of Moisture on Spontaneous Heating of. Katz
mil Foster. Gov. Pub
Coal, Stored. The Diffusion of Oxygen through Katz Gov Pub
Coal Tar and Creosote in Longleaf Pine. Tests of Absorption and
Penetration of Teesdale and McLean. Go\ Pub
Coal-Tar Industry, Methods of Analysis I -t .1 in Ih. I M Weiss
I— Crude Tars. 732; II— Distilled Tars and ruches. .hi:. Ill -Heavy
and Middle Oils. 911; IV— Benzols and 1 1 hi Oil
Coal-Tar Industry, Some Applications of Pliv .1 al l liemistrv in. W.
J. Huff ...........
Coal Tar. Oils from. Note
Coal-Tar Products for 1917 Note
Coal: The Santo Tomas Cannel Coal, Webb 1 " Texas Ashley
Gov Pub
Piling, Bituminous in Large House Heating Boilers I
Gov Pub
Coals, Weights of Various
Cobalt \r. Wave Lengths
and KieSS '.'.•. i'nii
tod Liver Oil, Newfoundland Note...
Coke. Determination of Moisture in
t old Shock, the Influence of, in the SI
I, I> Bushnell
. Construction
.590
236
418
172
646
946
937
649
861
569
942
1022
144
s74
313
,46
956
431
948
1030
586
938
412
245
nut,
1021
582
nil Selvig. Gov.
nli/iii. .11 ol Canned Foods.
Pub
1.1. Wax from Note
Color Blim Go Pub
1 oloi 1 1' if Oil Varnishes, Note 1
aphj • 1 ,11 ,,1
RBI . ■ 1917), HI,.
II,:, I
mi 764; July, H74, Auj list,
Hirniin
■in-lit I Iraintilt Durability
1 of Third Vet
1 Road
I ,i,l,i:.- , 1. 11 - ; ;
Mil
Reinforced Goldbeck and
al < ommitti ■ ' -'•■ Pub
' Through 1
to. I-: D Verj
» ontrolli 1 ii-
1111, 11 . Go I 'hi
Pub
• oppet
1, h, 41 1
-., pti ml
Mi. 1
Pub
P1.1,
1,1,1
!■
649
B79
412
Copper and Aluminum in Germany. Note
Copper Area. A New. Note
Copper Carbonate Ores, Zinc Carbonate and Related, at Oph
Utah. Loughlin. Gov. Pub
Copper in Eastern States in 1917. Gov Pub
Copper in Idaho and Washington in 1916 Gerry. Gov. Pub
Copper in the Central States. Dunlop and Butler. Gov. Pub
1916
In
Copper in 1916. Butler. Gov. Pub
Copper Production (1916). Gov Pub : Alaska, by Brooks, 246;
New Mexico, Texas, South Dakota, and Wyoming, by Henderson,
246; California and Oregon, by Yale. 246; Arizona and Montana,
by Heikes, 246; Eastern States, bv Hill, 240; Colorado, by Hender-
son, 409; Utah and Nevada, by Heikes
Copper Products, Brass and Bronze. Gov. Pub.
Copper: Swedish Industrial Developments. Note
Copper: Zinc Carbonate and Related Copper Carbonate Ores at
■ Ophir. Utah. Loughlin. Gov. Pub:
Corn and Sorghums, Comparative Transpiration of. Miller and
Coffman, Gov. Pub
Corn and Wheat Products, Phosphorus as an Indicator of the Vitamine
Content of. Voegtlin and Myers. Gov. Pub
Corn and Wheat, The Growth-Promoting Properties of Foods Derived
from Voegtlin and Myers. Gov. Pub
Corn Cobs. Preparation of Several Useful Substances from. F. B.
LaForge and C. R. Hudson
Corn Silage. Velvet-Bean Meal, and Alfalfa Hay when Fed Singly and
111 Combinations, Digestibility of. Swing and Smith. Gov. Pub. .
Corrosion, Tar-Still, by Chlorine. Note
Cotton Linters, Batting, and Waste, Foreign Markets for. Gov. Pub.
Cotton Oil Industry in the War. D. Wesson
Cotton Plant, Chemistry of the. Vierhoever, el al. Gov. Pub
Cotton-Sampling Machine. Note
Cotton Standards for Grade, Manufacturing Tests of the Official.
Dean and Taylor. Gov. Pub
Cottonseed: Gossypol, the Toxic Substance in Cottonseed. Withers
and Carruth. Gov. Pub
Cottonseed Meal for Feeding Beef Cattle. Ward. Gov. Pub
Cottonseed Meal, Uniform Nitrogen Determination in. J. S. Mc-
Hargue
Cottrell Precipitator: Electric Furnace Smelting of Phosphate Rock
and Use of the Cottrell Precipitator in Collecting the Volatilized
Phosphoric Acid. J. N. Carothers
Coumarin in Factitious Vanilla Extracts, The Detection and De-
termination of. H. J. Wichmann
1 nun. il of National Defense. Gov. Pub 586,
Cranes and Transporters Note
Creosote and Coal Tar in Longleaf Pine. Tests of Absorption and
Penetration of. Teesdale and McLean Gov Pub
Cresol or Phenol Preservative in Serums. A Colorimetric Method for
the Estimation of. Elvove. Gov. Pub
The Three. The Estimation of Phenol in the Presence of. G.
W Knight, C. T Lincoln, G. Formanck and H. L. Follett.t); Cor-
rection
Creosote, Relative Resistance of Various Hardwoods to Injection with.
Teesdale and Mac-Lean Gov, Pub
Cryolite and Fluorspar in 1916 Huriliard Gov. Pub
Cucumber, Wild. Echinocystii Oregana, Seeds of. M. R. Daughters..
Current Industrial NBWs A McMillan;
.73, ISO, 228, 312, 394, 1x7. 572, 648, 744.
Cyanamide. Pure. Note
Cyanide. Sodium. Notes 011 W. J. Sharwood
Cycle Components, Tubular. Note
764
759
764
5 74
764
930
764
5 74
535
1037
861
959
245
DAMASCENE Steel Note
Decanting H. Tilliscb
DEDICATION in 1,11 mix HalX,, Universjtv of California
Introductory Address E ' ' \11ll
1. J. M Stillmun. VI', I. II Duschak
DeRoode Method for the Determination of Potash in Fertilizer Ma-
terials, A Study of the T E. Keitt and H. I-:. Shiver
Developing Agents, Organic, Examination of. 11. T. Clark
I InSUn I • !■■ ' - ti etWI a Gl IBS anil Rubber Tub-
ing C. C. fCiplinger
Diamonds, South African Note
liicvanin. Application of, to Photography of Stellai S]
lOI Pub
1, , . Pulmonary, among Miners in foplin District
Siliceous Dust ill Relation to lllggllls ,1 al GOV. I'nb
1 1,, , i in ,,1, Bla 11 I'" in- 1 "Him! Note
,11111 Tesiing Machine, New 1 Stimson and Neil]
Gov.
Pub
586
763
04')
ml, . I , I -.1 Pub
Disinfectants South Mucin Requirements Note
Disinfectants Theii I 1 Application in Prevention of O. minimi
- 1. 1 lintii ; ret ■■•■ bj '-I- Coy, 1
1
1 .,,,11 1 in mi ,1 .1.1.1 il" ii i u hite diurnal: '.
Illation of il.--- 11,
and C D vi righl
lant Cri ' •'•■ |,,m '<"
I ' SARCH ' ' ■ I ItO
. 1 ,,, , : , -,,,:, 1 1 Vbel 969
i- '-i - ' mhart, 971 ;
F [< Blared, 973 D w i..v tie, V< idli in 976
.573
1
Dye and 1 . . . /4.5
15.'
1 , Jones Midi
1
C lli-bilell
I
man
I., Mil
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. to, No. »
Dyestuff Industry, Organization within the. Editorial 256
Dyestuff Manufacture. British Progress in J Falconer 145
DyestufT Manufacturers' Association, American. Note 402
Dyestuff, Request for Definition of Term. A Record of Achievement.
Editorial 879
Dyestuff Situation in Textile Industries. Gov. Pub. ....... 504
Dyestufls Association. Note 324
Dyestupps, Symposium on Chp.mistry op (Cleveland Meeting,
Announcement. R. N. Shreve, 750; Introductory Remarks K II
Shreve 789
America's Progress in DycslufTs Manufacturing. L. J. Matos. . . . 790
The Development of the Dyestuff Industry since 1914. J F
Schoellkopf Jr 792
Application of Dyestuffs in Cotton Dyeing. J. M. Matthews . . . 794
Natural Dyestuff — Au Important Factor in the Dyestuff Situation.
E. S. Chapin 795
The Manufacture, Use, and Newer Developments of the Natural
Dyestuffs. C. R. Delaney 798
Photographic Sensitizing Dyes: Their Synthesis and Absorption
Spectra. L. E. Wise and E. Q. Adams 801
The Color Laboratory of the Bureau of Chemistry. H D. Gibbs. . 802
Problems in Testing Dyes and Intermediates. E. W. Pierce 803
On the Quantitative Analysis of Dyestuffs. A. H. Halland 804
Dyestuffs: The Modern Miracle. Editorial 508
EARTH: Its Figure, Dimensions, and Constitution of Its Interior.
Chamberlin, el al. Gov. Pub *. 245
Ecuador, Peru, and Bolivia, Textile Markets in. Tucker. Gov
Pub 664
Edgewood Arsenal Laboratory. Library for. W. L. Evans 868
Editorials: 2, 9.1, 172, 254, 336, 418, 508, 590, 672, 876, 966. (See
Herty, C. H., in Author's Index for Complete List of Titles;
Actual Subjects treated are to be found in place in this index.)
Eggs, Determination of Loosely Bound Nitrogen as Ammonia in.
N. Hendrickson and G. C. Swan 614
Kkenberg Peat Process. Note 312
Electric Arc Welding. Note 152
Electric Heater for Use in Analytical Distillation of Gasoline. E- W.
Dean 823
Electric Lamp Industry in France. Note 1021
Electrical Appliances, Shortage of. Note 396
Electrical Conductivity Recorder for Salinity Measurements. I-;.
E. Weibel and A. L. Thuras 626
Electrical Energy from the Volterra "Sofnoni." Note 487
Electrical Heating Apparatus, Automatic Controller for. Note 229
Electrical Machinery. Note 746
Electricity in Silk Industry. Note 862
Electrochemical Industries, Swiss. Note 398
Electrodes. Manufacture of. Note. 151
Electrolytic Process. Note 746
Electrometric -Titration, The Determination of Manganese in Steel
in the Presence of Chromium and Vanadium by. G. I.. Kelley,
M. G. Spencer, C. B. Illingworth and T. Gray. 19
Electrons in Cadmium Vapor, Resonance and Ionization Potentials for.
Tate and Foote. Gov. Pub 762
Electro-Steel Works in Germany. Note 75
Electro-Technical Industry in Japln. Note 228
Elliott. Arthur Henry. Obituaty. C. F. Chandler 498
Emetine Hydrochloride, On the Toxicity of. Special Reference to
the Comparative Toxicity of Various Market Preparations. Lake.
Gov. Pub 1037
Engineering, Chemical, in our Universities and Colleges Immediately
Prior to the Declaration of War, The Status of. H. F. Zoller 644
Engines, Detachable, for Ships. Note 314
Engines, Gas and Petrol. Note 940
Engines, Various Classes of. Note 573
England, Women in the Chemical Industries of. Note 1028
English Pottery Industry. Note 395
Enzymes of Milk and Butter. Thatcher and Dahlberg. Gov. Pub. 503
Equilibria in Solutions Containing Mixtures of Salts. I — The System
Water and the Sulfates and Chlorides of Sodium and Potassium.
W. C. Blasdale 344
Equivalents, Table of, Millimeters to Inches. Gov. Pub 413
Ether, Effect of. on Tetanus Spoies and on Certain Other Micro-
organisms. Corbitt, Gov. Pub 873
Ether Extract of Silage. Variation in. L. D. Haigh 127
Evaporator for Acid Liquids. E Hart 555
Evaporators, Multiple, for Sugar Factories. Theory and Practice in the
Design of A 1. Webre 191
I'm. Inn,, 11. Present Problem of Caullery. Gov. Pub 245
Experiment Station at American University, Transfer of, to the War
Department. W. Wilson, N. D. Baker.' Note, 654; Set Editorial 590
Explosive Chemicals. Note 745
Explosive, New Mining. Note 747
Explosive. Safety of TNT as an. J.M.Weiss. Note 1028
Explosives, Gov. Pub 409
Explosives and Chemical Divisions, War Industries Board. Note.. 654
Explosives and Their Ingredients, Licenses Required for. J. R. Hcaly.
Note. 2.<7, Ste Editorial, Important Notice 256
Explosives. High, Initial Priming Substances for. Taylor and Cope.
Gov. P.,b H . 958
Explosives Manufacture, School of, Ordnance Department, Columbia
University. Note 868
Explosives: Method of Calculating Comparative Strength and
Kfiiciciicv of High Explosives from Their Composition and Apparent
Densities C . E, Waller 448
Explosives. Modern. Note 650
Explosives. Use nl Permissibh . in i oal Minis of Illinois. Fleming
and Kostcr. Cm- Pub 958
Exposition up Chemical Industries, Fourth National:
New York City, September 23 to 28 1918. Editorials 592, 672,674;
Notes. 651, 826; Program an. I Lists of Exhibitors 749
Addresses: Permanent Chemical Independence C. H. Herty.. 826
The Exposition in War and in Peace P. J. 'lone 828
The Importance of Practical Chemistry O. W. Thompson 829
Symposiums micals
Development in Nitric Acid Manufacture in the 1'. S since 1914
B. J. Pranke 830
Recovery of Potash from Kelp C, A Higgins 832
Recovery of Potash from iiun Blasl Furnaces and Cement Kilns
by Electrical Precipitation. I.. Bradley 8.34
Potash from Desert Lakes and Alunitc. J. W. Hornsey 838
Potash from Searles Lake A. de Ropp, jr '..'.'. 839
Recent Developments in Ceramics. A. V. Bleininger. . . 844
Carborundum Refractories. S. C. Linbarger. . .' 847
Mclal Industries
The Pyrophoric Alloy Industry. A. Hirsch. 840
The Ferro-Alloys. J W. Richards .'..'.'.'.'.'.'.'.'. 851
Industrial Organic Chemistry
Advances in Industrial Organic Chemistry since the Beginning
of the War S P. Sadtler ... 8S4
Solvents from Kelp. C. A. Higgins 858
Wood Waste as a Source of Ethyl Alcohol. C. H. Tomlinson . . . . 859
Extracts, Non-Alcoliolic Flavoring, The Determination of Essential
Oils in. F. M. lioyles 537
FABRICS, Balloon, Determination of Permeability of Edwards
Gov. Pub ' 70J
Fabrics for Aeronautic Construction. Whalen. Gov. Pub 873
Fabrics, Water-Proof and Dust-Proof. Note 7s
Fat in Condensed Milk and Milk Powders, A Study of the Estimation
of. C. H Biesterfeld and O. L. Evenson Correction 15V
Fatigue Products, The Present Status of Our Knowledge of Scott
Gov. Pub 580
Fats and Oils, Commercial, Tentative Standard Methods for the
Sampling and Analysis of. W. D. Richardson 315
Fats and Oils in Germany. Note 94 j
Fats and Oils. Saponification of. Note 75
Fats. Edible, In War and Law. Address. D. Wesson
Fats, Foreign in Butter Fat, A Method for the Detection of. A.
Seidenberg 61 r
Fats, Saving, from Garbage. F. C. Bamman. Notes 320
Federal Trade Commission. Gov. Pub
Feed Residues: Study of the Physical Changes in Feed Residues
which Take Place in Cattle During Digestion. Ewing and Wright
Gov. Pub .' 7M
Feeds: Mineral Content of Southern Poultry Feeds and Mineral
Requirements of Growing Fowls. Kaupp. Gov. Pub 95^
Feldspar in 1917. Katz Gov. Pub 956
Fellowship, Du Pont 58 1
Fellowship, Research, State College of Washington. Note 753
Fellowship System, Industrial, The Growth of. Mellon Institute.
Note 401
Ferro-Concrete Shipbuilding. Note 395
Ferromanganese Manufacture in Spain. Note 1021
Ferrosilicons. Acid-Resisting. Note 939
Fertilizer: Decomposition of Green and Stable Manures in Soil.
Potter and Snyder. Gov. Pub 504
Fertilizer Industry, Licensing of, Ordered. President Wilson. Proc-
lamation 325
Fertilizer Materials, A Study of the DeRoode Method for the De-
termination of Potash in. T. E. Keitt and H. E. Shiver 219
Fertilizer Materials from Minor Sources, Conservation of. Fletcher.
Gov Pub 76"»
Fertilizer: Phosphate Rock, Our Greatest Fertilizer Asset. Wagga-
man. Gov. Pub 763
Fertilizer: Reverted Phosphate. C. C. James 33
Fertilizer Situation in the United States. Interpretation of. Mineral
Industries of the United States. Pogue. Gov Pub 84
Fertilizer: The Agricultural Availability of Raw Ground Phosphate
Rock. W. H. Waggaman and C. R Wagner 442
Fertilizers: Commercial Bordeaux Mixtures: How to Calculate
their Values. Wallace and Evans. Gov. Pub 959
Fertilizers: Commercial Stocks of Fertilizers and Fertilizer Ma-
terials in U. S. as Reported for October 1, 1917. Gov. Pub 763
Fertilizers: Comparison of Percentages of Nitrogen in Tops and Roots
of Head Lettuce Plants. H. A. Noyes 621
Fertilizers, Effect of, on Hydrogen-Ion Concentration in Soils. F.
W. Morse
Fertilizers from Industrial Wastes. Ross. Gov. Pub 763
Fertilizers. Sources of our Nitrogenous. Brown. Gov. Pub 763
Fertilizers: The Fertilizing Value of Activated Sludge. G. G.
Nasmith and G. P. McKay. 339; See Rudnick 400
Fibers, "Hard" Rope, Distinguishing Manila from all other. C. E.
Swett 227
Filter. Ultra-. Note 74"
Filtering Tube. Simple and Efficient. W. M Thornton. Jr 132
Fire-CIay Bodies. Effect of Size of Grog in. Kirkpatrick. Gov. Pub.
Fish, Commercial Freezing and Storing of. Clark and Almy. Gov.
Pub 7o3
Fish, Experiments on Digestibility of. Holmes. Gov. Pub 763
Fish Oil, Utilization of Note 487
Flours: Hydration Capacity of Gluten from "Strong" and "Weak"
Flours. Gortner and Doherty. Gov. Pub 764
Fluorspar and Cryolite in 1916. Burchard. Gov. Pub 24<-
Fluxes. Note 151
Food: Chemical Tests for Detection oftRancidity. R.H.Kerr 4"
Food Chemistry in the Service of Human Nutrition. Address. H.
C. Sherman 383
Food Conservation, A Problem in. The Deterioration of Raw Cane
Sugar. C. A. Browne 178
Food: Determination of Loosely Bound Nitrogen as Ammonia in
Eggs. N. Hendricksou and G C. Swan 614
Food Determination of the Hexabromide and Iodine Numbers of
Salmon ( iil as a Means of Identifying the Species of Canned Salmon.
II S Bailey and I M. lolmson °99
Food: Effect of Different Oxygen Pressures on Carbohydrate Metab-
olism of Sweet Potato. Hasselbring. Gov. Pub 959
Food: Enzymes of Milk and Butter. Thatcher and Dahlberg.
Gov. Pub 501
Food Influence of Age of Cow on Composition and Properties of
Milk and Milk Fat Ecklcs and Palmer. Gov. Pub 503
Food In War Time. Note 325
Food: Method (or the Detection of Foreign Fats in Butler Fat. A.
Seidenberg
Food: Occurrence of Carotin in Oils and Vegetables. A H .Gill ... 612
Food Products. Detection of Vegetable Gums in. A. A Cook and
A. G. Woodman 530
Food Products. Sulfured. Arsenic in. W. D. Collins 360
Food: Studv of the Streptococci Concerned in Cheese Ripening.
Evans. Gov. Pub 763
Foods, Canned. The Influence of Cold Shock in Sterilisation of.
L. D. Bushnell ... •>■'-'
Dec, iqi^
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Foods Derived from Corn and Wheat, The Growth-Promoting Proper-
ties of. Voegtlin and Meyers. Gov. Pub 75g
Foods. The Bureau of Markets in Its Relation to the Conservation'©!
C. J. Brand .' 66
Formaldehyde, Disinfection with. A Substitute for the Permanganate-
Formalin Method. C. C. Storm 123
Formulas, Conversion of. W. H. Cole 55s
France, A Chemists' Club for. Editorial
France, A Letter from. W. A. Hamor 495
France, Electric Lamp Industry in. Note 1021
France, Machinery for. Note 394
Frasch, Herman, Unveiling of Portrait of 326
Freezing-Point Method as an Index of Variations in the Soil Solution
Due to Season and Crop Growth. Hoagland. Gov. Pub 504
French Chemical Industries during 1916. F. J. LeMaistre 4>1
French Industries, The Great Effort of the. M. Knecht 423
French Orphans. A Golden Opportunity Editorial 967
Fruits: Some Constituents of the American Grapefruit (Citrus
decumana). H. F. Zoller 364
Fruits: The Composition of Loganberry Juice and Pulp. M. K
Daughters. Correction 159
Fruits: The Loganberry and the Acid Content of its Juice. M. R.
Daughters Mt
Fuel. Gov. Pub 409
Fuel Briquetting in 1917. Lesher 662
Fuel for Manufacture of Chemicals. E. Smith. Note 159
Fuel in the U. S. Gov. Pub 408
Fungi, Wood-Rotting, Pure Culture of, on Artificial Media. Long
and Harsch. Gov. Pub 504
Furnace, A Rocking Electric Brass. H. W. Gillett and A. E. Rhoads. 459
Furnace, Blast. Practice. Note 746
Furnace, Electric Zinc. Note 487
Furnaces, Design of, and Combustion of Coal. Kreisinger, et al. Gov.
Pub 412
"GARABED," The Demise of the. Editorial 590
Garbage Collection and Garbage Grease Recovery in American
Cities, Statistics of. R. Pearl 027
Garbage Disposal Industry, American, and Its Chemical Relation
R. Wells 567
Garbage, Saving Fats from. F. C. Bamman Notes 320
Garbage, Utilization, Municipal Contribution to Conservation
through. E. D. Very 563
Gas. Gov. Pub 409
Gas Analysis, Reagents for Use in:
VI — The Absorption of Hydrogen by Sodium Oleate. R. P.
Anderson and M. H. Katz 23
VII — The Determination of Benzene Vapor. R. P. Anderson.... 25
Gas Analysis, Use of the Interferometer in. Siebert and Harpster.
Gov. Pub 959
Gas and Oil Possibilities of the Hatchetigbee Anticline, Alabama.
Hopkins. Gov. Pub 247
Gas and Petrol Engines: Note 940
Gas Condensate, Natural, Formation of Aromatic Hydrocarbons
from. J. G. Davidson 901
Gas Exhausters, Water Lubrication of. Note 488
Gas-Fired Brazing Table. Note 1022
Gas: Geologic Structure in the Crushing Oil and Gas Field, Okla-
homa, and Its Relation to the Oil, Gas, and Water. Beal. Gov.
Pub 331
Gas in Glass Industry. Note 940
Gas Interferometer Calibration. Edwards. Gov. Pub 413
Gas-Mantle Lighting Conditions in Ten Large Cities in the U. S.
McBride and Reinicker. Gov. Pub 8*
Gas, Natural, and Its Constituents, Compressibility of, with Analyses
of Natural Gas from 31 Cities in the U. S. Burrell and Robertson.
Gov. Pub 332
Gas, Natural, in 1916. Northrop. Gov. Pub 662
Gas, Natural, Testing for Gasoline. G. G Oberfell 21 1
Gas: Recovery of Gasoline from Natural Gas by Compression and
Refrigeration. Dykema. Gov. Pub 958
Gas: Report of the Bureau of Standards on the Recovery of Light
Oils and Refining of Toluol s 1
Gas: Toluol by Cracking Solvent Naphtha in the Presence of Blue
Gas. G. Egloff 8
Gas: Toluol Recovery and Standards for Gas Quality. R. S.
McBride Ill
Gas Warfare. Methods of. Address. S. J M. Auld 297
Gas Warfare: Typical German Pronouncements Editorial 420c
Gases, A New Method for the Quantitative Hstimation of Vapors in.
H. S. Davis and M. D. Davis 7"''
Cases: Application of the Differential Pressure Method to the
Estimation of the Benzene and the Total Light Oil Content of
Gases. H. S Davis. M D. Davis, and D G. MacGregor 712
Gases, Measuring the Temperature of, in Boiler Settings. Kreisinger
and Barkley. Gov. Pub 959
Gases: Physiological Effect of Different Gases on Man. Burrell.
Cov. Pub 95'<
Gases. Studies on the Absorption of Light Oils from. II, S. Davis
and M. D. Davis "I*
Gasoline. Gov. Pub 409
Gasoline. A Convenient Electric Heater for Use in Analytical Dis-
tillation of. E W Dean ••••■ 823
Gasoline, Determination of Unsaturated II vlrocarbons in. Dean
and Hill. Gov. Pub 4I-'
Gasoline Engines in Mines, Suggestions foi the Safe operation of.
Kmllieh and Higgins Gov. Pub.. 41-
Gasoline from Natural Gas by Compression and Refrigeration, Re-
covery of. Dykema. Gov Pub »5g
Gasoline, Testing Natural Gas for. G G 01 H Z'i
Gauges, Swedish Note J?J
mn. Gov Pub , ■•■• •■•. *[i7
Gelatin and Glue. Jelly Value of. A V. "I I, Dullois 707
Gelatin. Australian. Note ■••„• "'
Gelatin, The Reticulation of. S. E. Sheppard and P A Elliott .... . 727
Gems and Precious Stones. Shallcr. Go* Pub. In 1911. 955; in
1917 °57
Generator: Electric Heat Storage In Boilers Note 151
Generator, Hydrogen Sulfide. L. Sattlei . ■• <2'l
Generator. Hydrogen Sulfide. A New Port ible W. P. Munn. .. 130
Geologic Structure of Northwestern Part of Pawhuska Quadrangle,
Oklahoma Hcald. Gov Pub 40?
• Tological Survey; Director's Annual Report . . . . . • . ■ • 24/
Gov. Pub... 81. 165, 246,331,409.586,662, 759.873, 954
Geology and Oil Prospects of the Salinas Yalley-Parkfield Area
California. English. Gov. Pub 874
Geology, North American, Bibliography of, for 1916, with Subject
Index. Nickles. Gov Pub 33 !
Geology: Structure of Parts of the Central Great Plains, barton
Gov. Pub 586
German Enterprise in the Ukraine. Note 1021
German Potash and the War. Note 655
German Union of Technical and Scientific Societies 575
Germany, Alcohol Production in. Note 650
Germany, Catalytic Processes in. Note 939
Germany, Copper and Aluminum in. Note 649
Germany. Electro-Steel Works in. Note 75
Germany, Fats and Oils in. Note 942
Germany. New After-War Preparations in Chemical Industry of.
Translated from the French 1 025
Germany. New Sources of Oil Supply in. Note 747
Germany, Tanning Material in. Note 1022
Germany's Commercial Methods. Note 228
Gibbs Medal Award:
Editor's Note, 483; Introductory Address. L. M. Tolman 483
Chemistry in the Petroleum Industry. Medal Address. W. M.
Burton 484
Gilman Hall: The Research Unit of the Chemistry Group at the
University of California. M. Randall 634
Gilman Hall, University op California, Dedication op 391
Glass and Quartz, Compression Strength of. Note 942
Glass and Rubber Tubing, A Device to Insure Tight Connections
Between. C. C. Kiplinger 63 1
Glass. Demands for. Note 650
Glass Industry. Gas in. Note 940
Glassware. Chemical, Comparative Tests. Walker and Smither.
Gov. Pub 762
Glue and Gelatin, Jelly Value of. A. W. Clark and L. DuBois 707
Glue, Australian 487
Glues, Determining the Comparative Melting Points of, as a Measure
of the Jelly Strength. C. F. Sammet 595
Glues: Non-inflammable Plastic Material. Note 74
Gluten from "Strong" and "Weak" Flours, Hydration Capacity of
Gortner and Doherty. Gov. Pub 764
Glycerin and Soap Manufacture in India. Note 744
Glycerin as Used in Medicines, Conservation of. Note 495
Glycerin, Japanese. Note 75
Gold and Silver in 1916. McCaskey and Dunlop. Gov. Pub 956
Gold Coast. Exports from. Note 394
Gold in Eastern States in 1917. Hill. Gov. Pub 956
Gold in Idaho and Washington in 1916. Gerry. Gov. Pub 586
Gold Placers and Lode Deposits near'the Nenana Coal Field. Alaska.
Overbeck and Maddren. Gov. Pub 331
Gold Placers of the Anvik-Andreafski Region. Alaska. Harrington.
Gov Pub 331
Gold Placers of the Tolovana District, Alaska. Mertie Gov. Pub.. 331
Gold Production (1916). Gov. Pub. Alaska, by Brooks, 246. New
Mexico, Texas, South Dakota, and Wyoming, by Henderson, 246.
California and Oregon, by Yale, 246. Arizona and Montana, by
Heikes, 246. Eastern States, bv Hill, 246. Colorado, bv Hender-
son. 409. Utah and Nevada, by Heikes 409
Goods in Demand in Australia. Note 861
Gossypol, the Toxic Substance in Cottonseed. Withers and Carruth.
Gov. Pub 504
Government Publications. R. S. McBride:
84. 165, 245, 331, 408, 503. 586, 662. 758, 873. 954, 1037
Grain Relation of the Density of Cell Sap to Winter Hardiness in
Small Grains Salmon and Fleming. Gov. Pub 764
Grapefruit. American {Citrus decumana). Some Constituents of. H.
F. Zoller 364
Graphite for Boiler Scale Note 395
Graphite in 1917. Ferguson Gov. Pub 957
Gravel and Sand in IV K. Stone Gov. Pub 247
Gravel Deposits of the Caddo Gap and DeQueen Quadrangles. Arkan-
sas Miser and Purdue. Gov. Pub 954
Gravel. Flaxville, and its Relation to Other Terrace Gravels of the
Northern Great Plains. Collier and Thom. Gov. Pub 409
Grease Recovery. Note 650
Great Britain. Mineral Output of. Note 573
Great Britain. Preparation for Post- War Conditions in. Note 399
Greensand, Recovery of Potash from. H. W. Charlton 6
Grog in Fire-Clay Bodies, Effect of Size of Kirkpatrick. Gov. Pub 762
Guaiacol Sulfonate, Potassium, The Identification and Determination
Of. S. I'alkin h'0
Gums. Vegetable. The Detection of. in Food Products. A. A. Cook
and A. G. Woodman 530
Gun, Long-Range. Note 574
Guttapercha from the Shea Mutter Tree. Note 76
Gypsum Deposit in a Boiler Note ......... 488
Gvpsuni. Influence of, Upon Solubility '■! Potash in Soils. Mc.Miller.
Gov Pub 959
Gypsum in 1916. Stom Gov Pub "■
Gypsum Products: Their Preparation and Uses. Stone. Gov . Pu
HALL. C. M.. Portrait of, for Chemists' Club Note 947
Hardwood Thl ' 1 h. Yield of Products in the
Destruen 1 and H. Cloukey 262
Hardwoods Relativi Ri listai Various, to Injection with Creo-
solc T, Pub ....... 763
thl S leld of Products in the
Di ti Di [illation ol B I Palmei
olutions, Its
Re] ,tio "f Soils., and
Method [01 the Determination of Lime
n 1 ij
..,.,, itloni 1..1 it. bl I Ml 1 uh 1
. .' 151
Mitigation ..1 the Watkins. Gov. Pub 245
Hematite" nn- .,
centration Experiments with Singcwald Go« Pub '»
Hexamethyleneteti ,s,",',l.i,'\'" Syn' *n,
thetii Di ""' ' " Un>;'" S2S
Pub Ir?
1 -kins from Veni ■ "r
\ Modlfical I \" Improved Method IOI D
tennlnii ' •"•' " s ","""
1052
THE JOl l<\ 1/. Oh INDUSTRIAL AND ENGINEERING I HEMISTRY Vol
10. \o.
Holland. Margarine Industry in Note
Household, Materials for. Gov Pub
Household, Safety for, <'.<■ Pub
Humus in Mulched Basins, Relations ol Hu or
Production, and Effect of Mu tion fen sen
Gov. Pub.
Hydraulic Conversion Tables and Equivalents. Gov. Pub
Hydrocarbons, Aromatic, from Natural Gas Condensate fhi Porma
tion of i g i )avidson
Hydrocarbons, Desulfuration of. Note
Hydrocarbons in Gasoline, I asaturatcd, Determination ol
and Hill Gov. Pub
Hydros-.. mi< \ i i< i i ! I Fumi Ong ■ o - Pub
Hydrogen, Absorption of, by Sodium Oleate \I R
in Gas Analysis, R P. Anderson and M II Katz
Hydrogen Electrode, Relation ol I ■ ion Dioxide to toil Reacl
M'. i lured by the Hoagland ind 5h irp Gov Pub
Hydrogen Slectrod Si udies in Soil Ri ction [ndicated by the
Plum,,,, i i kn P il
Hydrogen in Coal and the Change in Weight of Coal on Drying,
Effect of Low Temperature Oxidation on. ECatz and Portei
Gov. Pub
Hydrogen-Ion Concentration in Soils, Effect of Fertilizers on. F W.
Morse
Hydro [en ! ulfid n rator. I. Sattlet
Hydrogen Sulfide Generator, A New Portable W F Munn
Hydrogen Sulfide Stopcock \n Automatii C II. Classen ..
Hydrosulfites Note
IGNEOUS Rocks i hemica) Lna] ton Gov Pub .
Illuminator, New, (or Microscopes A. Silverman
Incombustible Matl I oal and Rock-I.)ust Mixtures in Mines.
Quick Determination of. Fieldner, et al. Gov. Pub
India, Indigo Crop of. Note .
[ndia, Oil-Pressing Plant for. Note ......
India, Soap and Glycerin Manufacture En. Note
Indian <',:., I , ,i ,
Indian Resin Note. .......
Indigo Crop of India. Note
Indigo Industry, Natural. Note
Industrial Developments in Japan Note
Industrial 1 developments, South African Note
Industrial Efficiency. Lee, Gov Pub
Industrial Efficiency, Research as an Aid to
Industrial Notes:
82, 162, 243, 329, 406 !,"95l,
Industries. Chemical and Allied. Gov Pub
Industries, Clay Working, and Building ' operations in the Larger
Cities in 1916. Middleton. Gov. Pub
Industries, Prench, Great Effort of. M Knechl
Industries, New Norwegian. Note
Industries, New South African Note
Industry and Research, Organic Reagents for. C E. K
Notes 656, 1
Industry and Science, The Collaboration of. Translation of liddn
by V. Grignard
Industry, Chemical, in China, Note
Industry, Chemical, in the Netherlands Note
Industry. Cotton Oil, in the War. D Wesson
Industry. Electric Lamp, in France. Note
Industry, Planning a Research Laboratory for an. C. K K Mees.
Inseri ICggs. Toxicity of Volatile Organic Compounds to Moore and
Graham. Gov. Pub
Insecticides A Contribution to the Composition of Linn
Solutions, O. B, Winter
Insecticides, Contact, Physical Properties Governing the Effica
Moon and Graham Gov. Pub
Insecticides. Determination of Arsenic in, bj Potassium lodate G
Insignia, c_ hemistry. Editorial
Instill i, Collar, for Chemical Warfare Service Note
Instrument Optical The Properties and Testing of Gov. Pub
Insulating Material. Note
Insulation on Steam Drums, Effect of. Note
Interferoi i G I alibration. Edwards Gov Pub
terferometer in Gas Analysis, i se ol the. Siebert and Hat
958
488
197
744
39 7
_■ JO
24S
493
123
93Q
943
930
1021
476
r,(
Pub
'"■'Mi " tlirl
Invention Problems Note
Iota Sig 'i I ....
I .ue luiee, The Role of.
F. W. Zerban
Iron and
Iron and Steel Industry Duriti riod, Trend of '■
Frequi m % Rates in Chaney. Go* Pub
Iron ind Stee! fndu il i j in fapan Note
el. Sulfur in, A Standard i Determination of
od H B Pulsifi -
• i trade in Vden, Note
ths in Red and Infi i Red Spectra of. Meggers
959
314
413
959
245
1023
Note
i and Ste
■
I
and k,
Iron, I >el ei tninal ion ol i •
i . , Norwi ian Note
i. hard Go> Pub
i on i ii i Note
i> Pub
Iron, P Burchard. Gov. Pub
1
On Studies on Capacities ol
New Method for Determining Volume Weight, fsi
l ,. p
Isothe
Italian ' •
J \ p \ \' Ele< trie Lamp Trade in Note
; ; i ■ ■ . adust! j in. Nol c
lip in I urn and Steel Indu
I .pan Peppermint Cultivation Note
[ap in, Raiiwaj * i i ite
lap, mi, Rubber [ndustrj in Note
I Lpan Vegel
japan. Zinc Refining in, Note
313
t! 1
■
i amphoi Not< 1022
Nitrate Enterprise. Note y^i
Glycerin Note
relopraents No
jelly Strength, Determining the I omparative M ■ Glues
as a Measure of the C F -ainniet 595
JeUy Value of Gelatin ind Glut \ W Clark an. 1 I. DuBou
ditorship An
appreciation and a Greeting. Editorial 95
Journals of the American Chemical Goldthwait
Xo,L- 1026
lute Produi tion in China Note g^|
Jul. Sacks for Argentina. Note
nel A Physical and Chemical Study of the. Bid well. Gov.
KAI-TR Ke
Pub .
Kelp, On the Preparation of an Active Dei rbon from P
W. Zerban and E ( Fteeland gi?
Khaki. Dyeing of, in the United States J C Hebdcn
Kjeldahl Digestion flasks A Simple and Entirely Adjustable Rack
for. F. H Rice ...... $3]
Kjeldahl-Gunning Method, The Use of Sodium Sulfate- in the
Dowell and W G Friedman, 599
Korea. Machinery for. Note ?30
,'/; LABORATORY AND PLANT
Laboratory Resea
Laboratory Specir
nient Hasselti
Laboratory Suppli
Laboratorv Ware.
Pub
38. 128. 222. 292, 374. 459, 545, '■-''■ 732, 817, 911.
ch, for an Industry C. E. K Mi 1
iens. Public Health Their Preparation and Ship-
«. Gov Pub
S. ( '.ov Pub
Porcelain, Comparati
Tests of Waters. Gov.
Lamp Industry. Electric, in France. Note
Lamp Test- Note...
Lampblack Manufacture. Note
Lamps: Approved Electric Lamps for Miners. Clark and
Gov Pub
Lamps Electric Lamp Trade in Japan. Note.
Lamps, Incandescent. Note
Lamp-, Incandescent Electric. Tungsten and Carbon. Standard
Specifications for. Gov. Pub
Lead in I 1 tern S1 ites in 1917. Hill Gov Pub
Lead in Idaho aria Washington in 1916, Gerry. Gov. Pub..
Lead in the Central States. Dunlop and Butler. Gov. Pub, In
1916 7
Lead Production (1916] Gov Pub : Alaska, by Brooks, 24o. \*ew
Mexico Texas, South Dakota, and Wyoming, by Henderson. 246.
C alifornia and Oregon, by Vale. 2-iu Arizona and Montana by
Heikes !46 Eastern Mates, by Hill. 246. Colorado, bv Hender-
son, 409. Utah and Nevada, by Heikes
Lead, Silver-, Antimonial, Veins of the Arabia District, N
Knopf Gov. Pub
Leather and Hide Situation. Gov. Pub
Leather. Imitation, for Switzerland. No1
Leather Industry. Gov. Pub
Leal Ih-t I 1 illation of Waste Boots. Note
I \ ml Aberrations of Tillyer and Shull
Lettuce Plants. Head. Comparison of Percentages of Nitrogen in Tops
and Roots of. H A Noj s
Levenstein Limited. Report of Progress
Library for Edgewood Arsenal Laboratory. W L. I-*vau<
Light, Atmospheric Scattering of Fowle Gov. Pub
Lighl ing Factory. Note
Lime Agricultural, Determination of Value of. S. D. Conner
Lime Cal Analysis, A Quick Method for. A. N. Clark
Lime in 1916. Loughlin. Gov Pub
Lime Reaction of Hawaiian Soils with Calcium Bicarbonate Solu-
tions, Its Relation to the Determination of I.nue Requires
Soils, and a Rapid Approximate Method for the Determination of
Lime Rcquin ■ M. O. Johnson
Lime. Valuation of. for Various Purposes R K
Limestone H. Iderl entral Pennsylvania. Reeside
Pub
Lime Sulfur Solutions, A Contribution to Composition of. 0. B.
Winter
Liming ol Soils, Principles of Shorey Gov Pub...
Linseed 1 Ml Influence Oil ol Geographical Source and
tj ol Fla* Rabak. Gov. Pub
Liquids Metallii Note
Lode Deposits and Gold Placers near the Ncnana Coal Field
:k and M iddren I to* Pub
Lod< Mining in the Fail Alaska Mertie. Gov, Pub.
1 ind the Acid Content of its Juice M. R Daught
rrj Juice and Pulp. The Composition of. M R Datlf
C01 rection
Vole
Lubricating 1 til, Note
lite, Dye from. Note
MACHINE, Cotton-Sampling Note
New Disinfectanl
and Neill. Gov
Machinery and Materials. Construction, in Colombia. Hv\ing. Go
Pul
Machinery for Prance. Note
Note
Machine) j For Venezuela Note
Machinerj in South America Note .
i . ' 1 Canadian l.aV
Magnesia Bricks, Refractor) Properties of Mote
Magnesite Gov Pub. In [916, Vale and Gale 247; in \->
tite and Chrome Ore, Trans* aal Deposit
Magnesites, Nol t
turn Alloy, New Not<
iura and Calcium, Influence ol Carbonates of. on Bacteria of
Certain Wisconsin Soils. Kulmer Gov Pub
Magnesium Chloride and Cement Mortars. Note
iium Oxide, On the Influence of the Temperature of Burning
Hydration of E DeM Campbell
Magnetic Separations and the Rarer Metals Note
Dec, 191S THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Note
Magneto Ignition. Note
Magneto Machines for Pocket Torche
Magnets. Chromium Steel for. Note.
Malay States. Mineral Deposits in. Note.
" ingsten in. Note
and Manganiferous fires in 1916. Hewett. Gov
at Butte, Montana. Pardee. Gov. Pub
Deposits in Madison County. Montana Par'de
Malaya. Tt
Manganese anci Mangamlerous < >res in 191ce Hewett. Gov. Pub.
Mangane
Manganese Deposits in Madison County, Montana. Pardee. Gov.
Pub 954
Manganese in Steel, The Determination of. in the Presence of Chro-
mium and Vanadium by Electrometric Titration. G. I. Kclley M
G. Spencer, C. B. IUingworth and T. Gray 19
Manganese Ore, Possibilities for, on Certain Undeveloped Tracts in
Shenandoah Valley, Virginia. Hewett. el al. Gov. Pub 409
Manila Rope. Distinguishing from all other "Hard" Rope Fibers ^
E. Swett . ^27
Manufactures. Census of, (19141; Petroleum Refining. Gov. Pub 412
Manufacturers and Universities. Cooperation Between. R. E Oesper
Note 1027
Manures, Decomposition of Green and Stable, in Soil. Potter and
Snyder. Gov. Pub 504
Manures. Green. Soil Acidity as Influenced by. White. Gov. Pub 765
Maple Sugar; Composition. Methods of Analysis, Effect of En-
vironment. Bryan, el al. Gov. Pub 503
Margarine Industry in Holland. Note 396
Market Report. .90, 170, 252. 334, 416, 506, 588, 670, 766, 876, 964, 1040
Massachusetts Institute ok Technology:
Four Hundred Thousand Dollar Gift to. Note 581
Readjustments to meet War Conditions. Note 238
Meal, Check. Contest. Note. 656
Medical and Surgical Supplies, Staple, List of. Gov. Pub 586
Medicinals; War Chemistry in the Alleviation of Suffering. Edi-
torial 673
Medicine. Preventive, The Debt of, to Chemistry. G W. Goler 303
Medicines and Compounds, Patent and Proprietary, and Druggists'
Preparations. Gov. Pub 958
Medicines. Conservation of Alcohol. Glycerin, and Sugar as Used
in. Note 495
Mellon Institute. Growth of Industrial Fellowship System Note 401
Melting Points, Comparative, of Glues as a Measure of the Telly
Strength. C. F. Sammet 595
Menhaden Industry of the Atlantic Coast Greer. Gov. Pub 166
Metal-Spray Process. Schoop. Notes 939, 1022
Metallurgical Works in the I". S. during the Calendar Year 1916,
Accidents at. Fay. Gov. Pub 412
Metals and Other Materials Made in Ordnance Laboratory at Water-
town Arsenal, Mass., Fiscal Year 1916. Report of Tests of. Gov.
Pub 245
Metals, Antifriction. Note 941
Metals. Platinum, from Canadian Nickel, Recovery of. Note 76
Metals. Rarer, Magnetic Separations and. Note 313
Meteorology and Aeronautics. Blair. Gov. Pub 873
Methane Accumulations from Interrupted Ventilation. Smith and
Hamon. Gov. Pub 959
Mica. Schaller Gov Pub. In 1916. 240; in 1917. 957
Microorganisms, The Use of, to Determine the Preservative Value of
Different Brands of Spices F. M. Bachmann 121
Microscopes, A New Illuminator for. A. Silverman 1013
Microscopic Qualitative Chemical Analysis, The Use of Textile Fibers
in. E. M. Chamot and II I Cole 48
Microscopy, Chemical. E. M. Chamot. Address 60
Milk: A Comparison of the Proximate and Mineral Analysis of
Desiccated Skim Milk with Normal Cows' Milk E. P. Harding
and H. Ringstrom 295
Milk, Added Water in, Research on the Determination of. H.
Durand and R. Stevenson 26
Milk and Butter. Enzymes „f Thatcher and Dahlberg. Gov. Pub 503
Milk and Milk Fat, Influence of Age of Cow on Composition and
Properties of. Eckles and Palmer. Gov Pub siii
Milk, Condensed, and Milk Powders, A Stuclv of the Estimation of Fat
in. C. H. Biesterfeld and O L. Evenson Correction 159
Milk Manufacture of Casein from Buttermilk or Skim Milk. Dahl-
berg. Gov Pub 763
Milk Ordinance, A Guide for Formulating Gov Pub 332
Milk Powder. Dried Gov Pub 758
Mine Fire. Some Results of Analysis of Airs from. A. G. Blakeley
and H II Geist 552
Mineral Content of Southern Poultry Feeds and Mineral Requirement
of Growing Fowls ECaupn Gov. Pub 959
Mineral Deposits in Malay States Not' 397
Mineral Industries of the I. S. Gov Pul I Pi iducU, An
Object Lesson in Resource Administration ' > Coal.
Resource and Its Full Utilization. Gilberl and Pogue, 409, Inter-
ition of Fertilizer Situation in the I S Pogue, 84, Sulfur.
impleof Industrial Independence . I'o [Ui 245
Mineral Output of Great Britain Noti 5?3
Mineral Production in Canada. Note 74
Mineral Production of Victoria Note 151
Mineral Resources: The Lake Clark-Central Kuskokwim Region,
Alaska, Smith. Go> Pub
Mineral Springs of Alaska Chemical Character of Some Surface
Watt r of Alaska, Waxi Pub
Mineral Waters in 1916. Ellis G,,s Pub
Minerals, Rare-Earth, and Zirconium in 1916 Schaller Gov. Pi
Miners Siliceous I in unong
Miners in loplin District Missouri Hi| in • oi < ,o% Pub
|
Approved Elei trii I imp foi ""1 Ilsley
Metal-Mine Accidi nl in the 1
Pul.
• .I In
I
Determinal
Rock- Dual Mixtures in
Kudlicli and Mi Pub.
Mining i
n Mask:., t hapin i
Mining District, Dunklebi n I Iraniti i
Mining Industry, Alaskan in 9
Muni.. I
S'.s.r 1916 Smith ' io Pub
Mining in the Lo
Sound ; Gov. Pub
, insull
'nl
ninth
Pub
i h. i dendar
958
M
165
409
Mining, Lode, in Fairbanks District, Alaska. Mertie Gov Pul,
Molasses, Notes on the Analysis of H. S. Walker
Monazite Sand Deposits. Russian Note.
Monazite Sands. Burmese. Note ].....[...
Morocco, Soap Demand in. Note
Motor, New Steam. Note
Muntz Metal: Thermal Expansion of Alpha- and Beta- Brass Be
twecn 0° and 600° C. in Relation to Mechanical Propert
Heterogeneous Brasses of the Muntz Metal Type Merici
573
1020
395
943
..I
i the Presence of Blu
, Toluol by Crackii
Schad. Gov. Pub
Muntz Metal (60:40 Brass), Typical Case of the Deterioration of bv
Selective Corrosion. Rawdon. Gov. Pub
Naphtha. Solvent,
G. Egloff
Naphtha, Solvent. Recovery of. Note
Naphthol and Naphthylamine Sulfo Acids, Action of Tetraiodi-o-
Tolylmethane Chloride upon. J. H. Stebbins
Naphthol Resin— Substitute for Shellac. Note
Naphthylamine Sulfo Acids and Naphthol, Action of Tetrazodi o-
Tolylmethane Chloride upon. J. H. Stebbins
Natal, Cane By- Products in. Note
National Exposition of Chemical Industries, New York, Sep
tember 23-28, 1918. Editorials. 592. 672, 674; Notes, 651, 826'
Program and List of Exhibitors, 749; Addresses
National Fertilizer Association:
25th Annual Convention, Atlantic City, Julv 15 to 18, 1918. Pro-
gram
National Museum. Gov. Pub 84. 245.
National Research Council, Special Chemicals and Apparatus Avail
able through the Chemistry Committee of. M. T. Bogert. Note
National War Savings Committee, Chemical Division of. Organized.
Gov. Pub
Natural Gas in 1916. Northrop, Gov. Pub....
Natural Gas. Recovery of Gasoline from, bv Compression and Re-
frigeration. Dykema Gov Pub
Naval Consulting Board Editorial
o-Arsphenamine and Arsphenamine. Some Qualitative and Quanti-
Meyers and Du Mez. Gov Pub
tative Tests fo
Neo-Arsphenamine (Neo-Salvarsan) and Arsphenamine (Salvarsanl.
Gov Pub
Nephelometry. Technical Applications of. P. A. Sober
Netherlands. Beechnut Oil in. Note
Netherlands. Chemical Industry in. Note
Newfoundland Cod Liver Oil. ' Notes 5o7
New Journals
New Publications:
I. DeMattv .89, 169, 251. 333, 415, 505, 587, 669,
C. M. Guppy .
New Zealand and Australia. Railway Materials. Equipment, and
Supplies in. Rhea, Gov. Pub
Niagara Falls Wasting Waters Editorial
Nichols Menu. Award;
ouncement
Introductory Address.
Presentation Address
Acceptance of Medal
s— The
C II Herty
\\ II Nichols
I 1 1 1'iliiison
Development of Pyrimidine Chemistry.
Medal Addr
T B. John;
< Mi ssagi M T. Bogerl
Nichols, w, H, Leader in
Nickel Arc. Wave Lengths ii
and Kic-s Gov Pub
Nickel Canadian, Recovery of Platinum Metals from.
Nickel. Colloidal. Note
Niter take Note
Niter Cake. A Summary of the Literature on the Solubility of Sj 5t< ms
Related to II W P
Niter cake A Summary of the Proposals for Utilization of. J.
Johnston
Niter Cake, The RecrystaUization of. 13. Saxton
Niter Cake. The Utilization of E. Hart. Note
Niter Cake, Utilization of. Note
nterprist fapanest ( hi Kan. Note
Nitrates on Nitrogen Assimilating Bacteria. Influence of. Hill
Gov Puli
Nitric Acid, Effect ■>; Icetylene bridation of Ammonia to
B. Taylor and I II c.tj.ps
Nitric Acid from Niti Prod n ol i B
J. II i 'ir and A Coolidgi
Nitrogen, Comparison ol Percei rops and Roots ol H< <<i
Lettuce Planl I II \ Noyi
Nitrogen, Loosely Bound, as Ammonia in 1.
N Hendrickson and '", c Swan
ii Nitric, and Annie I . i ions in Soil I
.111,1 PI
Nitrogen, I inform Determination of. in Cottonseed Meal I s
758
586
556
1022
947
939
89
105
ti>5
106
9S9
76
168
2 )8
ni I
i, HO
I Concerning u I Hali
North Carolina Acadbhv or <i
Meeting Greensboro, N C ' 1918
Program "i Papi i 492
* 939
Note 31 I
Nutrition Human, H. ( Shei
•
194
3 I '.
654
OlHTl ARIES
ii,i ,,i,,i i ... I'os.ii.ilni. ..i ill. Hatchetigbee Anticlii
Hopkin Gob Pub
i in \iu„ lines in tie W)
,i , I
, ,,; Vpplii ation <•! Hi. 1 liffi rential Pn »un Mi thod I
ii
i . i , I 1 1 i ' . ndD. I i
i°54
THE JOl A'.V.l/. OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 12
Oil, Beechnut, in the Netherlands. Null- 1022
Oil-Break Switchgcar Note 398
oilier. Note 572
Oil, Cod I.ivcr. Newfoundland. Notes 397, 939
Oil: Cotton Oil Industry in the War. D. Wesson 930
Oil: Dclermination of the Ilexahromide and Iodine Numbers of
Salmon < Ml as .i Means of Identifying the Species of Canned Salmon
II S Bailey and I M. Tohnsnn 999
Oil Field, The Salt Creek Wyoming. Wegmann. Gov. Pub 760
i: uion of. Note 487
Oil: Geologic Structure in the Ciishiiig oil and Gas Field, Oklahoma,
and Its Relation to the Oil, Gas. and Water Beal (.... Pub... 331
Oil: Influence of Time of Harvest. Drying and Freezing of Spearmint
upon the Yield and Odorous Constituents of the Oil F. Rabak . . 275
Oil: Influence on Linseed Oil of Geographical Source and Variety
of Flax. Rabak. Gov. Pub 763
Oil in Paint. Substitute for. Note 152
Oil. Lubricating. Note 937
Oil: Methods of Analysis Used in the Coal-Tar Industry. IV-Ben-
zolsand Light oil. J. M. Weiss 1006
Oil: Nesson Anticline, Williams County, North Dakota. Collier.
Gov. Pub 955
Oil Nuts New. Note 313
Oil of Cassia, On Constituents of. II. F.D.Dodge 1005
Oil of Cloves. Note 648
Oil. Olive, Stability of. Holland, el al. Gov. Pub 764
Oil-Pressing Plant for India. Note 397
Oil Producers. Cost Accounting for. Smith. Gov. Pub 412
Oil Prospects of the Salinas Valley-Parkfield Area. California. Eng-
lish. Gov. Pub 874
Oil. Rubber-Seed. Note 938
Oil Sands, Methods for Increasing the Recovery from. Lewis. Gov.
Pub 332
Oil Shale of the Uinta Basin. Northeastern Utah, and Results of Dry
Distillation of Miscellaneous Shale Samples. Winchester. Gov.
Pub 874
Oil Shales, Phosphatic, near Dell and Dillon, Beaver Head County,
Montana. Bowen. Gov. Pub 409
Oil Storage Tanks and Reservoirs. Bowie. Gov. Pub 958
Oil Supply in Germany. New Sources of. Note 747
Oil: The Menhaden Industry of the Atlantic Coast. Greer. Gov.
Pub 166
Oil Varnishes. Notes on Color Designation of. F. A. Wertz 475
Oil, Waterproof Varnish from. Note 152
Oils and Fats, Commercial, Tentative Standard Methods for the
Sampling and Analysis of. Report of A. C. S. Committee. W.
D. Richardson 315
Oils and Fats in Germany. Note 942
Oils and Fats. Saponification of. Note 75
Oils and Nuts from Gold Coast. Note 394
Oils and Vegetables. The Occurrence of Carotin in. A. H. Gill 612
Oils at Room Temperature. Relative Viscosity of. C. F. Sammet. 632
Oils, Catalytical Bleaching of. Note 313
Oils: Digestibility of Some Seed Oils. Holmes Gov. Pub 959
Oils. Essential, in Non-Alcoholic Flavoring Extracts, The Determina-
tion of. F M. Bovles 537
Oils. Fish. Butter Substitute from. Note 397
Oils from Coal Tar. Note 1021
Oils. Light, Recoverv of, and Refining of Toluol. Report of the
Bureau of Standards 51
Oils: Methods of Analysis Used in Coal-Tar Industry. Ill — Heavy
and Middle Oils. J M. Weiss 911
Oils, Nut. Studies on Digestibility of. Holmes. Gov. Pub 763 «
Oils: Pipette Used in Titration of Oils for Acidity. J. Jacobsen. . . 633
Oils: Studies on the Absorption of Light Oils from Gases. H. S
Davis and M. D. Davis 719
Oils: The Palestine Salt Dome. Anderson County, Texas. The
Brenham Dome, Washington and Austin Counties, Texas Hop-
kins. Gov. Pub 85
Oils, Vegetable, in Japan. Note 862
Oilseed Industry of Rhodesia. Note 744
Oilseeds. Indian. Note 397
Oleomargarine or Butter. Detection of Added Color in. H. A Lubs 436
Orange Production: Humus in Mulched Basins, Relations of Humus
Content to Orange Production, and Effect of Mulches on Orange
Production. Jensen. Gov. Pub 763
Ordnance Department, School of Explosives Manufacture, Columbia
University 868
Ore Deposits of the Northwestern Part of the Garnet Range, Mon-
tana. Pardee. Gov. Pub 409
( ire. Low -Grade, utilization. Note 76
Ore, Sources of. Note 940
■Organic Developing Agents. Examination of. H. T. Clarke 891
Organic Matter, An Accurate Loss-On-Ignition Method for the De-
termination of. in Soils. J. B. Rather 439
Organic Reagents for Research and Industry. C. E. K. Mees.
Notes 656. 1027
Original Papers. . .6, 96, 176, 258, 339, 425, 511, 593, 707, 809, 891, 982
Ovens. Drying. Note 943
Oxidases and Iron in Color Changes of Sugar Cane Juice, The R61e
of. F. W. Zerban 814
Oxides, Nitrogen. The Production of Nitric Acid from. G. B. Tay-
lor, J. II. Capps and A. S. Coolidgc 270
Oxygen in Iron. Determination of. Note 745
Oxygen through Stored Coal. Diffusion of. Katz. Gov. Pub 959
Ozone. The Application of, to the Purification of Swimming Pools.
Manheimcr Gov. Pub 409
PAINT and Varnish. Gov. Pub 413
Paint, Substitute for Oil in. Note 152
Paint, White. Discoloration of. Note 940
Pan American Union. Gov. Pub 586
Paper. A Method for Determining the Absorbency of. E. O. Reed. . 44
Paper and Sorghum. Note 396
Paper. Blue and Brown Print Characteristics. Tests and Specifi-
cations F. P. Veitch. C. F. Sammet and E. O. Reed 222
Paper Exports, British. Note 769
Paper Some Experiments on the Pulping of Extracted Yellow Pine
Chips by the Sulfate Process. O. Kress and C. K. Textor 268
Paper Textiles, etc., A Constant Temperature and Humidity Room
for the Testing of. P. P. Veitch and E 0 Reed 38
Para Cymene. 1 — Nitration. Mononitrocymenc. 1-CHj, 2-NOi,
4-CH(CHl)l. C.E.Andrews 453
Patent Abuse. Editorial 1"3
Patent Applications under Trading with the Bkhhy Act:
243, 329, 406. 501, 659, 757. 952
Peace Preparations. Note. Skoda Works 74*
Peat Fuel. Note 1020
Peat in 1916. Turp. Gov. Pub |6}
Peat: Inorganic Composition of a Peat and of the Plant from Which
It Was Formed. Miller Gov. Pub 764
Peat Process. The Ekcnberg Note. ...
Pencil Factory. Chinese Note .. 942
Pentane, Petroleum. Manufacture of Amy! Acetate and Similar Sol-
vents from B. T. Brooks. D. F Smith and H Essex 511
Peppermint Cultivation, lapan. Note.. ;:
Perfume Plant, A Chinese. Note. 1022
Perfumery for Siam. Note .... 73
1'erkin Medal Award Announcement. .... 80
Introductory Address J. Alexander. . 138
Mr. A. J. Rossi and His Work. F. A. J. FitzGerald 138
Presentation Address W.H.Nichols 140
Address of Acceptance. A. J. Rossi 141
Permanganate: The Preparation of .V/100 Permanganate Solutions.
J. O. Halverson and O. Bcrgeim 119
Permanganate-Formalin Method. A Substitute lor. Disinfection
with Formaldehyde. C. G Storm 1 23
Personal Notbs:
81, 161, 241, 327. 404, 499, 583, 658, 755, 871. 949. 1035
Peru, Bolivia. Ecuador. Textile Markets in. Tucker. Gov. Pub. . . . 664
Peterson. Andrew P. Obituary. F. W. Willard 755
Petrol and Gas Engines. Note 940
Petroleum Gov. Pub 409
Petroleum and Allied Substances, 1915, Bibliography of. Burroughs.
Gov. Pub 958
Petroleum Industry, Chemistry in the. Medal Address. W
Burton 484
Petroleum in 1916. Northrup. Gov. Pub 662
Petroleum in the British Empire. Note . . 572
Petroleum Pentane. Manufacture of Amy! Acetate and Similar Sol-
vents from B. T. Brooks, D. F. Smith and H. Essex
Petroleum Refining; Census of Manufactures, 1914. Gov Pub
Petroleum Resources of the U. S. Arnold. Gov. Pub 24 =
Petroleum, Roumanian. Note 39S
Phenol in the Presence of the Three Cresols, the Estimation of. G.
W. Knight, C. T. Lincoln, G. Formanek and H. L. Follett, 9; Cor-
rection
Phenol or Cresol Preservative in Serums, A Colorimetric Method for
the Estimation of. Elvove. Gov. Pub 24s
Phenol. Synthetic. A. G. Peterkin, Jr
Phenols as Preservatives of Antipneumococcic Serum. Pharmaco-
logical Study. Voegtlin. Gov. Pub 873
Phosphate: A Geologic Reconnaissance of the Uinta Mts., North-
ern Utah, with Special Reference to Phosphate. ShulU 873
Phosphate. Reverted. C. C. James
Phosphate Rock, Electric Furnace Smelting of. and Use of the Cot-
trell Precipitator in Collecting the Volatilized Phosphoric Acid.
J. N Carothers, 35, Correction 23V
Phosphate Rock, Our Greatest Fertilizer Asset. Waggaman. Gov
Pub
Phosphate Rock, Raw Ground, The Agricultural Availability of. W.
II Waggaman and C. R. Wagner *+2
Phosphate, Tiicalcium. Effect of Nitrifying Bacteria on the Solubility
of. Kelly. Gov. Pub
Phosphates "Mine Run," The Use of, in the Manufacture of Soluble
Phosphoric Acid. W. H. Waggaman and C. R. Wagner
Phosphoric Acid: Critical Elaboration of Quantitative Pre-
cipitation Methods: Exemplified bv a Method for Determination of
Phosphoric Acid. H. Heidenhain
Phosphoric Acid: Electric Furnace Smelting of Phosphate Rock and
Use of the Cottrell Precipitator in Collecting the Volatilized Phos-
phoric Acid. J. N. Carothers, 35; Correction
Phosphoric Acid, Soluble, The Use of "Mine Run" Phosphates in the
Manufacture of. W. H. Waggaman and C. R Wagner M3
Phosphorus as an Indicator of the Yitamine Content of Corn and
Wheat Products. Voegtlin and Myers. Gov. Pub
Photoelectric Sensitivity of Bismuthinite and Various other Sub-
stances. Coblentz. Gov. Pub '
Photography, Color, Screens. Note ',4U
Phthalic Anhydride in Crude Phthalic Acid, The Determination of.
C. K. Downs and C.G. Stupp
Physiological Effect of Different Gases on Man. Burrell. Gov. Pub. 9>9
Physiological Solutions and Soil Extracts. Ammonia and Nitric Nitro-
gen Determinations in. B S. Davisson """
Pigments of the Tomb of IVrneb. M. Toch. - M»
Pigweed, Common 1-4 maranthus Retroficxus L). A Proximate Anal-
ysis of Seed of. E. P. Harding and W. A. Egge j. . 529
Pine Chips, Yellow, Some Experiments on the Pulping of. by the Sul-
fate Process. O. Kress and C. K. Textor ■ -°*
Pine, Longleaf, Tests of Absorption and Penetration of Coal Tar and
Creosote in. Teesdale and McLean. Gov. Pub 9
Pipette I sed in Titration of Oils for Acidity. J. Jacobsen. ...... . . 633
Pipette-Washing Device. An Improved Automatic A. \ . Fuller ..
Pitches: Methods of Analysis Used in the Coal-Tar Industry. II—
Distilled Tars and Pitches. J. M. Weiss
Plants and Soils, The Relation of Some of the Rarer fc,lcments in
Robinson, cl al. Gov. Pub ""';
Plastic Compound. A New. Note '*'
Plastic Material, Non-inflammable. Note '*
Platinum and Allied Metals in 1917. Hill. Gov. Pub 954
Platinum, As to. J. L. Howe. Note
Platinum at White Heat. Editorial
Platinum. Government Control of W. F Hillebrand Note SB
Platinum in Sp On. Note
Platinum Living from Hand to Mouth. Editorial V
Platinum Met. ,ls from Canadian Nickel, Recovery 01 Nolc g
Platinum oscillations. Editorial '
Platinum . .. B
Platinum Resolution by the Argentine Chemical society. G. t
.nd V, II Nichols. Letters ......... ■>-'
Platinum Resolution bv the State Council of Defense for Cabfor:
J. George ..jo
Platinum Resolutions. G. F Kunz Note. "*J
Platinum, Russia's Production of A R. Men
Platinum Scraps. Editorial
Platinum Substitute. Note ;■_
Platinum. Theft of. Note
Dec, igi8
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
Platinum: The Great Gamble. Editorial
Platinum Wanted by the Government. R. T. Baker
Platinum: Women's National League for the Conservation of Plat-
inum. Note, including letter from L. S. Y. Weill
Poisons. Economic, in California in 1916, The Consumption and Cost
of. G. P. Gray
Polariscope Situation and Need of an International Saccharimetric
Scale. C. A. Browne
Ponceau 3R(By) and Scarlet S3R(B), The Structure of. H. W
Stiegler
Porcelain Laboratory Ware, Comparative Tests of. Waters. Gov.
VII — The Determination of Benzene Vapor. E
Reagents, Organic, for Research and Industry.
Notes.
916
600
Pub.
Portland Cement, Standard Specifications and Tests for. Gov. Pub.
Potash and Magnesia from Canadian Lake. Recovery of. Note
Potash and Other Constituents from Sea Water Bittern, The Extrac-
tion of. J. H. Hildebrand
Potash: An Inexpensive Ash Leaching Plant. W. D. Turner and
B. G. Nichols
Potash as a By-Product in the Cement Industry, The Recovery of.
Ross, el al. Gov. Pub
Potash: A Study of Sources of Error Incident to the Lindo-Gladding
Method for Determining Potash. T E. Keitt and H. E. Shiver .
Potash, Cement Mill, Effect of Coal Ash on the Liberation and Na-
ture of. N. S. Potter, Jr., and R. D. Cheesman. See Letters
Potash from Greensand. Recovery of. H W. Charlton
Potash from Raw Materials Containing only a Trace of this Element,
The Concentration of. by Means of the Electric Precipitation of
Flue Dust and Fume Cement Kilns. B. F. Erdahl
Potash, German, and the War. Note
Potash in Fertilizer Materials, A Study of the DeRoode Method for
the Determination of. T E. Keitt and H. E. Shiver
Potash in Soils, Influence of Gypsum upon Solubility of. McMiller.
Gov. Pub
Potash Leasing Act. Regulations under the. "Note
Potash Lye. Note
Potash Salts and Brines, Nebraska, Some Methods of Analysis for.
A. H. McDowell
Potash Salts in Chile. Note
Potash: Searles Lake Open to Lease Application. Note
Potash Situation. A. W. Stockett
Potash: The Direct Heat Treatment of Cement Mill Dust to In-
crease Its Water-Soluble Potash Content. A. R. Merz
Potassium and Sodium, Improved Methods for Estimation of. S. N.
Rhue
Potassium and Sodium. The Separation of Chlorides and Sulfates of ,
by Fractional Crystallization. W. C. Blasdale
Potassium: Equilibria in Solutions Containing Mixtures of Salts.
I — The System Water and the Sulfates and Chlorides of Sodium and
Potassium. W. C. Blasdale
Potassium Guaiacol Sulfonate, The Identification and Determination
of. S. Palkin
Potassium Permanganate: The Preparation of Ar/100 Permanganate
Solutions. J. O. Halverson and O. Bergeim
Potato: Effect of Different Oxygen Pressures on Carbohydrate
Metabolism of Sweet Potato. Hasselbring. Gov. Pub
Potatoes, Effect of Frost and Decay upon the Starch in. H. A. Ed-
Potteries at Shek Waan, near Canton, China. C. N. Laird
Pottery Industry, English. Note
Power from Refuse. Note
Power: Wasting Waters. Editorial
Precipitation, Electric: The Concentration of Potash from Raw Ma-
terials Containing only a Trace of this Element by Means of the
Electric Precipitation of Flue Dust and Fume Cement Kilns. B.
F Erdahl
Precipitation Methods, Critical Elaboration of Quantitative, Exem-
plified by a Method for Determination of Phosphoric Acid. H.
Heidenhain
Precipitations Suggestions on Some Common. G. H. Brother
Preparation for After thb War. Address. B. C. Hesse,
881 ; See Editorial
Preservative Value of Different Brands of Spices, The Use of Micro-
organisms to Determine. F. M. Bachmann
Preservatives. Industrial Alcohol, and Chemistry. Gov. Pub
Preservatives of Biological Products. Studies in. Neill. Gov. Pub...
Preservatives: Toxicity of Certain Preservatives Used in Serums,
Viruses, and Vaccines. Leake and Corbitt. Gov. Pub
Preserving and Canning. Gov. Pub
Pressure Control, Diesel Engine Blast. Note
Primers, Military and Sporting Arms, Antimony Sulfide as a Con-
stituent in. A S. Cushman
Primus Stoves. Note
Product Patents. K P. McElroy
Propellers, Air, Experimental Research on. Durand. Gov. Pub...
Protactinium: New Radioactive Element. Note
Public Health Service Gov. Pub. . .84, 245. 409, 586, 758, 873, 954,
Publicity, An Experiment in. Editorial
Pulp, Soda and Sulfite. Note
Pyrhcliometer, Marvin, Some Characteristics of the. Foote. Gov.
Pub
994
1030
959
400
572
937
494
918
106
429
347
344
610
725
568
395
245
332
228
376
650
257
873
938
1037
967
1021
762
410
958
QUARRY Accidentsin U. S. during 1916. Fay. Gov. Pub
Quartz and Glass. Compression Strength of. Note
Quicksilver Deposits of Phoenix Mountains, Arizona. Schrader.
Gov. Pub
pie and Entirely Adjustable, for Kjeldahl Digestion
RACK, A
Flasks. I
Radio Instruments
Radioactive Elemen
Radiometry, Instru
Pub
Radium, The Bisulfate Method of De
Railway Material for Japan. Note
Measurements
:w Note
s and Method
631
Gov. Pub 762
938
Used in. Coblentz. Gov.
762
mining. H H. Barker 525
395
Railway Materials, Equipment, and SuppI
Zealand. Rhea. Cov. Pub
Rams.v Memorial Fund. W. H. Nichols Note
Rancidity. Chemical Tests for Detection ol. R. H. Kerr.
Reagents for Use in Gas Analysis:
VI — The Absorption of Hydrogen l.y Sodium Oleate
derson and II II EatI
in Australia and New
236
471
Recent Journal Articles:
I. DeMatty 89, 169. 251, 333, 415, 505, 587, 669
C. M. Guppy 875. 963,
Recorder. Electrical Conductivity, for Salinity Measurements. E.
E. Weibel and A. L. Thuras
Recorder, Riveting. Note
Recovery op Licht Oils and Repining op Toluol. Report Pre-
pared by the Bureau of Standards
Refractometer, A Differential. G. A. Shook
Refraetometer. Dipping, Note on the Use of. E. W. Randall
Refractory Material from Bauxite. Note
Refrigerating Plants. Relation between Efficiency of, and the Purity
of their Ammonia Charge. F. W. Frerichs
Remington, Joseph Price. Obituary. S. P. Sadtler
Rensselaer Polytechnic Institute. Meeting War Conditions at. Note.
Research and Industry. Organic Reagents for. C. E. K. Mees. Notes
.656,
Research and the Tar Baby. Editorial
Research as an Aid to Industrial Efficiency
Research. Chemical, in the Various Countries Before the War and in
1917. E J. Crane. Note
Research Fellowship, State College of Washington. Note
Research Information Committee. Note
Research, Permanence as an Ideal of. Address. S. R. Scholes
Research Work, An Embargo on. Editorial
Resin. Indian. Note
Rheostats. Starting. Note
Rhodesia. Oilseed Industry in. Note
Road Materials. Standard Forms for Specification, Tests, Reports,
and Methods of Sampling for. Gov. Pub
Rocks. Igneous, Chemical Analyses of. Washington. Gov. Pub....
Rocks: The Upper Chitina Valley, Alaska. Moffit. Gov. Pub
Rope Fiber: Distinguishing Manila from all other "Hard" Rope
Fibers. C. E. Swett
Rosin and Turpentine, Increased Yield of, from Double Chipping.
Schorger and Pettigrew. Gov. Pub
Roumanian Petroleum. Note
Rubber: Catalysts in Vulcanization. D. Spence
Rubber Industry in Japan. Note
Rubber-Seed Oil. Note
Rubber, Soft, Compounds, Volumetric Determination of Free Sulfur
in. H. S. Upton
Rubber. Synthetic. Note
Rubber Tubing and Glass, A Device to Insure Tight Connections be-
tween. C. C. Kiplinger
Rubber. Vulcanization of. by Selenium. C. R. Hoggs
Rubidium and Caesium in Plant Ash, A Proximate Quantitative
Method for the Determination of. W. O. Robinson
Russian Asbestos Industry. Note
Russian Monazite Sand Deposits. Note
Russia's Production of Platinum. A. R. Merz
Rust Prevention, New. Note
SACCHARIMETRIC Scale, International, the Need of, and the
Polariscope Situation. C. A Browne
Salinity Measurements. Electrical Conductivity Recorder for. E. E.
Weibel and A. L. Thuras
Salmon: Determination of the Hexabromide and Iodine Numbers of
Salmon Oil as a Means of Identifving the Species of Canned Salmon.
H. S Bailey and J. M. Johnson
Salt in 1917. Stone. Gov. Pub
Salt Requirements for Young and for Mature Buckwheat Plants in
Solution Cultures, Comparative Study of. Shive and Martin.
Gov. Pub
Salvarsan (Arsphenamine) and Neo-Arsphenamine (Neo-Salvarsan).
Gov. Pub
Salvarsan (Arsphenamine): Licenses Ordered and Rules and Standards
Prescribed for Its Manufacture. Gov. Pub
Sand and Gravel in 1916. Stone. Gov. Pub
Sand-Lime Brick in 1917. Middleton. Gov. Pub
Saybolt Universal Viscosimeter, Standardization of the. Herschel.
Gov Pub
Scale in Boilers, Prevention of. Note
Scale. International Saccharimetric. The Need of. C. A. Browne. . . .
Scarlet S3R(B) and Ponceau 3R(By), The Structure of. H. W.
Stiegler
Schoop Metal-Spray Process. Notes 939,
Science and Industry, The Collaboration of. Address. V Grignard.
Scientific and Technical Societies. The German Union of
Scientific Societies 77, 153. 315. 489, 575, 651, 748, 863, 944,
Screens. Color Photography. Note
Searles Lake Open to Lease Application. Note
Seeding Method of Graining Sugars. H. li. Zitkowski
Seeds of the Echinocystis Orcsana (Wild Cucumber). M. R. Daugh-
5S3
629
862
202
240
325
1027
420.J
493
390
968
747
941
744
503
331
954
397
573
920
313
243
247
956
137
575
1023
649
494
992
ters.
Umpleby. Gov. Pub. In 1916, 409; in 1917.
Selenium, Vulcanization of Rubber by. C. R Hoggs
Separators: Magnetic Separations and the Rarer Metals. Note
Serum. Human. Ohservati—
boceptor in. with Refercn
Neill. Gov Pub
Serums. A Colorinu-tric Method for the Estimation of the Cresol or
Phenol i ICIvove, Gov, Pub
listunenU Licensed for Propagatiot
„ on the Significance of Anti Sheep Am-
! to Complement Fixation Test for Syphilis.
and Sale of. Gov.
Pub.
Serum I of Antipneumococcus and Antimeningocnccus.
Gov. Pub • • ■ • ' ' i
Serums Viruses, and Vaccines. Toxicity of Certain Preservatives Used
in. Leake and Corbitt. Oo». Pub
Sewage: Grease Recovery. Note .&••,£■ V.'
Sewage The Fertilizing Value of Activated Sludge. G. G. Nasmith
and (". I' McKay, 139; St* Rudnlck
Buttet Tree. Gutta-Percha from. Note
Shellai I urn .lives. Note • • ■
Shellac Substitute. Notes 648
Shep.ird, Jemea Henry Obituary, w. Frear
.mcrctc. Note ...........
.imunication to the American
i.ical Society
Perfumery for. Note
B62
1056
I III; TOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10. No. 12
Signals. Air Raid Note 941
I. I> Haigh 127
ing Miners in
loplin District Missouri Higgins, el al. Gov. Put. 958
Silk [ndustry. Go\ Pub -'32
ry, Electrii itj in Noti
Silver and Gold in 1916. McCaske] and Dunlop Go\ Pub 956
Silver in the Central stale. Dunlop and I Pub.
In 1916 ... 84
Silver in the Eastern States in 1917. Hill '.,., ]■,,!. 956
Silver-Lead, Antimonial, Wins ,,f t h. Arabia District, Nevada.
Knopf Gov Pub ... 331
i 'induction (1916 i b Uaska bj Brooks 246;
New Mi ii o 'i i a h 1 1 il ol i nd V li i b Hi
!46; California and Oregon, i ind Montana,'
by Heikes, 246; Easten I olorado, by Hendei
son, 409; Utah and N es, 409; Idaho and Washing-
i '.errv
[fide, Some Electrical Properties of. Vinal. Gov Pub.... 86
tralian, Note 487
Hides from Venezuela. Note 228
Skoda Works Peace Preparations. Note ■-li
. it; 1 'bli toi Bla i i " ■ Work. Feild and Royster.
... Pub 959
•I 1 i. <'■"'. Pub 956
. Activated, Fertilizing Value of. G. G Nasmith and G. P.
McKay, 339; See Rudnick 400
Smithsonian Institution;
Administration and Activities of. Clark, Gov Pub 245
Annual Report of the Hoard of Regents of. Gov. Pub 408
Government Publications '45, 108, 764
Smithsonian Physical Tables. Gray Gov. Pub .64
Soap and Glycerin Manufacture in India Note 744
1 in Morocco Note 395
Soap, Sugar and. Editorial 175
Soap, Water in. An Improved Distillation Method for the Determina-
tion of. R. Hart 598
Soapstone and Talc in 1917. Diller. Coy. Pub 955
S..CIKTE I.I-: ChIHZB iNDUSTRIBtl I
Organization of New York Section 154
First Meeting of New York Section:
i onditions of the French Chemical Industries during 1916. F.
I I.eMaistre 421
The Great Effort of the French Industries. M Knccht 423
Society of Chemical Industry: New York Section Resolution. 1023
Society of Cotton Pa ers Analysts: Check Meal Contest.
Note 656
Soda and Sulfite Pulp Note ... 1021
Sodium and Potassium, Improved Methods fOI Estimation of. S X.
Rhue 429
Sodium and Potassium, The Separation of. and Chloride Sulfates of,
by Fractional Crystallization. W C. Blasdale 347
Sodium Cyanide, Notes on W. I Sharwood 292
Sodium: Equilibria in Solutions Containing Mixtures of Salts. I —
The System Water and the Sulfates and Chlorides of Sodium and
Potassium. W. C. Blasdale 344
Sodium Oleate, The Absorption of Hydrogen by. VI — Reagents for
Use in Gas Analysis. R. P. Anderson and M II Katz 23
Sodium Sulfate. The Use of, in the Kjeldahl Gunning Method. C. T.
Howell and W. G. Friedeman 599
Soil n Mil v and Hvdrolvtic Ratio in Soils. Sporway, Gov. Pub... 503
Soil Acidity as Influenced bv Green Manures. White. Gov. Pub 763
Soil, Decomposition of Green and Stable Manures in. Potter and •
Snyder Pov. Gub 504
Soil Extract, Effect of Season and Crop Growth in Modifying the.
Stewart Gov. Pub 504
Soil Extracts and Physiological Solutions. Ammonia and Nitric Nitro-
gen Determinations in. B. S Davisson 600
Soil Reaction and Growth of Azotobacter. Gainey. Gov. Pub 959
Soil Reaction as Indicated by the Hydrogen Electrode, Studies in.
Plummer. Gov. Pub . 504
Soil Reaction as Measured bv the Hydrogen Electrode, Relation of
Carbon Dioxide to. Hoagland and Sharp. Gov. Pub 504
Soil Solution Due to Season and Crop Growth. The Freezing- Point
Method as an Index of Variations in the. Hoagland. Gov. Pub. . 504
Soils, Alkali, Durability of Cement Draintile and Concrete in. (Con-
taining Results of Third Year's Tests.) Wig, el al. Gov. Pub 85
Soil., An Accurate I.oss-on-Iguition Method for Determination of Dr-
eam,- Matter in I B. Rather 439
Soils and Plants. Relation of Some of the Rarer Elements in. Robinson,
el al. Gov. Pub 503
Sods. Effect of Fertilizers on Hydrogen-Ion Concentration in. F. W.
, Morse 125
Soils: Influence ol Carl Magnesium and Calcium on Bac-
teria of Certain Wisconsin Soils. Fulmer. Gov. Pub 763
luence of Gypsum upon Solubility of Potash in. McMiller.
959
Soils. Movement Of Soluble Salts through. McCool and Wheeting.
i .... Pub 503
Soils, Principles of Liming Go Pub 763
Soil Ri "i I Hawaiian Soils with Calcium Carbonate Solutions,
Its Relation to the Deieriinuai Requirements of Soils,
and a Rapid Approximate Method for the Determination of Lime
Requirements of Soils M. O Johnson 31
1 irious
Sails ami Concentration of Soil Solution in Different Classes of
Vlillai Goi Pub 763
.a Irrigation Water, and on
a New Method for Determining Volume Weight. Israelsen.
i.,... Pub 763
ons of. as Criteria of Their Crop-Producing
Powei Bui i ' .■• Pub 04
Soldiers in Training Camps, Chemistry I'm I W, Beckman 869
From An Vapoi Mixtures Recovery of. E. 1. Knoedler and
i I. Dodg. 593
Sorghum and Paper.
Sorghums and < a of Miller and Coff-
nian I'.,,. Pub 7o4
Si it i i, - i . , I ill' Hop
... 887
South Ah
rii an Industrial Develop 10
South African Industries 943
South African Iron Oi 395
South African I' Note
South America, Chemical Markets of, O. P. Hopkins:
Chemical Trade of Argentine, Brazil, ami Uruguay
Chemical Trad [I and Bolivia.
uador, the Guianas, Venezuela,
and Paraguas
South America. Machinery in Not
South America, Water Proof Goods for. Note
.pun Perromanganese Manufacture in. Note
Platinum in N ote
Spearmint: Influence of Tunc of Harvest. Drying and Freezing of,
upon the yield and i idorou t onstituents of the Oil F. Rabat .
pectra Application of Dicyanifl to the Photography of Stellar
Merrill. Gov pal.
I from 5600 A to 9600 A., Wave Length Measurements in.
Meggi i i iov 1 '■.:'.
( !
F, ,M. Bachmann
Spirits, Distil!, i
Spruce, Effect i ."king Conditions in Production
Of Sulfite Pulp
Spruce Turpentim to thi Fori Editorial
star, li in . tit; Calf Shaw, el al. Gov. Pub . . .
Starch, Effect of Time of Digestion on Hydrolysis of Casein in Pres-
ence of. McHargue. Go\ Pub
Starch in Potato Prosl and Decay upon. H. A. Edson...
Statistical Abstract of II S. 1917. Gov. Pub
Steam. Volcanic, Electrical Energy from. Note
Steel and Iron
Steel and Iron Industry during the War Period, Trend of Accident
Frequency Rates in. Chaney. Gov Pub
Steel and Iron [ndustry in Japan. Note
Steel and Iron. Sulfur in. A Standard Apparatus for Determination of,
by Evolution Method. H. B. Pulsil- r
Steel and Iron Trade in Aden. Note
Steel, Carbon and High Speed. Liquids for Heating, Quenching, and
Temp, ring of. Note
Steel, Carbon Hardening. Note
Steel, Chromiuti foi Magnets Note
■ .in. is. ene Note
Steel, Determination of Manganese in in the Presence of Chromium
and Vanadium bv Electrometric Titration. G. L. Kelley. M G.
Spencer, c I; [Uingworth and T Graj
Steel, Electro-. Works in Germany. Note.
Steel. Microscopic Examination of. Gov. Pub.
Steel, Nickel. Note-
Steel Production (1916). Hurchard. Gov. Pub
Steel, Rapid Determination of Carbon in. by Barium Carbonate
Titration Method. J. R. Cain and I. C. Maxwell
Hardened Carbon, Effect of Annealing on Electrical Resistance
of. I P. Parkhurst
Steels. Tool Note. .
Stones of Minnesota, The Structural and Ornamental. Bowles. Gov.
S04
725
874
487
040
574
229
Pub
Stopcock. Hydrogen Sulfide, An Automatic C. H. Classen
Stopcock. Special, for Dropping Liquids Arranged for Equalizing
Pressure above and below the Outlet in the Stopcock. H. L.
Fisher
Stoves, Primus. Note
Stream Pollution, Gov. Pub
Streptoecoci, Concerned in Cheese Ripening. Study of. Evans. Gov.
Pub
Strontianite Deposits near Barslow. Californi
Strontium in I'M 7. Hill. Gov Pub
Sudan-Grass Hay, Composition and Digestibility of.
MeCandlish. Gov. Pub
Sugar and Soap. Editorial
Sugar as I sed in Medicines. Conservation of. Note
Sugar Cane luice. The Role of Oxidases and Iron in Color Changes of
F W Zerban
Sugar Factories, Theory and Practice in the Design of Multiple
Evaporators for, A. L. Webre
Sugar, Maple: Composition. Methods of Analysis. Effect of En-
vironment. Bryan, ct al Gov. Pub
Sugar: The Deterioration of Raw Cane Sugar:
Conservation. C A. Browne
. The Seeding Method of Grainng. II. E. Xitkowski
5, Raw Valuation of. W. D. Home
- Various, American Sources of Supply for. C. S. Hudson.
Knopf. Gov Pub.
Gaessler and
A Problem in Food
Stis.it
Silent
Sugar
Address
Sulfate of Ammonia, Production of. Note
Sulfate 1'r.n.ss, Some Experiments on the Pulping of Extracted
Yellow I'm. Chips by the, I > Kress and C K, TextOI
Sulfates and Chlorides of Sodium and Potassium. The Separation of.
by Fractional Crystallization, W. C. Blasdale
Sulfates Equilibria in Solutions Containing Mixtur.
The S1 sti m Water and the Sulfates and Chlorides of Sodium and
Potassium V. C Blasdale
Sulfite Lye, V m of. Note
Sulfite Lyes I lye from. Note
Sulfit. i Note
Sulfite Pulp fi ..in Spin trying Certain Cooking Condi-
tions in Production oi Lunak. Gov. rub
Sulfite '! nti ntine A W Schorger
Sulfur A Contribution to the Composition of Liinc-Sulfur folu-
WlllUT
Sulfur, Andean Deposits. Miller anil Singewald, Jr i '...-. I'
Sulfur, in Example ..t Industrial Independei
of the LSI Pub
Sulfur. Free, Volumetric Determination of.
pounds lis I Fpton.
Sulfur in Iron and Steel. Determination .a bv the Evolution Method.
A Standard Appai itus for. II B. Pulsifer
Sulfur Production 1916). Smith Goi Pub
Sulfur. Pyrites, and Sulfurii \. id Smith. Gov. Pol
Sulfur.! Arsenic in. W D Collins
Sulfuric Acid, Avoidable Waste in th< Production of, by
Note
i, >.| tndustx]
Sulfuric Acid Prod Pub .
,1 Sulfur Smith. Gov Pub
...v Pub
.ml Medical Supplies, Staple, List ot GOV. Pub
1014
650
4lio
763
409
-'.I
OsC,
4'iS
sl 4
178
809.
Mineral Industries
Soft Rub
Cham-
41"
Dec.
THE JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
1057
Sweden, Bichromate Manufacture i
Sweden, Trade Developments in,
Swedish Gauges. Note
Swedish Industrial Developments,
Swiss Electrochemical Industries. 1
Switchgear. Oil-Break. Note
Switzerland, Imitation Leather for.
Synthetic Market. Note
Synthetic Materials. Note. 314; Correction.
Syphilis: Observations on the Significance of Anti-Sheep Ambocepto
Note .
Hui
nplement Fixation Test
TALC and Soapstone in 1917. Diller. Gov. Pub 955
Tannin and Timber. Note 229
Tanning. Chrome. Note 74,,
Tanning Material in Germany, Note 1022
Tar. Notes on "Free Carbon" of. J. M. Weiss and C. R. Downs 400
Tar-Still Corrosion by Chlorine. Note
Tar. Vacuum, Alcohols and Bases in. Note
Tariff Commission. Gov. Pub 504
Tariff Commission and the Dye Industry G. Jones. Address. .
Tariff Commission. Facts for the. Editorial 173
Tariff Commission. I'. S.. Inquiry in Regard to Chemical Industries . 158
Tars: Methods of Analysis Used in the Coal-Tar Industry. J M
Weiss.
I — Tars, 732 ; II — Distilled Tars and Pitches 817
Technical and Scientific Societies, The German Union of .
Technical Association of the Pulp .
nual Meeting, New York City, February 5 to 7,
Third Annual Spring Meeting. Announcement 403
Technical Education in Foreign Countries Smith and Jesian. Gov.
Pub ... 403
Technical Men and Skilled Operatives Wanted for I". S. Army Ord-
nance. Note 954
Tellurium CJmpleby. Gov. Pub. In 1916, 409; in 1917
Temperature-Viscosity Relations in Ternary System CaO-AIsOa-SiO:.
Feild and Royster. Gov. Pub 959
Temperatures, High. The Automatic Control and Measurement of.
R. P. Brown 153
Ternary System CaO-AlsOr-SiOa, Temperature-Viscosity Relations
in the. Feild and Royster. Gov. Pub ... 059
Tetanus Antitoxin. Destruction of, by Chemical Agents. Berg and
Kelser. Gov. Pub 764
Tetanus Spores. Effect of Ether on. Corbitt. Gov. Pub 87 s
Tetrazodi-o-Tolvlmethane Chloride. Action of. upon Naphthol and
Naphthvlamine Sulfo Acids. J. H. Stebbins, Jr 44s
Textile Exposition. Sixth National 491
Textile Fibers, The Use of, in Microscopic Qualitative Chemical
Analysis. E. M. Chamot and H. I. Cole 4S
Textile" Industries. The Dyestuff Situation in. Gov. Pub 504
Textile Markets of Bolivia. Ecuador, and Peru. Tucker. Gov.
Puh 664
Textiles. Gov. Pub 1037
Textiles. Miscellaneous. Gov. Pub 332
Textiles, Paper, etc., A Constant Temperature and Humidity Room
for the Testing of. F. P. Veitch and E. O. Reed 38
Textiles: W'ater-Proof and Dust-Proof Fabrics. Note 7s
Theobromine. Estimation of. Studies in Synthetic Drug Analysis — V.
W. O. Emery and G. C. Spencer 605
Thermit Welding. Note 150
Thermite: Modern Explosives, Note 650
Timber and Tannin. Note 229
Timber, Pit, Preservation of. Note 397
Timing Device for Simplifying the Thermometric Reading of Calori-
metric Determinations. C. A. Myers. Ir 1015
Tin, Conservation of. Conservation Begins at Home. Editorial. . . 879
Tin Production Knopf. Gov. Puh. In 1916 410
Tin, Recovery of. Note 746
Tin Resources of the Kings Mountain District. North Carolina and
South Carolina. Keith and Sterretl Gov. Pub 351
TN'T as an Explosive, Safety of. J. M Weiss Note 1028
Tobacco: Effects of Various Salts. Acids Germicides, etc.. Upon the
Infectivitv of the Virus Causing the Mosaic Disease of Tobacco.
Allard. Gov Pub 764
Toluol bv Cracking Solvent Naphtha in the Presence of Blue Gas.
G. Egloff 8
Toluol from Spruce Turpentine. A S. Wheeler 359
Toluol Recovery ami Standards for Gas Qu ility R. S. McBride. ... Ill
Toluol Recovery: fin with the Investigation. Editorial 93
Toluol. Refining of. and Recovery of Light 1 'Ms Report of the
Bureau of Standards 5 1
Toluol: Spruce Turpentine to the Fore Editorial 174
Tomato Seeds and Skins Waste. Utilization of. Rabak. Gov. Pub sol
Tool Steels. Note . 942
Torches. Pocket, Magneto Machines F01
Toxins and Analogous Products, Establishments Licensed for the
Propagation and Sale of. Gov. Pub . 758
Tkaih 231
Trade British Board of. Notes:
16 151, 2M\. HI. 398, 488, 574, 650. 747
Trade, British: Register of Overseas Buyers Note 573
i's Export Note
Trade Developments in Sweden. Note 396
Current, A Method for Testing. Silsbee. Gov. Pub.. 86
861
31 \
Trinitrotoluol. Pr 1. tii Poinl in
Gov. Pub
Tube n of. Note.
574
Turpentine ami I ol from 1 ble I hipping
. >v. Pub 132
Turpi ■
Turpentine, Spruce. Editorial.
iluol from. A s a/he 1- <
174
Turpentini Sulfite A W. Schorger
709
41 !
152
47s
862
6 1 2
UKRAINE. German Enterprise in the. Note 10?1
Ultra-Filter. Note . . . 74 7
United States Shipping Board: Communication to the Ami
Chemical Society 864
United States Tariff Commission: Coal-Tar Products for
Note ... 582
LTnited States Tariff Commission Inquiry in Regard to Chemical In-
dustries 158
Universities and Manufacturers, Cooperation Between, R, E.
Oesper. Note 1027
Uruguayan Markets. Note 650
VACCINE, Anti-tvphoid.'The Standardization of. McCoy. Gov
Pub
Vaccines. Viruses, and Serums, Toxicity of Certain Preservatives Used
in. Gov. Pub 245
Valve. Safety. E. Rittenhouse 633
Vanilla Extracts. Factitious. The Detection and Determination of
Coumarin in. H.J. Wiehmann 535
Vapor-Air Mixtures. Recovery of Solvents from. E. L. Knoedler
and C. A. Dodge 50!
Vapors in Gases. A New MetHod for the Quantitative Estimation of
H. S. Davis and M. D. Davis
Varnish and Paint. Gov. Pub .
Varnish, Waterproof, from Oil. Note
Varnishes. Oil, Notes on Color Designation of. F \ H
Vegetable Oils in Japan. Note
Vegetables and Oils, The Occurrence of Carrotin in. A II loll
Velvet- Bean Meal, Corn Silage, and Alfalfa Hay when Fed -
and in Combinations, Digestibility of. Ewing and Smith
Pub 7M
Venezuela, Hides and Skins from. Note 228
Venezuela, Instruments and Tools for Note . 398
Venezuelan Trade Inquiries. Note . . 957
Victoria, Mineral Production of. Note 1 si
Viruses, Establishments Licensed for Propagation and Sale of. Gov.
Pub ... 758
Viruses, Vaccines, and Serums, Toxicity of Certain '
Used in. Leake and Corbitt. Gov. Pub. 245
Viscosimeter, Savbolt Universal, Standardization of the. Herschel
Gov. Pub
Viscosimeters, Short-Tube. Determination of Absolute Viscosity by
Herschel. Gov. Pub ss
Viscosity. Relative, of Oils at Room Temperature C F Sammet.... 632
"Vitamine. Antiiieuritic," The Dietary Deficiency of Cereal 1
with Reference to Their Content in, Voegtlin, el at. Gov. Pub.. 586
Vitamine Content of Corn and Wheat Products. Phosphorus as an
Indicator of. Voegtlin and Myers. Gov. Put. 750
Voltaic Cell. New Note 744
Volumenometer, A. J. S. Rogers and R. W Frey 554
Volumeter. Anaerobic Culture. Z. Northrup 624
Vulcanization, Catalysts in. D. Spence 115
Vulcanization of Rubber by Selenium. C. R. Boggs 117
WAR Chemistry in the Alleviation of Suffering. Editorial 673
War Gas Investigators, Civil Service Rules Waived for. W Wilson
Note 755
War Industries Board. Chemical and Explosi
War Service. Chemists in, 'See under Che
Washington Letter p. Wooton:
80, 160. 259, 325, 403, 496, 582, 656, 753 f
Washington Notes Editorial
Waste. Reduction of. J. Stieglitz. .SVr Gray
Wastes Industrial. Fertilizers from. Ross. Gov Pub
Water. Bacteriological Examination of . Comparative Stu.lv of Media
Used Hasseltine Gov. Pub
Water. Distilled. The Carhonation of. Carbonation Studies II
II E Patten anrl G. H Mains
Water: Geologic Structure in the Cashing nil and Gas Field, Okla-
homa, and Its Relation to the Oil, Gas .111. 1 Water. Beal, Gov
Pub
Water in Milk Added. Research on the Determination of.
Dur&nd and k Stevenson
Water in Soap. An Improved Method for the Determination of.
II
Hart
1-:
Water Lubrication of Gas Exhausters. Note
Water-Power u Developments in
111 Alaska Chapill. .7 n! Gov Pub
1 Goods tot South At
Waters Investigation of the Pollution of Certain Tidal u il
New Jersey, New ^- di
Bathing Beaches and Shellfish-Bearing An
Pub
Imeral. in 1916 Elli ' '■"* Pub
0 1 lie Intermount tit
and C. T Hirst
Waters. Surface. Chemical Character of Some, of Alaska
Springs 01 Alaska. Warin Gi int.
Watertown Arsenal Go\ Pub
Red Hid Infra-Red Spectra of Iron.
N'ickel ! I'ub
I
"I Corn I'roilm '
Wheal and
rived from Voegtlin and Myers G01 Pun
I'llb
Wood w 1
u \ I
W.k.i Manufactui
X RAY \ r
152
633
1
ios8
\
THE JOURNAlSdF INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 10, No. 12
ZINC Carbonate and Re.atcd Copper CarbonaVe Ores at Opbir, %?£%£*& SS^rSSS^TftfihttS
Utah. Loughlin. Gov. Pub I ^ rado by Henderson. 409; Utah and Nevada, by Heikes, 409;
Zinc, Electric Furnace. Note V ■ 396 Idaho and Washington, by Gerry 586
^fa*32£?&l£l£i»l? HiU tv«. Inm69S1 l^u^^'R^Eartn^eralsiniVloVSonaUer: C.v Pub MS
jygjMiNU ot^io AUb 1 9 W
TP I&EG. Industrial and
1 engineering chemistry
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